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Production method of spherical cellulose acetate butyrate

A technology for the production of acetic acid butyric acid and its production method, which is applied in the production field of spherical cellulose acetate butyrate, can solve the problems of poor reaction effect, high viscosity of reaction liquid, poor mixing effect of reaction liquid, etc., so as to improve the mixing effect and product yield High, elegant appearance effect

Inactive Publication Date: 2014-12-10
SICHUAN NITROCELLULOSE CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In addition, in the reaction process of these prior art, the viscosity of the reaction liquid is relatively high, and the mixing effect of the reaction liquid is poor, so that the reaction effect is relatively poor.

Method used

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  • Production method of spherical cellulose acetate butyrate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0057] Prepare spherical cellulose acetate butyrate as follows:

[0058] Put 300g of refined cotton in the activation machine, spray 200g of acetic acid on the refined cotton, and activate it at room temperature for 2 hours; at the same time, mix 1500g of butyric anhydride, 160g of acetic anhydride, and 12g of concentrated sulfuric acid and cool to 0°C; the activated refined cotton Put it into the cooled mixed solution, then add 600mL of dichloromethane, keep the system temperature at 47°C, and acylate for 120min; add 210g of acetic acid aqueous solution with a mass fraction of 60% acetic acid to the acylated solution, hydrolyze for 4 hours, and then add 127g The mass fraction is 15% magnesium acetate aqueous solution; Finally, slowly add 3000mL of 5% dilute acetic acid under the stirring speed of 300r / min, at this moment just precipitate out spherical cellulose acetate butyrate with uniform particle size, then in 80 Maintain at ℃ for 1 hour to evaporate and recover the dichlo...

Embodiment 2

[0061] Prepare spherical cellulose acetate butyrate as follows:

[0062] Put 300g of fluffy wood pulp in the activation machine, spray 200g of acetic acid on the refined cotton, and activate it at room temperature for 2 hours; at the same time, mix 800g of butyric anhydride, 500g of acetic anhydride, and 9g of concentrated sulfuric acid and cool it down to 0°C; Put the good refined cotton into the cooled mixed solution, then add 600mL of ethyl acetate, keep the system temperature at 60°C, and acylate for 120min; Then add 71.7g mass fraction of 20% magnesium acetate aqueous solution to neutralize the sulfuric acid reacted; finally, slowly add 5% dilute acetic acid 3000mL under the stirring speed of 600r / min, at this moment, the precipitate with uniform particle size Spherical cellulose acetate butyrate, and then maintained at 80°C for 1 hour to evaporate and recover the ethyl acetate in the precipitated solution, and the spherical cellulose acetate butyrate gradually hardened; ...

Embodiment 3

[0065] Prepare spherical cellulose acetate butyrate as follows:

[0066]Put 300g of fluffy wood pulp in the activation machine, spray 200g of acetic acid on the refined cotton, and activate it at room temperature for 2 hours; at the same time, mix 1650g of butyric anhydride and 12g of concentrated sulfuric acid and cool to 0°C; the activated refined cotton Put it into the cooled mixed solution, then add 600mL of butyl acetate, keep the system temperature at 45°C, and acylate for 150min; 20% aqueous solution of sodium acetate to neutralize the reacted sulfuric acid; finally, slowly add 3000mL of 5% dilute acetic acid at a stirring speed of 300r / min, at this time, spherical acetate butyrate fibers with uniform particle size are precipitated Then maintain at 80°C for 1 hour to evaporate and recover the ethyl acetate in the precipitated solution, and the spherical cellulose acetate butyrate gradually hardens; then obtain spherical cellulose acetate butyrate with uniform particle s...

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Abstract

The invention belongs to the technical field of organic acid ester cellulose preparation, in particular relates to a production method of spherical cellulose acetate butyrate, and solves the technical problem of low product yield. The production method comprises the following steps: a, treating velvet wood pulp or cellulose acetate grade refined cotton by acetic acid; b, mixing butyric anhydride, acetic anhydride and concentrated sulfuric acid, cooling to obtain cooled mixed liquid, adding the treated velvet wood pulp or cellulose acetate grade refined cotton into the cooled mixed liquid, and adding a solvent for acylation; c, adding hydrolysis liquid into acylation reaction liquid for hydrolysis, and neutralizing; d, precipitating, hardening, performing solid-liquid separation, washing, stewing, and drying to obtain a spherical cellulose acetate butyrate product. According to the method provided by the invention, the apparent viscosity of materials in reaction liquid can be effectively reduced, the mixing effect of the materials can be improved, the reaction performance of the materials can be improved, and the reaction yield of the materials can be increased.

Description

technical field [0001] The invention belongs to the technical field of organic acid ester cellulose production, in particular to a production method of spherical cellulose acetate butyrate. technical background [0002] Cellulose acetate butyrate (CAB for short) has toughness, weather resistance and cold resistance, good electrical insulation, easy processing, and also has excellent moisture resistance, UV resistance, cold resistance, oil resistance, flexibility, transparency, electrical insulation Insulation and other properties, and good compatibility with resins and high boiling point plasticizers, mainly used in leather brighteners, wood coatings, automotive paints, motorcycle paints, plastic thermosetting powder coatings, printing inks, etc. [0003] The preparation method of cellulose acetate butyrate is generally divided into homogeneous method and heterogeneous method. The homogeneous method generally uses ionic liquids such as DMF, DMAC and other organic solvents to...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08B3/18
Inventor 阳洪谭春雷夏晓玉彭欢宋世杰
Owner SICHUAN NITROCELLULOSE CORP
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