Preparation method of high-acid-content carbon-based solid acid

A technology of carbon-based solid acid and high acid content, which is applied in the preparation of carboxylic acid esters, the preparation of organic compounds, chemical instruments and methods, etc. It can solve the problems of poor thermal stability of carbon materials, low acid strength, and limited acid content. Achieve the effect of simple equipment, easy process, and extended industrial chain

Inactive Publication Date: 2012-10-10
TAIYUAN UNIV OF TECH
View PDF6 Cites 9 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this route can only use the limited surface hydroxyl groups produced by carbonization to interact with concentrated sulfuric acid to introduce sulfonic acid groups, that is, the amount of acid is limited by the number of surface groups.
The higher the carbonization temperature, the fewer the number o...

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

Examples

Experimental program
Comparison scheme
Effect test

Embodiment approach 1

[0017] Take 20g of medium-temperature coal tar pitch, add 40ml of xylene, stir to dissolve, then add 50g of trichloroacetic acid and 60ml of 30% H 2 o 2 , ultrasonicated for 50 minutes at a temperature of 80°C, filtered and dried to obtain chlorinated coal tar pitch containing 20 wt% chlorine; then pulverized the chlorinated coal tar pitch, sieved 200 mesh (74 microns), and put it into a beaker , add 100g of concentrated sulfuric acid, place it in a heat-conducting oil bath, control the reaction temperature to 165°C, react for 12 hours, cool to room temperature, filter with a sand core funnel, and then wash the sulfonated product with distilled water until the pH of the filtrate is neutral In order to obtain a solid acid with a surface acid content of 7.3 mmol / g, it was dried in a drying oven at 110°C for 4 hours.

Embodiment approach 2

[0019] Take 20g of high-temperature coal tar pitch, add 60ml of xylene, stir to dissolve, then add 60g of dichloroacetic acid and 80ml of 30% H 2 o 2 , ultrasonicated for 60 minutes at a temperature of 90°C, filtered and dried to obtain chlorinated coal tar pitch containing 18.6 wt% chlorine; then crushed chlorinated coal tar pitch, sieved to 200 mesh (74 microns), and put into a beaker , add 172g of concentrated sulfuric acid, place it in a heat-conducting oil bath, control the reaction temperature to 170°C, react for 12 hours, cool to room temperature, filter with a sand core funnel, and then wash the sulfonated product with distilled water until the pH of the filtrate is neutral In order to obtain a solid acid with a surface acid content of 7.5 mmol / g, it was dried in a drying oven at 110°C for 4 hours.

Embodiment approach 3

[0021] Take 20g of high-temperature coal tar pitch, add 80ml of xylene, stir to dissolve, then add 50g of monochloroacetic acid and 100ml of 30% H 2 o 2 , ultrasonicated for 40 minutes at a temperature of 70°C, filtered and dried to obtain chlorinated coal tar pitch with a chlorine content of 19.5 wt%; then pulverized the chlorinated coal tar pitch, sieved to 200 mesh (74 microns), and put it into a beaker , add 149.0g concentrated sulfuric acid, place it in a heat conduction oil bath, control the reaction temperature to 170°C, react for 12 hours, cool to room temperature, filter with a sand core funnel, and then wash the sulfonated product with distilled water until the pH of the filtrate is Neutral, placed in a drying oven at 110 ° C for 4 hours to obtain a solid acid with a surface acid content of 7.3 mmol / g.

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 relates to a preparation method of high-acid-content carbon-based solid acid, which comprises the steps of: firstly oxidizing coal tar pitch by using hydrogen peroxide under the effect of ultrasonic waves, using chloroacetic acid as chlorinating agent, introducing chlorine atoms in benzene ring structures of aromatic compounds through reaction and sulphonating the aromatic compounds to introduce more sulfonic acid groups, so as to increase carbon-based surface acid content, improve acid strength and enhance acid catalytic capability. Since the solid acid is prepared by introducing high-content sulfonic acid groups at more active sites which are provided by the chlorine atoms and can be substituted by the sulfonic acid groups and by fully using the characteristic that the major components, i.e. large ring aromatic compounds in the coal tar pitch are sulphonated, the esterification rate of ethanol and acetic acid esterification reaction can reach 87 percent, the esterification rate is not decreased after the solid acid is repetitively used for five times, the acid content of the solid acid is two times of the acid content of solid acid reported by open literature, and the solid acid has the characteristics of high acid content, acid and alkali resistance and high thermal stability.

Description

technical field [0001] The invention relates to a method for preparing a carbon-based solid acid, especially a method of using coal tar pitch as a raw material, oxidizing and pretreating by adding oxidant hydrogen peroxide under the assistance of ultrasonic waves, and then chlorinating to make the chlorine content reach 18-20wt%. Grinding, sieving, and then sulfonating the target product. The method improves the degree of sulfonation and the amount of surface acid through advance chlorination treatment, thereby improving the acid strength and thermal stability, and expanding the application range of the prepared solid acid. technical background [0002] The efficient utilization of resources and the development of environment-friendly catalysts have become one of the important goals pursued by many scientists in the world today. Acids are widely used as catalysts for many reactions, such as alkyd esterification, bio-oil preparation, cyclohexanone oxime to caprolactam, etc. ...

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): B01J31/02C07C67/08C07C69/14
Inventor 曹青靳利娥解小玲张怀平俞蕙
Owner TAIYUAN UNIV OF TECH
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