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Preparation method of acetic acid 2-hydroxyl-3-chloro-propyl ester compound

A technology of acetic acid and hydroxyl group, applied in the field of preparation of acetate compounds, can solve problems such as high production cost, equipment corrosion, environmental pollution of waste water, etc., and achieve the effects of easy product separation, low production cost and high reaction yield

Inactive Publication Date: 2018-05-18
瑞通高分子科技(浙江)有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This process has high production costs, serious equipment corrosion, many side reactions, difficult product separation, and the generated wastewater will cause environmental pollution.

Method used

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  • Preparation method of acetic acid 2-hydroxyl-3-chloro-propyl ester compound
  • Preparation method of acetic acid 2-hydroxyl-3-chloro-propyl ester compound
  • Preparation method of acetic acid 2-hydroxyl-3-chloro-propyl ester compound

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preparation example Construction

[0024] A kind of preparation method of acetic acid 2-hydroxyl-3-chloro-propyl ester, this method is raw material with acetic acid and epichlorohydrin, under the catalysis of phase transfer catalyst, reaction prepares acetic acid 2-hydroxyl-3-chloro-propyl ester, The molar ratio of acetic acid and epichlorohydrin is 1:1.02-1.05, and the catalyst is added. The reaction temperature is controlled at 105-110°C for 3 hours, and the temperature is controlled at 115-125°C for 3 hours. The acid value is less than 5mg / gKOH , and then evacuated at 100-105°C for 2 hours at a pressure of -0.04-0.06MPa to obtain high-purity 2-hydroxy-3-chloro-propyl acetate. Wherein said catalyzer is a phase transfer catalyst, preferably quaternary ammonium salt but not limited to: bisdecyldimethylammonium bromide, benzyltriethylammonium chloride in quaternary ammonium salt, consumption is 2-2 of the total amount of this step 3%.

[0025] The reaction temperature is divided into two temperature control pro...

Embodiment 1

[0033] Embodiment 1 Synthetic acetic acid 2-hydroxyl-3-chloro-propyl ester

[0034] Table 1, synthetic formula table

[0035]

[0036] Add components 1, 2, 3, and 4 into the flask, heat and control the temperature at 105-110°C for 3 hours, then control the temperature at 115-125°C for 4 hours and then detect that the acid value is less than 5mg / gKOH , and then evacuated at 100-105°C for 2 hours at a pressure of -0.04-0.06MPa to obtain the target product 2-hydroxyl-3-chloro-propyl acetate.

[0037] Product index: colorless liquid, viscosity---15cps / 25℃, refractive index---1.4582(23℃).

[0038] The infrared spectrum of the product is shown in figure 1 .

Embodiment 2

[0039] Embodiment 2 Synthetic acetic acid 2-hydroxyl-3-chloro-propyl ester

[0040] Table 2, synthetic formula table

[0041]

[0042] Add components 1, 2, 3, and 4 into the flask, heat and control the temperature at 105-110°C for 3 hours, then control the temperature at 115-125°C for 4 hours and then detect that the acid value is less than 5mg / gKOH , and then evacuated at 100-105°C for 2 hours at a pressure of -0.04-0.06MPa to obtain the target product 2-hydroxyl-3-chloro-propyl acetate.

[0043] Product index: colorless liquid, viscosity---15cps / 25℃, refractive index---1.4582(23℃).

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Abstract

The invention provides a preparation method of acetic acid 2-hydroxyl-3-chloro-propyl ester. The invention provides the acetic acid 2-hydroxyl-3-chloro-propyl ester generated by reacting acetic acid with epichlorohydrin by a phase transfer catalyst. The preparation method of a substance comprises the following steps: under the condition that the molar ratio of the acetic acid to the epichlorohydrin is 1 to (1.02 to 1.05), adding the catalyst, and controlling the reaction temperature at 105 to 110 DEG C for 3 hours; then controlling the temperature at 115 to 125 DEG C for 3 hours; under the conditions that the temperature is 100 to 105 DEG C and the pressure is 0.04 to 0.06 MPa, vacuumizing for 2 hours to obtain high-purity acetic acid 2-hydroxyl-3-chloro-propyl ester. The catalyst is the phase transfer catalyst, preferable quaternary ammonium salt but not limited to didoctyl dimethyl ammonium bromide and benzyl triethyl ammonium in quaternary ammonium salt; the use amount of the preferable quaternary ammonium salt is 2 to 3 percent of the total amount in the step. The acetic acid 2-hydroxyl-3-chloro-propyl ester prepared by the preparation method has the advantages of high conversion rate, high selectivity, good stability and suitability for industrial production.

Description

technical field [0001] The invention relates to the field of fine chemicals, in particular to a preparation method of acetate compounds. Background technique [0002] The chemical formula of 2-hydroxy-3-chloro-propyl acetate is: CH 3 COOCH 2 -CH(OH)CH 2 Cl. [0003] 2-Hydroxy-3-chloro-propyl acetate is a colorless oily liquid with a special aroma. It has good solubility in resins, especially some insoluble cellulose ethers, polyurethane resins and thermoplastic acrylic resins. It is used to dissolve, so it can be used as an excellent solvent for paints, paints, etc., and as a spice ingredient in the food industry and cosmetics. [0004] In addition to being used as a solvent, since 2-hydroxy-3-chloro-propyl acetate is a compound containing a hydroxyl group, it can be used as a functional compound of a hydroxyl compound, so it can be used for esterification reactants, polyurethane reactants and polyurethane compounds. chain agent. [0005] 2-Hydroxy-3-chloro-propyl acet...

Claims

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Application Information

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IPC IPC(8): C07C67/26C07C67/48C07C67/52C07C69/16
CPCC07C67/26C07C67/48C07C67/52C07C69/16
Inventor 余宗萍余宗宝黄世斌杨鹏飞
Owner 瑞通高分子科技(浙江)有限公司
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