CN1180589A - Catalyzer for preparing propylene-glycol ether acetate - Google Patents
Catalyzer for preparing propylene-glycol ether acetate Download PDFInfo
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- CN1180589A CN1180589A CN 96116545 CN96116545A CN1180589A CN 1180589 A CN1180589 A CN 1180589A CN 96116545 CN96116545 CN 96116545 CN 96116545 A CN96116545 A CN 96116545A CN 1180589 A CN1180589 A CN 1180589A
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- catalyzer
- ether acetate
- glycol ether
- propylene
- karb
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)
Abstract
A catalyst for preparing propanediol ether acetate is AlCl3 carried by cationic exchange resin with the Al content of 0.5-2.0 Wt.%, and features high activity, low reaction temp and less corrosion.
Description
The present invention relates to be used to prepare the catalyzer of propylene-glycol ether acetate, particularly about being used to prepare the cation exchange resin catalyst of propylene-glycol ether acetate.
Propylene-glycol ether acetate is a kind of low toxicity advanced industrial solvent of excellent property.Because its toxicity is low, solubility property is good, development abroad is very fast in recent years, is progressively substituting to be extensive use of at present but the higher glycol ether acetic ester of toxicity.It can be widely used in industries such as coating, printing, Shan China ink, clean-out system, textile dyestuff and leather retanning agent.Made the used catalyzer of propylene-glycol ether acetate in the past H was arranged
2SO
4, HNO
3, HCl, BF
3Deng Lewis acid, react with homogeneous phase.The advantage that aforesaid method has is with low cost, reactive behavior is high, but side reaction is serious, corrodibility is high.Introduced load AlCl on ion exchange resin on the 17th～19 page of document " Speciality Petrochemicals " 1993 1 phase
3The solid super acid catalyst technology, but the document does not have to disclose the effect what reaction this solid super acid catalyst can be used for and can reach.
The purpose of this invention is to provide a kind of catalyzer that is used to prepare propylene-glycol ether acetate, it is good that this catalyzer has reactive behavior, and temperature of reaction is low, the characteristics that corrodibility is little.
The objective of the invention is to realize by following technical scheme: a kind of catalyzer that is used to prepare propylene-glycol ether acetate, on Zeo-karb load aluminum chloride, by weight percentage, aluminium content is 0.5～2.0%.
Zeo-karb is Phenylsulfonic acid resin, p-methyl benzenesulfonic acid resin, dry hydrogen resin in the technique scheme.The aluminum chloride amount of load on the Zeo-karb, by weight percentage, aluminium content preferable range is 1.0～1.5%.
Catalyzer of the present invention is to prepare by following method: Zeo-karb is dropped in the there-necked flask, slowly add the aluminum chloride ethanolic soln, be heated to 78 ℃ of boilings, naturally cool to room temperature after 5 hours, add deionized water and fully stir, make unnecessary aluminum chloride hydrolysis, take out and filter, use washing with acetone, be washed till no chlorion with deionized water again, vacuum-drying, the cation exchange resin catalyst of load aluminum chloride.
The present invention is the load aluminum chloride on Zeo-karb, and essence is that aluminum chloride has been sloughed a hydrogenchloride between two sulfonic groups of two resins, thereby has formed a strong proton donor, has become a kind of solid super-strong acid.When therefore being used to prepare propylene-glycol ether acetate, had very high activity, can under lower temperature, react simultaneously, adapt to resin and be difficult for resistant to elevated temperatures characteristics, in addition because the aluminium atom of aluminum chloride is a form with complexing exists, therefore make the corrodibility of this catalyzer very little, increased the strength of acid of Zeo-karb on the contrary, obtained effect preferably.
Further specify below by embodiment.[embodiment 1]
Get load 20 milliliters of the dry hydrogen resins of aluminum chloride in tubular microreactors, the aluminium content of load aluminum chloride is 1.5% by weight percentage in the dry hydrogen resin.Feed the mixture of raw material propylene glycol monomethyl ether and acetic acid in this reactor, wherein propylene glycol monomethyl ether: acetic acid is 1: 3 (moles/mole), reacts under normal pressure, 115 ℃ of conditions of temperature, and the liquid air speed is 5 hours
-1After reaction finishes, with chromatography the reaction solution composition is analyzed, its result is 67.7% for the transformation efficiency of propylene glycol monomethyl ether, and the selectivity of 1-Methoxy-2-propyl acetate is 98.0%.[comparative example 1]
20 milliliters of dry hydrogen resins getting load aluminum chloride not are in tubular microreactors, in this reactor, feed raw material: the mixture of propylene glycol monomethyl ether and acetic acid, propylene glycol monomethyl ether wherein: acetic acid is 1: 3 (moles/mole), reacts under normal pressure, 115 ℃ of conditions of temperature, and the liquid air speed is 5 hours
-1After reaction finishes, with chromatogram the reaction solution composition is analyzed, its result is 66.8% for the transformation efficiency of propylene glycol monomethyl ether, and the selectivity of 1-Methoxy-2-propyl acetate is 95.0%.[embodiment 2]
Get load 20 milliliters of the Phenylsulfonic acid resins of aluminum chloride in tubular microreactors, the aluminium content of load in the Phenylsulfonic acid resin is 0.5% by weight percentage.Other condition is with embodiment 1, and the result is 67.0% for the transformation efficiency of propylene glycol monomethyl ether, and the selectivity of propylene-glycol ether acetate is 97.0%.[embodiment 3]
Get load 20 milliliters of the p-methyl benzenesulfonic acid resins of aluminum chloride in tubular microreactors, the aluminium content of load in the p-methyl benzenesulfonic acid resin is 1% by weight percentage.Other condition is with embodiment 1, and the result is 67.9% for the transformation efficiency of propylene glycol monomethyl ether, and the selectivity of 1-Methoxy-2-propyl acetate is 98.2%.
Claims (5)
1, a kind of catalyzer that is used to prepare propylene-glycol ether acetate, the aluminum chloride that it is characterized in that on Zeo-karb load, by weight percentage, aluminium content is 0.5～2.0%.
2,, it is characterized in that Zeo-karb is the Phenylsulfonic acid resin according to the catalyzer of the described preparation propylene-glycol ether acetate of claim 1.
3,, it is characterized in that Zeo-karb is the p-methyl benzenesulfonic acid resin according to the catalyzer of the described preparation propylene-glycol ether acetate of claim 1.
4,, it is characterized in that Zeo-karb is the dry hydrogen resin according to the catalyzer of the described preparation propylene-glycol ether acetate of claim 1.
5, according to the catalyzer of the described preparation propylene-glycol ether acetate of claim 1, it is characterized in that the aluminum chloride amount of load on the Zeo-karb, by weight percentage, aluminium content is 1.0～1.5%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN96116545A CN1074314C (en) | 1996-10-22 | 1996-10-22 | Catalyzer for preparing propylene-glycol ether acetate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN96116545A CN1074314C (en) | 1996-10-22 | 1996-10-22 | Catalyzer for preparing propylene-glycol ether acetate |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1180589A true CN1180589A (en) | 1998-05-06 |
| CN1074314C CN1074314C (en) | 2001-11-07 |
Family
ID=5123644
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN96116545A Expired - Fee Related CN1074314C (en) | 1996-10-22 | 1996-10-22 | Catalyzer for preparing propylene-glycol ether acetate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1074314C (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101337885B (en) * | 2008-08-08 | 2011-07-20 | 德纳（南京）化工有限公司 | Method for preparing 1-Methoxy-2-propyl acetate by continuous esterification reaction |
| CN103008014A (en) * | 2013-01-08 | 2013-04-03 | 哈尔滨工业大学 | Preparation method of catalyst and method for preparing 190# solvent oil by use of catalyst |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6099073A (en) * | 1983-11-02 | 1985-06-01 | 帝人株式会社 | Treatment of polyester fiber |
| FR2585812B1 (en) * | 1985-07-30 | 1987-10-23 | Jeumont Schneider | THERMAL MACHINE WITH ADSORPTION-DESORPTION |
| CN1052848A (en) * | 1989-04-10 | 1991-07-10 | 齐鲁石油化工公司研究院 | The manufacture method of methyl methacrylate (MMA) |
| CN1053598C (en) * | 1994-05-16 | 2000-06-21 | 北京化工大学 | Zirconium oxide catalyst used in glycol series monoether acetate synthesis |
-
1996
- 1996-10-22 CN CN96116545A patent/CN1074314C/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101337885B (en) * | 2008-08-08 | 2011-07-20 | 德纳（南京）化工有限公司 | Method for preparing 1-Methoxy-2-propyl acetate by continuous esterification reaction |
| CN103008014A (en) * | 2013-01-08 | 2013-04-03 | 哈尔滨工业大学 | Preparation method of catalyst and method for preparing 190# solvent oil by use of catalyst |
| CN103008014B (en) * | 2013-01-08 | 2014-08-27 | 哈尔滨工业大学 | Preparation method of catalyst and method for preparing 190# solvent oil by use of catalyst |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1074314C (en) | 2001-11-07 |
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