CN102964223A - Preparation method of propylene glycol monomethyl ether - Google Patents
Preparation method of propylene glycol monomethyl ether Download PDFInfo
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- CN102964223A CN102964223A CN2012104922606A CN201210492260A CN102964223A CN 102964223 A CN102964223 A CN 102964223A CN 2012104922606 A CN2012104922606 A CN 2012104922606A CN 201210492260 A CN201210492260 A CN 201210492260A CN 102964223 A CN102964223 A CN 102964223A
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- monomethyl ether
- glycol monomethyl
- propylene glycol
- preparation
- reaction
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Abstract
The invention relates to a method in the field of chemical synthesis, in particular to a preparation method of propylene glycol monomethyl ether, which comprises the steps of: heating epoxypropane and methanol in the presence of a catalyst, wherein the reaction temperature is 180-200 DEG C, the reaction pressure is 1-2MPa, the molar ratio of the epoxypropane to the methanol is 1:(2-3), the catalyst is kieselguhr embedded with ferric chloride; and then carrying out reduced pressure distillation, and separating to obtain the propylene glycol monomethyl ether. The kieselguhr embedded with the ferric chloride is selected as the catalyst, is good in catalysis effect; kieselguhr can enlarge the contact area of a reactant and the catalyst and can influence the catalyst direction of the ferric chloride, and the yield of the propylene glycol monomethyl ether is remarkably larger than that of 2-methoxy-propanol. Through controlling the reaction condition, the temperature is 180-200 DEG C, the reaction pressure is 1-2MPa, and the yield of the propylene glycol monomethyl ether reaches 98 percent.
Description
Technical field
The present invention relates to a kind of method of the field of chemical synthesis, the preparation method of the propylene glycol monomethyl ether that particularly a species specificity is high.
Background technology
Glycol ether is the widely used industrial solvent of a large class, because the eighties is found the toxicity problem of glycol ethers solvent, therefore, hypotoxic propylene glycol product was developed rapidly within the short more than ten years, more and more came into one's own.
The structural formula of propylene glycol monomethyl ether is:
The main fine solvent that is used as the resol of nitrocellulose, Synolac and cis-butenedioic anhydride modification is used as the additive of jet fuel antifreezing agent and brake fluid etc.; Main as solvent, dispersion agent and thinner, also as fuel antifreezing agent, extraction agent etc.
The synthetic principle of propylene glycol monomethyl ether is as follows:
If synthesis condition is not controlled, synthetic product is the mixture of propylene glycol monomethyl ether and 2-methoxyl group-propyl alcohol, and not only combined coefficient is low, and the separating difficulty of product is large, causes production cost large, is unfavorable for expanding the scale of production.
Summary of the invention
It is high that the technical problem to be solved in the present invention provides a kind of yield, the preparation method of the propylene glycol monomethyl ether that product purity is high.
Content of the present invention is to comprise the steps:
Propylene oxide and methyl alcohol are heated under the condition of catalyzer, and temperature of reaction is 180-200 ℃, and reaction pressure is 1-2MPa, the mol ratio of propylene oxide and methyl alcohol is 1: 2-3, described catalyzer are the diatomite that is inlaid with iron(ic) chloride, then underpressure distillation, separate, get propylene glycol monomethyl ether.
The weight of described iron(ic) chloride is the 0.5-2% of propylene oxide weight.
Reaction times is 20-100 minute.
Described temperature of reaction is 190 ℃.
Described reaction pressure is 1.5MPa.
The mol ratio of described propylene oxide and methyl alcohol is 1: 3.
The invention has the beneficial effects as follows, the present invention selects the diatomite that is inlaid with iron(ic) chloride as catalyzer, its catalytic effect is good, diatomite has not only strengthened the contact area of reagent and catalyzer, and diatomite is also influential to the catalysis direction of iron(ic) chloride, and the productive rate of the propylene glycol monomethyl ether of its product is obviously greater than 2-methoxyl group-propyl alcohol.By the control reaction conditions, so that temperature of reaction is 180-200 ℃, reaction pressure is 1-2MPa, and the productive rate of product propylene glycol monomethyl ether reaches 98%.
Embodiment
Embodiment 1
Content of the present invention is to comprise the steps:
Propylene oxide and methyl alcohol are heated under the condition of catalyzer, temperature of reaction is 190 ℃, reaction pressure is 1.5MPa, reaction times is 50 minutes, and the mol ratio of propylene oxide and methyl alcohol is 1: 3, and described catalyzer is the diatomite that is inlaid with iron(ic) chloride, the weight of described iron(ic) chloride is 2% of propylene oxide weight, then underpressure distillation separates, and gets propylene glycol monomethyl ether.
Described product propylene glycol monomethyl ether yield be 98.2%, purity is 99.1%.
Embodiment 2
Content of the present invention is to comprise the steps:
Propylene oxide and methyl alcohol are heated under the condition of catalyzer, temperature of reaction is 180 ℃, reaction pressure is 1MPa, reaction times is 20 minutes, and the mol ratio of propylene oxide and methyl alcohol is 1: 2, and described catalyzer is the diatomite that is inlaid with iron(ic) chloride, the weight of described iron(ic) chloride is 0.5% of propylene oxide weight, then underpressure distillation separates, and gets propylene glycol monomethyl ether.
Described product propylene glycol monomethyl ether yield be 97.4%, purity is 98.3%.
Embodiment 3
Content of the present invention is to comprise the steps:
Propylene oxide and methyl alcohol are heated under the condition of catalyzer, temperature of reaction is 200 ℃, reaction pressure is 2MPa, reaction times is 100 minutes, and the mol ratio of propylene oxide and methyl alcohol is 1: 2.5, and described catalyzer is the diatomite that is inlaid with iron(ic) chloride, the weight of described iron(ic) chloride is 1% of propylene oxide weight, then underpressure distillation separates, and gets propylene glycol monomethyl ether.
Described product propylene glycol monomethyl ether yield be 96.5%, purity is 98.1%.
Claims (6)
1. the preparation method of a propylene glycol monomethyl ether, it is characterized in that, propylene oxide and methyl alcohol are heated under the condition of catalyzer, temperature of reaction is 180-200 ℃, and reaction pressure is 1-2MPa, and the mol ratio of propylene oxide and methyl alcohol is 1: 2-3, described catalyzer is the diatomite that is inlaid with iron(ic) chloride, then underpressure distillation separates, and gets propylene glycol monomethyl ether.
2. the preparation method of propylene glycol monomethyl ether according to claim 1 is characterized in that, the weight of described iron(ic) chloride is the 0.5-2% of propylene oxide weight.
3. the preparation method of propylene glycol monomethyl ether according to claim 1 is characterized in that, the reaction times is 20-100 minute.
4. the preparation method of propylene glycol monomethyl ether according to claim 1 is characterized in that, described temperature of reaction is 190 ℃.
5. the preparation method of propylene glycol monomethyl ether according to claim 1 is characterized in that, described reaction pressure is 1.5MPa.
6. the preparation method of propylene glycol monomethyl ether according to claim 1 is characterized in that, the mol ratio of described propylene oxide and methyl alcohol is 1: 3.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012104922606A CN102964223A (en) | 2012-11-13 | 2012-11-13 | Preparation method of propylene glycol monomethyl ether |
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| Application Number | Priority Date | Filing Date | Title |
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| CN2012104922606A CN102964223A (en) | 2012-11-13 | 2012-11-13 | Preparation method of propylene glycol monomethyl ether |
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| CN102964223A true CN102964223A (en) | 2013-03-13 |
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| CN2012104922606A Pending CN102964223A (en) | 2012-11-13 | 2012-11-13 | Preparation method of propylene glycol monomethyl ether |
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Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN85104661A (en) * | 1985-06-14 | 1987-07-08 | 南开大学 | A kind of solid acid catalyst that can be used for producing gylcol ether |
| CN1362396A (en) * | 2001-01-05 | 2002-08-07 | 中国石油化工股份有限公司 | Synthesis of propylene glycol ether and the catalyst applied |
| JP2002338511A (en) * | 2001-05-16 | 2002-11-27 | Kyowa Yuka Co Ltd | Distillation apparatus for propylene glycol monoalkyl ether and method for distilling the same |
| CN1764622A (en) * | 2003-04-16 | 2006-04-26 | 高砂香料工业株式会社 | Process for producing 2-(l-menthoxy)ethanol compound |
| CN100999448A (en) * | 2007-01-05 | 2007-07-18 | 华东师范大学 | Synthesis method of propylene glycol ether |
| CN101190878A (en) * | 2006-11-21 | 2008-06-04 | 中国石油化工股份有限公司 | Method for preparing propylene glycol ether |
| CN101550069A (en) * | 2009-05-25 | 2009-10-07 | 哈尔滨师范大学 | Method for synthesizing propylene glycol methyl ether |
| WO2010099300A1 (en) * | 2009-02-26 | 2010-09-02 | Dow Global Technologies Inc. | Alkoxylation processes and catalysts therefor |
-
2012
- 2012-11-13 CN CN2012104922606A patent/CN102964223A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN85104661A (en) * | 1985-06-14 | 1987-07-08 | 南开大学 | A kind of solid acid catalyst that can be used for producing gylcol ether |
| CN1362396A (en) * | 2001-01-05 | 2002-08-07 | 中国石油化工股份有限公司 | Synthesis of propylene glycol ether and the catalyst applied |
| JP2002338511A (en) * | 2001-05-16 | 2002-11-27 | Kyowa Yuka Co Ltd | Distillation apparatus for propylene glycol monoalkyl ether and method for distilling the same |
| CN1764622A (en) * | 2003-04-16 | 2006-04-26 | 高砂香料工业株式会社 | Process for producing 2-(l-menthoxy)ethanol compound |
| CN101190878A (en) * | 2006-11-21 | 2008-06-04 | 中国石油化工股份有限公司 | Method for preparing propylene glycol ether |
| CN100999448A (en) * | 2007-01-05 | 2007-07-18 | 华东师范大学 | Synthesis method of propylene glycol ether |
| WO2010099300A1 (en) * | 2009-02-26 | 2010-09-02 | Dow Global Technologies Inc. | Alkoxylation processes and catalysts therefor |
| CN101550069A (en) * | 2009-05-25 | 2009-10-07 | 哈尔滨师范大学 | Method for synthesizing propylene glycol methyl ether |
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Application publication date: 20130313 |