Method for synthesizing 2,2-dimethoxypropane

A technology of dimethoxypropane and a synthesis method, which is applied in 2 fields, can solve the problems of complex process, reduced yield, strong corrosion of equipment, etc., and achieves the effects of simple equipment requirements, easy scale and environmental friendliness

Inactive Publication Date: 2008-04-09
ZHEJIANG SCI-TECH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The traditional synthesis methods of DMP include direct synthesis method and indirect synthesis method of acetone and methanol. The above two methods are complex in process, relatively large in equipment investment, long in reaction time, low in yield, azeotropic in methanol and product, and difficult to separate and purify the product. .The traditional catalysts for DMP synthesis reaction are sulfuric acid, hydrochloric acid, etc., but due to strong corrosion, serious environmental pollution and other reasons, its application has been limited
In 2001, Yang Shumin et al. reported the synthesis of DMP with acetone and trimethyl orthoformate under the action of solid acid, but the application of the solid acid was limited due to the cumbersome preparation of solid acid, strong corrosion to equipment, and high cost.
Our experiments and data show that acetone and trimethyl orthoformate are an equilibrium reaction. In a relatively closed system, even if the amount of acetone is 10 times excessive, the conversion rate of trimethyl orthoformate is only about 70%. Under the temperature of the post-reaction treatment stated, the product DMP will decompose and produce many by-products, which also greatly reduces the yield, and it is difficult to reach the yield in the literature

Method used

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  • Method for synthesizing 2,2-dimethoxypropane

Examples

Experimental program
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Effect test

Embodiment 1

[0018] Take a reactor with a rectification device, add 20g of p-toluenesulfonic acid catalyst and 500mL of acetone in the reactor, start stirring, add 825mL of trimethyl orthoformate dropwise, control the temperature at 30-40°C, and collect methyl formate at the top of the tower , reacted for 3 to 4 hours, after the reaction solution was neutralized by adding sodium carbonate, rectification under reduced pressure (30mmHg), keep the temperature in the reactor at 30 to 35°C, circulate the refrigerated medium to cool the fraction, collect DMP, the product content > 95%, Yield 85~92%.

Embodiment 2

[0020] Take a reactor with a rectification device, add 30g of catalyst potassium bisulfite and 700mL of acetone into the reactor, start stirring, add 120mL of trimethyl orthoformate dropwise, control the temperature of the reactor at 10-15°C, and control the pressure (50mmHg ), cooling and collecting methyl formate by circulating refrigeration medium at the top of the tower, reacting for 7 to 8 hours, filtering out the catalyst, adding sodium carbonate to the filtrate to neutralize, rectifying under reduced pressure (25mHg), keeping the temperature in the reactor at 25 to 30°C, and circulating Refrigeration medium cools the distillate, collects the medium boiler and the product DMP, the medium boiler can be applied mechanically, the product DMP content is > 95%, and the yield is 85-90%.

Embodiment 3

[0022] Take the same device as in Example 1, and the same operation, add 1000 mL of trimethyl orthoformate dropwise to 15 g of catalyst ammonium chloride and 75 mL of acetone, control the temperature of the reactor at 30 to 40 ° C, collect methyl formate at the top of the tower, and react After 3-4 hours, filter the catalyst, neutralize the filtrate with sodium carbonate, rectify under reduced pressure (40mmHg), keep the temperature in the reactor at 35-40°C, cool with circulating refrigeration medium, collect the product DMP, and recycle the substrate. Product DMP content > 95%, yield 85-92%

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Abstract

The invention discloses a method of synthesizing a 2, 2-dimethyoxypropane. Under the effect of catalyst, acetone and trimethyl orthofomate are synthesized through reactive distillation; and the invention has the feeding mol ratio that the proportion between the acetone and the trimethyl orthofomate is 1:10 to 10:1. The reaction utilizes dynamics balance principle, and continuously transforms a product in reaction process by reaction distillation device, to lead the reaction to go along the direction of producing. The method, realizing high conversion, has the advantages of simple device and small corrosivity as well as being easy for large-scale producing and environment-friendly.

Description

technical field [0001] The invention relates to a method for synthesizing 2,2-dimethoxypropane. Background technique [0002] 2,2-dimethoxypropane (English name 2,2-dimethoxy propane, referred to as DMP), has a wide range of uses in the research and industrial production of fine chemical products such as medicine, pesticides, and natural products. Propylene, pseudoionone, ionone, isophytol, vitamin A, vitamin E and other key intermediates of pharmaceutical, chemical and feed products, can be used as cyclizing agent, condensation agent, dehydrating agent, protective agent and polymer catalyst composition etc. [0003] The traditional synthesis methods of DMP include direct synthesis method and indirect synthesis method of acetone and methanol. The above two methods are complex in process, relatively large in equipment investment, long in reaction time, low in yield, azeotropic in methanol and product, and difficult to separate and purify the product. . The traditional catal...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C43/303C07C41/50
CPCY02P20/10Y02P20/582
Inventor 朱锦桃王朝阳
Owner ZHEJIANG SCI-TECH UNIV
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