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Method of preparing fluorine-containing demoulding additive with industrial side product terpinene

A technology of by-product terpinene and mold release additives, which is applied in the direction of carboxylate preparation, carboxylic acid amide preparation, chemical instruments and methods, etc., can solve problems such as difficult to produce economic benefits and separation difficulties, and achieve sufficient raw material sources, Improved processing efficiency, simple and easy reaction operation

Inactive Publication Date: 2017-06-27
修建东
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Synthesis of terpineol with turpentine as raw material will produce a large amount of by-product terpinene, which accounts for about 20% to 30% of the output of terpineol. my country is rich in turpentine resources and is the country with the largest output of rosin and turpentine One, the amount of by-product terpinene produced by the synthesis of terpineol is huge every year. Terpinene is a mixture of isomers with very similar properties. It is very difficult to separate, so it can only be used as a low-grade solvent use, it is difficult to produce greater economic benefits

Method used

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  • Method of preparing fluorine-containing demoulding additive with industrial side product terpinene
  • Method of preparing fluorine-containing demoulding additive with industrial side product terpinene
  • Method of preparing fluorine-containing demoulding additive with industrial side product terpinene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] In a four-necked flask equipped with a stirring device, a reflux condensing device and a thermometer, add 30 grams of terpinene, 1.5 grams of toluenesulfonic acid and 0.5 grams of concentrated sulfuric acid, and after stirring for 0.5 to 1 hour, add 21 grams of 2-methanol Base-2-pentenoic acid, heat up to 170°C-180°C for reflux reaction for 5 hours to generate methylpentenoic acid terpinene addition compound, cool down to 60-70°C, add 25 grams of hydrogen peroxide, 5 grams Glacial acetic acid and 0.5 gram of concentrated sulfuric acid carried out epoxidation reaction for 4 hours to generate epoxidized 2-methyl-2-pentenoic acid terpinene addition compound, then hydrolyzed with 3 times the volume of hot water, and allowed to stand , take the oil layer to generate dihydroxyl products, add 150mL of toluene and 120g of hexafluoropropylene oligomer, start stirring, slowly add 1.5g of N,N-dimethylcyclohexylamine, and carry out prophylaxis at a temperature of 20°C to 35°C. Afte...

Embodiment 2

[0038] Add 30 grams of terpinene, 1.8 grams of p-toluenesulfonic acid and 1.2 grams of sulfamic acid into a four-neck flask equipped with a stirring device, a reflux condensing device and a thermometer, and after stirring for 0.5 to 1 hour, add 18 grams of crotonic acid , heated up to 150°C-160°C for reflux reaction for 4 hours to generate crotonyl terpinene addition compound, cooled to 65-75°C, added 21 grams of hydrogen peroxide, 5.5 grams of glacial acetic acid and 0.6 grams of concentrated sulfuric acid, and carried out Epoxidation reaction 3 hours, generate epoxidized butenoic acid terpinene addition compound, carry out hydrolysis with the hot water of 3 times volume then, leave standstill, get oily layer, generate double hydroxyl product, add 120mL toluene and 110 grams of six Fluoropropylene oligomer, start stirring, slowly add 2 grams of N,N-dimethylcyclohexylamine, carry out nucleophilic substitution reaction at a temperature of 20°C to 35°C for 6 to 8 hours, distill t...

Embodiment 3

[0040] In a four-neck flask equipped with a stirring device, a reflux condensing device and a thermometer, add 30 grams of terpinene, 1 gram of p-toluenesulfonic acid and 1.5 grams of sulfamic acid, stir for 0.5 to 1 hour, then add 24 grams of 2-hexane Acrylic acid, heat up to 160°C-170°C for reflux reaction for 6 hours to generate hexenoic acid terpinene addition compound, cool down to 70-80°C, add 24 grams of hydrogen peroxide, 6.5 grams of glacial acetic acid and 0.7 grams of concentrated sulfuric acid , carry out epoxidation reaction for 5 hours, generate epoxidized 2-hexenoic acid terpinene addition compound, then hydrolyze with 3 times the volume of hot water, let it stand, take the oil layer, generate dihydroxy product, add 100mL toluene and 105 grams of hexafluoropropylene oligomer, start stirring, slowly add 1 gram of N,N-dimethylcyclohexylamine, carry out nucleophilic substitution reaction at a temperature of 20°C to 35°C for 6 to 8 hours, and distill out toluene , to ...

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Abstract

The invention discloses a method of preparing a fluorine-containing demoulding additive with an industrial side product terpinene. The method includes the steps of: 1) performing isomerization to alpha-pinene, dipentene and isoterpinolene in the terpinene to obtain alpha-terpinene; 2) performing an addition reaction to the main component, alpha-terpinene, in the terpinene and the terpinene, which is generated through continuous isomerization, with (methyl) alkenyl acid to generate a (methyl) alkenyl acid terpinene addition compound; 3) performing an epoxidation reaction with H2O2 to generate an epoxidized (methyl) alkenyl acid terpinene addition compound; 4) performing hydrolysis to obtain a bis-hydroxyl product, which is then subjected to a nucleophilic substitution reaction with a hexafluoropropylene oligomer to prepare a hexafluoropropylene oligomer substituted product; 5) performing an amidation reaction to the hexafluoropropylene oligomer substituted product with diethanol amine to prepare an amidation product; and 6) finally performing esterification to the amidation product with phosphoric acid to prepare an esterified product, which is the fluorine-containing demoulding additive.

Description

technical field [0001] The invention relates to the technical field of mold release additive synthesis, in particular to a method for preparing a fluorine-containing mold release additive by using industrial by-product terpinene. Background technique [0002] The mold release agent is a functional substance between the mold and the organic polymer substance or other products, which is to prevent the molded products, laminated products, spinning parts, etc. A type of processing aid that is bonded to the surface of the mold or metal plate and is easy to release. In the field of polymer processing, the use of a release agent is essential and is usually used as the main release agent The active substances are mainly hydrocarbons or polysiloxane-type organosilicon compounds. The release agents formulated with hydrocarbons are rich in sources and cheap in price. The products after demoulding can be directly processed for secondary processing. However, long-term use It will cause ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/11C07D303/40C07C5/25C07C13/23C07C5/27C07C51/353C07C61/29C07C51/367C07C62/06C07C231/02C07C235/40B29C33/62
Inventor 修建东
Owner 修建东
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