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A preparation method of modified mixed cellulose ether and products obtained by the method

A technology of mixing cellulose and cellulose powder, which is applied in the preparation of mixed cellulose ether, the preparation of modified mixed cellulose ether, and the field of modified mixed cellulose ether, which can solve the problem of low light transmittance and difficulty in making high viscosity products. , reducing the viscosity of the solution, etc., to achieve the effects of broad market prospects, excellent water retention, and fewer by-products

Active Publication Date: 2019-07-05
广东龙湖科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, HPMC and HEMC have the following problems in production and use: 1. It is not easy to increase the viscosity (above 180,000); 2. After the viscosity is increased, the viscosity of the solution decreases; 3. The specific gravity is low, and the solubility is not easy to control; 4. The product Low light transmittance; 5. Low crushing efficiency and high energy consumption; 6. No anti-sagging effect; 7. Poor film forming, water retention, stability, and mildew resistance; 8. Formation of dimethylformamide in the production process Ether, α-propylene glycol, propylene glycol and other by-products that cause great trouble to post-processing
With the modern society's increasing emphasis on energy and quality in all walks of life, the production process, quality and function requirements of the important additive cellulose ether are getting higher and higher, and the existing mixed cellulose ether can no longer meet the requirements

Method used

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  • A preparation method of modified mixed cellulose ether and products obtained by the method

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] 1) Preparation of lye: first configure 700 parts of mixed solvent, the ratio of the mixed solvent is isopropanol:toluene=1:4, add 400 parts of mixed solvent, 40 parts of sodium hydroxide, and 30 parts of water into the reactor, Raise the temperature to 80°C, stir the sodium hydroxide to dissolve it completely, and keep it warm for 30 minutes;

[0017] 2) Alkalization: Lower the temperature of the reactor to 30°C, add 80 parts of refined cotton powder and 1 part of starch, and spray the material with the remaining mixed solvent. After the feeding is completed, vacuumize and fill with nitrogen for 3 replacements, and then keep the reaction Stir at 28°C for 90 minutes;

[0018] 3) Etherification: after alkalization, vacuumize again, add 18 parts of propylene oxide, 58 parts of methyl chloride and 3 parts of ethylene oxide in sequence, keep the temperature of the reactor at 28°C, stir for 20 minutes, and raise the temperature of the reactor to Keep warm for 90 minutes at 4...

Embodiment 2

[0024] 1) Preparation of lye: first configure 800 parts of mixed solvent, the ratio of which is isopropanol:toluene=1:5, add 500 parts of mixed solvent, 50 parts of sodium hydroxide, and 40 parts of water into the reactor, Raise the temperature to 85°C, stir the sodium hydroxide to dissolve it completely, and keep it warm for 40 minutes;

[0025] 2) Alkalization: Lower the temperature of the reactor to 35°C, add 85 parts of refined cotton powder and 2 parts of starch, and spray the materials with the remaining mixed solvent. The reactor temperature was stirred at 25° C. for 100 minutes;

[0026] 3) Etherification: after alkalization, vacuumize again, add 20 parts of propylene oxide, 70 parts of methyl chloride and 4 parts of ethylene oxide in sequence, keep the temperature of the reactor below 24°C, stir for 25 minutes, and put the reactor into When the temperature rises to 45±1°C, 70±1°C, and 90±1°C, keep it warm for 100 minutes;

[0027] 4) Desolventization and acid adjust...

Embodiment 3

[0032] 1) Preparation of lye: first configure 900 parts of mixed solvent, the ratio of which is isopropanol:toluene=1:6, add 600 parts of mixed solvent, 60 parts of sodium hydroxide, and 45 parts of water into the reactor, Raise the temperature to 90°C, stir the sodium hydroxide to dissolve it completely, and keep it warm for 50 minutes;

[0033] 2) Alkalinization: Lower the temperature of the reactor to 40°C, add 88 parts of refined cotton powder and 2.5 parts of starch, and spray the material with the remaining mixed solvent. After the feeding is completed, vacuumize and replace with nitrogen for 3 times, and then keep the reaction Stir at 22°C for 110 minutes;

[0034] 3) Etherification: After the alkalization is completed, vacuumize again, add 22 parts of propylene oxide, 90 parts of methyl chloride and 5 parts of ethylene oxide in sequence, keep the temperature of the reactor below 22°C, stir for 28 minutes, and put the reactor into When the temperature is raised to 50±1...

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Abstract

The invention provides a preparation method of modified mixed cellulose ether, the preparation method includes alkalization, etherification, desolvation and acid adjustment and post-treatment, and the alkalinization is to use lye to carry out alkali activation treatment on cellulose powder and starch , etherification is to use methyl chloride, propylene oxide and ethylene oxide as etherification agents to alkalized cellulose powder and starch at 30‑54±1°C, 65‑80±1°C, 85‑95±1°C Etherification at ℃ for 90‑120 minutes respectively. Desolventization and acid adjustment is to add acid and hot water first and then desolventization. The desolventization temperature is 80‑90℃, and the pH value of the material after desolventization is 5‑7; cellulose powder The parts by weight of starch, methyl chloride, propylene oxide and ethylene oxide in the formula are 80-95 parts of cellulose powder, 1-3 parts of starch, 58-100 parts of methyl chloride, and 18-25 parts of propylene oxide , 8-10 parts of ethylene oxide. The preparation method of the invention has a short production cycle, and the obtained product has excellent water retention, dispersibility, solubility, film-forming property, stability, mildew resistance, sagging resistance and easy crushing property. The present invention also provides a mixed modified cellulose ether obtained by the above preparation method.

Description

technical field [0001] The present invention relates to a preparation method of cellulose ether, in particular to a preparation method of mixed cellulose ether, and more particularly to a modified mixed cellulose ether which adopts mixed raw materials and various etherification agents for one-step reaction method of preparation. The present invention also relates to a modified mixed cellulose ether obtained by the above method. Background technique [0002] Cellulose ether is the most commonly used additive in dry powder mortar. As a water retaining agent, it can prevent the moisture in the wet mortar from evaporating prematurely or being absorbed by the base layer, and ensure that the cement is fully hydrated, thereby ensuring the mechanical properties of the mortar. Cellulose ether is generally prepared from cellulose powder through processes such as alkalization, etherification, desolvation and acid adjustment, and post-treatment. The alkalization step is to activate the...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08B11/193C08B31/12C08J3/24C08L1/28C08L3/08C08K5/07C04B24/38
CPCC04B24/383C08B11/193C08B31/12C08J3/246C08J2301/28C08J2403/08C08L1/28C08L2312/00C08L3/08C08K5/07
Inventor 刘晓清洪永顺
Owner 广东龙湖科技股份有限公司
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