Application of hydrophobic modified solid acid catalyst in acetylation reaction of cellulose acetate

A solid acid catalyst, cellulose acetate technology, applied in molecular sieve catalysts, physical/chemical process catalysts, organic compound/hydride/coordination complex catalysts, etc., can solve problems such as weak interaction, improve efficiency, replace low degree of effect

Active Publication Date: 2022-08-02
NANJING FORESTRY UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Through the interaction analysis, it can be known that the surface property relationship between the solid superacid material and the low-substituted cellulose acetate molecule has a large difference in polarity, which leads to a weak interaction between the two, which makes it difficult for the low-substituted cellulose acetate molecular chain to be in the solid superacid. The surface continues to react

Method used

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  • Application of hydrophobic modified solid acid catalyst in acetylation reaction of cellulose acetate
  • Application of hydrophobic modified solid acid catalyst in acetylation reaction of cellulose acetate
  • Application of hydrophobic modified solid acid catalyst in acetylation reaction of cellulose acetate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment approach

[0037] As an embodiment, the cellulose is pretreated with alkali.

[0038] There are no special requirements for acetylating reagents in this application. On the basis of not violating the inventive concept of this application, any known acetylating reagents suitable for acetylation of cellulose can be used in this application, including but not limited to acetylation reagents. One or more of acid anhydride, acetyl chloride and acetic acid.

[0039] It can be understood that, on the basis of not violating the inventive concept of the present application, any technical solution for carrying out the acetylation reaction by a multi-step reaction method is within the protection scope of the present application.

[0040] There is no special requirement for the type of cellulose in this application, and any known cellulose with industrial value for acetylation reaction can be acetylated by the method of this application.

[0041] Surprisingly, due to the hydrophobicity of the gener...

Embodiment 1

[0044] Preparation of Modified Sulfuric Acid Accelerated Solid Superacid

[0045] Combining concentrated sulfuric acid with carrier TiO 2 Follow SO 4 2- with TiO 2 The mass ratio is 3:100, TiO 2 Mix it with deionized water at a ratio of 0.67g / mL, heat and stir until it becomes viscous; after drying, it is calcined at 450°C for 2h to obtain SO 4 2- / TiO 2 Sulfuric acid-promoted solid super acid. Then, octadecyltrichlorosilane was prepared into anhydrous toluene solution of octadecyltrichlorosilane with a concentration of 10%, and SO was added to the solution according to the amount of 1.0g / mL solid-liquid ratio. 4 2- / TiO 2 The powder was continuously and rapidly stirred at 25 °C; after 1 h, the powder was collected by solid-liquid separation, and then the powder was washed with a large amount of anhydrous toluene, and then dried in an oven to obtain octadecyltrichlorosilane-modified SO 4 2- / TiO 2 Solid super acid. The reaction performance data of the prepared sol...

Embodiment 2

[0058] Preparation of modified sulfuric acid-promoted solid superacid:

[0059] Zirconium oxychloride (ZrOCl 2 ·8H 2 O) (Sinopharm Chemical Reagent) as a zirconium source to prepare Zr(OH) 4 . Zr(OH) 4 ZrO was prepared by calcining at 650℃ for 2h in a muffle furnace 2 , sulfuric acid and ZrO 2 Follow SO 4 2- with ZrO 2 The mass ratio is 3:100, ZrO 2 Mix with deionized water at a ratio of 0.67g / mL, heat and stir until it becomes viscous, dry and calcinate at 450°C for 2h to obtain SO 4 2- / ZrO 2 Sulfuric acid-promoted solid super acid. Then, a 6% vinyltriethoxysilane / ethyl acetate solution was prepared, and SO was added to the mixed solution at a solid-liquid ratio of 0.8 g / mL. 4 2- / ZrO 2 Powder; continuously and stably stirred at 40°C for 12 hours, and the solid samples were separated and collected by suction filtration, rinsed with a large amount of ethyl acetate, and dried to obtain vinyltriethoxysilane-modified SO 4 2- / ZrO 2 .

[0060] Evaluated using t...

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Abstract

The invention relates to application of a solid acid catalyst in acetylation reaction of cellulose acetate. The solid acid catalyst comprises solid acid and a modified group, the modifying group at least has a C1-C20 carbon chain, and the contact angle of the solid acid catalyst to water is 120 degree lt; theta < lt >; by adopting the scheme of the invention, the problems of low cellulose acetylation conversion rate and low reaction yield caused by poor interface bonding force of solid acid and cellulose in the prior art are solved.

Description

technical field [0001] The invention relates to the technical field of acetylation reaction of cellulose acetate, in particular to the application of a solid acid catalyst in the synthesis of cellulose acetate. Background technique [0002] Cellulose acetate is widely used and is a bulk product with great international competitive value. At present, the production of cellulose acetate mainly uses concentrated sulfuric acid as a catalyst. Since the sulfuric acid cannot be separated from the reaction system, a large amount of water resources are consumed in the process, and there are problems of large amount of pollution and high energy consumption, and technical innovation is urgently needed. In response to this problem, people from all walks of life generally hope to use solid super acid to replace liquid sulfuric acid, and the solid super acid and the product system can be effectively separated and recycled, thereby reducing the generation of waste water and simplifying the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/053B01J31/02B01J29/40B01J31/06B01J31/10C08B3/06
CPCB01J27/053B01J31/0274B01J31/0275B01J29/405B01J29/40B01J31/0272B01J31/06B01J31/10B01J23/002C08B3/06B01J2523/00B01J2229/186B01J2523/31B01J2523/47B01J2523/842Y02P20/584
Inventor 李力成索娜佘洁吴臻煜马娜李倩倩李小保
Owner NANJING FORESTRY UNIV
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