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
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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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