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    • 专利摘要:
    To prepare decaffeinated tea, a tea which is adjusted to a water content of 15 to 50 % by weight is first extracted at 50 to 70 DEG C with moist CO2 at 260 to 350 bar, the caffeine is then reextracted from the caffeine-containing CO2 in the same pressure range using active carbon, and the caffeine-free CO2 is then recycled via the tea which has already been extracted, and the tea is separated from the CO2 and dried. <IMAGE>
    公开号:SU1602385A3
    申请号:SU853877651
    申请日:1985-04-10
    公开日:1990-10-23
    发明作者:Шютц Эрвин；Фолльбрехт Хайнц-Рюдигер；Клима Хубертус
    申请人:Скв Тростберг Аг (Фирма)；
    IPC主号:
    专利说明:

    The invention relates to the production of decaffeinated black tea.
    The purpose of the invention is to simplify the method, increase efficiency and reduce energy consumption.
    FIG. 1 shows an installation for carrying out the method; in fig. 2 - autoclave, general view.
    If, when coffee is decaffeinated, the raw material is used as raw material, i.e. When raw coffee beans are used, when tea is decaffeinated, it is necessary to use as a starting material a product that has already been fermented and therefore has a certain aroma, which, as a rule, after removal of caffeine, usually deteriorates significantly.
    Methods for removing caffeine using organic solvents are known. However, a common drawback of the methods is the removal, together with caffeine, of a significant part of the flavor, as well as the difficulty of complete, without residue, 1 of the solvent used.
    The method of decaffeinating tea is known, in which, at the first stage of the process, aromatic substances are removed from the dry tea using supercritical CO-j, and then, in the second stage, caffeine is selectively extracted with moist supercritical CO-j and after days 1Ha the removed from it in the first stage aromatic substances. Extraction of this method should be carried out at 40--60 ° C, so as not to disturb apoO5 O HCHE
    CO 00
    sd

    U4
    mate, and only after the removal of aromatic substances can processes be carried out at a higher temperature. Extraction of caffeine should be carried out at pressures of 200-250 bar. The separation of caffeine from CO2 is then carried out by lowering the temperature and pressure below the critical limit.
    The disadvantage of this method is that the aromatic substances have to be removed under as mild conditions as possible before one can proceed, under somewhat more severe temperature conditions in the second stage, to the removal of caffeine. Another disadvantage of this method is its two-step process. In addition, the separation of caffeine by reducing pressure and temperature is expensive, because a significant expenditure of energy is required to return CO2 to the supercritical zone. There is a method in which caffeine is removed from CO2 in the supercritical pressure range using ion exchangers. The two-stage extraction is known, which remains unchanged, with a temperature of 40 ° C and a pressure of 200 bar being used.
    Therefore, the proposed method is based on the task of creating a simpler one-step method for obtaining decaffeinated tea, in which only caffeine is selectively extracted without extracting aromatic substances and without the need to change supercritical and subcritical temperature and pressure conditions with a CO2 extracting agent.
    The goal is achieved by obtaining decaffeinated tea by extraction with supercritical CO2 (in relation to the temperature and temperature) in the presence of water. The proposed method is characterized in that the extraction is carried out in one stage using humid CO2 at a pressure of 260-350 bar and a temperature of 50-70 ° C, from the caffeine-containing CO2 activated carbon at a specified pressure range, the caffeine is again removed, thus obtained decaffeinated CO2 The tea is again passed through tea, which is free from caffeine, the latter is separated from COz and dried.
    The proposed method is based on the fact that under the conditions of the indicated pressure and temperature, if a certain moisture content in tea is observed, only one caffeine can be selectively extracted, as a result of which the operation of separate extraction of aromatic substances becomes more distinct and therefore the tea retains its natural taste and loses its inherent aroma. Therefore, with such selective extraction, it became possible to use cheap activated carbon to remove the extracted caffeine from CO2 instead of ion exchangers.
    In the proposed method, as a rule, ordinary dried tea is used, which is moistened with the addition of water to a moisture content () of 15-50% by weight. You can set the required moisture content in tea by simply adding to the dried tea the right amount of water in the mixing device, with which you can evenly distribute the moisture in the tea. It is advisable to set the water content in tea to be 25-40 wt.%, And the best results are obtained when the water content in tea is 28-35 wt.%. CO2 is used under supercritical conditions in the wet state. The pressure should be 26.0-35.0 MPa, but preferably 27.0-29.0 MPa. This temperature range of 50-70 ° C is critical. If the temperature is below 50 ° C, a sharp decrease in the amount of extracted caffeine is observed, the method is unprofitable and requires an extended extraction time. If 70 ° C is exceeded, undesirable changes in the aroma of tea occur.
    The amount of CO2 used depends on the amount of extractable caffeine in the tea. Since under these conditions of pressure and temperature approximately 0.2 g of caffeine per kilogram of CO2 can be obtained, it is advisable to use 2–20 kg of CO2, preferably 5–10 kg of CO2 per gram of extractable caffeine in tea.
    After the extraction, which lasts 2–20 hours, the CO2 containing caffeine is directed while maintaining the pressure and temperature conditions at specified intervals for contact with activated carbon, used as a free flowing mass. In this operation, caffeine goes into activated charcoal. Decaffeinated CO-2 is again directed, under extraction pressure, to tea already extracted, and about the same amount of moisture that was removed from it during the extraction carried out before it is introduced. The method is expedient to carry out when using several extraction autoclaves, which can be connected to each other in parallel or in series and separated one by one from the process cycle. After the end of the introduction of COj to tea, a wet tea is obtained with a greatly reduced caffeine content and almost initial aromatic content. This tea is then dried at 60-80 ° C and immediately after drying it is ready for use.
    Adsorption of caffeine with activated carbon should be carried out at 50-70 ° C. Passing the CO2 through the already extracted tea while simultaneously moistening it is advisable to carry out 50-70 ° C, preferably at 60-70 ° C.
    Extraction of tea can be carried out in an autoclave, which is charged with tea and then CO2 is passed in the direction of the longitudinal axis. Such an extraction autoclave has a suitably cylindrical shape with a ratio of length to diameter of approximately 3: 1 to 8: 1. Constructions
    of the internal flow in a cylindrical extraction autoclave, and at the end, upon reaching the internal hollow space, approximately five times larger, depending on the diameter of the internal hollow space. Accordingly, also, n, the velocity of the gas flow between adjacent particles of material is low. With a mea-change of cm of average processing time inside the autoclave, the duration of the contact autoclaves is significantly increased and it is easy to load them into the gas flow separately with the particle material to be extracted. through a removable cover.
    However, in extraction autoclaves of this design it is often observed that this type of installation significantly reduces the mechanical load on the loaded bulk material. The pressure loss has a square weight seal of the loaded material. In this form of installation, the mechanical load on the loaded bulk material is significantly reduced. The pressure loss is square dependent. The reason for the seal is that the bridge of the flow rate into the pipes and directly from the water, like most others, is proportional to the flow through the liquid.
    Natural substances exist due to the shape of their particles; high stickiness. TO
    of the way. In the extraction method of the radial flow, the path covered by carbon dioxide is therefore about 1/10 hours and a pair of 1 track of the path traveled 20 with the axial passage of the core method, i.e. the degree of moistening, the gas flow through the autoclave. Thanks
    This eliminates the possibility of compressing the bulk material. Activated carbon can be placed in the hollow interior of the cylinder. For the sake of the increase in the capacity of the CO2 flow, the pressure and rate of change of the volume flow, the height of the autoclave and the filter area at the outlet of the autoclave
    As the loaded material compresses this, pressure losses in the
    thirty
    Rial increases the pressure loss during the passage of gas through the loaded material, which leads to further hardening of this material. As a result, a channel or channels are formed in the loaded material, which, in turn, determine the non-uniformity of the degree of extraction per cross section of the autoclave and its height. This can lead to a significant - lengthening of the time required for the extraction.
    To eliminate the drawbacks, the tea is arranged in the form of a hollow cylinder and the extraction is carried out concentrically, the passage does not contain CO2 impurities from the side of the surface of the cylinder. The CO2 received impurity is collected on the other side of the cylinder surface and from there is supplied to activated carbon. It is advisable to make a supply of CO2 from the outer cylindrical surface. With proper execution of the hollow cylinder, it is possible
    the pipelines between the extraction and the separation autoclaves and it becomes possible to particularly advantageous operation of the extraction device.
    The apparatus includes a mixer 1 for moistening tea, associated with a cylindrical autoclave 2 for extracting tea. At the same time, a cylindrical autoclave 2 is connected with adsorbertem 3 to form a closed circuit including a heat exchanger 4 and a pump 5 installed in the section connecting the outlet of the adsorber to the inlet of the autoclave 2. The reserve tank 6 for the liquid with carbon dioxide contained in it enters the installation gas, pump 7 and valve 8 forming a circulation loop.
    The cylindrical autoclave 2 comprises a supply pipe 9 for the extracting agent, a cover 0 and a discharge pipe 11 for the extracting agent. In the autoclave, two perforated inserts 12 and 13 are installed for extractable
    ability to position activated carbon material (with perforated walls)
    inside the hollow cylinder, thereby creating favorable conditions for gas flow.
    Due to this radial gas flow method, the cross section through which the flow passes is constantly changing along the path from one surface of the hollow cylinder to the other regardless of the direction in which the gas flow passes. With the passage of the gas stream with ext
    and located along the longitudinal axis and made in the form of a perforated collecting cylinder - for the extracting agent, which is connected to the pipeline 11 - for the extracting agent. The perforated collecting cylinder for the extracting agent can be made in the form of a pipe. The extracting agent is collected and directly from the extraction autoclave through, releasing
    They are transferred in a separate section to private cars in the inner part of the side surface of 55 claves filled with activated carbon. bulk solids through which an assembly cylinder for extracting
    agent contains activated roofing, thanks to what a separating autoclave
    gas flows, 15–20 times larger than the axial flow of the gas flow in a cylindrical extraction autoclave, and at the end, when reaching the inner hollow space, approximately five times larger, depending on the diameter of the inner hollow space. Accordingly, also, n, the velocity of the gas flow between adjacent particles of material is low. With meismeasurement of cm / m, the average processing time inside the autoclave significantly increases the duration of contact with the gas flow of an individual particle.
    tact with the gas flow of a separate particle.
    In this form of installation, the mechanical load on the loaded bulk material is significantly reduced. The pressure loss has a square dependence on the flow velocity in the tube e and is directly proportional to the flow through the fluid.
    the pipelines between the extraction and the separation autoclaves and it becomes possible to particularly advantageous operation of the extraction device.
    The apparatus includes a mixer 1 for moistening tea, associated with a cylindrical autoclave 2 for extracting tea. At the same time, a cylindrical autoclave 2 is connected with adsorbertem 3 to form a closed circuit including a heat exchanger 4 and a pump 5 installed in the section connecting the outlet of the adsorber to the inlet of the autoclave 2. The reserve tank 6 for the liquid with carbon dioxide contained in it enters the installation gas, pump 7 and valve 8 forming a circulation loop.
    The cylindrical autoclave 2 comprises a supply pipe 9 for the extracting agent, a cover 0 and a discharge pipe 11 for the extracting agent. In the autoclave, two perforated inserts 12 and 13 are installed for extractable
    material (with perforated walls)
    0
    and located along the longitudinal axis and made in the form of a perforated collecting cylinder - for the extracting agent, which is connected to the pipeline 11 - for the extracting agent. The perforated collecting cylinder for the extracting agent can be made in the form of a pipe. The extracting agent is collected and directly from the extraction autoclave through, releasing
    25
    20 MPa, after which the pump is removed from the cycle. After switching on the pump 5, COA is circulated through the extraction autoclave and the adsorber, and the temperature in the extraction autoclave due to the heat exchanger 4 rises to 63 ° C. The pressure in the extraction autoclave is 29 MPa. The adsorber operates at a pressure of 28 MPa and at 6GS. The circulating amount of CO2 is 800 kg / h. 2.5 hours later
    10, the extraction is interrupted; the CPS from the extraction autoclave is discharged to the CO2 storage tank until the pressure is equalized and then discharged to the atmosphere. Tea is removed from the extraction autoclave and dried in a dryer at 70 ° C. The analysis gives a residual moisture of 4.5% H2O and 0.08% caffeine.
    Example 2. 10 kg of Ceylon Blends grade tea with 5.9% H2O and 3.3% caffeine is moistened in 20 mixer 1 with 3.5 l of water and then introduced into an extraction autoclave 2. Adsorber 3 is charged with 7 kg of activated coal The extraction autoclave and the adsorber are brought to a pressure of 16 MPa by means of CO2 from the tank 6 for liquid using a pump 7, after which the pump 7 is taken out of the cycle. After switching on the pump 5, the CO2 is circulated through the extraction autoclave and the adsorber, and the temperature in the extraction autoclave rises to 56 ° C due to the heat exchanger 4. The pressure in the extraction autoclave is 26 MPa. The adsorber operates at a pressure of 25 MPa and at 55 ° C. The circulating amount of CO2 is 800 kg / h. After 2.5 hours, the extraction is interrupted, the CO2 is released from the extraction autoclave until the pressure is equalized into the CO2 storage tank and then into the atmosphere. Tea is removed from the extraction autoclave and dried in a dryer at 80 ° C. The analysis gives a total moisture content of 4.1% water and 0.15% caffeine.
    40
    Example 3. 10 kg of Ceylon- grade tea, B lends with 5.9% water and 3.3% caffeine in a mixer are moistened with 3.5 liters of water and then injected into an extraction autoclave 2. Adsorption v, ic .nv.D, .j,., w..x.pber 3 load 7 KG activated carbon.
    until the tea contains 45 The extraction autoclave and the adsorber are brought to a pressure of 24 MPa with the aid of C02 from the reservoir 6 for the liquid using a pump 7, after which the pump is removed from the cycle. After switching on the pump 7, the CO2 is circulated through the extraction autoclave and the adsorber, and the temperature in the extraction autoclave rises to 61 ° C due to the heat exchanger 4. The pressure in the extraction autoclave is 32 MPa. The adsorber operates at a pressure of 31 MPa and at 61 ° C. The circulating amount of CO2 is 800 kg / h. After 2.5 hours, extraction is stopped, CO2 is removed from the extraction autoclave until leveling.
    new in this case is superfluous. Thus, the inserts are fixed in an autoclave concentrically with the formation of a gap 14 for the extractant, an annular cavity for tea and a cavity for activated carbon. In the installation, a uniform flow of gas flow to the material to be extracted is ensured.
    The insert 12 for the material to be extracted (cha) can be installed in the autoclave 2 rigidly or with the possibility of extraction. Depending on this, loading with the material to be extracted is carried out either in a cylindrical autoclave or else outside of the latter in a tank for the material to be extracted. The collecting cylinder for the extracting agent is designed in such a way that it can be removed from the device when loading bulk material. This facilitates emptying of bulk material. Before new loading the pipe is put back again. If necessary, the collecting cylinder can be installed rigidly. The autoclave contains an annular cover 15.
    The proposed method and installation with a stream that passes through the extractable material radially is suitable for treating any bulk material that needs to be extracted with a CO2 extracting agent under high pressure conditions.
    The installation works as follows.
    The tea to be decaffeinated is moistened in mixer 1 and sent for extraction into a cylindrical autoclave 2. Carbon dioxide with caffeine contained in it is passed through activated carbon in adsorber 3. Activated carbon absorbs caffeine, carbon dioxide released from it goes out the adsorber 3 and through the pump 5 it is re-directed through the heat exchanger 4 to the extraction cylindrical autoclave 2. Consequently, the carbon dioxide is circulated in a closed loop. An extraction process, in which carbon dioxide passes through the plant, is repeated until
    very small amount of caffeine. After the extraction is completed, the CO2 is passed through valve 8 to reserve tank 6 or is expanded and only after that, i.e. after pressure equalization, the carbon dioxide is released into the atmosphere.
    Example I. 10 kg of Ceylon Blends grade tea with 5.9% H2O and 3.3% caffeine is moistened with 3.5 l of water in mixer 1 and then introduced into an extraction autoclave 2. Adsorber 3 is charged with 7 kg of activated carbon . The extraction autoclave and adsorber with C02 from the reservoir 6 for the liquid using a pump 7 is brought to pressure 30
    35
    50
    55
    pressures are released into the reserve; al for CO2 and then into the atmosphere. Tea is extracted from an extraction autoclave and dried in a dryer at 70 ° C. The analysis gives a residual moisture of 5.9% water and 0.07% caffeine.
    Example 4. 10 kg of Ceylon-Ble grade tea, nds with 5.9% water and 3.3% caffeine in a mixer are moistened with 2.7 liters of water and then injected into an extraction autoclave 2. 7 kg are loaded into adsorber 3 activated carbon The extraction autoclave and the adsorber are brought to a pressure of 20 MPa by means of CO2 from the tank 6 for liquid using a pump 7, after which the pump is taken out of the cycle. After switching on the pump 5, the CO2 is circulated through the extraction autoclave and adsorber, and the temperature in the extraction autoclave rises to 63 ° C due to heat exchanger 4. The pressure in the extraction aktoklav is 29 MPa. The adsorber operates at a pressure of 28 MPa and at 61 ° C. The circulating amount of CO2 is 800 kg / h. After 2.5 hours, the extraction is stopped, the CO from the extraction autoclave, until the pressure is equalized, is withdrawn to the reserve tank for CO, and then released to the atmosphere. Tea is extracted from the extraction autoclave and dried in a systelka at 70 ° C. The analysis gives a residual moisture of 3.7% water and 0.09% caffeine.
    Example 5. 10 kg of Ceylon-Blends grade tea with 5.1% water and 2.9% caffeine is moistened in a mixer with 1.0 l of water and then introduced into an extraction autoclave 2. Adsorber 3 is charged with 7 kg of activated carbon . The extraction autoclave and adsorber are brought to a pressure of 16 MPa by means of CO2 from the reservoir b for liquid using a pump 7, after which the pump is taken out of the cycle. After switching on the pump 5, the CO2 is circulated through the extraction autoclave and the adsorber, and the temperature in the extraction autoclave, due to the heat exchanger 4, reaches up to 65 ° C. The pressure in the extraction autoclave is 29 PAWS. The adsorber operates at a pressure of 28 MPa and at 64 ° C. The circulating amount of CO2 is 1280 kg / h. After 4 hours, the extraction is stopped, the CO2 is removed from the extraction autoclave until the pressure in the reserve tank for CO- is equalized and then released to the atmosphere. Tea is removed from the extraction autoclave and dried in a dryer at 70 ° C. The analysis gives a residual moisture content of 6.3% water and 1.12% caffeine.
    Example 6. 9 kg of Ceylon-Blends grade tea with 5.1% water and 2.9% caffeine in a mixer are moistened with 7.0 l of water and then injected into an extraction autoclave 2. 7 kg are loaded into adsorber 3 activated carbon The extraction autoclave and the adsorber are brought to a pressure of 16 MPa by means of CO2 from the tank 6 for the liquid using a pump 7, after which the pump is taken out of the cycle.
    After VK;:;; -, MI pump 5 CO: circulates through e; ..: iiaKiiMfVitibU autoclave and adsorber, n |) i-; ; o.M t {..; The oratory in the extraction autoclave due to heat exchanger 4 rises to 63 ° C. The pressure in the extraction autoclave is 28 MPa. The adsorber operates at a pressure of 27.NPa and at 61 ° C. The circulating amount of CO2 is 800 kg / h. After 2.5 hours, the extraction is stopped, CO2 is removed from the extractive actoclave until pressure is equalized in the CO2 storage tank and then released to the atmosphere. Tea is removed from the extraction autoclave and dried in a dryer at 70 ° C. The analysis gives a residual moisture of 6.7%
     water and 0.18% caffeine.
    Example 7. 10 kg of Ceylon-Blends grade tea with 5.1% water and 2.9% caffeine in a mixer are moistened with 3.5 liters of water and then injected into an extraction autoclave 2. Adopt sorber 3 is charged 7 kg of activated carbon. The extraction autoclave and adsorber are brought to a pressure of 22 AARP with the aid of CO2 from the tank 6 for the liquid using a pump 7, after which the pump is taken out of the cycle. After turning on the pump 5, CO2 is circulated
    5 through an extraction autoclave and an adsorber, the temperature in the extraction autoclave, due to the heat exchanger 4, rises to 50 ° C. The pressure in the extraction autoclave is 30 A lna. The adsorber operates at a pressure of 29 MPa and at 49 ° C. The circulating amount of CO2 is 800 kg / h. After 2.5 hours, the extraction is stopped, CO2 is removed from the extraction autoclave until pressure presses are flattened into a storage tank for CO. and then released into the atmosphere. Tea izv. Squeeze from the extraction autoclave 5a and dry in a bottle at. . Analysis will give a residual moisture content of 5.3% water and 0.25% caffeine.
    Example 8. 10 kg tea grade Ceylon Blends
    0, with 5.1% water and 2.9% caffeine in the mixer, is moistened with 1.57 liters of water and then introduced into an extraction autoclave 2. Adsorber 3 is charged with 7 kg of activated carbon. The extraction autoclave and the adsorber are brought to a pressure of 6 MPa by means of CO2 from the tank 6 for liquid using a pump 7, after which the pump is taken out of the cycle. After turning on the pump 5 CO., It circulates through the extraction autoclan and adsorber, and the temperature in the extraction autoclave due to the heat exchanger 4 rises to 65 ° C. Pressure in the extraction auto. the seam is 29 .. The adsorber operates under a pressure of 28 MPa and at 64 C. The circulating amount of CO2 is 1280 kg / h. After 4
    The g extraction is stopped, the CO2 is removed and the extraction autoclave until the pressure is equalized to the CO2 storage tank and then released to the atmosphere.
    five
    0
    feru. Tea is removed from the extraction autoclave and dried in a dryer at 70 ° C. The analysis gives a residual moisture of 6.4% water and 0.51% caffeine.
    Example 9. 10 kg of Ceylon-Blends grade tea with 5.1% pod and 2.9% caffeine in a mixer are moistened with 1.94 l of water and then injected into an extraction autoclave 2. 7 kg of activated carbon are charged to adsorber 3 . The extraction autoclave and the adsorber are brought to a pressure of 16 MPa by means of CO2 from the tank 6 for the liquid using a pump 7, after which the pump is taken out of the cycle. After switching on the pump, the 5CO2 circulates through the extraction autoclave and the adsorber, and the temperature in the extraction autoclave rises to 65 ° C due to the heat exchanger 4. The pressure in the extraction autoclave is 29 MPa. The adsorber operates at a pressure of 28 MPa and at 64 ° C. The circulating amount of COA is 1280 kg / h. After 4 hours, the extraction is stopped, CO2 is removed from the extraction autoclave until pressure is equalized to the CO2 storage tank and then released to the atmosphere. Tea is removed from the extraction autoclave and dried in a dryer at 70 ° C. The analysis gives a residual moisture of 6.7% water and 0.21% caffeine.
    Example 10. 10 kg of Ceylon Blends grade tea with 5.1% water and 2.9% caffeine in a mixer are moistened with 2.17 liters of water and then injected into an extraction autoclave 2. Adsorber 3 is charged with 7 kg of activated carbon . The extraction autoclave and the adsorber are brought to a pressure of 16 MPa by means of CO2 from the tank 6 for the liquid using a pump 7, after which the pump is taken out of the cycle. After switching on the pump 5, the CO2 is circulated through the extraction autoclave and the adsorber, and the temperature in the extraction autoclave rises to 65 ° C due to the heat exchanger 4. The pressure in the extraction autoclave is 29 MPa. The adsorber operates at a pressure of 28 MPa and at 64 ° C. The circulating amount of CO2 is 1280 kg / h. After 4 hours, the extraction is stopped, the CO2 from the extraction autoclave is withdrawn until the pressure in the CO2 storage tank is equalized and thereafter released to the atmosphere. Tea is removed from the extraction autoclave and dried in a dryer at 70 ° C. The analysis gives a residual moisture of 6.2% water and 0.13% caffeine.
    Example P. 10 kg of Ceylon.Blends grade tea with 5.1% water and 2.9% caffeine in a mixer is moistened with 4.94 L of water and then injected into an extraction autoclave 2. Adsorber 3 is charged with 7 kg of activated carbon . The extraction autoclave and the adsorber are brought to a pressure of 16 MPa by means of CO2 from the tank 6 for the liquid using a pump 7, after which the pump is taken out of the cycle. After switching on the pump 5, the CO2 is circulated through the extraction autoclave and the adsorber, and the temperature in the extraction autoclave rises to 60 ° C due to the heat exchanger 4. The pressure in the extraction autoclave is 26 MPa. The adsorber operates at a pressure of 25 MPa and at 58 ° C. The circulating amount of CO2 is 800 kg / h. 2.5 hours later
    the extraction is stopped, CO2 is removed from the extraction autoclave until the pressure in the reserve tank for CO2 is equalized and thereafter released into the atmosphere. Tea is removed from the extraction autoclave and dried in a dryer at 70 ° C. The analysis gives a residual moisture of 6.9% water and 0.16% caffeine.
    Example 12: 10 kg of Ceylon-Blends grade tea with 5.1% water and 2.9% caffeine in a blender are moistened with 5.85 liters of water and then
    is introduced into an extraction autoclave 2. Adsorber 3 is charged with 7 kg of activated carbon. The extraction autoclave and the adsorber are brought to a pressure of 16 MPa by means of CO2 from the tank 6 for the liquid using a pump 7, after which the pump is taken out of the cycle. After switching on the pump, the CO2 is circulated through the extraction autoclave and the adsorber, and the temperature in the extraction autoclave rises to 60 ° C due to the heat exchanger 4. The pressure in the extraction autoclave is 26 MPa. The adsorber operates at a pressure of 25 MPa and at 58 ° C. The circulating amount of CO2 is 800 kg / h. After 2.5 hours, the extraction is stopped, the CO2 is removed from the extraction autoclave until the pressure is equalized to the CO2 storage tank and then released to the atmosphere. Tea is removed from the extraction autoclave and dried in a dryer at 70 ° C. The analysis gives residual moisture.
    7.1% water and 0.18% caffeine.
    Example 13. 10 kg of Ceylon-Blends grade tea with 5.1% water and 2.9% caffeine in a mixer are moistened with 7.05 liters of water and then introduced into an extraction autoclave 2. Adsorber 3 is charged with 7 kg of activated carbon . The extraction autoclave and the adsorber are brought to a pressure of 16 MPa by means of CO2 from the tank 6 for the liquid using a pump 7, after which the pump is taken out of the cycle. After switching on the pump 5, the CO2 is circulated through the extraction autoclave and the adsorber, and the temperature of the extraction autoclave rises to 60 ° C due to the heat exchanger 4. The pressure in the extraction autoclave is 26 MPa. . Absorber operates under pressure
    25 MPa and at 58 ° C. The circulating amount of CO2 is 800 kg / h. After 2.5 hours, extraction is stopped, CO2 is removed.
    i 3 13
    extraction autoclave until the pressure in the reserve tank for CO2 is equalized and then released into the atmosphere. Tea is removed from the extraction autoclave and dried in a dryer at 70 ° C. The analysis gives a residual moisture of 6.8% water and 0.21% caffeine.
    Example 14. 10 kg of Ceylon- grade tea: B lends with 5.1% water and 2.9% caffeine in a mixer are moistened with 8.6 l of water and then injected into an extraction autoclave 2. Adsorber 3 is charged 7 kg of activated carbon. The extraction autoclave and the adsorber are brought to a pressure of 16 MPa by means of CO2 from the tank 6 for the liquid using a pump 7, after which the pump is taken out of the cycle. After switching on the pump 5, COA is circulated through the extraction autoclave and the adsorber, and the temperature in the extraction autoclave rises to 60 ° C due to the heat exchanger 4. The pressure in the extraction autoclave is 26 MPa. The adsorber operates at a pressure of 25 MPa and at 58 ° C. The circulating amount of CO2 is 320 kg / h. After 1 h, the extraction is stopped, the CO2 from the extraction autoclave is released into the storage tank for CO2 until the pressure is equalized and thereafter to the atmosphere. The experience is interrupted as the tea is crumpled and clogged the pipelines.
    Example 15. 10 kg of Ceylon-Blends grade tea with 5.1% water and 2.9% caffeine in a mixer are moistened with 3.65 l of water and then injected into an extraction autoclave 2. Adsorber 3 is charged with 7 kg of activated carbon . The extraction autoclave and the adsorber are brought to a pressure of 16 MPa by means of CO2 from the tank 6 for the liquid using a pump 7, after which the pump is taken out of the cycle. After switching on the pump 5, the CO2 is circulated through the extraction autoclave and adsorbate {5 and the temperature in the extraction autoclave due to the heat exchanger 4 rises to 65 ° C. The pressure in the extraction autoclave is 35 MPa. The adsorber operates at a pressure of 34 MPa and at 64 ° C. The circulating amount of CO2 is 800 kg / h. After 2.5 hours, the extraction is stopped, the COA from the extraction autoclave is discharged to the reserve tank for CO2 until the pressure is equalized and thereafter to the atmosphere. Tea is removed from the autoclave and dried in a dryer at .70 ° C. The analysis gives a residual
    moisture content of 6.1% water and 0.04% caffeine. Example 16. 10 kg of Ceylon-Blends grade tea with 5.1% water and 2.9% caffeine in a mixer are moistened with 3.75 liters of water and then injected into an extraction autoclave 2. Adsorber 3 is charged with 7 kg of activated carbon . The extraction autoclave and the adsorber are brought to a pressure of 16 MPa by means of CO2 from the tank 6 for the liquid using a pump 7, after which the pump is removed from


    0
    385
    -h
    cycle. After switching on the ICT, the CO2 is circulated through the extraction flax and adsorber, and the temperature in the extraction autoclave due to the heat exchanger 4 rises to 70 ° C. The pressure in the extraction autoclave is 29 MPa. The adsorber operates at a pressure of 28 MPa and at 68 ° C. The circulating amount of CO2 is 800 kg / h. After 2.5 hours, the extraction is stopped, CO2 is removed from the extraction autoclave until the pressure in the storage tank for CO2 is equalized and thereafter to the atmosphere. Tea is extracted from the extraction autoclave and dried in a dryer at 70 ° C. The analysis gives a residual moisture of 6.9%
    5 water and 0.06% caffeine.
    Example G /. 0.5 kg of Ceylon-Blends grade tea with 5.1% water and 2.9% coffe in mix. The mixture was moistened with 0.2 l of water and then introduced into an extraction autoclave. 2.
    Q Adsorber 3 is charged with 0.4 kg of activated carbon. The extraction autoclave to the adsorber is brought to a pressure of 16 MPa by means of CO2 from the tank 6 for liquid x by means of the pump 7, after which the pump is taken out of the cycle. After turning on the pump 5
    5 is circulated through an extraction autoclave and an adsorber, and the temperature in the extraction autoclave due to the heat exchanger 4 rises to 65 ° C. The pressure in the extraction autoclave is 29 MPa. The adsorber operates under pressure.
    0 28 MPa and at 64 C. The circulating amount of CO2 is 320 kg / h. After the extraction is interrupted, the CO is discharged from the extraction autoclave until the pressure in the storage tank for CO2 is equalized and thereafter to the atmosphere. Tea
    5 is removed from the extraction autoclave and dried in a dryer at 7G ° C. The analysis gives a residual moisture of 6/1% and 0, caffeine.
    40
    Example 18. 1 kg of Ceylon-Blends grade tea with 5.1% water and 2.9% caffeine in a mixer is moistened with 0.38 liter of veda. then they are introduced into the extraction autoclave 2. Adsorber 3 is charged with 1 kg of activated carbon. Extraction autoclave and adsorber
    45 using CO2 from reservoir 6 for a liquid is brought to a pressure of 16 MPa by means of a pump 7, after which the pump is taken out of the cycle. After switching on the pump 5, the CO2 is circulated through the extraction autoclave and the adsorber, and the temperature in the extraction auto 50 increases to 65 ° C due to the heat exchanger 4. The pressure in the extraction autoclave is 29 MPa. The adsorber operates at a pressure of 28 MPa and at 64 ° C. The circulating amount of CO2 is 640 kg / h. After 2 hours, the extraction is stopped, CO2 is released from the extraction autoclave until pressure is equalized to the reserve tank.
    55
    CO2 and then into the atmosphere. Tea is removed from the extraction autoclave and dried in a dryer at 70 ° C. The analysis gives a residual moisture of 7.0% water and 0.12% caffeine.
    Example 19. 10 kg of Ceylon Blends grade tea with 5.1% water and 2.9% caffeine is moistened in a mixer with 3.7 liters of water and introduced into an extraction autoclave 2. Adsorber 3 is charged with 7 kg of activated carbon. The extraction autoclave and adsorber with CO2 from the tank 6 for the liquid are brought to a pressure of 16 MPa by means of the pump 7, after which the pump is taken out of the cycle. After switching on the pump 5, the CO2 is circulated through the extraction autoclave and the adsorber, and the temperature in the extraction autoclave rises to 60 ° C due to the heat exchanger 4. The pressure in the extraction autoclave is 26 MPa. The adsorber operates at a pressure of 25 MPa and at 58 ° C. The circulating amount of CO2 is 640 kg / h. After 2 hours, the extraction is stopped, CO2 is released from the extraction autoclave until the pressure in the storage tank for CO2 is equalized and thereafter to the atmosphere. Tea is removed from the extraction autoclave and dried in a dryer at 70 ° C. The analysis gives a residual moisture of 6.8% water and 0.43% caffeine.
    Example 20. 10 kg of Ceylon-Blends grade tea with 5.1% water and 2.9% caffeine in a mixer are moistened with 3.85 l of water and then injected into an extraction autoclave 2. Adsorber 3 is charged with 7 kg of activated carbon . The extraction autoclave and the adsorber are brought to a pressure of 16 MPa by means of CO2 from the tank 6 for the liquid using a pump 7, after which the pump is taken out of the cycle. After switching on the pump 5, the CO2 is circulated through the extraction autoclave and the adsorber, and the temperature in the extraction autoclave rises to 60 ° C due to the heat exchanger 4. The pressure in the extraction autoclave is 26 MPa. The adsorber operates at a pressure of 25 MPa and at 58 ° C. The circulating amount of CO2 is 800 kg / h. After 2.5 hours the extraction is stopped, CO2 is released from the extraction autoclave and the adsorber is brought up with CO2 from the liquid reservoir 6 by means of the pump 7 to a pressure of 6 MPa, after which the pump is removed from the circulation. After switching on the pump 5, CO2 is pumped through the extraction autoclave and the adsorber, and the temperature in the extraction autoclave is raised through the heat exchanger 4 to 65 ° C. The pressure in the extraction autoclave is 29 MPa. AdsorUber operates at a pressure of 28 MPa and at 64 ° C. The circulating amount of CO2 is 1280 kg. After 4 h, the extraction is stopped, CO2 from the extraction autoclave, before pressure equalization, is dropped into
    .R. a collection of CO2 and then into the atmosphere. Tea is taken from the extraction autoclave and it is grown in a tree at 70 ° C. The analysis gives a residual moisture of 6.3% H2O and 1.12% caffeine. Thus, the amount of CO2 per gram of caffeine removed is 7.2 kg.
    20 Example 22. 10 kg of varieties of Ceylon blends with 5.1% H2O and 2.9% caffeine are moistened with 5.85 L of HgO in a mixing unit so that the tea has a moisture content of 40% by weight and then placed in an extraction autoclave 2. Load adsorber 3
     7 kg of activated carbon. The extraction autoclave and adsorber are brought by means of CO2 and a liquid tank 6 by means of a pump 7 to a pressure of 16 MPa, after which the pump is taken out of circulation. After switching on the pump 5, CO2 is pumped through the extraction autoclave and the adsorber, and the temperature in the extraction autoclave is raised through the heat exchanger 4 to 60 ° C. The pressure in the extraction autoclave is 26 MPa. The adsorber operates at 25 MPa and at 58 ° C. The circulating amount of CO2 is 800 kg. After 2.5 h, the extraction is stopped, the CO2 from the extraction autoclave is discharged into the CO2 collection until the pressure is equalized and thereafter to the atmosphere. Tea is taken from
    40 extraction autoclave and exist in a substance at 70 ° C. The analysis gives a residual moisture of 7.1% H2O and 0.18% caffeine. Thus, the amount of CO2 per gram of caffeine removed is 2.9 kg.
    Example 23. 0.5 kg Ceylon tea grade
    li UCf lJalJ-l.oivJ 1, fJDiii. I no. ".R. . “-, .. ..-.
    The ZING autoclave, up to leveling-° mixtures with 5.1% H2O and 2.9% caffeine, moisturize the pressure in the reserve tank for CO2 and then into the atmosphere. Tea is extracted from the extraction autoclave and dried in a nodule at 70 ° C. The analysis gives a residual moisture content of 6.5% water and 0.14% Q caffeine.
    Example 21. 10 kg of Ceylon blend tea with 5.1% H2O and 2.9% caffeine is moistened with 1.0 L H2O in a mixing unit so that the tea has a moisture content of 55–15% by weight and then placed in a conventional extraction autoclave 2. Adsorber 3 load 7 kg of activated carbon. Extract with the aid of 0.2 l of H2O in a mixing plant so that the tea has a moisture content of 32.2 wt.%, And then placed in an extraction autoclave 2. Adsorber 3 is charged with 0.4 kg of activated carbon. The extraction autoclave and adsorber are brought by means of CO2 from the liquid tank 6 by means of the pump 7 to a pressure of 16 MPa, after which the pump is taken out of circulation. After switching on the pump 5, the CO2 is pumped through the extraction autoclave and the adsorber, and the temperature in the extraction autoclave is raised through the heat exchanger 4 to 65 ° C. Extraction pressure
    The cancer autoclave and the adsorber are brought by means of CO2 from the liquid reservoir 6 by means of the pump 7 to a pressure of 6 MPa, after which the pump is taken out of circulation. After switching on the pump 5, CO2 is pumped through the extraction autoclave and the adsorber, and the temperature in the extraction autoclave is raised through the heat exchanger 4 to 65 ° C. The pressure in the extraction autoclave is 29 MPa. The adsorber operates at a pressure of 28 MPa and at 64 ° C. The circulating amount of CO2 is 1280 kg. After 4 h, the extraction is stopped, CO2 from the extraction autoclave, before pressure equalization, is dropped into
    R. a collection of CO2 and then into the atmosphere. Tea is taken from the extraction autoclave and it is grown in a tree at 70 ° C. The analysis gives a residual moisture of 6.3% H2O and 1.12% caffeine. Thus, the amount of CO2 per gram of caffeine removed is 7.2 kg.
    0 Example 22. 10 kg of varieties of Ceylon blends with 5.1% H2O and 2.9% caffeine are moistened with 5.85 L of HgO in a mixing unit so that the tea has a moisture content of 40% by weight and then placed in an extraction autoclave 2. Load adsorber 3
     7 kg of activated carbon. The extraction autoclave and adsorber are brought by means of CO2 and a liquid tank 6 by means of a pump 7 to a pressure of 16 MPa, after which the pump is taken out of circulation. After switching on the pump 5, CO2 is pumped through the extraction autoclave and the adsorber, and the temperature in the extraction autoclave is raised through the heat exchanger 4 to 60 ° C. The pressure in the extraction autoclave is 26 MPa. The adsorber operates at a pressure of 25 MPa and at 58 ° C. The circulating amount of CO2 is 800 kg. After 2.5 h, the extraction is stopped, the CO2 from the extraction autoclave is discharged into the CO2 collection until the pressure is equalized and thereafter to the atmosphere. Tea is taken from
    0 extraction autoclave and exist in a substance at 70 ° C. The analysis gives a residual moisture of 7.1% H2O and 0.18% caffeine. Thus, the amount of CO2 per gram of caffeine removed is 2.9 kg.
    Example 23. 0.5 kg Ceylon tea grade
    l ".r. . “-, .. ..-.
    ° Mixtures with 5.1% H2O and 2.9% caffeine with a mixture with 5.1% H2O and 2.9% caffeine are moistened with 0.2 L H2O in a mixing unit so that the tea has a moisture content of 32.2% by weight. %, and then placed in an extraction autoclave 2. In adsorber 3 load 0.4 kg of activated carbon. The extraction autoclave and adsorber are brought by means of CO2 from the liquid tank 6 by means of the pump 7 to a pressure of 16 MPa, after which the pump is taken out of circulation. After switching on the pump 5, the CO2 is pumped through the extraction autoclave and the adsorber, and the temperature in the extraction autoclave is raised through the heat exchanger 4 to 65 ° C. Extraction pressure
    the autoclave is 29 MPa. The adsorber operates at a pressure of 28 MPa and at 64 ° C. The circulating amount of CO2 is 270 kg. After 1 h, the extraction is stopped, the CO2 from the extraction autoclave is released into the CO2 collector before pressure is equalized and thereafter to the atmosphere. Tea is taken from the extraction autoclave and dried in a dryer at 70 ° C. The analysis gives a residual moisture of 6.4% H2O and 0.21% caffeine. Thus, the amount of CO2 per gram of caffeine removed is 20 kg.
    权利要求:
    Claims (2)
    [1]
    Claims. A method for decaffeinating tea, involving extraction with CO2 in an autoclave in the supercritical state by pressure and temperature in the presence of water, followed by separation of caffeine in the adsorber and drying tea, characterized in that, in order to simplify the process, increase efficiency and reduce energy consumption , before extraction, tea is moistened to a moisture content of 15-40% by weight, then the wetted mass of tea in the autoclave is molded into a cylinder, and CO2
    0
    passed through this cylinder and then sent to an adsorber with activated carbon and then back to the autoclave for circulation, the extraction being carried out at 26-35 MPa, 50-70 ° C and CO2 consumption of 2-20 kg per I g extractable caffeine.
    [2]
    2. A plant for decaffeinating tea, including a cylindrical extraction autoclave, a container for liquid CO 2 connected to the autoclave using a high-pressure pump, and an adsorber, in order to improve efficiency and reduce energy consumption, The adsorber is interconnected to form a closed loop, which has a heat exchanger and a pump installed in the area connecting the adsorber outlet to the autoclave inlet, while the autoclave is equipped with two perforated inserts chno placed in a cylinder with a gap for supplying obrazovanie.m extractant annular cavity for ca and capacity for the activated carbon, and the installation is provided with a mixing device for moistening tea, associated with the autoclave.
    0
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    同族专利:
    公开号 | 公开日
    EP0159724A2|1985-10-30|
    JPS60234548A|1985-11-21|
    EP0159724B2|1998-01-07|
    EP0159724B1|1991-07-03|
    DE3415844A1|1985-10-31|
    CA1248812A|1989-01-17|
    JPH053258B2|1993-01-14|
    DE3583354D1|1991-08-08|
    DE3415844C2|1994-02-03|
    AT64825T|1991-07-15|
    EP0159724A3|1988-07-20|
    引用文献:
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    US10426178B2|2014-03-26|2019-10-01|Infré Sa|Decaffeination methods and systems|CH535543A|1970-02-05|1973-04-15|Studiengesellschaft Kohle Mbh|Process for decaffeinating green coffee|
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    DE2727191B2|1977-06-16|1980-07-03|Hag Ag, 2800 Bremen|Process for the selective extraction of caffeine from plant materials|
    DE3339181A1|1983-10-28|1985-05-09|Uhde Gmbh, 4600 Dortmund|METHOD AND DEVICE FOR DECAFFINATING TEA LEAVES|
    DE3414767C2|1984-04-18|1989-06-15|Hopfenextraktion Hvg Barth, Raiser & Co, 8069 Wolnzach, De|
    EP0167399A3|1984-07-06|1987-08-26|General Foods Corporation|Decaffeination of fermented unfired tea|DE3339181A1|1983-10-28|1985-05-09|Uhde Gmbh, 4600 Dortmund|METHOD AND DEVICE FOR DECAFFINATING TEA LEAVES|
    DE3515740C2|1985-05-02|1993-07-29|Skw Trostberg Ag, 8223 Trostberg, De|
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    DE3640967A1|1986-11-29|1988-06-09|Sueddeutsche Kalkstickstoff|METHOD FOR DEAROMATIZING AND THEN REAROMATIZING TEA|
    AT388114B|1987-05-20|1989-05-10|Ver Edelstahlwerke Ag|METHOD AND ARRANGEMENT FOR LOADING A PRINT SPACE|
    DE3838952C2|1988-11-17|1993-08-19|Hopfenextraktion Hvg Barth, Raiser & Co, 8069 Wolnzach, De|
    DE4400096C2|1994-01-04|1997-06-12|Barth Raiser Hopfenextraktion|Process for decaffeinating black tea|
    DE19524481C2|1995-07-05|2000-03-02|Hopfenextraktion Hvg Barth, Raiser & Co|Procedure for decaffeinating black tea|
    CA2572995C|2004-07-09|2010-12-07|Nateco2 Gmbh + Co. Kg|Method for decaffeinating tea|
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    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    DE3415844A|DE3415844C2|1984-04-27|1984-04-27|Process for the production of decaffeinated tea|
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