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Preparation method of ultrahigh-sulfonic-acid-density biomass carbon solid acid

A technology of biomass carbon and ultra-high sulfonic acid, which is applied in the preparation of organic compounds, carboxylic acid ester preparation, chemical instruments and methods, etc., and can solve the problems of limited solid acid catalytic performance, low yield, and low content of sulfonic acid groups, etc. question

Active Publication Date: 2017-06-20
HUNAN NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It is currently reported that the sulfonic acid group density of bio-based solid carbon sulfonic acid prepared by the above three methods is generally below 3 mmol / g, and the limited amount of acid limits the improvement of the catalytic performance of this type of solid acid.
[0004] For carbonized monosaccharides, the conditions for direct carbonization of natural biomass are harsher and the process is more complicated, and the yield after general carbonization is low, and the content of sulfonic acid groups after sulfonation is also low

Method used

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  • Preparation method of ultrahigh-sulfonic-acid-density biomass carbon solid acid

Examples

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Effect test

Embodiment 1

[0017] This example is used to illustrate the method for preparing ultra-high sulfonic acid density biomass carbon solid acid by using bamboo powder and the obtained ultra-high sulfonic acid density biomass carbon solid acid.

[0018] (1) Pretreatment: Weigh 6 g of bamboo powder into the lining of a 100 mL crystallization kettle, weigh 3.6 g of ferric chloride and dissolve it in 20 mL of deionized water, add 4 drops of concentrated hydrochloric acid to prevent hydrolysis, add 1.2 g of phenol, Stir with a glass rod to make it evenly mixed, then seal the crystallization kettle and put it in an oven at 60°C for 12 hours;

[0019] (2) Hydrothermal carbonization: In an oven, the crystallization kettle was heated to 150°C, and the reaction time was 9 h. After the reaction, cool down to room temperature naturally, take out the inner lining, wash it twice with deionized water, once with dilute hydrochloric acid, and twice with deionized water, dry the obtained biomass carbon solid at ...

Embodiment 2

[0032] This example is used to illustrate the use of 180 ° C carbonization temperature for the preparation of HBC-SO 3 The impact of H-II.

[0033] (1) Pretreatment: Weigh 6 g of bamboo powder into the lining of a 100 mL crystallization kettle, weigh 3.6 g of ferric chloride and dissolve it in 20 mL of deionized water, add 4 drops of concentrated hydrochloric acid to prevent hydrolysis, add 1.2 g of phenol, Stir with a glass rod to make it evenly mixed, then seal the crystallization kettle and put it in an oven at 60°C for 12 hours;

[0034] (2) Hydrothermal carbonization: In an oven, the crystallization was heated to 180 °C, and the reaction time was 9 h. After the reaction, it was cooled down to room temperature naturally, and the lining was taken out, washed twice with deionized water, once with dilute hydrochloric acid, and twice with deionized water, and dried to obtain 3.2 g of solid carbon material;

[0035] (3) Sulfonation: Take 2 g of the solid carbon material obtai...

Embodiment 3

[0056] This example is used to illustrate that while using ferric chloride, add other Lewis acid catalytic carbonization-sulfonated bamboo powder to prepare HBC-SO 3 H's method.

[0057] (1) Pretreatment: Weigh 6 g of bamboo powder into the lining of a 100 mL crystallization kettle, weigh 3.0 g of ferric chloride and 0.6 g of copper chloride and dissolve them in 20 mL of deionized water, add 4 drops of concentrated hydrochloric acid to prevent hydrolysis , add 1.2g of phenol, stir with a glass rod to make it evenly mixed, then seal the crystallization kettle, put it in a 60°C oven for 12h;

[0058] (2) Hydrothermal carbonization: In an oven, the crystallization was heated to 180 °C, and the reaction time was 9 h. After the reaction, cool down to room temperature naturally, take out the inner lining, wash it twice with deionized water, once with dilute hydrochloric acid, and twice with deionized water, and dry the obtained solid to obtain 3.2 g;

[0059] (3) Sulfonation: Take...

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Abstract

The invention relates to the field of catalytic material synthesis, and discloses a preparation method of ultrahigh-sulfo-group-density biomass carbon solid acid HBC-SO3H and a method for synthesizing dioctyl adipate by catalytic esterification. The preparation method of HBC-SO3H comprises the following steps: carrying out hydrothermal carbonization on wood fiber biomass under the catalytic actions of Lewis acid and phenol, and sulfonating by using concentrated sulfuric acid or fuming sulfuric acid. The preparation method of HBC-SO3H has the advantages of short procedure, mild reaction conditions, low cost, high catalyst yield and low environmental pollution, and is simple to operate. The sulfo-group density of the HBC-SO3H is generally 3 mmol / g or above, and can reach 5 mmol / g at the maximum. When being used for catalyzing the synthesis of dioctyl adipate, the HBC-SO3H has excellent catalytic esterification activity and excellent recoverability and reusability.

Description

technical field [0001] The invention belongs to the field of preparation of novel biomass carbon materials, and in particular relates to an ultra-high sulfonic acid density biomass carbon solid acid catalyst HBC-SO 3 The preparation method of low-temperature hydrothermal carbonization, oleum / concentrated sulfuric acid sulfonation of H, and the use of the HBC-SO 3 H catalyzed esterification method for synthesizing dioctyl adipate. Background technique [0002] With the aggravation of the energy crisis, renewable and pollution-free biomass resources are getting more and more attention from all over the world. Biomass forms carbon materials through various carbonization techniques, among which bio-carbon-based solid sulfonic acid is a new type of high-efficiency solid protonic acid catalyst obtained by introducing sulfonic acid groups on the surface of carbon materials. The advantages of high activity, good selectivity, low corrosion to equipment and good chemical stability m...

Claims

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Application Information

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IPC IPC(8): B01J27/02C07C69/44C07C67/08
CPCB01J27/02C07C67/08C07C69/44
Inventor 伏再辉张荣陈增添张超刘亚纯王云
Owner HUNAN NORMAL UNIVERSITY
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