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Catalyst for preparing glycidyl neodecanoate and application thereof

A technology of glycidyl ester and neodecanoic acid, applied in physical/chemical process catalysts, organic compound/hydride/coordination complex catalysts, organic chemistry, etc. The problem of low rate and other problems, to achieve the effect of shortening the reaction time, fast reaction speed and high product purity

Active Publication Date: 2019-10-18
SOUTHWEST RES & DESIGN INST OF CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In order to solve the problems of large amount of existing catalysts, high strength, easy generation of by-products, and low reaction yield, the invention provides a catalyst for preparing glycidyl neodecanoate and its application

Method used

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  • Catalyst for preparing glycidyl neodecanoate and application thereof
  • Catalyst for preparing glycidyl neodecanoate and application thereof
  • Catalyst for preparing glycidyl neodecanoate and application thereof

Examples

Experimental program
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Effect test

example 1

[0042] Add 20.32 g (0.0767 mol) of neodecanoic acid-1-chloroglyceride into a 250 ml three-necked flask equipped with a magnetic stirrer, a thermometer, a dropping funnel, and a condenser, stir and raise the temperature to 40 ° C, and add 17.51 ​​g of catalyst DBU, Dropping in, adopt the method of first slow, medium fast and then slow, control the dropping time to 20 minutes, keep the temperature at 40°C, count 0.5 hours from the start of dropping, keep the temperature at 40°C, then add water 101.6 to the organic phase g, wash for 10 minutes, stop stirring, let stand to separate layers, and remove the water phase. The organic phase was distilled under reduced pressure to remove water to obtain 17.10 g of a colorless and transparent liquid product. Based on neodecanoic acid-1-chloroglyceride, the yield is 97.60%, and the epoxy equivalent value is 236.1 g / mol (purity: 96.8%).

[0043] figure 1 The infrared spectrogram of the glycidyl neodecanoate product prepared for this examp...

example 2

[0045] Add 46.78 g (0.1767 mol) of neodecanoic acid-1-chloroglyceride into a 500 ml three-necked flask equipped with a magnetic stirrer, a thermometer, a dropping funnel, and a condenser, stir and raise the temperature to 40 ° C, and add a catalyst DBU32.25 g, Dropping in, using the method of slow, medium, fast and then slow, control the dropping time to 20 minutes, keep the temperature at 40°C, count 0.5 hours from the start of dropping, keep the temperature at 40°C, and then add water 233.9 to the organic phase g, wash for 10 minutes, stop stirring, let stand to separate layers, and remove the water phase. The organic phase was distilled under reduced pressure to remove water to obtain 38.92 g of a colorless and transparent liquid product. Based on neodecanoic acid-1-chloroglyceride, the yield is 96.70%, and the epoxy equivalent value is 236.3g / mol (purity 96.8%).

example 3

[0047] Add 20.32 g (0.0767 mol) of neodecanoic acid-1-chloroglyceride into a 250 ml three-necked flask equipped with a magnetic stirrer, a thermometer, a dropping funnel, and a condenser, stir and raise the temperature to 50 ° C, and add 9.62 g of catalyst DBN, Dropping in, using the method of slow, medium, fast and then slow, control the dropping time to 20 minutes, keep the temperature at 50°C, count 1 hour from the start of dropping, keep the temperature at 50°C, and then add water 20.32 to the organic phase g, wash for 10 minutes, stop stirring, let stand to separate layers, and remove the water phase. The organic phase was distilled under reduced pressure to remove water to obtain 17.01 g of a colorless and transparent liquid product. Based on neodecanoic acid-1-chloroglyceride, the yield is 97.10%, and the epoxy equivalent value is 236.5 g / mol (purity: 96.6%).

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Abstract

The invention provides a catalyst for preparing glycidyl ester of neodecanoic acid and belongs to the technical field of catalysts. The catalyst is DBU (1,8-diazacyclo hendecene) or DBN (1.5-diazabicyclo [4.3.0]-5-nonylene). A preparation method of using the catalyst for the glycidyl ester of neodecanoic acid comprises the following steps of heating neodecanoic acid-1-chlorinated glyceride, addingthe catalyst for reaction, adding water in a reaction liquid, performing washing to neutral, performing static stratification to remove a water phase, and after removing water from an oil phase, performing reduced pressure distillation to obtain a glycidyl ester product of the neodecanoic acid. The catalyst provided by the invention is high in catalytic activity, rapid in reaction speed and mildin condition. By applying the catalyst to preparation of the glycidyl ester of neodecanoic acid, the reaction time can be effectively shortened, an amount of reaction byproducts is small, a separationstep is omitted, and the reaction yield is increased at the same time. The DBU and DBN catalysts are stable, are good in quality of products and higher in yield and product purity, can lower the costthrough recovery and reusing and provide a better selection for industrial production.

Description

technical field [0001] The invention belongs to the technical field of catalysts, in particular to a catalyst for preparing glycidyl neodecanoate and an application thereof. Background technique [0002] Glycidyl neodecanoate is an ester compound composed of a tertiary carbon structure and a glycidyl group structure. It is a mixture of isomers, wherein R1 and R2 are alkyl groups, and the sum of their carbon numbers is 7. Mainly through the polymerization of propylene into tripropylene, and then carbonylation to prepare neodecanoic acid, and then catalyze the preparation of neodecanoic acid-1-chloroglyceride, which is obtained after dehydrochlorination. The special tertiary carbon structure and epoxy group of glycidyl neodecanoate make it have low viscosity and high boiling properties, and can be widely used in the coating industry. [0003] [0004] Glycidyl neodecanoate has epoxy functionality and is widely used in solvent-borne formulations for automotive OEM and refi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/02C07D301/28C07D303/16
Inventor 肖英李毅
Owner SOUTHWEST RES & DESIGN INST OF CHEM IND
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