Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Preparation method of isooctyl salicylate

A technology of isooctyl salicylate and methyl salicylate, which is applied in the field of compound preparation, can solve problems such as high reaction temperature and limited economic benefits, and achieve the effects of high purity, improved economic benefits, and low production cost

Active Publication Date: 2012-11-14
江苏普源化工有限公司 +1
View PDF5 Cites 4 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There is still a small amount of methyl salicylate at the end of this method reaction, and its reason is that sodium methylate can attack the carbocation of salicylic acid parent as a kind of strong nucleophile, causes there to be a reaction balance in transesterification reaction, methyl salicylate Esters cannot be completely converted to isooctyl salicylate
And this method reaction temperature is higher, and economic benefit is subject to certain restriction in industrialized production

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Preparation method of isooctyl salicylate

Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0020] A kind of preparation method of isooctyl salicylate of the present invention comprises the following steps:

[0021] In the first step, add isooctyl alcohol solution with a purity of 70% to 99.9% to the methyl salicylate solution with a purity of 70% to 99.9%, and methyl salicylate and isooctyl in the methyl salicylate solution The molar ratio of isooctyl alcohol in the alcohol solution is 1:1-1:3, and the mixture is stirred for 1-3 hours to form a uniformly mixed raw material solution.

[0022] As preferably, in the first step, the molar ratio of the methyl salicylate in the methyl salicylate solution to the isooctyl alcohol in the isooctyl alcohol solution is 1:2.

[0023] In the second step, a solid inorganic base catalyst is added to the raw material solution prepared in the first step, and the mass of the inorganic base catalyst is 0.2%-1.0% of the mass of the raw material solution to form a reaction solution.

[0024] In the second step, the inorganic base cataly...

Embodiment 1

[0031] Add 20 mL of 99.9% pure methyl salicylate solution and 40 mL of 99.9% pure isooctyl alcohol solution into a 150 mL three-necked bottle, stir for 1 hour, and form a uniformly mixed raw material solution after stirring. Add 0.3 g of NaOH to the raw material solution to form a reaction solution; and install a distillation head, a condenser tube, a tail joint tube and a receiving bottle on the three-necked flask respectively. Heat the reaction solution to 150°C, stir and react for 10 hours, recover the methanol in the receiving bottle, cool the three-necked flask to 80°C, wash the reaction solution twice with 100°C hot water, separate and extract the organic phase. with anhydrous Na 2 SO 4 Dry the organic phase and remove the Na in the organic phase after standing for 8 hours 2 SO 4 . Carry out oil pump decompression distillation: first use the oil pump to remove the foreboiler isooctyl alcohol in the organic phase, then heat the container containing the organic phase t...

Embodiment 2

[0038] Add 40 mL of methyl salicylate solution with a purity of 70% and 80 mL of iso-octanol solution with a purity of 85% into a 250 mL three-necked bottle, stir for 3 hours, and form a uniformly mixed raw material solution after stirring. Add 0.6 g of NaOH to the raw material solution to form a reaction solution; and install a distillation head, a condenser tube, a tail joint tube and a receiving bottle on the three-necked flask. Heat the reaction solution to 100°C, stir and react for 4 hours, recover the methanol in the receiving bottle, cool the three-necked flask to 20°C, wash the reaction solution three times with hot water at 50°C, separate and extract the organic phase. with anhydrous Na 2 SO 4 Dry the organic phase and remove the Na in the organic phase after standing for 12 hours 2 SO 4 . Carry out oil pump decompression distillation: first use the oil pump to remove the foreboiler isooctyl alcohol in the organic phase, then heat the container containing the orga...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention discloses a preparation method of isooctyl salicylate, which comprises the following steps: 1. adding an isooctyl alcohol solution into a methyl salicylate solution, and stirring for 1-3 hours to form a raw material solution; 2. adding an inorganic alkali catalyst into the raw material solution to form a reaction solution; 3. heating the reaction solution to 100-200 DEG C, stirring to react for 4-10 hours, cooling the reaction solution to 20-80 DEG C, washing the reaction solution with 50-100 DEG C hot water, separating, and extracting an organic phase; and 4. adding anhydrous Na2SO4 into the organic phase to dry the organic phase, standing, removing the Na2SO4 in the organic phase, adding the organic phase into a flask, carrying out vacuum distillation with an oil pump, and collecting the 174-178 DEG C / 1.0kPa fraction which is the isooctyl salicylate. The isooctyl salicylate prepared by the preparation method disclosed by the invention has the advantages of high recovery rate, high purity and low preparation cost.

Description

technical field [0001] The present invention relates to a kind of preparation method of compound, specifically, relate to a kind of preparation method of isooctyl salicylate. Background technique [0002] 2-Hydroxy-benzoic acid (2-ethylpentyl) ester (isooctyl salicylate) chemical formula is as follows: [0003] [0004] Isooctyl salicylate (also known as 2-ethylpentyl salicylate) is an important chemical product. It is a colorless to pale yellow transparent liquid with a slightly aromatic smell. It is resistant to UVB (Chinese: outdoor Ultraviolet rays) have absorption and are widely used in perfume, soap, sunscreen cosmetics, and pharmaceutical industries. They can also be used as organic solvents and organic synthesis intermediates. At present, my country mainly relies on imports. [0005] The industrial synthesis of isooctyl salicylate mainly uses salicylic acid as raw material, and concentrated sulfuric acid is used as a catalyst for direct esterification. This method...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
IPC IPC(8): C07C69/84C07C67/03
Inventor 孙柏旺王燕徐冰左荣林
Owner 江苏普源化工有限公司
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com