CN1095396C - Catalyst carrying inorganic potassium compound - Google Patents
Catalyst carrying inorganic potassium compound Download PDFInfo
- Publication number
- CN1095396C CN1095396C CN00118436A CN00118436A CN1095396C CN 1095396 C CN1095396 C CN 1095396C CN 00118436 A CN00118436 A CN 00118436A CN 00118436 A CN00118436 A CN 00118436A CN 1095396 C CN1095396 C CN 1095396C
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- CN
- China
- Prior art keywords
- inorganic potassium
- catalyst
- potassium compound
- catalyzer
- hours
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 150000003112 potassium compounds Chemical class 0.000 title claims abstract description 16
- 239000003054 catalyst Substances 0.000 title claims abstract description 12
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910044991 metal oxide Inorganic materials 0.000 claims abstract description 5
- 150000004706 metal oxides Chemical class 0.000 claims abstract description 5
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 15
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 8
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims description 8
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims description 5
- 239000000292 calcium oxide Substances 0.000 claims description 5
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 5
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical group O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 4
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Substances [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 4
- 239000004323 potassium nitrate Substances 0.000 claims description 4
- 235000010333 potassium nitrate Nutrition 0.000 claims description 4
- 239000011787 zinc oxide Substances 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 2
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims 1
- 229910000027 potassium carbonate Inorganic materials 0.000 claims 1
- 229910001928 zirconium oxide Inorganic materials 0.000 claims 1
- 238000006243 chemical reaction Methods 0.000 abstract description 13
- 239000000203 mixture Substances 0.000 abstract description 8
- 239000007864 aqueous solution Substances 0.000 abstract description 3
- 238000001914 filtration Methods 0.000 abstract description 3
- 238000002360 preparation method Methods 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract description 2
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 15
- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 description 10
- 239000000243 solution Substances 0.000 description 6
- 238000004587 chromatography analysis Methods 0.000 description 5
- RUOJZAUFBMNUDX-UHFFFAOYSA-N propylene carbonate Chemical compound CC1COC(=O)O1 RUOJZAUFBMNUDX-UHFFFAOYSA-N 0.000 description 5
- 230000009466 transformation Effects 0.000 description 5
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- 206010013786 Dry skin Diseases 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 235000015320 potassium carbonate Nutrition 0.000 description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 238000001994 activation Methods 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 150000008044 alkali metal hydroxides Chemical class 0.000 description 1
- 150000004703 alkoxides Chemical class 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 230000002860 competitive effect Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- CXHHBNMLPJOKQD-UHFFFAOYSA-M methyl carbonate Chemical compound COC([O-])=O CXHHBNMLPJOKQD-UHFFFAOYSA-M 0.000 description 1
- 238000005554 pickling Methods 0.000 description 1
- 235000011118 potassium hydroxide Nutrition 0.000 description 1
- 239000011541 reaction mixture Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000011949 solid catalyst Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
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- Catalysts (AREA)
Abstract
一种负载无机钾化合物的催化剂，其重量百分比组成为10-20%的无机钾化合物和80-90%金属氧化物或活性炭。将催化剂载体在400℃下焙烧2小时，然后按催化剂的组成将载体浸渍到无机钾化合物的水溶液中，抽真空，静置24小时，经120℃干燥，在550℃下焙烧4小时得到催化剂。本发明的催化剂具有制备简单、用量少、无污染、活性与选择性较高、反应结束后催化剂通过过滤得到分离、且具有可重复使用的特点。A catalyst supporting inorganic potassium compounds, the composition of which is 10-20% by weight of inorganic potassium compounds and 80-90% of metal oxides or activated carbon. Calcinate the catalyst carrier at 400°C for 2 hours, then impregnate the carrier into an aqueous solution of inorganic potassium compound according to the composition of the catalyst, vacuumize it, let it stand for 24 hours, dry it at 120°C, and bake it at 550°C for 4 hours to obtain the catalyst. The catalyst of the invention has the characteristics of simple preparation, less consumption, no pollution, high activity and selectivity, the catalyst can be separated by filtration after the reaction, and has the characteristics of reusability.
Description
The invention belongs to a kind of solid catalyst of the carrying inorganic potassium compound from methyl alcohol and propylene carbonate Synthesis of dimethyl carbonate.
As a kind of eco-friendly organic synthesis intermediate and gasoline dope, methylcarbonate (Dimethyl Carbonate is called for short DMC) synthetic be subjected in recent years paying attention to widely with using (Y.Ono., Appl.Catal.A:, 1997,155,133).Synthesizing DMC from propylene carbonate and methyl alcohol through transesterify, because process is simple, and can generate dibasic alcohol, thereby is competitive method (A.G.Shaikh, S.Sivaram, Chem.Rev., 1996,96,951).
Propylene carbonate (being called for short PC) is as follows with the methyl alcohol reaction formula:
In this reaction, much more general with (Jiang Qi etc., gas chemical industry, 1997,22 (5), 1) such as alkali metal hydroxide, carbonate, alkoxide as catalyzer.But, cause difficulty for the separation and the repeated use of catalyzer because of this reaction is a homogeneous reaction.
The purpose of this invention is to provide a kind of catalyzer from methyl alcohol and propylene carbonate Synthesis of dimethyl carbonate, this catalyzer is easy to separate from product.
Goal of the invention of the present invention be achieved in that adopt inorganic potassium compound be impregnated into burning, on the activated carbon, the weight percent of its catalyzer consists of:
Inorganic potassium compound 10-20%
Metal oxide or gac 80-90%
Aforesaid inorganic potassium compound is potassium hydroxide, saltpetre or salt of wormwood.
Aforesaid metal oxide is aluminum oxide, zinc oxide, zirconium white or calcium oxide.The specific surface area of aforesaid gac is a 700-1000 rice
2/ gram, particle diameter is less than 80 orders.
Preparation method of the present invention adopts pickling process, with support of the catalyst 400 ℃ of following roastings 2 hours, then by the composition of above-mentioned catalyzer with carrier impregnation in the aqueous solution of inorganic potassium compound, vacuumize, left standstill 24 hours, and, obtained catalyzer in 4 hours 550 ℃ of following roastings through 120 ℃ of dryings.
Catalyzer of the present invention and other catalyzer relatively have preparation simply, and catalyst levels is few, environmentally safe, and have characteristics such as higher activity and selectivity.After reaction finished, catalyzer obtained separating by filtration, and it is reusable.
Embodiments of the invention are as follows:
Embodiment 1
400 ℃ of following roastings 2 hours, is 10% by potassium hydroxide then with calcium oxide, and calcium oxide is that 90% composition (weight percent) is impregnated into calcium oxide in the aqueous solution of potassium hydroxide, vacuumize, left standstill 24 hours, and, obtained catalyzer in 4 hours at 550 ℃ of following calcination activations through 120 ℃ of dryings.Add methyl alcohol and propylene carbonate by certain mole proportioning in reaction vessel, the add-on of catalyzer is 4% of a reaction mixture weight, under agitation condition, is warming up to 120 ℃, 2 hours reaction times.Cooling, filtration make catalyzer separate with reaction solution, the reaction solution gas chromatographic analysis, and the productive rate of DMC is 29.6%, the transformation efficiency of PC is 33.7%.
Embodiment 2
400 ℃ of following roastings 2 hours, is 10% by salt of wormwood then with zinc oxide, and zinc oxide is 90% composition, makes catalyzer, and all the other are with embodiment 1, the reaction solution gas chromatographic analysis, and the productive rate of DMC is 39.2%, the transformation efficiency of PC is 43.4%.
Embodiment 3
400 ℃ of following roastings 2 hours, is 18% by saltpetre then with aluminum oxide, and aluminum oxide is 82% composition, makes catalyzer, and all the other are with embodiment 1, the reaction solution gas chromatographic analysis, and the productive rate of DMC is that the transformation efficiency of 32.6%PC is 37.5%.
Embodiment 4
400 ℃ of following roastings 2 hours, is 16% by potassium hydroxide then with zirconium white, and zirconium white is 84% composition, makes catalyzer, and all the other are with embodiment 1.Reaction solution gas chromatographic analysis, the productive rate of DMC are 36.4%, and the transformation efficiency of PC is 40.1%.
Embodiment 5
400 ℃ of following roastings 2 hours, is 20% by saltpetre then with gac, and gac is 80% composition, makes catalyzer, and all the other are with embodiment 1, the reaction solution gas chromatographic analysis, and the productive rate of DMC is 39.9%, the transformation efficiency of PC is 43.7%.
Claims (4)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN00118436A CN1095396C (en) | 2000-06-21 | 2000-06-21 | Catalyst carrying inorganic potassium compound |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN00118436A CN1095396C (en) | 2000-06-21 | 2000-06-21 | Catalyst carrying inorganic potassium compound |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1304791A CN1304791A (en) | 2001-07-25 |
| CN1095396C true CN1095396C (en) | 2002-12-04 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN00118436A Expired - Fee Related CN1095396C (en) | 2000-06-21 | 2000-06-21 | Catalyst carrying inorganic potassium compound |
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| CN (1) | CN1095396C (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103664620B (en) * | 2012-09-03 | 2015-09-16 | 中国石油化工股份有限公司 | The preparation method of a kind of bis--terephthalate |
| CN104248944B (en) * | 2013-06-27 | 2016-09-28 | 中国石油化工股份有限公司 | For adsorbing cleanser of volatile oxidn and preparation method thereof in MTP tail gas |
| CN103752270B (en) * | 2014-01-24 | 2015-08-05 | 上海方纶新材料科技有限公司 | For the special-purpose activated charcoal that chlorine is separated with Oxygen Adsorption |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6157361A (en) * | 1984-07-27 | 1986-03-24 | Fujitsu Ltd | Impact type dot printer platen |
| JPH049356A (en) * | 1990-04-27 | 1992-01-14 | Asahi Chem Ind Co Ltd | Production of dialkyl carbonate |
| CN1103862A (en) * | 1993-07-15 | 1995-06-21 | 拜尔公司 | Process for the preparation of dimethyl carbonate |
| CN1228358A (en) * | 1998-03-06 | 1999-09-15 | 中国科学院山西煤炭化学研究所 | Catalyst for synthetising dimethyl carbonate from methanol and propylidene carbonate |
| CN1242356A (en) * | 1998-07-20 | 2000-01-26 | 中国科学院山西煤炭化学研究所 | Method for producing dimethyl carbonate by direct synthesizing carbon dioxide and methanol |
-
2000
- 2000-06-21 CN CN00118436A patent/CN1095396C/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6157361A (en) * | 1984-07-27 | 1986-03-24 | Fujitsu Ltd | Impact type dot printer platen |
| JPH049356A (en) * | 1990-04-27 | 1992-01-14 | Asahi Chem Ind Co Ltd | Production of dialkyl carbonate |
| CN1103862A (en) * | 1993-07-15 | 1995-06-21 | 拜尔公司 | Process for the preparation of dimethyl carbonate |
| CN1228358A (en) * | 1998-03-06 | 1999-09-15 | 中国科学院山西煤炭化学研究所 | Catalyst for synthetising dimethyl carbonate from methanol and propylidene carbonate |
| CN1242356A (en) * | 1998-07-20 | 2000-01-26 | 中国科学院山西煤炭化学研究所 | Method for producing dimethyl carbonate by direct synthesizing carbon dioxide and methanol |
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| Publication number | Publication date |
|---|---|
| CN1304791A (en) | 2001-07-25 |
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