Method of preparing Octocrilene

A technology of dehydrating agent and catalyst, which is applied in the field of octocrylene preparation, can solve problems such as low yield, octocrylene cannot meet the technical requirements for the manufacture of anti-ultraviolet additives, environmental pollution, etc., and achieve simple treatment and convenient production Effects on operation, ergonomics and energy utilization

Inactive Publication Date: 2012-09-19
南京寒武纪科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • 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-ultraviolet additives, secondly to solve the technical problem of low yield, and thirdly to solve the problem of environmental pollution and provide A kind of preparation method of octocrylene with high purity and low luster

Method used

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  • Method of preparing Octocrilene

Examples

Experimental program
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Effect test

Embodiment 1

[0026] Add 364g (2.0mol) of benzophenone, 400g (2.0mol) of isooctyl cyanoacetate, 600ml of n-hexane, 247g (2.4mol) of acetic anhydride and 10g of ammonium acetate into a 2L four-necked flask, and install the water separator. Slowly raise the temperature to 85°C for reflux, separate the acetic acid-water-n-hexane solution, and reflux the n-hexane into the reaction system. GC online analysis of isooctyl cyanoacetate content is less than 0.5%, stop the reaction.

[0027] Cool down to room temperature, add cold water, stir for 30 minutes, statically separate the lower aqueous layer containing acetic acid-ammonium acetate, neutralize with ammonia water to pH 7, and concentrate to dryness to obtain ammonium acetate as a by-product. (The claim is heating and vacuum concentration, so how much degree 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 is concentrated to recover n-he...

Embodiment 2

[0029] Add 509.6g (2.8mol) of benzophenone, 400g (2.0mol) of isooctyl cyanoacetate, 600ml of n-hexane, 247g (2.4mol) of acetic anhydride and 10g of ammonium acetate into a 2L four-necked flask, and install the water separator. Slowly raise the temperature to 85°C for reflux, separate the acetic acid-water-n-hexane solution, and reflux the n-hexane into the reaction system. GC online analysis of isooctyl cyanoacetate content is less than 0.5%, stop the reaction.

[0030] Cool down to room temperature, add cold water, stir for 30 minutes, statically separate the lower aqueous layer containing acetic acid-ammonium acetate, neutralize with ammonia water to pH 7-8, concentrate to dryness, and obtain ammonium acetate as a by-product. The oil layer was concentrated to recover n-hexane, and the concentrated solution was distilled under reduced pressure. Collection: 180-190°C / 0.1mmHg, to obtain 685.9g of light yellow viscous oily liquid with a yield of 95% and a purity of 99.5% (GC). ...

Embodiment 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-necked flask, and install the water separator. Slowly raise the temperature to 85°C for reflux, separate the acetic acid-water-n-hexane solution, and reflux the n-hexane into the reaction system. GC online analysis of isooctyl cyanoacetate content is less than 0.5%, stop the reaction.

[0033] Cool down to room temperature, add cold water, stir for 30 minutes, statically separate the lower aqueous layer containing acetic acid-ammonium acetate, neutralize with ammonia water to pH 7, and concentrate to dryness to obtain ammonium acetate as a by-product. The oil layer was concentrated to recover cyclohexane, and the concentrated solution was distilled under reduced pressure, collected at 180-190°C / 0.1mmHg to obtain 655g of a light yellow viscous oily liquid with a yield of 90.7% and a purity of 99.5% (GC)...

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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 is1-5 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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Patent Type & Authority Patents(China)
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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