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Sulfonated cross-linked chitosan resin type solid acid catalyst and preparation method thereof

A technology of sulfonated cross-linked chitosan and solid acid catalyst, which is applied in the direction of physical/chemical process catalysts, carboxylate preparation, chemical instruments and methods, etc. It can solve the problems of poor mechanical properties and molding properties, and separation of catalysts and reaction liquids Difficulty, limited application range and other problems, to achieve good mechanical properties and thermal stability, effective catalytic active centers, and excellent physical and chemical properties

Inactive Publication Date: 2012-08-01
江苏宜海环保科技工程有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The main disadvantages of this chitosan sulfate catalyst are: 1. poor thermal stability, resulting in limited application range
The maximum use temperature of the catalyst is only 120°C. Above this temperature, the catalyst will be carbonized and deactivated, so it is not suitable for reactions with higher temperatures.
② Low acid capacity, resulting in low catalytic efficiency
③ Poor mechanical properties and formability, only powder products can be used
Due to the small particle size and strong water absorption of the product, on the one hand, it is difficult to filter and wash during preparation; on the other hand, it is difficult to separate the catalyst from the reaction solution after the reaction, which may easily lead to incomplete recovery.

Method used

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  • Sulfonated cross-linked chitosan resin type solid acid catalyst and preparation method thereof
  • Sulfonated cross-linked chitosan resin type solid acid catalyst and preparation method thereof
  • Sulfonated cross-linked chitosan resin type solid acid catalyst and preparation method thereof

Examples

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Effect test

Embodiment 1

[0027] A kind of preparation method of sulfonated cross-linked chitosan resin type solid acid catalyst, the concrete steps of described method are as follows:

[0028] (1) Preparation of cross-linked chitosan

[0029]With commercially available (deacetylation degree ≥ 95%) chitosan as raw material, by the quality (g) of chitosan: the volume (ml) of cross-linking agent (concentration is 100% glutaraldehyde): mass concentration 2% The volume (ml) of dilute hydrochloric acid solution: the ratio of the mass (g) of the calcium carbonate powder of purity 99.0% is the ratio of 1: 0.5: 50: 0.5, chitosan is joined in described dilute hydrochloric acid solution earlier, stir Chitosan dilute hydrochloric acid solution is prepared until chitosan dissolves. Finally, according to the ratio of Tween-80: dilute chitosan hydrochloric acid solution: the volume ratio of liquid paraffin is 1: 400: 400, first add Tween-80 to the paraffin, stir for 7 minutes and then add dilute chitosan under stir...

Embodiment 2

[0033] A kind of preparation method of sulfonated cross-linked chitosan resin type solid acid catalyst, with embodiment 1, wherein:

[0034] In the (1) step, the quality (g) of described chitosan: the volume (ml) of cross-linking agent (concentration is 100% glyoxal): the volume (ml) of the dilute hydrochloric acid solution of mass concentration 2%: The ratio of the calcium carbonate powder mass (g) of purity 99.0% is 1: 0.1: 70: 0.6, according to Tween-80: chitosan dilute hydrochloric acid solution: the volume ratio of liquid paraffin is 1: 500: 480, the Tween The stirring time for adding -80 to paraffin is 5 minutes, and the stirring time for adding chitosan dilute hydrochloric acid solution is 10 minutes. Add the cross-linking agent and the calcium carbonate powder to the dispersion, and continue stirring for 35 minutes. , heating the reaction solution to 65°C, adjusting the pH value of the system to 9, continuing to stir at a constant temperature of 65°C for 2.3h, and lett...

Embodiment 3

[0037] A kind of preparation method of sulfonated cross-linked chitosan resin type solid acid catalyst, with embodiment 1, wherein:

[0038] In the (1) step, the quality (g) of described chitosan: the volume (ml) of linking agent: the volume (ml) of the dilute hydrochloric acid solution of mass concentration 2%: the calcium carbonate powder quality of purity 99.0% ( g) the ratio is the ratio of 1: 0.4: 60: 0.8, according to the ratio of Tween-80: chitosan dilute hydrochloric acid solution: the volume of liquid paraffin is the ratio of 1: 470: 500, Tween-80 is added to the stirring in the paraffin The time is 10min, the stirring time of adding dilute chitosan hydrochloric acid solution is 5min, the reaction solution is heated up to 70°C, and continues to stir for 2h at a constant temperature at 70°C, according to the quality (g) of the filter cake: the mass concentration is The ratio of the volume (ml) of 2% hydrochloric acid solution is 1: 1.5, and the stirring reaction time t...

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Abstract

The invention provides a sulfonated cross-linked chitosan resin type solid acid catalyst and a preparation method thereof, which belong to the technical field of solid acid catalysts of organic reaction. According to the invention, the catalyst is a sulfonated cross-linked chitosan polymer; and according to the method, the method comprises the steps of first preparing cross-linked chitosan by using commercial chitosan as raw material, carrying out sulfonation reaction on the cross-linked chitosan, washing the cross-linked chitosan by using distilled water and drying the cross-linked chitosan to obtain the product. The sulfonated cross-linked chitosan resin type solid acid catalyst provided by the invention has the advantages of simple method, mild reaction condition, low energy consumption and low cost and is beneficial for environmental protection; the prepared product has the advantages of acid capacity of high up to 4.05-4.38 mmol / g, use temperature of high up to 130-150 DEG C, higher catalytic activity and capability of being recycled for multiple times; the method provided by the invention can be widely applied to the preparation of the chitosan resin type solid acid catalyst; and the product prepared by the method provided by the invention can be widely used for the petrochemical industry and the fine chemical industry.

Description

technical field [0001] The invention belongs to the technical field of solid acid catalysts used in organic reactions, and in particular relates to a sulfonated crosslinked chitosan resin type solid acid catalyst and a preparation method thereof. technical background [0002] Solid acid catalysts are widely used in the production process of many petrochemical and fine chemical industries such as hydrocarbon cracking, reforming, isomerization, olefin hydration, alkyd esterification, etc., in the production of resins, coatings, flavors and fragrances, cosmetics, medicine, surface Active agents and other organic products. It overcomes the shortcomings of liquid acid, and has the characteristics of easy separation from the liquid phase reaction system, no corrosion of equipment, simple post-treatment, environmental friendliness, and high selectivity. Among various solid acid catalysts, resin-type solid acid catalysts have the advantages of low activity temperature and good reus...

Claims

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Application Information

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IPC IPC(8): B01J31/06C07C67/08C07C69/704C07C69/14C08B37/08C08J3/24
Inventor 董立春徐玉婷江寒梅唐成黎李俊宏
Owner 江苏宜海环保科技工程有限公司
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