Solid superacid catalyst and method for preparing iso-octyl p-methoxycinnamate by using same

A technology of methoxycinnamic acid and solid superacid, which is applied in the preparation of carboxylic acid esters, chemical instruments and methods, and the preparation of organic compounds. It can solve the problems of complicated synthesis methods and waste water generation, and achieve easy recycling and increase Effects of specific surface area and enriched mesoporous structure

Pending Publication Date: 2022-02-11
WANHUA CHEM GRP CO LTD
View PDF9 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The synthetic method is complicated, and a large amount of waste water is produced

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
  • Solid superacid catalyst and method for preparing iso-octyl p-methoxycinnamate by using same

Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0032] Specifically, a preparation method of isooctyl p-methoxycinnamate comprises the following steps:

[0033] Under normal pressure, add a certain amount of p-methoxybenzoic acid, isooctyl alcohol, alkane compound and catalyst X-SO 4 2- / Cr 2 o 3 -SiO 2 , heat up to a certain temperature for heat preservation reaction, reflux and water separation, after the reaction, remove the catalyst X-SO by filtration 4 2- / Cr 2 o 3 -SiO 2 , successively add saturated sodium carbonate solution and distilled water to wash until the solution becomes neutral, remove the solvent and excess isooctyl alcohol, and rectify to obtain isooctyl p-methoxycinnamate.

[0034] Wherein, the molar ratio of p-methoxybenzoic acid to isooctyl alcohol is 1.0-4.0:1, for example including but not limited to 1:1, 1.5:1, 2:1, 2.5:1, 3:1, 3.5 :1,4:1, preferably 1.5-2.0:1; the alkane solvent is selected from at least any one of n-pentane, isopentane, n-hexane, cyclohexane, dodecane, preferably cyclohexan...

Embodiment 1

[0052] 1) Preparation of X-SO 4 2 - / Cr 2 o 3 -SiO 2 catalyst:

[0053] Add 0.35g graphene (0.07wt%) to 500g deionized water, add 80% sulfuric acid to adjust pH to 3, then add 8.75g (25 times of graphene quality) chromium picolinate (with Cr 2 o 3 In terms of), add 4.375g ethyl orthosilicate (as SiO 2 In terms of), the amount added is the mass of chromium (in terms of Cr 2 o 350wt% of total), the temperature was adjusted to 60°C, and the hydrolysis reaction was carried out for 3 hours; then the precipitate obtained in the above hydrolysis reaction was filtered to obtain a catalyst precursor, which was dried and immersed in 120mL of 0.7mol / L sulfuric acid for 1.8h (solid-liquid Ratio is 10mL sulfuric acid / 1g solid), after centrifugal drying, equal volume is placed in 4wt% Ti(NO 3 ) 4 solution, soaked for 4 hours; finally, the impregnated solid was filtered and washed, then placed in an air roaster for roasting, the roasting condition was 700 ° C, and the time was 8 hou...

Embodiment 2

[0057] 1) Preparation of X-SO 4 2 - / Cr 2 o 3 -SiO 2 catalyst:

[0058] Add 0.35g graphene (0.07wt%) to 500g deionized water, add 80% sulfuric acid to adjust pH to 3, then add 8.75g (25 times of graphene quality) chromium picolinate (with Cr 2 o 3 In terms of), add 4.375g ethyl orthosilicate (as SiO 2 In terms of), the amount added is the mass of chromium (in terms of Cr 2 o 3 50wt% of total), the temperature was adjusted to 60°C, and the hydrolysis reaction was carried out for 3 hours; then the precipitate obtained in the above hydrolysis reaction was filtered to obtain a catalyst precursor, which was dried and immersed in 120mL of 0.7mol / L sulfuric acid for 1.8h (solid-liquid Ratio is 10mL sulfuric acid / 1g solid), after centrifugal drying, equal volume is placed in 4wt% Ti(NO 3 ) 4 solution, soaked for 4 hours; finally, the impregnated solid was filtered and washed, then placed in an air roaster for roasting, the roasting condition was 700 ° C, and the time was 8 ho...

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 solid superacid catalyst and a method for preparing iso-octyl p-methoxycinnamate by using the solid superacid catalyst. The method is characterized in that iso-octyl p-methoxycinnamate is prepared by taking p-methoxycinnamic acid and isooctanol as raw materials and an alkane compound as a solvent under the action of the solid superacid catalyst, wherein the catalyst is an X-SO4 < 2-> / Cr2O3-SiO2 solid superacid which is prepared by taking Cr2O3-SiO2 as a composite carrier, graphene as a hard template and sulfuric acid as a sulfur source through transition metal X modification. The solid acid catalyst used in the method not only reduces the reaction temperature, but also improves the conversion rate and selectivity of the p-methoxycinnamic acid; and after transition metal modification, the strength of the catalyst is greatly improved, and the service life of the catalyst is greatly prolonged.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, and in particular relates to a solid superacid catalyst and a method for preparing isooctyl p-methoxycinnamate with it. Background technique [0002] The human body is exposed to ultraviolet radiation for a long time without taking effective protective measures, which will cause different degrees of damage to the skin, such as: erythema, skin pigmentation, skin tumors, and skin photoaging. It has become a global consensus to take active and effective protective measures to reduce the disease burden caused by overexposure. [0003] The sunscreen absorbs isooctyl methoxycinnamate at 290-320nm, has a high absorption rate, has good solubility in lipophilic materials, is easy to use, has no irritation to the skin, and is safe. It is almost an ideal sunscreen. Sunscreen, its structure is as follows: [0004] [0005] At present, there are many synthesis methods of isooctyl p-methoxycinna...

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): B01J27/053C07C67/08C07C69/734
CPCB01J27/053C07C67/08C07C69/734Y02P20/584
Inventor 刘连才郭云峰姜鹏张德旸张永振
Owner WANHUA CHEM GRP CO LTD
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

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

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap