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Process for producing hydroxy propyl cellulose with high substitution degree

A technology of hydroxypropyl and cellulose, which is applied in the field of producing highly substituted hydroxypropyl cellulose, can solve the problems of high concentration of propylene oxide, difficult control of side reactions, and difficult purification of by-products, etc., so as to improve the quality Stability, improving labor efficiency and production safety, and reducing labor intensity

Inactive Publication Date: 2014-05-07
邸勇
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] At present, the domestic preparation of hydroxypropyl cellulose is all one-step process, using natural refined cellulose under the action of solvent and alkali, adding a sufficient amount of propylene oxide at one time, and reacting in stages, the concentration of propylene oxide in the system is relatively high , the side reaction is severe and difficult to control, and a large amount of by-products are produced, which is not easy to purify in the later stage

Method used

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  • Process for producing hydroxy propyl cellulose with high substitution degree

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] 1) Pulverization: Unpack 600 parts by mass of natural refined cellulose, pulverize it with a rotary knife pulverizer, and separate it through a cyclone separator to reach 0.03-0.15mm (about 80 meshes). ;

[0038] 2) Alkalinization: Add 8500 parts by mass of benzene solvent and 2000 parts by mass of ethanol solvent into the reaction kettle, start the mixer to stir, add 120 parts by mass of caustic soda, heat up to 60°C to alkalize, after the alkalizes , cool down to normal temperature, add the pulverized refined cellulose prepared in step 1), and alkalize at 20°C for 1 hour;

[0039] 3) Reaction: Add 1200 parts by mass of propylene oxide to the reactor, and the reaction is carried out in two steps:

[0040] In the first step, 55% propylene oxide is added to the reaction kettle. The reaction is divided into two stages. The reaction temperature of the first stage is 50°C, and the reaction time is 2 hours. The reaction temperature of the second stage is 75°C. The reactio...

Embodiment 2

[0049] 1) Pulverization: Unpack 600 parts by mass of natural refined cellulose, pulverize it with a rotary knife pulverizer, and separate it through a cyclone separator to reach 0.03-0.15mm (about 80 meshes). ;

[0050] 2) Alkalinization: Add 8500 parts by mass of toluene solvent and 1500 parts by mass of isopropanol solvent into the reaction kettle, start the mixer to stir, add 150 parts by mass of caustic soda, and heat up to 78°C to alkalize and alkalize After the end, cool down to normal temperature, add the pulverized refined cellulose prepared in step 1), and alkalize at 30°C for 0.8 hours;

[0051] 3) Reaction: Add 1500 parts by mass of propylene oxide to the reaction kettle, and the reaction is carried out in two steps:

[0052] In the first step, 40% propylene oxide is added to the reaction kettle. The reaction is divided into two stages. The reaction temperature of the first stage is 55°C, and the reaction time is 3 hours. The reaction temperature of the second sta...

Embodiment 3

[0061] 1) Pulverization: Unpack 600 parts by mass of natural refined cellulose, pulverize it with a rotary knife pulverizer, and separate it through a cyclone separator to reach 0.03-0.15mm (about 80 meshes). ;

[0062] 2) Alkalinization: Add 9000 parts by mass of xylene solvent and 1500 parts by mass of n-propanol solvent into the reaction kettle, start the mixer to stir, add 180 parts by mass of caustic soda, heat up to 70°C to catalyze the alkali, and After the alkali is finished, cool down to normal temperature, add the pulverized refined cellulose prepared in step 1), and alkalize at 25°C for 0.5 hours;

[0063] 3) Reaction: Add 1800 parts by mass of propylene oxide to the reactor, and the reaction is carried out in two steps:

[0064] In the first step, 50% propylene oxide is added to the reaction kettle. The reaction is divided into two stages. The reaction temperature of the first stage is 50°C, and the reaction time is 4 hours. The reaction temperature of the second...

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Abstract

The invention discloses a process for producing hydroxy propyl cellulose with high substitution degree, which relates to the field of fine chemistry. Natural refined cellulose is alkalified through the action of a binary composite solvent and alkali, epoxy propane is added in twice according to the requirement of the substitution degree, the reaction is performed in two stage after adding the epoxy propane each time, and the whole reaction process is controlled by set computer programs, thereby ensuring the concentration of the epoxy propane in a system to be stabilized in a certain range, controlling the side reaction speed to be in a low state, facilitating stable performing of positive reaction, and simultaneously greatly improving uniformity degree of macromolecule substitution and quality stability of products. The whole reaction process is controlled by the computer distributed control system (DCS) programs, the labor intensity is reduced, a production device with same size can save 12 fixed workers, and labor efficiency and production safety are improved.

Description

technical field [0001] The invention relates to the field of fine chemicals, in particular to a process for producing hydroxypropyl cellulose with a high degree of substitution. Background technique [0002] At present, the domestic preparation of hydroxypropyl cellulose is all one-step process, using natural refined cellulose under the action of solvent and alkali, adding a sufficient amount of propylene oxide at one time, and reacting in stages, the concentration of propylene oxide in the system is relatively high , The severe side reaction is not easy to control, and the production of a large number of by-products is not easy to purify in the later stage. Contents of the invention [0003] In order to solve the above-mentioned technical problems, the present invention provides a process for producing highly substituted hydroxypropyl cellulose, using natural refined cellulose in the presence of a binary composite solvent composed of an aromatic solvent and an aliphatic a...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08B11/08C08B1/08
Inventor 刘传荣邸勇邸蓉
Owner 邸勇