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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 glycidyl tertiary carbonic acid in the prior art, and provide a method for preparing glycidyl tertiary carbonic acid

Method used

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

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Embodiment 1: as figure 1 Shown, a kind of preparation method of glycidyl tertiary carbonate comprises the following steps:

[0038] A. Add 100g of ethanol, 100g of water and 69.4g of epichlorohydrin to a four-necked 1L flask with stirring, thermometer and reflux, heat to 55°C, and mix 129.3g of tertiary carbonic acid and 12.3g of sodium hydroxide solution ( Sodium hydroxide (50% by weight) was added dropwise in the flask, and the feeding time was controlled to be 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 24g of sodium hydroxide and 74g of water, and 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, then add 20mL of water for stripping, keep the pressure at 5KPa, and the temperature is 140°C for 10 minutes to remove excess epichlorohydrin , solvent and the w...

Embodiment 2

[0042] Embodiment 2: as figure 1 Shown, a kind of preparation method of glycidyl tertiary carbonate comprises the following steps:

[0043] A. Add 400g of isopropanol, 605g of water and 300g of epichlorohydrin to a four-necked 2L flask with stirring, thermometer and reflux, heat to 80°C, mix 500g of tertiary carbonic acid and 47.6g of sodium hydroxide solution ( Sodium hydroxide weight percentage is 50%) dropwise in the flask, and feed time is controlled as 20 minutes, and reaction is carried out 100 minutes under 80 ℃ of conditions;

[0044] B. Cool the reaction mixture obtained in step A to 60°C, separate the water phase, add 93g of sodium hydroxide and 280g 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 to distill under reduced pressure until the pressure is 5KPa and the temperature is 140°C to remove excess epichlorohydrin, solvent and react...

Embodiment 3

[0047] Embodiment 3: as figure 1 Shown, a kind of preparation method of glycidyl tertiary carbonate comprises the following steps:

[0048] A. Add 124.9g of tert-butanol, 100g of water and 234.9g of epichlorohydrin to a four-necked 1L flask with stirring, thermometer and reflux, heat to 65°C, and oxidize 129.3g of tertiary carbonic acid and 12.3g of hydrogen Sodium solution (sodium hydroxide weight percent is 50%) is added dropwise in the flask, and the feeding time is controlled as 20 minutes, and the reaction is 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 24.0 g of potassium hydroxide and 74 g of water, and 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 to distill under reduced pressure until the pressure is 5KPa and the temperature is 140°C to remove excess epichlorohy...

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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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