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Method for preparing solid sulfonic acid from reproducible vegetable material

A solid and sulfonic acid technology, which is applied in chemical instruments and methods, chemical/physical processes, physical/chemical process catalysts, etc., can solve problems such as limited production and application, and achieve improved resource utilization, less energy consumption, and slow down energy consumption. The effect of the crisis

Inactive Publication Date: 2007-02-21
HUNAN NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In the situation of increasingly scarce energy, this shortcoming will limit their future production and application

Method used

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  • Method for preparing solid sulfonic acid from reproducible vegetable material
  • Method for preparing solid sulfonic acid from reproducible vegetable material

Examples

Experimental program
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Effect test

Embodiment 1

[0017] Embodiment 1: Get 4.0kg of sawn bamboo chips, dry, add 12.64kg of 95% sulfuric acid solution, stir, 60 ℃ of constant temperature reaction 3h, wash with deionized water after cooling until the filtrate is neutral, dry, obtain bamboo charcoal 1.39kg. Bamboo charcoal 1.0kg, add 10kg of 50% (mass percentage) chlorosulfonic acid, sulfonate at a constant temperature of 100°C for 2h, add deionized water to terminate the reaction, wash until the filtrate is neutral, wash with BaCl 2 There was no precipitation in the solution detection, and bamboo charcoal sulfonic acid was obtained by drying at 100°C, and the acid content was 2.0mmolg by titration -1 .

Embodiment 2

[0018] Example 2: Get 4.0kg of sawdust, add 42.7kg of 75% (mass percent) sulfuric acid, control the carbonization temperature at 80°C, stir and react at a constant temperature for 3h, add deionized water to wash until the filtrate is neutral after cooling, and dry to obtain sawdust. Charcoal 1.42kg. Take 1.0kg of sawn charcoal, add concentrated sulfuric acid at a mass ratio of 7:1, sulfonate at 120°C for 2 hours, add deionized water to terminate the reaction, wash until the filtrate is neutral, and wash with BaCl 2 The solution detected no precipitation, and dried at 100° C. to obtain 1.33 kg of saw charcoal sulfonic acid. The amount of sulfonic acid obtained by titration is 1.82mmol g -1 .

Embodiment 3

[0019] Embodiment 3: Take 4.0 kg of absorbent cotton, add 40.0 kg of 80% (mass percentage) sulfuric acid, control the carbonization temperature at 100 ° C, stir and react at a constant temperature for 1 hour, wash with deionized water after cooling until the filtrate is neutral, and dry to obtain cotton charcoal 1.58kg. Take 1.0kg of cotton charcoal, add 50% (mass percent) oleum at a mass ratio of 5:1, sulfonate at 80°C for 2 hours, add deionized water to terminate the reaction, wash until the filtrate is neutral, wash with BaCl 2 The solution detected no precipitation. Dry at 100° C. to obtain 1.10 kg of cotton-based sulfonic acid. The amount of cotton carbonyl sulfonic acid obtained by titration is 2.28mmol g -1 .

[0020] The obtained product cotton charcoal sulfonic acid is identified by FT-IR and XPS as a solid sulfonic acid containing sulfonic acid groups.

[0021] From the gained Cottonyl Sulfonic Acid FT-IR collection of spectra, it can be seen that ( figure 1 ): ...

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Abstract

A process for preparing solid sulfonic acid from the regeneratable vegetative raw material, such as wood bits and bamboobits, includes such steps as drying the vegetative raw material containing cellulose and lignin, breaking, proportionally mixing it with sulfuric acid, stirring at 40-200 deg.C for 1-20 hr, cooling, washing with deionized water until it becomes neutral, baking, proportionally adding sulfonating agent, sulfonating at 30-150 deg.C for 1-20 hr, cooling, washing with deionized water until it becomes neutral, testing no deposition in BaCl2 solution, and baking.

Description

technical field [0001] The invention belongs to a preparation method of a catalyst, in particular to a preparation method of solid sulfonic acid. Background technique [0002] As a strong protic acid catalyst, sulfonic acid is widely used in various acid-catalyzed reactions such as esterification, etherification, dehydration, hydration, and isomerization. [0003] Common solid sulfonic acid catalysts include p-toluenesulfonic acid, sulfamic acid, sulfonic acid resin, etc. In organic reactions, p-toluenesulfonic acid and sulfamic acid catalysts, especially in the presence of water, both dissolve to a certain extent and become liquid acid catalysts. Although liquid sulfonic acid has high acid strength and high reactivity, it is difficult to separate and corrode. strong, environmental pollution and other shortcomings. Sulfonic acid resin is difficult to withstand high temperature, and it is easy to break and lose under long-term stirring. In recent years, some people have in...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/053B01J21/18
Inventor 尹笃林徐琼毛丽秋兰支利王季惠王艺娟张锋
Owner HUNAN NORMAL UNIVERSITY
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