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Production method of 2-hydroxy-4-methoxy benzophenone

A technology of methoxybenzophenone and hydroxyl, which is applied in the production field of benzophenone ultraviolet absorber 2-hydroxy-4-methoxybenzophenone, can solve the problem of excessive toluene solvent residue and production cost High-level problems, to achieve process optimization, production cost reduction, and the effect of environmental protection

Active Publication Date: 2008-12-17
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

[0012] The above-mentioned production method easily causes the toluene solvent residue to exceed the standard, and the production cost is relatively high

Method used

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  • Production method of 2-hydroxy-4-methoxy benzophenone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] 1. BP-3 crude:

[0042] a. Raw material ratio:

[0043] BP-1 crude product 100Kg

[0044] n-Hexane 120Kg

[0045] Sodium carbonate 40Kg

[0046] Dimethyl sulfate 20Kg

[0047] Water 200Kg

[0048] b. Mix the crude product of BP-1, n-hexane, and sodium carbonate in the reaction kettle in proportion, then add dimethyl sulfate and heat to generate 2-hydroxy-4-methoxybenzophenone. The reaction temperature is 60 -68°C, the reaction time is 4 hours.

[0049] c. Add water to the reaction kettle to separate the liquid layers, heat to 68-70°C, distill and separate n-hexane, and discharge waste water; continue to heat at 110-120°C to generate BP-3 distilled crude product, lower it to normal temperature, and obtain BP- 3 Crude product, product content 95%, light red.

[0050] 2. BP-3 refining:

[0051] a. Once refined. Add crude BP-3 to methanol solution, heat at 55-60°C until the crude BP-3 is fully dissolved, remove impurities by centrifugation, cool to 0-5°C to crystal...

Embodiment 2

[0054] 1. BP-3 crude:

[0055] a. Raw material ratio:

[0056] BP-1 crude product 100Kg

[0057] n-Hexane 90Kg

[0058] Sodium carbonate 30Kg

[0059] Dimethyl sulfate 15Kg

[0060] Water 150Kg

[0061]b. Mix the crude product of BP-1, n-hexane, and sodium carbonate in the reaction kettle in proportion, then add dimethyl sulfate and heat to generate 2-hydroxy-4-methoxybenzophenone. The reaction temperature is 45 -46°C, the reaction time is 6 hours.

[0062] c. Add water to the reaction kettle to separate the liquid layers, heat to 100-110°C, distill and separate n-hexane, and discharge waste water; continue to heat at 180-210°C to generate BP-3 distillation crude product, lower it to normal temperature, and obtain BP- 3 Crude product, product content 95%, light red.

[0063] 2. BP-3 refining:

[0064] a. Once refined. Add crude BP-3 to methanol solution, heat at 58-68°C until the crude BP-3 is fully dissolved, remove impurities by centrifugation, cool to 5-10°C for cr...

Embodiment 3

[0067] 1. BP-3 crude:

[0068] a. Raw material ratio:

[0069] BP-1 crude product 100Kg

[0070] n-Hexane 110Kg

[0071] Sodium carbonate 35Kg

[0072] Dimethyl sulfate 18Kg

[0073] Water 180Kg

[0074] b. Mix the crude product of BP-1, n-hexane, and sodium carbonate in the reaction kettle in proportion, then add dimethyl sulfate and heat to generate 2-hydroxy-4-methoxybenzophenone. The reaction temperature is 60 -68°C, the reaction time is 5 hours.

[0075] c. Add water to the reaction kettle to separate the liquid layers, heat to 68-70°C, distill and separate n-hexane, and discharge waste water; continue to heat at 110-120°C to generate BP-3 distilled crude product, lower it to normal temperature, and obtain BP- 3 Crude product, product content 95%, light red.

[0076] 2. BP-3 refining:

[0077] a. Once refined. Add crude BP-3 to methanol solution, heat at 55-60°C until the crude BP-3 is fully dissolved, remove impurities by centrifugation, cool to 4-8°C for crysta...

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Abstract

The invention relates to a production method of 2-hydroxy-4-methoxyl benzophenone (BP-3) which is an ultraviolet ray absorbent. The production process mainly comprises rough preparation of BP-3: BP-1 crude product is reacted with dimethyl sulfate in a normal hexane solution with sodium carbonate as a neutralizing agent to produce the BP-3; preparation of BP-3 crude product by heating distillation; refinement of the BP-3: the BP-3 crude product can be prepared into BP-3 fine product in a methanol solution through heating, crystallization by cooling and filtration and finished product can be gained through drying with product content of not less than 99.9 percent. The production method of the 2-hydroxy-4-methoxyl benzophenone (the BP-3) provided by the invention reduces residue of solvent, with no residue of toluol existing in the products, thus improving the safety of the products. In addition, production procedures are reduced so as to reduce production cost.

Description

technical field [0001] The invention relates to the field of light stabilizer production, in particular to a production method of benzophenone ultraviolet absorber 2-hydroxyl-4-methoxybenzophenone (hereinafter referred to as BP-3). Background technique [0002] In recent years, as the earth's ozone layer has been destroyed more and more seriously, the radiation of the sun's ultraviolet rays on the earth has become more and more intense. Foreign countries have made very strict regulations on the addition of ultraviolet absorbers to various products, and my country has also begun to pay attention to ultraviolet rays. The content of absorbent in various articles. 2-Hydroxy-4-methoxybenzophenone (BP-3) is a new type of light stabilizer, which can efficiently absorb ultraviolet light at 290-400 nanometers, hardly absorb visible light, and has good light and thermal stability. It does not decompose at 200°C and is widely used in plastics, paints, coatings and cosmetics industries....

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C49/84C07C45/64C09K15/06
Inventor 赵定春孙大明
Owner 宜都市华阳化工有限责任公司
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