Method for preparing versatate glycidyl

A technology of glycidyl ester and tertiary carbonic acid is applied in the field of preparation of glycidyl tertiary carbonate, can solve the problems of low yield of glycidyl tertiary carbonate and high preparation cost, and achieves a product with good product quality, low preparation cost and high purity. Effect

Active Publication Date: 2012-04-11
SOUTHWEST RES & DESIGN INST OF CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to overcome the low yield and high production cost of glycidy

Method used

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  • Method for preparing versatate glycidyl
  • Method for preparing versatate glycidyl
  • Method for preparing versatate glycidyl

Examples

Experimental program
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Example Embodiment

[0037] Example 1: Such as figure 1 As shown, a method for preparing glycidyl tertiary carbonate includes the following steps:

[0038] A. Into a four-necked 1L flask with stirring, thermometer and reflux, add 100g ethanol, 100g water and 69.4g epichlorohydrin, heat to 55℃, add 129.3g tertiary carbonic acid and 12.3g sodium hydroxide solution ( Sodium hydroxide (50% by weight) was added dropwise to the flask, the feeding time was controlled to 20 minutes, and the reaction was carried out at 55°C for 2.0 hours;

[0039] B. Cool the reaction mixture obtained in step A to 40°C, separate the water phase, add 24 g of sodium hydroxide and 74 g of water, and then react at 40°C for 80 minutes;

[0040] C. Distill the reaction mixture obtained in step B at a pressure of 5KPa and a temperature of 120°C, and then add 20mL of water for steam stripping. Keep the pressure at 5KPa and a temperature of 140°C for 10 minutes to remove excess epichlorohydrin. , Solvents and water and chloride salts ge...

Example Embodiment

[0042] Example 2: Such as figure 1 As shown, a method for preparing glycidyl tertiary carbonate includes the following steps:

[0043] A. Into a four-necked 2L flask with stirring, thermometer and reflux, add 400g isopropanol, 605g water and 300g epichlorohydrin, heat to 80℃, add 500g tertiary carbonic acid and 47.6g sodium hydroxide solution ( Sodium hydroxide (50% by weight) was dropped into the flask, the feeding time was controlled to 20 minutes, and the reaction was carried out at 80°C for 100 minutes;

[0044] B. Cool the reaction mixture obtained in step A to 60°C, separate the water phase, add 93 g of sodium hydroxide and 280 g of water, and then react at 60°C for 100 minutes;

[0045] C. Distill the reaction mixture obtained in step B at a pressure of 95.4KPa and a temperature of 120°C, and then continue vacuum distillation until the pressure is 5KPa and a temperature of 140°C. Remove excess epichlorohydrin, solvent and reaction products The water and chloride salt to obta...

Example Embodiment

[0047] Example 3: Such as figure 1 As shown, a method for preparing glycidyl tertiary carbonate includes the following steps:

[0048] A. Add 124.9g tert-butanol, 100g water and 234.9g epichlorohydrin to a four-necked 1L flask with stirring, thermometer and reflux, and heat to 65°C, add 129.3g tertiary carbonic acid and 12.3g hydrogen hydroxide Sodium solution (50% by weight of sodium hydroxide) was dropped into the flask, the feeding time was controlled to 20 minutes, and the reaction was carried out at 65°C for 30 minutes;

[0049] B. Cool the reaction mixture obtained in step A to 55°C, separate the water phase, add 24.0g potassium hydroxide and 74g water, and then react at 55°C for 30 minutes;

[0050] C. Distill the reaction mixture obtained in step B at a pressure of 95.4KPa and a temperature of 120°C, and then continue vacuum distillation until the pressure is 5KPa and a temperature of 140°C. Remove excess epichlorohydrin, solvent and reaction products The water and chloride...

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Abstract

The invention discloses a method for preparing versatate glycidyl, which comprises the following steps of: A. dropwise adding versatic acid and an alkali metal hydroxide or an alkali metal alkoxide with the mol ratio is 1: 0.1-0.5 into chloroepoxy propane with a mol ratio of 1: 1.01-10 to the versatic acid, and carrying out reaction for 0.3-2.0 hours at the temperature of 45-110 DEG C in the presence of water and an organic solvent; B. carrying out aqueous-phase separation on a reactant mixture obtained from the step A, adding the alkali metal hydroxide or the alkali metal alkoxide again until the mol ratio of the total amount of the alkali metal hydroxide or the alkali metal alkoxide added in the step A and the step B to that of the versatic acid reaches 1.01-2.5: 1, and then, carrying out reaction for 0.5-3.0 hours at the temperature of 20-90 DEG C; and C. distilling a reactant mixture obtained from the step B to remove superfluous chloroepoxy propane, superfluous solvent, and water and chloride salts produced by the reaction, and obtaining the required versatate glycidyl. With the adoption of the method, the yield of the versatate glycidyl is high, the purity is high, and the cost for preparation is low.

Description

technical field [0001] The invention relates to a preparation method of glycidyl tertiary carbonate. Background technique [0002] The structural formula of glycidyl tertiary carbonic acid ester is: , where R 1 , R 2 , R 3 Respectively represent the same or different alkyl groups with a straight chain or branched chain structure containing 1 to 20 carbon atoms, at least one of which is methyl, more commonly R 1 +R 2 +R 3 =C8. Glycidyl tertiary carbonic acid ester has epoxy functional end groups, and is widely used in solvent-based formulations for automotive original paint and refinish paint. The main advantage of using glycidyl tertiary carbonic acid ester is that it can reduce the viscosity of the synthesized resin and improve the viscosity of the resin. Fullness, weatherability (alkali and water resistance) and adhesion, especially for acrylic and polyester resins. [0003] There are mainly one-step reaction system and two-step reaction system in the production m...

Claims

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Application Information

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IPC IPC(8): C07D303/16C07D301/26
CPCC07D303/16
Inventor 李毅肖英朱林刘杨黄超明陈春玉程长明王玲
Owner SOUTHWEST RES & DESIGN INST OF CHEM IND
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