![]() Method of preparing beta-dextrose
专利摘要:
A method for the production of an anhydrous powdered dextrose containing large amounts of anhydrous crystals of beta -form dextrose, characterized by concentrating aqueous solutions of dextrose, or aqueous solutions containing dextrose up to a sugar concentration of 90 to 98%, adding anhydrous crystals of beta -dextrose or powdered dextrose containing large amounts of anhydrous beta -dextrose as seed crystals to this concentrate at temperatures above 60 DEG C., maintaining the temperature above 60 DEG C., and while stirring gently, eliminating the free water by vacuum dehydration from the time of formation of microcrystals by adequately reducing the pressure. 公开号:SU751333A3 申请号:SU772528901 申请日:1977-10-03 公开日:1980-07-23 发明作者:Майз Есинари;Томимура Эйдзиро 申请人:Спс Интернэшнл Инк (Фирма); IPC主号:
专利说明:
(54) METHOD OF OBTAINING B-DVKTROSY one This invention relates to methods for producing anhydrous powdered dextrose containing, in large quantities, anhydrous dextrose from dextrose solutions. It is known that there are three types of dextrose crystals: anhydrous a-dextrose crystals, a-dextrose monohydrate crystals and anhydrous f) -dextrose crystals. Of these, anhydrous dextrose has an advantage over the others, since it dissolves faster, is more soluble in cold water, and lumps less when dissolved than monohydrate and anhydrous CL-dextroses. The advantage of anhydrous f-dextrose is also that, compared to dextrose monohydrate, it can be used regardless of the moisture content, while the moisture content. in dextrose monohydrate, it is about as crystallization water. The closest to the proposed technical essence is the method of obtaining crystalline anhydrous f-dextrose, which consists in concentrating the initial aqueous solution of dextrose, which is used as a starch hydrolyzate with a dextrose content of 95-97%, under reduced pressure to a concentration of 8891 ° Brix , heated to a temperature of 85-110 ° C, seeded in the form of powder of anhydrous f-dextrose crystals at a temperature of 85-110 ° C and stirring and subjected to further dehydration the resulting mass 1. Dehydration uschestvl kristallomassy by centrifugation. Liquid (mother liquor), removed by centrifugation, contains dissolved dextrose, this dextrose is not removed. As a result, the final yield for crystalline dextrose is not high. The purpose of the invention is to increase the yield of p-dextrose. For this, in the proposed method, the concentration of the initial solution is carried out to 90-98% CB, and the dehydration of the concentrated solution with the seed is carried out under vacuum at a pressure of 200
权利要求:
Claims (6) [1] 20 250 mmHg Art. with stirring until a crystalline mass is formed, followed by a decrease in pressure to 50-100 mm Hg. by holding the mass at this pressure and further reducing the pressure to 15-30 mm Hg. Art. until the product has a moisture content of 0.5-1.0%. As a starting solution, saccharified starch solution can be used. The proposed method is as follows. The original aqueous solution of dextrose may contain various substances. For example, potato starch, wheat starch, and the like, can be saccharified by an acid-enzyme hydrolysis method or an enzyme-saccharification enzyme process to produce a saccharified starch solution. From these saccharified starch solutions, various dextrose-containing solutions can be obtained. Purified or partially purified solid dextroses can be redissolved in water and aqueous solutions of dextrose can be obtained, which can be used as the starting material for the production of p-dextrose. The purified or crude dextrose solution is concentrated to 90-98% CB, heated to 80-95 ° C and stirred at this temperature in a mixer. Seed crystals without aqueous dextrose or powdered dextrose containing large amounts of dextrose are then introduced into the solution. The seed crystals in size should be no more than about 100 bricks (US sieve standard). The proportion of anhydrous f-dextrose in the seed should be greater than 85%, better than 90%. It is also possible to use the powdered anhydrous dextrose obtained by the proposed method as seed crystals. From the point of view of priming and profitability, this is the best way. The amount of seed crystals should be at least 0.2% based on the dry matter of the sugar solution. It is advisable that the amount of seed crystals be at least 10%. Of course, large amounts can be used, but this is hardly advisable. The degree of crystallization of anhydrous dextrose depends on the JOT temperature at which crystallization occurs. For example, if anhydrous -dextrose is used as a primer, the anhydrous dextrose content in the product is 93% at 97 ° C, 890/0 at 10 ° C, 85% at and 59% at 40 ° C. Thus, it is possible to vary the degree of crystallization of anhydrous p-dextrose by changing the operating temperature. Crystal formation usually begins quickly, i.e. 10 minutes after the addition of seed crystals. The mass becomes layered and contains white microcrystals. In addition, when microcrystals are formed, the amount of free water increases in accordance with the number of crystals formed, and therefore the concentration of the sugar solution decreases. The concentrated solution with the seed is dehydrated under vacuum at a pressure of 200-250 mm Hg. Art. with stirring. Thus, with the continuous formation of microcrystals, the formation of free water and the removal of free water, the amount of water gradually decreases and at the same time the substance itself becomes crystalline and becomes a solid powder. The reduced pressure should be sufficient to remove free water. It is better to apply such pressure so that when a large amount of free water suddenly evaporates, the temperature of the mass will not decrease. For example, at 90-95 ° C it is necessary to maintain a pressure of 200-250 mm Hg. (absolute). If a significantly lower pressure is used than in the initial stage, the temperature drops and the degree of crystallization of the anhydrous-dextrose decreases. The stripping of free water continues until almost all of the dextrose crystallizes. This usually takes about 0.5 hours. The work of the agitator causes a flowable powder to form from the dehydrated mass. To improve product stability, it is better to dry the product under reduced pressure. The pressure is further reduced and, with good drying, the flowability of the powder is improved. The pressure at this stage is 50-100 mm Hg. century, the mass is maintained and then the pressure is reduced to 1530 mm Hg. Art. In this way, a free flowing anhydrous powdered dextrose is obtained which contains a large amount of anhydrous microcrystalline dextrose with a moisture content of about 0.5-1% and less. Powdered dextrose crystals, which are microcrystals, can be obtained by the proposed method, since crystallization occurs under conditions of a very high sugar concentration, i.e. 90-98%. For this reason, in comparison with the products obtained by other crystallization methods, this powdered dextrose has a large specific surface area and is characterized by a greater dissolution rate. Further, according to the proposed method, the whole solid fraction of the sugar solution can be powdered without affecting the formation of microcrystals, since centrifugation or washing is not used. Therefore, this method provides powdered dextrose containing a large amount of dextrose, at a low production cost. Example 1. Technical anhydrous dextrose is dissolved in water and the solution is concentrated to 96% in an evaporator at 90 ° C. Then the solution is fed into the mixer and stirred (5 rpm) at 90 ° C. The mixer is equipped with a device for temperature control and for vacuum distillation of water. The anhydrous p-dextrose is then ground to a size of about 100 mesh, warmed to 90 ° C and added to the concentrated sugar solution in the mixer in an amount of 0.2% by weight of the solid fraction in the indicated sugar solution. After 10 minutes, when the whole solution turns into a white plastic paste, the water begins to distil under vacuum at 200-250 mmHg. Art. After another 10 minutes, when the mass turns into a white microcrystalline powder mass, the pressure is further reduced to about 100 mm Hg. Art. Even after 5 minutes, when the fluidity of the powder increases, the pressure is reduced to 20 mm Hg. Art. and less and lead further dehydration. The measurement of the optical rotation of powdered dextrose thus obtained shows that it contains about 92% anhydrous 6-dextrose with a moisture content of 0.5% and below. Example [2] 2. Technical anhydrous dextrose is dissolved in water and concentrated in an evaporator to 96% at 90 ° C. Then it is fed into the mixer and stirred (5 rpm) as in example 1, at 90 ° C. Then, the microcrystalline powder obtained in Example 1 was milled to 100 mesh and added to the concentrated sugar solution in the mixer in an amount of 0.2% by weight of the solid fraction in the specified solution. Further processing is carried out as in Example 1. Thus obtained, powdered dextrose contains about 90% anhydrous A-dextrose and 0.5% / v of moisture. Example [3] 3. Technical corn starch is cooked with a technical enzyme preparation, and a saccharified starch solution is obtained (DE 95.5). It is cleaned with activated carbon and ion exchange resin according to the standard procedure, evaporated to 96% in an evaporator at 95 ° C. This concentrated solution is then transferred to a mixer as in Example 1, in which the temperature is maintained at 95 ° C. The anhydrous β-dextrose is then ground to 100 mesh and added to the concentrated sugar solution in a blender in an amount of 10% by weight of the solid fraction in the solution. Treatment is carried out as in Example 1. The resulting powdered dextrose contains about 89% anhydrous -dextrose and 0.5% moisture. Example [4] 4. Technical corn starch is cooked with a technical enzyme and get the saccharified starch solution (DE 95.5). It is cleaned with activated carbon and ion exchange resin according to standard methods and evaporated in an evaporator to a concentration of 96% at a temperature of 95 ° C. This concentrated solution is then fed to the mixer, as in example 1, at a temperature of 95 ° C. The dextrose powder obtained in Example 3 is then milled to 100 mesh and added to the concentrated sugar solution in a mixer in an amount of 10% by weight of the dry phase in this solution. Treatment is carried out as in Example 1. The resulting powdered dextrose contains 89% anhydrous -dextrose and 0.5% moisture. Example [5] 5. Technical corn starch is cooked with a technical enzyme and get the saccharified starch solution (DE 95.5). It is cleaned with activated carbon and ion-exchange resin in the usual manner and evaporated in an evaporator to a concentration of 96% at a temperature of 95 ° C. This concentrated solution was transferred to a mixer, as in Example 1, at 95 ° C. The powdered dextrose obtained in Example 3 is then ground to about 100 mesh and added to the concentrated sugar solution in the specified mixer in an amount of 10% by weight of the solids in piacTBOpe. After 10 minutes, when the entire solution becomes a white, mobile paste-like mass, it is dehydrated in vacuum at a pressure of 200-250 mm Hg. Art. After another 10 minutes, when the mass turns into a white microcrystalline powder, the pressure is reduced to 50 mm Hg. (absolute) or less and continue to dehydrate. The dextrose thus obtained contains about 88% p-dextrose and 0.5% moisture. Example [6] 6. Sugar solution DE 98, obtained by enzymatic saccharification of corn starch, is crystallized by the standard method. After removing the crystals, the first molasses is cleaned with activated carbon and ion exchange resin according to the standard procedure and evaporated in an evaporator to a concentration of 96% at 95 ° C. This concentrated solution is then transferred to a mixer as in Example 1, in which the temperature is maintained at 95 ° C. Then, the dextrose powder obtained in Example 3 is milled to about 100 mesh and added to the concentrated sugar solution in the mixer in an amount of about 10% by weight of the solid fraction in the solution. Further, the treatment is carried out as in Example 1. Powdered dextrose thus obtained contains 84% p-dextrose and 0.5% moisture. Claims 1. A method of producing p-dextrose, comprising concentrating a solution containing dextrose, maintaining the solution at a temperature of 80-95 ° C, the introduction of a seed containing p-dextrose, and dehydration of the concentrated solution with a seed, characterized in that, in order to increase the yield of dextrose, the concentration of the initial solution is carried out to 90-98% CB, and the dehydration the concentrated solution with the seed is carried out under vacuum at a pressure of 200250 mm Hg. Art. and when moving to form a crystalline mass with a subsequent decrease in pressure to 50100 mm Hg. by holding the mass at this pressure and further reducing the pressure to 15-30 mm Hg. Art. until the product has a moisture content of 0.5-1.0 / o2. A method according to claim 1, characterized in that the saccharified starch solution is used as the initial solution. Sources of information taken into account in the examination 1. French patent number 2005688, cl. From 13 to 1/00, published. 1969 (prototype).
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同族专利:
公开号 | 公开日 CH634109A5|1983-01-14| FR2366361A1|1978-04-28| MX4373E|1982-04-19| FI772905A|1978-04-05| JPS5352637A|1978-05-13| ATA702777A|1980-03-15| MY8000082A|1980-12-31| HU176497B|1981-03-28| RO72591A|1981-06-26| SE7711022L|1978-04-05| NZ185327A|1979-10-25| FR2366361B1|1983-02-04| US4297146A|1981-10-27| NL7710831A|1978-04-06| BE859296A|1978-04-03| DK436577A|1978-04-05| TR19659A|1979-09-17| FI62337B|1982-08-31| FI62337C|1982-12-10| YU237677A|1982-10-31| JPS5719960B2|1982-04-26| GB1542167A|1979-03-14| ES462861A1|1978-06-01| CA1094058A|1981-01-20| AR212892A1|1978-10-31| ZA775869B|1978-11-29| IT1087724B|1985-06-04| AU2934177A|1979-04-12| AU511587B2|1980-08-28| DE2744099A1|1978-04-06| AT359446B|1980-11-10|
引用文献:
公开号 | 申请日 | 公开日 | 申请人 | 专利标题 RU2521510C1|2012-12-29|2014-06-27|Государственное научное учреждение Всероссийский научно-исследовательский институт крахмалопродуктов Российской академии сельскохозяйственных наук|Method of obtaining crystalline anhydride glucose|US2324113A|1941-07-01|1943-07-13|American Maize Prod Co|Method of making dextrose| FR1052692A|1951-09-22|1954-01-26|Corn Prod Refining Co|Beta-dextrose production process| US3085914A|1959-06-30|1963-04-16|Corn Products Co|Novel crystalline sugar products| US3197338A|1962-06-21|1965-07-27|Staley Mfg Co A E|Method of producing dried starch conversion product| NL300874A|1962-11-23| FR1384712A|1963-11-22|1965-01-08|Corn Products Co|New manufacturing process for dextrose| GB1252523A|1968-04-06|1971-11-03| FR2027545A1|1968-11-22|1970-10-02|Hayashibara Co| US3748175A|1969-04-06|1973-07-24|Tokai Togyo Kk|Process for preparing crystalline anhydrous beta dextrose| US3650829A|1969-08-06|1972-03-21|Cpc International Inc|Method of producing granular dextrose| US3752877A|1969-08-27|1973-08-14|Parsons Co Ralph M|Recovery of sulfur compounds from tail gases| GB1461070A|1970-07-17|1977-01-13|Shell Int Research|Process for reducingthe total sulphur content of claus- off- gases| US3864460A|1973-07-12|1975-02-04|Nrg Inc|Method for removing hydrogen sulfide from hydrocarbon gas streams without pollution of the atmosphere| US3981739A|1974-08-30|1976-09-21|Amstar Corporation|Continuous crystallization| US4059460A|1975-11-07|1977-11-22|A. E. Staley Manufacturing Company|Solid anhydrous dextrose| US4041130A|1975-12-29|1977-08-09|The Ralph M. Parsons Company|Process for desulfurization of coke oven gas|US4888060A|1985-06-21|1989-12-19|A. E. Staley Manufacturing Company|Enrichment of fructose syrups| DK159488A|1988-03-23|1989-09-24|Danske Sukkerfab|Apparatus for stretching of reinforcement lock strips| FI97625C|1995-03-01|1997-01-27|Xyrofin Oy|Method for crystallization of xylose from aqueous solutions| FI952065A0|1995-03-01|1995-04-28|Xyrofin Oy|Foilfarande Foer tillvaratagande av en kristalliserbar organisk foerening| US6527868B2|1999-12-15|2003-03-04|Roquette Freres|Dextrose in powder form and a process for the preparation thereof| FR2787811B1|1998-12-24|2001-03-02|Roquette Freres|POWDER DEXTROSE AND PROCESS FOR THE PREPARATION THEREOF| FR2877186B1|2004-10-29|2007-02-09|Roquette Freres|NON-FOOD AND NON-PHARMACEUTICAL USE OF A SELECTED ANHYDROUS DEXTROSE COMPOSITION| WO2020112159A1|2018-11-30|2020-06-04|Amerilab Technologies, Inc.|Rapidly disintegrating effervescent tablets and methods of making the same|
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申请号 | 申请日 | 专利标题 US05/729,325|US4297146A|1976-10-04|1976-10-04|Method for the production of powdered dextrose| 相关专利
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