Unlock instant, AI-driven research and patent intelligence for your innovation.

Green synthesis method of allyl phenoxyacetate

A green synthesis, pineapple ester technology, applied in chemical instruments and methods, preparation of carboxylate, preparation of organic compounds, etc., can solve the problems of increasing environmental protection pressure and increasing production costs, and achieve low production costs and reduced production costs. , Process green effect

Inactive Publication Date: 2018-03-06
江苏馨瑞香料有限公司
View PDF6 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purification of the product after the second step transesterification needs to neutralize the catalyst and wash with water, which increases the pressure on environmental protection and increases the production cost

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
  • Green synthesis method of allyl phenoxyacetate
  • Green synthesis method of allyl phenoxyacetate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Put 6000kg of methyl cyclohexyl propionate, 4430kg of allyl alcohol and 40kg of p-toluenesulfonic acid into a synthesis kettle to carry out transesterification reaction at 90-100°C. During the reaction, methanol is in a state of partial reflux. Central control sampling When the mass content of methyl cyclohexyl propionate is less than or equal to 5%, methanol and allyl alcohol are removed by atmospheric distillation, and then vacuum distillation is carried out to obtain pineapple ester, and p-toluenesulfonic acid remains in the synthesis kettle and can be used many times . The finished product analysis pineapple ester content is 99.34%,

Embodiment 2

[0017] Put 6650kg of methyl cyclohexyl propionate, 4760kg of allyl alcohol and 50kg of recovered p-toluenesulfonic acid into the tower reactor to carry out transesterification at 100-120°C. When the top temperature of the tower reactor is between 64°C and 70°C, the reflux ratio is 100:1 and the material is discharged until the top temperature of the tower reactor is 70°C, and the reaction ends. Turn on the vacuum pump to make the pressure of the tower reactor ≤ -0.09MPa, raise the temperature so that the temperature of the kettle is 130-150°C to start rectification, and the rectification ends to obtain pineapple ester with a mass content of 99%.

Embodiment 3

[0019] Throwing into industrial grade mass fraction in reactor is 99.4% methyl cyclohexenyl propionate 3400Kg and activated Raney nickel 50Kg, feeds H in the reactor 2 The pressure of the reactor is 5MPa, and the temperature is raised to 130-140°C for reaction, and H is continuously added during the reaction. 2 , so that the pressure in the kettle is maintained at 5±0.2MPa, when the pressure in the kettle is basically unchanged, stop adding H 2 . Stop adding H 2 When the pressure in the rear kettle decreased by no more than 0.1Mpa per hour, a sample was taken for chromatographic analysis. The mass fraction of methyl cyclohexylpropionate was 99.12%. After cooling, the product was weighed to 3517.2Kg, and the yield was 98.3%.

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 provides a green synthesis method of allyl phenoxyacetate. The method comprises the step of carrying out transesterification on the following components in parts by mass: 100 parts of dimethyl cyclohexylmalonate, 50 to 200 parts of allylalkohol, and 0.5 to 5 parts of para-toluenesulfonic acid at the temperature of 90 to 120 DEG C. The green synthesis method of the allyl phenoxyacetate has the advantages of green process and low production cost.

Description

technical field [0001] The invention relates to a production method of pineapple esters, in particular to a green synthesis method of pineapple esters. Background technique [0002] Allyl 3-cyclohexylpropionate, also known as pineapple ester, has a mild pineapple fragrance and is used as a flavoring agent, mainly for the preparation of fruit flavors such as pineapple. Existing pineapple ester production technology is to take the concentrated sulfuric acid as catalyst, carry out esterification reaction with cyclohexyl propionic acid and allyl alcohol. After the synthesis of this method, steps such as water washing and alkali washing are required to improve the product purity, and a large amount of washing waste water is produced which does not meet the environmental protection requirements. The invention patent application publication number is CN85102572A, and the invention title is the patent application for the synthesis of pineapple ester by using 4-vinyl cyclohexene. ,...

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
Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/608C07C67/03C07C67/303C07C67/54
CPCC07C67/03C07C67/303C07C67/54C07C69/608
Inventor 应登宇应思斌赵建标席建忠翁卫栋
Owner 江苏馨瑞香料有限公司