CN1095396C - Catalyst carrying inorganic potassium compound - Google Patents

Catalyst carrying inorganic potassium compound Download PDF

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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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potassium compound
inorganic potassium
catalyzer
catalyst
hours
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CN00118436A
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CN1304791A (en
Inventor
韩怡卓
常雁红
杨彩虹
李文彬
王心葵
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Shanxi Institute of Coal Chemistry of CAS
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Shanxi Institute of Coal Chemistry of CAS
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Abstract

The present invention relates to a catalyst carrying an inorganic potassium compound, which is composed of 10 to 20% of inorganic potassium compound and 80 to 90% of metal oxide or activated carbon in weight percentage. A catalyst carrier is accelerated for 2 hours at the temperature of 400 DEG C, then the carrier is immersed in a water solution of the inorganic potassium compound according to the composition of the catalyst, the carrier and the water solution are pumped to be a vacuum state and statically placed for 24 hours, and the catalyst is obtained after the carrier and the water solution are dried at the temperature of 120 DEG C and are accelerated for 4 hours at the temperature of 550 DEG C. The catalyst of the present invention has the characteristics of simple preparation, less dosage, no pollution, higher activity and selectivity and repeated use; furthermore, the catalyst can be separated by filtration after the reaction is completed.

Description

A kind of catalyzer of carrying inorganic potassium compound
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:
Figure C0011843600031
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)

1. the catalyzer of a carrying inorganic potassium compound is characterized in that the weight percent of catalyzer consists of:
Inorganic potassium compound 10-20%
Metal oxide or gac 80-90%.
2. the catalyzer of a kind of carrying inorganic potassium compound according to claim 1 is characterized in that described inorganic potassium compound is potassium hydroxide, saltpetre or salt of wormwood.
3. the catalyzer of a kind of carrying inorganic potassium compound according to claim 1 is characterized in that described metal oxide is aluminum oxide, zinc oxide, zirconium white or calcium oxide.
4. the catalyzer of a kind of carrying inorganic potassium compound according to claim 1, the specific surface area that it is characterized in that described gac is a 700-1000 rice 2/ gram, particle diameter is less than 80 orders.
CN00118436A 2000-06-21 2000-06-21 Catalyst carrying inorganic potassium compound Expired - Fee Related CN1095396C (en)

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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)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS6157361A (en) * 1984-07-27 1986-03-24 Fujitsu Ltd Platen for impact type dot printer
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

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS6157361A (en) * 1984-07-27 1986-03-24 Fujitsu Ltd Platen for impact type dot printer
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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