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A kind of synthetic method of photoinitiator isopropyl thioxanthone

A technology for isopropyl thioxanthone and crude isopropyl thioxanthone, which is applied in organic chemistry and other fields, can solve the problems of high cost of raw materials, harsh reaction conditions, and low inhibition yield, and achieve less waste, The effect of stable quality control and high conversion rate of raw materials

Active Publication Date: 2019-08-06
宁夏沃凯珑新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

They all have many disadvantages: expensive raw materials, high cost, harsh reaction conditions, difficult to control, difficult to suppress side reactions, low yield, large amount of waste acid, etc.

Method used

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  • A kind of synthetic method of photoinitiator isopropyl thioxanthone
  • A kind of synthetic method of photoinitiator isopropyl thioxanthone
  • A kind of synthetic method of photoinitiator isopropyl thioxanthone

Examples

Experimental program
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Effect test

Embodiment 1

[0023] The specific steps of the synthesis method are as follows: primary chlorination: add 1000 ml of dichloroethane, 2,2'-dithiodibenzoic acid dithio 150g of salicylic acid, add 125g of thionyl chloride dropwise at 65-70°C, drop it for about 2-2.5 hours, then keep it warm at 70-75°C for 1 hour, sample and analyze, the raw material dithiosalicylic acid disappears, The reaction is completed; secondary chlorination: after the one-step chlorination reaction is qualified, the temperature is lowered to 10-15°C, and about 72g of chlorine gas is passed into the reaction liquid at a rate of 20-25g / h, Insulate the reaction for 0.5h, take a sample to judge the end point of the reaction, if it is qualified, stop the chlorine flow; Friedel-Crafts: After the chlorine flow is completed, lower the temperature to below 10°C, control the temperature at 7-10°C and add 154g of anhydrous aluminum trichloride in batches, and drop it at the same time Add 135 g of cumene, add 9 g of cumene dropwise...

Embodiment 2

[0025] The specific steps of the synthesis method are as follows: primary chlorination: add 1000 ml of dichloroethane, 2,2'-dithiodibenzoic acid dithio For 150g of salicylic acid, add 120g of thionyl chloride dropwise at 65-70°C, drop it for about 2-2.5 hours, then keep it warm at 70-75°C for 1 hour, sample and analyze, the raw material dithiosalicylic acid disappears, The reaction is completed; secondary chlorination: after the one-step chlorination reaction is qualified, the temperature is lowered to 10-15°C, and about 68 chlorine gas is introduced into the reaction liquid at a rate of 20-25g / h, Heat preservation reaction for 0.5h, take a sample to judge the end point of the reaction, if it is unqualified, prolong the heat preservation time for 0.5h, then take a sample for analysis, if it is qualified, stop the chlorine flow; Friedel-Crafts: After the chlorine flow is completed, cool down to below 10°C, and control the temperature at 7-10°C Add 147g of anhydrous aluminum tri...

Embodiment 3

[0027] The specific steps of the synthesis method are as follows: primary chlorination: add 1000 ml of dichloroethane, 2,2'-dithiodibenzoic acid dithio For 150g of salicylic acid, add 120g of thionyl chloride dropwise at 65-70°C, drop it for about 2-2.5 hours, then keep it warm at 70-75°C for 1 hour, sample and analyze, the raw material dithiosalicylic acid disappears, The reaction is completed; secondary chlorination: after the one-step chlorination reaction is qualified, the temperature is lowered to 10-15°C, and about 72g of chlorine gas is passed into the reaction liquid at a rate of 20-25g / h, Heat preservation reaction for 0.5h, take a sample to judge the end point of the reaction, if it is unqualified, prolong the heat preservation time for 0.5h, then take a sample for analysis, if it is qualified, stop the chlorine flow; Friedel-Crafts: After the chlorine flow is completed, cool down to below 10°C, and control the temperature at 7-10°C Add 154g of anhydrous aluminum tri...

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Abstract

The invention discloses a synthesis method of photoinitiator isopropylthioxanthone. According to the method, an isopropylthioxanthone crude product is prepared from raw materials including dithiosalicylic acid and isopropylbenzene with a chlorination-friedel-crafts reaction synthesis route, and a product is obtained through high-vacuum distillation purification. The raw and auxiliary materials are easy to obtain, reaction conditions are mild, the operation is safe, simple and convenient, the conversion rate of the raw materials is high, and the product quality is stable.

Description

[0001] Technical field: [0002] The invention relates to a synthesis method of a light stabilizer, in particular to a synthesis method of a photoinitiator isopropylthioxanthone. [0003] Background technique: [0004] Photoinitiators are mainly used for the initiation of monomers in radiation (UV) curable coatings. Due to the advantages of fast curing speed, energy saving, low pollution, and good physical properties, UV curable coatings have been applied in many fields such as wood coating, printing glazing, ink curing, and optical fiber manufacturing to coatings for automobiles and aircraft metal parts. . In recent years, the application of UV curing coatings has grown at a rate of 18-20%. [0005] Isopropylthioxanthone is a highly efficient photoinitiator and is an important component of UV-curable coatings. For a long time, its application and industrialization have been limited due to its high cost. At present, the synthesis methods of isopropylthioxanthone at home and...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D335/16
CPCC07D335/16
Inventor 郭徐良万学明
Owner 宁夏沃凯珑新材料有限公司
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