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Method for synthesizing isooctyl salicylate with sodium salicylate

A technology of isooctyl salicylate and a synthesis method, applied in the field of daily chemical industry, can solve the problems of complex catalyst preparation process, unfavorable industrialized production, too long reaction time, etc. The effect of processing simplification

Active Publication Date: 2020-03-17
ANHUI SHENGNUOBEI CHEM TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The second process route is to use methyl salicylate and isooctyl alcohol to carry out transesterification reaction to synthesize isooctyl salicylate, which will produce a large amount of methanol by-product
[0008] Both of these two processes use concentrated sulfuric acid as the traditional esterification catalyst. Although they have the advantages of low catalyst price, good catalytic effect, and mature technology, they also have the characteristics of corroding equipment, polluting the environment, dark product color, and many side reactions.
[0009] In recent years, a lot of research and development have been done on the synthesis process of isooctyl salicylate. Most of the research focuses on exploring new and efficient catalysts to replace the use of concentrated sulfuric acid. The developed catalysts mainly include solid acid, solid super acid, Phosphoric acid, sulfonic acids, HY molecular sieves, and rare earth solid superacids, etc., although higher conversion rates of salicylic acid can be obtained, and catalysts have their own strengths, there are still problems such as high catalyst cost, long reaction time or catalyst preparation. Problems such as complex process are not suitable for industrial production

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  • Method for synthesizing isooctyl salicylate with sodium salicylate
  • Method for synthesizing isooctyl salicylate with sodium salicylate
  • Method for synthesizing isooctyl salicylate with sodium salicylate

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preparation example Construction

[0024] The invention provides a kind of industrial synthesis method of isooctyl salicylate, the method comprises the following steps:

[0025] Step 1, adding chloroisooctane, sodium salicylate and a catalyst into a solvent, heating and reacting to obtain a reaction solution;

[0026] Step 2, post-processing the reaction solution to obtain isooctyl salicylate.

[0027] The present invention is specifically described below.

[0028] Step 1, adding chloroisooctane, sodium salicylate and a catalyst into a solvent, heating and reacting to obtain a reaction liquid.

[0029] The said chloroisooctane, sodium salicylate and catalyst are added into the solvent step by step sequentially. Firstly, after the chloroisooctane is uniformly dissolved in the solvent, then the catalyst is added until the catalyst is completely dissolved to form a homogeneous mixture. After the organic solution, add sodium salicylate solid powder for dispersion.

[0030] The solid-liquid phase reaction system ...

Embodiment 1

[0083] Preparation of sodium salicylate:

[0084] Add 94g of phenol into a four-neck flask, then add 160g of 25% sodium hydroxide aqueous solution to convert phenol into sodium phenate, stir for 0.5h, then add 200g of toluene and raise the temperature to 130°C, and reflux to bring the water out until No water comes out of the water separator.

[0085] The toluene was distilled off under reduced pressure using a water pump to obtain a solid sodium phenate. Then put the sodium phenoxide solid into the autoclave, pass carbon dioxide gas into the autoclave, the reaction temperature is 110°C, and the reaction pressure is 0.8-1Mpa. After 8 hours of reaction, the obtained sodium salicylate solid is directly used in water without purification. Synthesis of isooctyl sylate.

Embodiment 2

[0087] Preparation of chloroisooctane: Add 130.2g of isooctyl alcohol into the reaction vessel, keep the temperature at 2-3°C, add 120.2g of thionyl chloride dropwise under the condition of stirring, and continue the heat preservation reaction for 1h after the dropwise addition. At this time, the mass fraction of isooctyl alcohol was lower than 0.1%, and 145.8 g of chloroisooctane was obtained by vacuum distillation with an oil pump, with a yield of 98%.

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Abstract

The invention provides an industrial synthesis method of isooctyl salicylate. In the method, sodium salicylate and 3-(chloromethyl)heptane are utilized to form a solid-liquid phase reaction system, and the isooctyl salicylate is synthesized in the presence of a catalyst. According to the synthesis method, processes of sodium salicylate acidification and subsequent esterification are simplified, and use of sulfuric acid is greatly reduced, thereby reducing the generation of acidic wastewater. Sodium chloride produced during the process can be automatically precipitated in the reaction system, and the remaining solvent, the catalyst, and the residual small amount of raw materials can be recovered and reused. The post-processing step is simplified, the production of three wastes is reduced, the production cost is reduced, and the need of green clean production can be satisfied.

Description

technical field [0001] The invention belongs to the technical field of daily chemical industry, and in particular relates to a method for synthesizing isooctyl salicylate by solid-liquid phase reaction. Background technique [0002] Isooctyl salicylate, also known as 2-ethylhexyl salicylate, is an important daily chemical product, which can be used as a blending fragrance of soap, perfume, daily cosmetics, organic solvent and organic synthesis intermediate Wait. Isooctyl salicylate can absorb wavelengths near 300nm and has a slight aromatic smell. As one of the most commonly used and effective ultraviolet absorbers at present, it is widely used in sunscreens. The industrial synthesis of isooctyl salicylate mainly uses concentrated sulfuric acid as a catalyst for direct esterification. This method has the disadvantages of dark product color, serious equipment corrosion, and unfavorable clean production. [0003] The current industrialization route mainly utilizes salicylic ...

Claims

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Application Information

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IPC IPC(8): C07C67/11C07C67/54C07C69/84C07C37/66C07C39/235C07C51/15C07C65/10
CPCC07C67/11C07C67/54C07C69/84C07C37/66C07C51/15C07C39/235C07C65/10
Inventor 陈和平徐阳
Owner ANHUI SHENGNUOBEI CHEM TECH