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A kind of synthetic method of dimer acid glycidyl ester

A technology of glycidyl ester and synthesis method is applied in the field of synthesizing dimer acid glycidyl ester, can solve the problems to be further improved and the like, and achieve the effects of stable product index, low viscosity and high epoxy value

Active Publication Date: 2015-11-18
SHANDONG SHENGQUAN NEW MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] "C 36 Synthesis of dimer acid diglycidyl ester epoxy resin" (Nie Xiaoan et al., Thermosetting Plastics, No. 3, P11) discloses two preparation methods of dimer acid glycidyl ester epoxy resin. Among them, the one-step method The reaction temperature is 110°C, the reaction time is 3h, the epoxy value of the obtained product is 0.229 equivalent / 100g, the organic chlorine content is 0.038 equivalent / 100g, and the viscosity is 0.95Pa·s; the reaction temperature of the two-step method is 30°C, and the reaction time is For 12h, the epoxy value of gained product is 0.145 equivalent / 100g, and organochlorine content is 0.084 equivalent / 100g, and viscosity is 1.4Pa s; But from the result of two kinds of methods, the organochlorine content and viscosity of gained product are relatively High, the performance needs to be further improved

Method used

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  • A kind of synthetic method of dimer acid glycidyl ester

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Add 178g of dimer acid, 569g of epichlorohydrin and 2.5g of NaOH into a 1L reaction flask, stir, raise the temperature to 90°C, and maintain the reaction temperature at 90°C for 2h to obtain an intermediate with a chlorohydrin ester structure, and continue to add 2.67g of NaOH to the system. g benzyltrimethylammonium chloride, then raise the vacuum degree of the system to 140torr, control the temperature at 65°C, add 53.36g of 50% NaOH solution dropwise at a constant speed within 3 hours, and continue stirring at this temperature after the dropwise addition is completed React for 1 hour. After the reaction was completed, break the vacuum, add 200g of 80°C deionized water, stir for 5 minutes and let stand, separate liquid to remove salt, remove excess unreacted epichlorohydrin, and filter to obtain 202g of dimer acid glycidyl ester. Epoxy equivalent 412g / eq, hydrolyzed chlorine 3850ppm.

Embodiment 2

[0021] Add 178g of dimer acid, 569g of epichlorohydrin, and 5g of NaOH into a 1L reaction bottle, stir, raise the temperature to 85°C, and maintain the reaction temperature at 85°C for 4h to obtain an intermediate with a chlorohydrin ester structure, and continue to add 5.34g of benzyl to the system Triethylammonium chloride, then raise the vacuum degree of the system to 140torr, control the temperature at 65°C, add 49.48g of 50% NaOH solution dropwise at a constant speed within 2 hours, and continue stirring at this temperature for 1 Hour. After the reaction, break the vacuum, add 200g of 80°C deionized water, stir for 5 minutes and let it stand, then separate the liquid to remove the salt and excess unreacted epichlorohydrin, and filter to obtain 196g of dimer acid glycidyl ester. Epoxy equivalent 425g / eq, hydrolyzed chlorine 4542ppm.

Embodiment 3

[0023] Add 178g of dimer acid, 569g of epichlorohydrin, and 5g of KOH into a 1L reaction bottle, stir, raise the temperature to 90°C, and maintain the reaction temperature at 90°C for 2h to obtain an intermediate with a chlorohydrin ester structure, and continue to add 2.67g of tetrachloride to the system. Methyl ammonium bromide, then the vacuum degree of the system was raised to 130torr, the temperature was controlled at 60°C, and 48.13g of 50% NaOH solution was added dropwise at a uniform speed within 2 hours. After the dropwise addition, the reaction was continued at this temperature for 1 hour. After the reaction is complete, break the vacuum, add 200g of 80°C deionized water, stir for 5 minutes and let stand, separate liquid to remove salt, remove excess unreacted epichlorohydrin, and filter to obtain 198g of dimer acid glycidyl ester. The epoxy equivalent is 436g / eq, and the hydrolyzed chlorine is 5210ppm.

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Abstract

The invention relates to a synthesis method of dimer acid glycidyl ester, which comprises the following steps: 1) under the action of a catalyst 1, carrying out addition reaction on dimer acid and epoxy chloropropane to obtain an intermediate containing chlorinol ester structure; and 2) under the action of a catalyst 2, esterifying the intermediate containing chlorinol ester structure in alkali liquor to obtain the dimer acid glycidyl ester. The synthesized dimer acid modified epoxy resin has the advantages of high epoxide number, low hydrolytic chlorine, low viscosity and the like; and the cured resin has the advantages of favorable flexibility, favorable bonding strength and stable product indexes, and can be used for industrial production.

Description

technical field [0001] The invention relates to a method for synthesizing glycidyl dimer acid, belonging to the field of resin preparation. Background technique [0002] In recent years, my country has developed a series of flexible epoxy resins, which can be divided into glycidyl ether epoxy resins and glycidyl ester epoxy resins. Glycidyl dimer acid is the glycidyl ester epoxy resin. a category of . Dimer acid is used to synthesize dimer acid glycidyl ester and its modified epoxy resin. The cured product has good elasticity and toughness, so it is also called flexible epoxy resin. [0003] Dimer acid glycidyl ester flexible epoxy resin is an epoxy resin with a completely new molecular structure, perfect formula design system and curing process conditions. Make its cured product have high bonding strength, shear strength, electrical insulation performance and chemical resistance. More importantly, the dimer acid glycidyl ester type flexible epoxy resin cured product syste...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G59/12
Inventor 唐一林江成真朱红军韩东明孟令波
Owner SHANDONG SHENGQUAN NEW MATERIALS CO LTD
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