Preparation method of 2,2'-dihydroxy-4-methoxybenzophenone

A technology of methoxybenzophenone and trihydroxybenzophenone, which is applied in the field of chemical synthesis, can solve the problems of low preparation yield, undisclosed preparation method for product purification, and high cost, so as to improve the preparation efficiency and solve the problem of product Effects of appearance problems, yield and quality improvement

Active Publication Date: 2015-09-30
宜都市华阳化工有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The starting material salicyloyl chloride of the preparation method has poor stability, high cost, and low preparation yield. The literature d

Method used

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  • Preparation method of 2,2'-dihydroxy-4-methoxybenzophenone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Weigh 50g of sulfolane, 20mL of phosphorus oxychloride, 30g (0.2mol) of anhydrous zinc chloride in a 250mL four-neck glass bottle, stir and heat to 50°C for 1 hour, then add 15.2g (0.11mol) of salicylic acid, Resorcinol 11.0g (0.1mol), heated up to 75°C and reacted for 2 hours. After the reaction was completed, 20mL of water was added dropwise under cooling to terminate the reaction. The reaction solution was poured into 250mL of ice water and stirred for 5 hours, cooled to crystallize, filtered and dried, and reassembled. 21.3g, the content of 2,2',4-trihydroxybenzophenone detected by HPLC is 96.58%, and the yield is 92.60%;

[0028] Take 21.3g of the prepared 2,2',4-trihydroxybenzophenone in a 250mL reaction flask, add 60mL of toluene, 12.7g (0.12mol) of sodium carbonate, stir and raise the temperature to 45°C, add dropwise dimethyl sulfate 16.4g (0.13mol), keep it warm for 2 hours after dripping, add 50mL of distilled water to wash, stir for 10 minutes and then separ...

Embodiment 2

[0031] Weigh 250g of sulfolane, 100mL of phosphorus oxychloride, 150g (0.2mol) of anhydrous zinc chloride, add to a stirred 1000mL reaction flask, heat to 55°C for 1 hour, then add 72.5g (0.53mol) of salicylic acid , resorcinol 55.0g (0.5mol), heated to 72 ° C for 2 hours, after the reaction was completed, 50 mL of water was added dropwise under cooling to terminate the reaction, the reaction solution was poured into 1000 mL of ice water and stirred for 10 hours, cooled and crystallized, filtered at room temperature The product was collected and weighed 108.3g after drying. The 2,2',4-trihydroxybenzophenone content was 95.20% as detected by GC, and the yield was 94.17%;

[0032] Take 108.3g of the prepared 2,2',4-trihydroxybenzophenone in a 1000mL reaction flask, add 300mL of toluene, 63.5g (0.60mol) of sodium carbonate, stir and raise the temperature to 45°C, add dimethyl sulfate dropwise 82.0 g (0.65 mol), keep it warm for 2 hours after dripping, add 250 mL of distilled wate...

Embodiment 3

[0035] Weigh 500kg sulfolane, 200L phosphorus oxychloride, 300kg (2000mol) anhydrous zinc chloride, add in 1000L enamel reaction tank, heat up to 50 ° C for 1 hour, then add 152kg (1100mol) of salicylic acid, resorcinol 110kg (1000mol), heated at 70-75°C to react for 2 hours. After the reaction, 100L of water was added dropwise to terminate the reaction. The reaction liquid was transferred to a 2000L enamel reaction tank that had been cooled and filled with 1000L of ice water, stirred for 8 hours, cooled and crystallized, and centrifuged. After drying, it weighs 208kg. The content of 2,2',4-trihydroxybenzophenone detected by HPLC is 97.15%, and the yield is 90.43%;

[0036] Take 208kg (904mol) of the prepared 2,2',4-trihydroxybenzophenone into a 2000L enamel reaction tank, add about 600kg of toluene, 127kg (1200mol) of sodium carbonate, stir and heat up to 45°C, add disulfuric acid di Methyl ester 164kg (1300mol), keep warm for 2 hours after dripping, add 30OL water to wash, s...

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Abstract

A preparation method of 2,2'-dihydroxy-4-methoxybenzophenone comprises the following steps: synthesizing 2,2'4-trihydroxybenzophenone from salicylic acid and resorcinol, and carrying out a methylation reaction on 2,2'4-trihydroxybenzophenone and dimethyl sulfate to prepare 2,2'-dihydroxy-4-methoxybenzophenone. The method has the advantages of high purification efficiency, good separation effect of byproducts, high product purity reaching 99.5%, and realization of industrial production requirements of the above product.

Description

technical field [0001] The invention belongs to the field of chemical synthesis and relates to the preparation of light stabilizers, in particular to a preparation method of 2,2'-dihydroxy-4-methoxybenzophenone, a benzophenone ultraviolet absorber. Background technique [0002] 2,2'-dihydroxy-4-methoxybenzophenone, hereinafter referred to as BP-8, is a kind of ultraviolet absorber. 330-370nm ultraviolet light has a strong absorption effect and a wide absorption range. It is suitable for the application of polymer materials polyvinyl chloride, ABS resin, acrylic resin, polyurethane, melamine resin, cellulose resin and cosmetics. [0003] There are few literature reports on the preparation method of BP-8. The following is the relevant literature about the synthesis method of BP-8. [0004] In the "Synthesis of 2,2'-dihydroxy-4-methoxybenzophenone" published by Liu Shumei and others, it is introduced that aluminum trichloride is used as a catalyst to make 2,4,2'-trimethoxybe...

Claims

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Application Information

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IPC IPC(8): C07C45/70C07C49/84
CPCC07C45/455C07C45/70C07C49/84C07C49/83
Inventor 徐明华赵定春覃华中
Owner 宜都市华阳化工有限责任公司
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