CN1142018C - Catalyst carrying potassium oxide - Google Patents
Catalyst carrying potassium oxide Download PDFInfo
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- CN1142018C CN1142018C CNB00117794XA CN00117794A CN1142018C CN 1142018 C CN1142018 C CN 1142018C CN B00117794X A CNB00117794X A CN B00117794XA CN 00117794 A CN00117794 A CN 00117794A CN 1142018 C CN1142018 C CN 1142018C
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- catalyst
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- carrier
- water solution
- molecular sieve
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Abstract
The present invention relates to a catalyst carrying potassium fluoride, which is composed of 5 to 20% of potassium fluoride and 80 to 95% of metal oxide, zeolite molecular sieve 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 KF water solution according to the composition of the catalyst, the carrier and the water solution are pumped to be a vacuum state and are statically placed for 12 hours, and the catalyst is obtained after the carrier and the water solution are dried at 120 DEG C and are accelerated and activated for 4 hours at 600 DEG C. The catalyst of the present invention has the characteristics of simple and facile preparation processes, higher activity and selectivity and repeated use; furthermore, the catalyst can be separated by filtration after the reaction is completed.
Description
The invention belongs to from the solid catalyst of methyl alcohol and propene carbonate Synthesis of dimethyl carbonate.
As a kind of eco-friendly organic synthesis intermediate and gasoline additive, dimethyl carbonate (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 propene carbonate and methyl alcohol through ester exchange, because process is simple, and can generate dihydroxylic alcohols, thereby is competitive method (A.G.Shaikh, S.Sivaram, Chem.Rev., 1996,96,951).
Propene carbonate (being called for short PC) is as follows with the methyl alcohol reaction equation:
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 catalyst.Though above-mentioned catalyst has catalytic activity preferably,, cause difficulty for the separation and the repeated use of catalyst because of it is a homogeneous reaction.
The purpose of this invention is to provide a kind of catalyst from methyl alcohol and propene carbonate Synthesis of dimethyl carbonate, this catalyst is easy to separate from product.
Goal of the invention of the present invention is achieved in that and adopts KF to be impregnated on metal oxide, zeolite molecular sieve, the active carbon that the percentage by weight of its catalyst consists of:
Potassium fluoride 5-20%
Metal oxide, zeolite molecular sieve or active carbon 80-95%.
Aforesaid metal oxide is aluminium oxide, zinc oxide, zirconia, calcium oxide, magnesia.
Aforesaid zeolite molecular sieve mol ratio consists of:
SiO
2∶Al
2O
3＝(2-50)∶1。
Aforesaid zeolite molecular sieve is preferably A, X, L, ZSM-5 type.
Aforesaid zeolite molecular sieve is Na, K type.
The specific area of aforesaid active carbon is a 700-1000 rice
2/ gram, particle diameter is less than 80 orders.
Preparation method of the present invention adopts infusion process, with catalyst carrier 400 ℃ of following roastings 2 hours, then by the composition of above-mentioned catalyst with carrier impregnation in the aqueous solution of KF, vacuumize, left standstill 12 hours, and, obtained catalyst in 4 hours at 600 ℃ of following calcination activations through 120 ℃ of dryings.
Aforesaid catalyst and other catalyst compare, and it is simple to have preparation process, and required reagent and carrier are easy to get, and this catalyst has higher activity and selectivity.After should finishing, reactant liquor is handled simple, and catalyst can obtain 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 KF then with calcium oxide, and calcium oxide is that 90% composition (percentage by weight) is impregnated into calcium oxide in the aqueous solution of KF, vacuumize, left standstill 12 hours, and, obtained catalyst in 4 hours at 600 ℃ of following calcination activations through 120 ℃ of dryings.Add methyl alcohol and propene carbonate by certain mole proportioning in reaction vessel, the addition of catalyst is 4% of a reactant mixture weight, under stirring condition, is warming up to 120 ℃ of reaction temperatures, 2 hours reaction time.Cooling is filtered, and catalyst is separated with reactant liquor, the reactant liquor gas chromatographic analysis, and the productive rate of DMC is 30.5%, the conversion ratio of PC is 33.8%.
Embodiment 2
400 ℃ of following roastings 2 hours, is 20% by KF then with zinc oxide, and zinc oxide is 80% composition, makes catalyst, and all the other are with embodiment 1, the reactant liquor gas chromatographic analysis, and the productive rate of DMC is 24.1%, the conversion ratio of PC is 29.5%.
Embodiment 3
400 ℃ of following roastings 2 hours, is 15% by KF then with 4A type molecular sieve, and 4A type molecular sieve is that 85% composition makes catalyst, and all the other are with embodiment 1.Reactant liquor gas chromatographic analysis, the productive rate of DMC are 38.6%, and the conversion ratio of PC is 39.5%.
Embodiment 4
400 ℃ of following roastings 2 hours, is 16% by KF then with zirconia, and zinc oxide is 84% composition, makes catalyst, and all the other are with embodiment 1.Reactant liquor gas chromatographic analysis, the productive rate of DMC are 32.4%, and the conversion ratio of PC is 37.4%.
Embodiment 5
400 ℃ of following roastings 2 hours, is 7% by KF then with NaX type molecular sieve, and NaX type molecular sieve is 93% composition, makes catalyst, and all the other are with embodiment 1.Reactant liquor gas chromatographic analysis, the productive rate of DMC are 31.1%, and the conversion ratio of PC is 32.3%.
Embodiment 6
400 ℃ of following roastings 2 hours, is 20% by KF then with active carbon, and active carbon is 80% composition, makes catalyst, and all the other are with embodiment 1.Reactant liquor gas chromatographic analysis, the productive rate of DMC are 31.5%, and the conversion ratio of PC is 36.4%.
Embodiment 7
400 ℃ of following roastings 2 hours, is 18% by KF then with aluminium oxide, and aluminium oxide is 82% composition, makes catalyst, and all the other are with embodiment 1.Reactant liquor gas chromatographic analysis, the productive rate of DMC are 35.2%, and the conversion ratio of PC is 38.4%.
Claims (2)
1. the catalyst of a carrying potassium oxide is characterized in that the percentage by weight of catalyst consists of:
Potassium fluoride 5-20%
Calcium oxide, magnesia or active carbon 80-95%
2. the catalyst of a kind of carrying potassium oxide according to claim 1, the specific area that it is characterized in that described active carbon is a 700-1000 rice
2/ gram, particle diameter is less than 80 orders.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB00117794XA CN1142018C (en) | 2000-06-21 | 2000-06-21 | Catalyst carrying potassium oxide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB00117794XA CN1142018C (en) | 2000-06-21 | 2000-06-21 | Catalyst carrying potassium oxide |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1304797A CN1304797A (en) | 2001-07-25 |
| CN1142018C true CN1142018C (en) | 2004-03-17 |
Family
ID=4587047
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB00117794XA Expired - Fee Related CN1142018C (en) | 2000-06-21 | 2000-06-21 | Catalyst carrying potassium oxide |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1142018C (en) |
Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100379492C (en) * | 2005-01-10 | 2008-04-09 | 顾明兰 | Super alkali composite catalyst for preparing superfine KF/Al2O3 using Sol-gel method |
| CN101773822A (en) * | 2009-01-14 | 2010-07-14 | 中国科学院大连化学物理研究所 | Catalyst used in preparation of propylene epoxide by utilizing 1,2-propylene glycol gas dehydration and application |
| CN101822992B (en) * | 2010-05-26 | 2012-02-29 | 华中科技大学 | Catalyst for synthesis of glycerol carbonate and preparation method thereof |
| CN102527427A (en) * | 2012-01-06 | 2012-07-04 | 厦门大学 | Modified molecular sieve catalyst for preparing propylene by methinehalide and preparation method of modified molecular sieve catalyst |
| CN109593076A (en) * | 2018-12-05 | 2019-04-09 | 常熟市常吉化工有限公司 | A kind of application of KF/NaY catalyst in synthesizing ethylene carbonate |
| CN109821560B (en) * | 2019-01-25 | 2022-04-22 | 中国科学院成都有机化学有限公司 | Catalyst for synthesizing dimethyl carbonate by ester exchange and application thereof |
| CN110003458A (en) * | 2019-04-29 | 2019-07-12 | 中国科学院成都有机化学有限公司 | A kind of load type solid body base catalyst and its application |
-
2000
- 2000-06-21 CN CNB00117794XA patent/CN1142018C/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| CN1304797A (en) | 2001-07-25 |
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