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Catalytic synthesis method of n-butyl glycolate

A technology of n-butyl hydroxyacetate and a synthesis method is applied in chemical instruments and methods, preparation of carboxylate, preparation of organic compounds, etc., can solve problems such as difficulty in washing out hydrogen ions, achieve improved yield and selectivity, Improved selectivity and low equipment requirements

Active Publication Date: 2017-01-25
山东广浦生物科技有限公司
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  • Abstract
  • Description
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AI Technical Summary

Problems solved by technology

In this process, most of the hydrogen ions on the surface of the resin are easily washed away, but the hydrogen ions in the resin pores are difficult to be washed away

Method used

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Examples

Experimental program
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Effect test

preparation example Construction

[0024] Preparation of acidic ion exchange resin:

[0025] The configuration of the buffer solution refers to the conventional buffer solution configuration method, and a series of buffer solutions with a pH range from 1 to 6 are obtained. The following are the representatives of the buffer solution:

[0026] Buffer (pH2.0): phosphoric acid-disodium hydrogen phosphate buffer;

[0027] Buffer (pH2.2): disodium hydrogen phosphate-citric acid buffer;

[0028] Buffer (pH3.0): acetic acid-lithium hydroxide buffer;

[0029] Buffer (pH4.5): acetic acid-sodium acetate buffer;

[0030] Weigh 30 grams of acidic ion exchange resin, soak it completely in 150 grams of buffer solution, let it stand at room temperature for 24 hours, filter, wash with deionized water, and dry it in vacuum at 50°C to obtain buffer solution-treated acidic ion exchange resin. resin. The acidic ion exchange resins treated with different buffers are marked with the pH value of the buffer solution used.

Embodiment 1

[0032] Add 200 grams of glycolic acid (70%) successively in the 1L four-neck flask that is equipped with thermometer, condenser, water separator, 580 grams of n-butanols and 4 grams of pretreated acidic ion exchange resins (pH=2.0), heat up To 120°C, adjust the vacuum degree of the system to maintain a certain reflux in the system. Use a water separator to separate the water generated by the reaction. After tracking the amount of separated water to the theoretical amount, stop the reaction, cool down to room temperature, filter, and wash the acidic resin with a small amount of n-butanol. After recovering n-butanol from the filtrate under reduced pressure, it was distilled to obtain 216 grams of n-butyl glycolate with a purity of 99.2% and a yield of 89%.

Embodiment 2

[0034] Add 200 grams of glycolic acid (70%) successively in the 1L four-necked flask that is equipped with thermometer, condenser, water trap, 580 grams of n-butanols and 10 grams of pretreated acidic ion exchange resins (pH=2.0), heat up To 120°C, adjust the vacuum degree of the system to maintain a certain reflux in the system. Use a water separator to separate the water generated by the reaction. After tracking the amount of separated water to the theoretical amount, stop the reaction, cool down to room temperature, filter, and wash the acidic resin with a small amount of n-butanol. After recovering n-butanol from the filtrate under reduced pressure, it was distilled to obtain 224 g of n-butyl glycolate with a purity of 99.5% and a yield of 92%.

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Abstract

The invention belongs to the technical field of chemical synthesis, and concretely relates to a catalytic synthesis method of n-butyl hydroxyacetate. The method comprises the following steps: carrying out a refluxing dehydrating esterification reaction on glycolic acid and an excess amount of n-butanol under the catalysis of acidic ion exchange resin, filtering, and distilling to synthesize n-butyl hydroxyacetate, wherein the acidic ion exchange resin is preprocessed by a buffer solution. Processing of the acidic ion exchange resin by the buffer solution with a certain pH value greatly improves the synthesis yield and selectivity of n-butyl hydroxyacetate. The method has the advantages of low device requirements, no corrosion and few three wastes, and is especially suitable for amplified production.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, and in particular relates to a catalytic synthesis method of n-butyl glycolate. Background technique [0002] With its unique molecular structure, n-butyl glycolate has functional groups such as ɑ-H, hydroxyl, and ester groups at the same time, making it have the chemical properties of alcohol and ester at the same time, and can undergo carbonylation reaction, oxidation reaction, hydrolysis reaction and ɑ- Substitution reactions, etc., become an important chemical raw material. It is easily soluble in nitrocellulose, cellulose acetate, and cellulose acetate propionate. At the same time, it is also an excellent solvent for many celluloses, resins, and rubbers. It can be used as a cleaning agent for semiconductors, an additive for cosmetics, and paints. Therefore, it is widely used in many fields such as chemical industry, medicine, pesticides, feed, dyes, and spices. The traditional s...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C67/08C07C69/675
CPCC07C67/08C07C69/675
Inventor 朱虎仇敏郝健李彦孙鹏
Owner 山东广浦生物科技有限公司
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