• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
  • 同族专利
  • 引用文献
  • 法律状态
  • 优先权
    • 专利摘要:
    Process for the production of shaped articles starting from industrial and mineral waste materials characterized in that it comprises depositing a layer of an aqueous slurry composed of a mixture of a fibrous component and a mineral component; controlling the water content of the slurry in order to produce a coherent agglomerated layer having a degree of wet strength; then shape the layer under pressure; and take out to produce a shaped article.
    公开号:SU936803A3
    申请号:SU782625600
    申请日:1978-06-15
    公开日:1982-06-15
    发明作者:Ваутер Каувенховен Германн；Хартман Юрриан Сторк Виллем；Схапер Ламберт
    申请人:Шелл Интернэшнл Рисерч,Маатсхаппий Б.В. (Фирма)；
    IPC主号:
    专利说明:

    (5) METHOD FOR OBTAINING AROMATIC HYDROCARBONS
    one
    The invention relates to methods for the preparation of Cg-C.pM aromatic hydrocarbons that can be used in the refining, petrochemical, oil shale and coking industries.
     .. ....
    A known method for producing aromatic hydrocarbons by reacting toluene with synthesis gas and
    The process is carried out, for example, at a pressure of 52.5 atm in the presence of a crystalline oxide catalyst containing Cr, 0-, ZnO mixed with zeolite.
    The disadvantage of this method is low yield of aromatic hydrocarbons Cg, not exceeding E, E. A method is known for producing p-xylene by conversion of isobutylene in the presence of an oxide catalyst containing MgO 2. I
    The disadvantage of the method is a low yield of p-xylene, not exceeding 71.
    io
    Closer to the present invention is a method for producing aromatic hydrocarbons by converting synthesis gas at 300-350 ° C, pressure
    5 36-52,5 atm in the presence of a crystalline oxide catalyst containing a mixture of oxides of copper and iron. chromium and type Y zeolite. In this case, 8.9 catalyzate is obtained, containing
    10%, 1% aromatic hydrocarbons 40.7; alkenes 39, paraffin hydrocarbons 20.3 GZ.
    However, this method of obtaining aromatic hydrocarbons does not have a 15% yield of aromatic hydrocarbons per raw material, which does not exceed 5. The purpose of the invention is to increase the yield of the target product.
    20 . This goal is achieved in that according to the method of producing chromatic hydrocarbons from a raw material selected from the group containing isobutylene or methanol, or W-hexadecane, or a gas mixture of hydrogen and carbon monoxide, or mixtures of toluene and methanol, by carrying out the process at a pressure of 30 atm using a crystalline shakat thermally stable at 600–1050 0, absorbing 6–8.2 weight of water at 25 ° C and pressure on the shielded water vapor and after vacuum in a vacuum and having a powder X-ray diffraction gram mu containing reflexes, given in Table. 1, containing the following components, weight D: 0.1-0.2 Sodium oxide 5.5-8.0 Iron oxide 1.7-2.2 Alumina 0.7-0.8 Silicon oxide Rest Sodium oxide 0, 05-0.2 0.8-8.0 Iron oxide 0.15-0.7 Water Rest Silicon oxide Crystalline silicate contains chromium oxide and zinc oxide. The results of powder diffraction of the 1st radiograph are given in tab. Table 3 Continued tabl, 1 Radiation, Note wavelength 0, HM.VS is very strong; Ssilny, M - medium; W - weak, - the value of the angle according to the Bragg law, Example. Receiving silicates 1-12. Silicate 1. A mixture of Fe (NOj), j, SiO, NaNOa and (NjCH in water, having the molar composition Nap 4,5 Fe ,, 1 Si02 ;. is heated with stirring for 48 hours in an autoclave at autogenous pressure. After cooling the reaction mixture, the resulting silicate is filtered, washed with water until the pH of the wash water is about 8, and dried for 2 hours at. The silicate 1 thus obtained has the following chemical composition: 0.67 L (C, H -,} О x xO, 23Nagb -FejO -SO SiOa-9 NdO Silicate 2. This silicate is obtained as silicate 1, but the raw material is taken up as a mixture having a molar leaving: - ", 5 G (C ,, H7) 4 NJO i (Q, 5 Fe2.0 29.1 468 lij). The silicate 2 thus obtained has the following chemical composition: 0.80 C (C5H, LN.p. 0.30 Na.O- Fe.O, x X 45 Si02..13 HjO: Silicate 3. This silicate is obtained as silicate 1, but the raw material is a drawn mixture, which in addition to FerNOj) contains ALCNOj) and has the following molar composition:., 5 - (-0.33, - 0.67.. 29.1 N3.0. The silicate 3 thus obtained has the following chemical composition: 0.55 (CjHyLNjiO- 0.45 Naap x X 0.67 - 0.33 Al, jO. 30 SiO x X 10 HiO. Silicate k. This silicate is obtained as silicate 3, but the initial material is an extracted mixture having the following molar composition: Na, 0 x X ".S 1 () Schur-0.5 AlaOj XX 0.5 Fe O 3-29.1 N , 0. The silicate f thus obtained has the following chemical composition: 0.86 CCCaH l NJjL O. 0.3 NagO 0.55 F & O X 0, Aii.0v 32 SiOi8. Silicate 5. This silicate is obtained as silicate 1, but the starting material is a stripped mixture containing A1 (Yuz) instead of FeCNOj) and having the following. molar composition: Nae.0 х 9 3 X i, 5 (СзН,)., 1 X Н-0. The silicate thus obtained has the following chemical composition: 0, (CjH,) 0.2 Na О X X. – 21.6 SiOa-. Silicate 6. This silicate is obtained as silicate I, but with the starting material, a precipitated mixture that does not contain PILTA, 3) and has the following molar composition:, 5CCCH III |) x 29.1 SiO. thirty . . The resulting silicates 1-6 have a powder X-ray diffraction of My, as indicated in table. 2.. Table 2
    Note. The values of the thermal stability of silicates 1-6 and the amount of water that they, after dehydration at lOO C, absorb in vacuum at 25 ° C and under saturated pressure of water vapor, are given in Table. 3 The composition of the obtained silicates in wt.% Are given in table. .
    Powder X-ray diffraction of silicate (radiation: CXa-KL, wavelength 0, nm). g
    Table 3
    the intensity of the strongest characteristic found in the radiograph, SP - sharp, SR - shoulder; NL - normal; BD - wide; Q is the angle according to the Bragg law.
    Silicates 7-12.
    Using silicates 1-6 as starting material, silicates 7-12 are obtained, respectively, by successive stages of calcining -6 silicates for k hours at 500 ° C, boiling with a 1.0 M solution of water, followed by boiling with 1 , 0 M solution of NbLNO and washing, drying for 2 h with and calcination for k h at. The composition of the obtained silicates, parts:
    Silicate 7 - 0.85 H, 0.05 Na O x X 30 SiOj.
    Silicate 8 - 1 ,, 0.05 Na, j, 0 x X Fe2.05 5 SiO.
    Silicate 9 - 0.95 0.05 Na / jO x X 0.67 Fe O 0, Of the silicates 1-12 described above, "only silicates 1-, 7-to are offered silicates. Silicates 5,6, 11 and 12, which do not contain iron, are not the object of the invention and are included for comparison. B50 of the proposed silicates, the negative electvalence of iron or / and aluminum is compensated for by replaceable cations in such a way that for each atom of iron and / or aluminum 55 there is one monovalent cation. EXAMPLE 2. Preparation of p-krilol from izobutylene. IM and 12 silicates are tested as catalysts in the preparation of rti-xylene from isobutylene. To this end, isobutylene is passed over a fixed layer of These silicates at atmospheric pressure, and the space velocity. The results of these experiments are shown in Table. five
    The results are shown in Table. show the advantage of iron-containing silicates as catalysts for the selective production of p-xylene from isobutylene (experiments 1-3) as compared with the corresponding non-iron silicates (experiments 5)
    The compositions of the liquid products, roller in experiments 1-5, are given below.
    Experience 1. The composition of the liquid product. weight.:. .
    Benzene0,3
    Toluene3 8
    p-Xylene6,4
    o-xylene3,3
    . NV-Xylene
    Cft-Aromatic hydrocarbons 20.3 and higher aromatic hydrocarbons Naphthenes + paraffins + f olefins 18.8
    Experience 2. The composition of the liquid product wt.%
    Benzene, 0.2
    / Toluene 3,0
    P-xylene11,3
    o-Xylene0,6
    M-Xylene 0.6
    Cft-aromatic hydrocarbons 16.3 and higher aromatic hydrocarbons35, 0 Naphthenes paraffins h + ole-Finm 331 P
    Experience 3. The composition of the liquid product
    %%: .
    Benzene, 0.2
    Toluene2,2
    . ; p-Xylene6,8
    O-xylene2,4
    M-Xylene 2,5, Cj-aromatic hydrocarbons 11.3 and higher aromatic hydrocarbons30, 7 Naphthenes + paraffins + olefins 3.3 Experience A. The composition of the liquid product,
    eD:
    Benzene, 0.2
    Toluene3
    P-Xylene3.9 O-Xylene6.9 M-Xylene6.8 CQ-aromatic hydrocarbons17.8 and above aromatic hydrocarbons38, 3 Naphthenes + paraffins + olefins22.7 Experience 5. Composition of the liquid product, EU. %:
    Benzene0,1
    Toluene 0.5
    p-Xylene0,4
    O-Xylene0,6
    M-Xylene 0.5 Cd-aromatic
    hydrocarbons2.9 and higher aromatic hydrocarbons6, 2 Naphthenes + paraffins + olefins 88.2 Example 3- Preparation of aromatic compounds from methanol. Silicate 8 was tested as a catalyzate for the preparation of aromatic compounds from methanol. To this end, the metal is passed over a fixed layer of 5 atm. Of this silicate at a pressure, and a space velocity of 1 h. 100 weight.h. 28.7 ve of a mixture of liquid oxygen-containing organic compounds is obtained as the starting material. The average number of carbon atoms in this mixture is 9.5. The mixture contains 59.6% of aromatic hydrocarbons distributed as follows in the form of various compounds, wt.%: Benzene Toluene P-Xylene M-Xylol o-Xylene Co-Aromatic hydrocarbons - Aromatic hydrocarbons Non-aromatic hydrocarbons are present in the liquid product §, trace quantities, wt.%, in terms of liquid product: Pentanes Cyclopentanes Hexanes Cyclohexanes Heptanes and higher boiling paraffins Cycloheptanes and others. Higher boiling naphthas Gas has the following composition, weight Propane Butanes p 4. Preparation of aroma N-hexadecane gasoline. Silicate 9 was tested as a catalyst in the preparation of aromatic gasoline from H-hexadecane. For this purpose, -hexadecane is passed over a fixed layer of this silicate at a pressure of 5 atm, 375 ° C and a volume growth of 1 h. The feed material is transformed into a product having the following composition, wt.,:, 0. , -Sur The resulting liquid product has the following composition, wt.%: Benzene Toluene P-Xylene o-Xylene M-Xylene C-Aromatic hydrocarbons and above aromatics17, 3 Å hydrocarbons Olefins 10.0 Naphthenes 20.0 Paraffins 25.0 Example 5 Receiving silicates 13-23. Silicates Silicate 13 is obtained as silicate 1, the only difference is that the aqueous mixture has the following molar composition: 0.8 (C3li, l4Nj-iO ..0.3 NaO-Fe-Q. X X 200 SiO-j .- 55 NgO. Silicate 13 produces silicate 1 in the same way that silicates of silicates 1-6 are obtained, respectively, and silicate 13 produces silicate 15 through successive calcination of silicate 13 for k h at 500 ° C, boiling with 1 , 0 M solution of washing with water, then boiling with 1.0 M solution of NaNO and washing, drying for 2 hours with roasting and for 4 hours at 500 ° C. The silicate 15 thus obtained has the following chemical composition: X 200 SiOj. Silicates .16 and 17. Silicate 16 is obtained in the same way as silicate 1, but the initial mixture is taken up as an aqueous mixture that does not contain NaNO and has the following molar composition: 1.5 UCjHy) NjjPFe p. ,, x x 205 310450-И2.0. Silica 17 is prepared from silicate j6, calcined for 4 hours at 500 ° C .; Silicates 18 and 19. The first mixture containing 6.18 g of I-butylamine, 6.2 g of water glass (28 SiOa., 8 Ph. O.) and
    56.2 g of water are mixed with a second mixture containing 1.3 g of Fe (804) 5-9 3.75 g of HjSQi and 77 g of water. The mixture thus obtained is stirred for 2 hours at room temperature, and then heated for 8 hours with stirring in an autoclave at an autogenous pressure. After cooling the reaction mixture, the resulting silicate is filtered.
    Powder x-ray diffraction (radiation CK, wavelength: O. nm), these silicates are given in Table. 7
    权利要求:
    Claims (3)
    [1]
    Table 7 Continued table. / Silicate 22. A mixture of Fe (NO) i, SiOj NaCH and (in water, having a molar composition of 16 32 (510, -7200 heated with stirring for 2k hours in an autoclave at 15 CgS under independent pressure. After cooling the reaction mixture, the ; silicate filters are washed, washed with water until the pH of the wash water reaches approximately B and dried for 2 hours at 120 C. Silicate 22, prepared in this way, has the following chemical composition: 0.7 (t (0 , 23 - РвзО ,; SiOa-9H ..... Silicate 23. Silicate 22 is calcined for 4 hours at 500 ° C, then boiled with 1.0 And ammonium nitrate solution and washed with water, then re-boiled with a 1.0 solution of ammonium nitrate. washed, dried for 2 hours and calcined for k hours with .. Silicate 23, thus obtained, has the following chemical composition: 0.9 HJJ X 0, 05 Fe2.0 "v340 SiO. Of silicates 13-23, only silicate 21, which is an amorphous product, is not covered by the scope of the present invention and is included for comparison. Silicate compositions are in weight. are given in table. k,. Example 6. Single-stage production of aromatic hydrocarbon mixture from the mixture. The catalyst is prepared by mixing silicate I with a mixture of 71.7 wt. ZnO and 28.6 ppA in a weight ratio of 1: 5. Both components are present in the catalyst in the form of particles with a diameter of 0.1-0.3 mm. The composition of the catalyst is as follows, wt.% 0.083 0.2167 SiO., 16.4167 H, 0. 0.0250 ZnO 59.5000 23.8333 This catalyst was tested for one stage, an aromatic hydrocarbon mixture from a mixture. The test was carried out in a 50 ml reactor, KotopoM contained a fixed catalyst bed of 7.5 ml. The mixture at a molar ratio of 2: 1 is contacted with a catalyst at a pressure of 30 atm and a space velocity of 1 ml of gas / l of catalyst / h. The results of this experiment are as follows: Conversion of CO, 75 Conversion of Hj,% 35 Composition of the obtained products, wt. Based on hydrocarbons, 8 Cj10.3 Cz15.9 C4t2.7 and above The resulting liquid products have the following composition, eec.% I Benzene0.2 Toluene 1.8 P-Xylene 6.7 o-Xylene 3,3 M-Xylene 3.4 C "-Aromatic hydrocarbons 25.0 C-aromatic hydrocarbons 15, 2 C. and higher aromatic hydrocarbons 7.9 Paraffin Ch-olefins 14.0 Naphthenes 22.5 Example 7- Production of aromatic, gasoline from aromatic n-hexadecane gasoline from i-hexadecane. For this purpose, I-hexadecane is passed over a fixed bed of this silicate at a pressure of 5 atm, 375 C and a space velocity of 1. The feed material is completely converted into a product having the following composition, weight. , 1 Cr 0; 6 p 9 The obtained liquid products are the following composition, wt.% Benzene 0.1 Toluene J, lt P-Xylene 3 6 o-Xylene 1; 7 m-K-s ol1,7 Cp-aromatic hydrocarbons 12.5 and higher aromatic hydrocarbons 16.7 Olefins10.0 Naphthenes .23.0 Paraffins27.0 Example 8. Preparation of P lola by methylation of toluene. Silicate 14 was tested as a catalyst for the production of p-xylene by meting toluene. For this purpose, a mixture of toluene and methanol in equivalent amounts is passed over the viscous layer, 5 m atm of this silicate, and a volume growth of 1 h. The results of the experiment are as follows: Toluene conversion, wt.%. Methanol conversion, wtD Selectivity to Cg aromatic hydrocarbons,% Amount of p-xylene in Cr-aromatic fraction,% The resulting total products have the following composition, weight: Methane0.1 Ethane + ethylene 0.5 Propane + propylene 1, 4 Butanes + butylenes 2, 0 Pentanes + pentenes 3.0 Benzene0.1 Toluene49.0 o-Xylene3.2 GL-Xylene3.3 P-Xylene26.5 C (, aromatic hydrocarbons 2.9-aromatic hydrocarbons 3.0 (and higher aromatic hydrocarbons 5.0 3 I Example 9. Production of aromatic compounds from methanol. Silicate 23 was tested as a catalyst for the preparation of arom For this purpose, methanol is passed over a fixed bed of this silicate under a pressure of 5 atm and a feed rate of 1 hour. Using 100 parts by weight of methanol as a raw material, 35 parts by weight of liquid, oxygen-free compounds are obtained. The average carbon number in the mixture is 8.7. The mixture contains 32 wt.% Cg and higher aromatics distributed in various compounds as follows, wt., C 0.1; С 2.9 П-СдЗ, 1; M-Cg 2.4; 0-Cg 4.0; C 12.5 C, about 7.0. . Thus, the use of crystalline ferrosilicates in the processes of producing aromatic hydrocarbons of 6 ° C allows an increase in the yield of mathematic hydrocarbons. Claim i. A method for producing aromatic hydrocarbons by converting a feedstock at elevated temperature and pressure in the presence of a crystalline oxide catalyst, characterized in that, in order to increase the yield of the target product, compounds selected from the group containing isobutylene or methanol, or Ktexadekan, or a gas mixture of hydrogen and carbon monoxide, or a mixture of toluene and methanol, and the process is carried out at 350–400 ° C, at a pressure of 130 atm, using 313 as catalysis a crystalline silicate torus thermally stable at 600–1050 ° C, absorbing 6–8.2% (w / w%) of water at and a pressure of saturated water vapor and after dehydrating in vacuum at having a X-ray diffraction of reflexes, containing . 1. containing the following components, weight: 0.1-0.2 Oxides; 5.5-8.0 Oxides of iron; 1.7-2.2; Oxides of aluminum: 0.7-0.8; Water Rest Silicon or 0.15-0, go sodium
    21 936803.22
    Iron oxide 0.8-8.0, 02.08.77tv as a source syVoda O, 15-0, / Or, use a gas mixture vordord
    Silicon oxide rest is carbon monoxide.
    [2]
    2. The way POP.1, distinguish-Sources of information
    w u and with the fact that crystalline s taken into account in the examination
    Cue silicate contains chromium oxide I1. US Patent (G Ц086289,
    zinc oxide 260-671N, publ. 1978
    Priority signs: 2. Japanese Patent H SB-ltOSS,
    16.12.76-B as initial sy-cl. 16 C 1, published. 1978
    pb use isobutylene or meta-10
    [3]
    3. US patent No. tl 39550,
    NOL, or H-hexadecay, or a mixture of To-Cl. 26Q-kk3, publ. 1979 (proto
    lurla and methanol. type of).
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    公开号 | 公开日
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    申请号 | 申请日 | 专利标题
    NLAANVRAGE7613957,A|NL175162C|1976-12-16|1976-12-16|PROCESS FOR PREPARING CRYSTALLINE SILICATES AND USE OF THE OBTAINED SILICATES AS CATALYST OR CATALYST CARRIER.|
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