Method of preparing Octocrilene

A dehydrating agent and catalyst technology, which is applied in the field of octocrylene preparation, can solve problems such as environmental pollution, low yield, and octocrylene cannot meet the technical requirements for the manufacture of anti-ultraviolet additives, so as to improve work efficiency and energy utilization , simple processing, and convenient production and operation

Inactive Publication Date: 2009-07-29
南京寒武纪科技有限公司
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  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

[0006] The purpose of the present invention is to solve the technical problem that the octocrylene produced by the prior art cannot meet the technical requirements for the manufacture of daily cosmetic grade anti-ultrav

Method used

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  • Method of preparing Octocrilene

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Example Embodiment

[0025] Example 1

[0026] Add 364g (2.0mol) benzophenone, 400g (2.0mol) isooctyl cyanoacetate 600ml n-hexane, 247g (2.4mol) acetic anhydride and 10g ammonium acetate into a 2L four-neck flask, and install a water separator. The temperature was slowly raised to 85°C and refluxed, the acetic acid-water-n-hexane solution was separated, and the n-hexane was refluxed into the reaction system. GC online analysis showed that the content of isooctyl cyanoacetate was less than 0.5%, and the reaction was terminated.

[0027] Cool to room temperature, add cold water, stir for 30 min, stand to remove the lower aqueous layer containing acetic acid-ammonium acetate, neutralize with ammonia water to pH 7, and concentrate to dryness to obtain by-product ammonium acetate. (The claim is heating and vacuum concentration, so how many degrees of heating should be given, and what is the degree of vacuum? Give specific numbers, and the following examples are also modified accordingly) The oil layer...

Example Embodiment

[0028] Example 2

[0029] Add 509.6g (2.8mol) benzophenone, 400g (2.0mol) isooctyl cyanoacetate 600ml n-hexane, 247g (2.4mol) acetic anhydride and 10g ammonium acetate into a 2L four-neck flask, and install a water separator. The temperature was slowly raised to 85°C and refluxed, the acetic acid-water-n-hexane solution was separated, and the n-hexane was refluxed into the reaction system. GC online analysis showed that the content of isooctyl cyanoacetate was less than 0.5%, and the reaction was terminated.

[0030] Cooled to room temperature, added cold water, stirred for 30 min, statically separated the lower aqueous layer containing acetic acid-ammonium acetate, neutralized with ammonia water to pH 7-8, concentrated to dryness to obtain by-product ammonium acetate. The oil layer was concentrated to recover n-hexane, the concentrated solution was distilled under reduced pressure, collected: 180-190°C / 0.1mmHg to obtain 685.9g of light yellow viscous oily liquid, yield 95%, ...

Example Embodiment

[0031] Example 3

[0032] Add 364g (2.0mol) of benzophenone, 400g (2.0mol) of isooctyl cyanoacetate, 600ml of n-hexane, 494g (4.8mol) of acetic anhydride and 10g of ammonium acetate into a 2L four-neck flask, and install a water separator. The temperature was slowly raised to 85°C and refluxed, the acetic acid-water-n-hexane solution was separated, and the n-hexane was refluxed into the reaction system. GC online analysis showed that the content of isooctyl cyanoacetate was less than 0.5%, and the reaction was terminated.

[0033] Cool to room temperature, add cold water, stir for 30 min, stand to remove the lower aqueous layer containing acetic acid-ammonium acetate, neutralize with ammonia water to pH 7, and concentrate to dryness to obtain by-product ammonium acetate. The oil layer was concentrated to recover cyclohexane, and the concentrated solution was distilled under reduced pressure. Collection: 180-190°C / 0.1 mmHg to obtain 655 g of light yellow viscous oily liquid wi...

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Abstract

The invention relates to a preparation method of Octocrilene. Iso-octyl cyanoacetate and benzophenone are used as raw materials. And under the function of catalysts, dehydrating agent is used in solvent for the reflux dehydration to obtain the Octocrilene. The molar ratio of iso-octyl cyanoacetate to benzophenone is 1-2 to 1-5. The molar ratio of iso-octyl cyanoacetate to the dehydrating agent is 1-5 to 1-5. A practical Octocrilene preparation method is provided. The product yield is 95 percent and the purity is 99.5 percent.

Description

Technical field: [0001] The invention relates to a preparation method of octocrylene, in particular to a preparation method of cosmetic grade octocrylene. technical background: [0002] Octocrylene, English abbreviation OCR, trade name N-539, is mainly used in daily chemicals and plastic additives as an anti-ultraviolet additive. At present, the methods for industrialized mass production of octocrylene at home and abroad are mainly transesterification and condensation. [0003] The transesterification method uses 2-cyano-3,3-diphenylimino ethyl acrylate and isooctyl alcohol to obtain octocrylene through transesterification under alkaline conditions. The published patent US5047571 on October 10, 1991 introduced the state of the art. After treatment, film evaporation was used to obtain a yield of 97%, and a GC purity of 99.8%. Similarly, there is no market industrialized product for 2-cyano-3,3-diphenylimino ethyl acrylate, and the process cost is relatively high. [0004]...

Claims

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Application Information

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IPC IPC(8): C07C255/41C07C253/30A61K8/40C08K5/315
Inventor 居沈贵薛峰
Owner 南京寒武纪科技有限公司
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