Method for preparing organic cellulose acid ester by solid acid catalysts

A solid acid catalyst and organic acid ester technology, which is applied in the field of preparing a series of cellulose organic acid esters, can solve the problems of catalyst corrosion to equipment, difficult separation and recovery of catalyst, and large environmental impact, so as to reduce equipment investment and operating costs, No environmental pollution, environmentally friendly effect

Inactive Publication Date: 2012-06-20
CHANGMAO BIOCHEMICAL ENG CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to use solid acid instead of concentrated sulfuric acid as a catalyst to prepare cellulose organic acid esters in view of the shortcomings of the existi

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Weigh 10.7gZrOCl 2 ·8H 2 O (or Zr(NO 3 ) 4 ·5H 2 O) Dissolve in 100mL distilled water, under vigorous stirring, add ammonia water (25-28%) drop by drop to pH=8-10, age at 0°C for 24 hours, transfer the aged liquid to the Seal in a lined autoclave, conduct hydrothermal treatment at 110°C for 24 hours, suction filter after cooling, and wash the filter cake with deionized water until there is no Cl - (or NO 3 - ), dried and ground with 1mol / L H 2 SO 4 Immerse for 4 hours and bake at 500°C for 3 hours to get SO 4 2- / ZrO 2 solid acid catalyst.

[0026] Weigh 10.0g of cellulose, add 125.0g of acetic acid and 6.5g of propionic acid mixed solution, activate at 50°C for 1 hour, filter with suction, filter cake, reaction solution and 0.3g of the above SO 4 2- / ZrO 2 The solid acid catalysts were all cooled in an ice-water bath for 0.5 hour, wherein the reaction solution was a mixture of 129.0 g acetic acid, 27.0 g propionic acid, 19.0 g acetic anhydride, and 72.0 g...

Embodiment 2

[0028] Weigh 4.2gZr(NO 3 ) 4 ·5H 2 O was dissolved in 60 mL of distilled water, and 4.0 g of Al was added 2 o 3 , under vigorous stirring, add ammonia water (25-28%) drop by drop to pH = 9, and the prepared precipitate is washed with deionized water until no NO 3 - , after drying and grinding, use 1mol / L H 2 SO 4 Immerse for 6 hours and bake at 500°C for 2 hours to get SO 4 2- / ZrO 2 -Al 2 o 3 solid acid catalyst.

[0029] Weigh 10.0g of cellulose, add 100.0g of acetic acid, activate at 30°C for 12 hours, filter with suction, filter cake, reaction solution and 0.2g of the above SO 4 2- / ZrO 2 -Al 2 o 3 The solid acid catalysts were all cooled in an ice-water bath for 1 hour, wherein the reaction solution was a mixture of 139.0 g acetic acid and 19.0 g acetic anhydride, which was esterified at 40 ° C for 3 hours, centrifuged, precipitated, filtered, washed, and dried to obtain The product cellulose acetate is 16.9g, and the acetyl group content is 43.0%.

Embodiment 3

[0031] 4.0g of dry wood powder was placed in a tubular resistance furnace, and carbonized at a constant temperature of 400°C for 1 hour under the protection of nitrogen. The obtained dark brown solid product was cooled and ground into powder; Concentrated sulfuric acid, sulfonate at 150°C for 1 hour, then cool naturally to room temperature; slowly add the mixture to distilled water, stir, stand, and filter, wash the filter cake with boiling distilled water until the pH is about 7, and dry at 105°C to obtain Biomass charcoal-based solid acid catalyst.

[0032] Weigh 10.0g of cellulose, add 120.0g of acetic acid and 6.5g of butyric acid mixture, activate at 50°C for 1 hour, filter with suction, and cool the filter cake, reaction solution and 0.3g of the above-mentioned biomass carbon-based solid acid catalyst in an ice-water bath 0.5 hours, wherein the reaction solution is a mixture of 129.0g acetic acid, 27.0g butyric acid, 12.0g acetic anhydride, and 36.0g butyric anhydride, e...

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Abstract

The invention discloses a method for preparing organic cellulose acid ester by solid acid catalysts, relating to the technical field for preparing organic cellulose acid ester. In the invention, the organic cellulose acid ester refers to cellulose formic acid, cellulose acetate, cellulose propionate, cellulose acetate butyrate, cellulose acetate propionate, cellulose acetate butyrate and cellulose acetate propionate butyrate. Three solid acids, namely, SO42-/MxOy solid acid, biomass carbon-based solid acid, phosphorus-aluminum molecular sieve solid acid; the organic acid is used as solvent and the organic acid anhydride is used as esterifying agent; the using amount of the catalyst is 0.01-5% of the reaction liquid; the organic cellulose acid ester is prepared under the conditions that the reaction temperature is 15-90 DEG C and the reaction time is 0.5-72 h. The method adopts the novel environment-friendly solid acid catalyst; the obtained product has good quality; the catalyst is easy to separate, recover and recycle; no device corrosion exists and the environment is protected.

Description

technical field [0001] The present invention prepares the technical field of cellulose organic acid ester, specifically refers to taking cellulose as raw material, SO 4 2- / M x o y A series of cellulose organic acid esters were prepared using type solid acid, biomass charcoal-based solid acid, and phosphorus-aluminum molecular sieve solid acid as catalysts. Background technique [0002] Cellulose organic acid esters are a series of products prepared by esterification of cellulose with organic acids and organic anhydrides in the presence of catalysts. Mainly used as film, X-ray film, rayon, auto parts, toys, tools and packaging. Among them, cellulose acetate is currently the most widely used cellulose derivative; cellulose propionate has high toughness and rigidity, and is mainly used in automotive decorations and electronic and electrical industrial accessories; cellulose acetate propionate has good air permeability It is widely used in petroleum, food, paint, film and ...

Claims

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Application Information

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IPC IPC(8): C08B3/02C08B3/04C08B3/06C08B3/08C08B3/16C08B3/18
Inventor 冷一欣李园园芮新生黄春香
Owner CHANGMAO BIOCHEMICAL ENG CO LTD
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