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Preparation method of sodium carboxymethylcellulose

A technology of sodium carboxymethyl cellulose and alkali cellulose, which is applied in the field of chemical modification of natural polymers, can solve the problems of prolonging the production cycle, difficulty in meeting demands, and high production costs, and achieve loose production equipment requirements, reduce preparation costs, Good product performance

Active Publication Date: 2014-04-30
CHINA UNIV OF PETROLEUM (BEIJING)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But the viscosity of the product obtained in CN101548733A is low, and the viscosity of the 2% aqueous solution is less than 50mPa·s; although the viscosity of the product obtained in CN101747441A is higher, a crosslinking agent is added in the reaction process, and the crosslinking agent is not described in this patent document The specific circumstances of (such as the structure or name of the substance, the addition amount, etc. are not mentioned)
However, the disadvantages of this method are also obvious: ①The cost of solvent is too high
First of all, the cost of isopropanol is significantly higher than the ethanol commonly used in other patents; in addition, the liquid-solid ratio of the reaction described in this method is also high (the mass ratio of isopropanol to raw material is about 11:1~15:1 )
②Complicated process
The weak point of this method is that the amount of organic solvent consumed is relatively large. In the given example, 4g of raw material will use about 60mL of high-concentration ethanol solution (volume concentration is 95%) to complete the reaction, and the production cost is high.
The product viscosity that this method obtains is very high, but too loaded down with trivial details to the pretreatment step of raw material, prolong production cycle greatly; And reaction uses more expensive high-concentration isopropanol solution, and liquid-solid ratio is also very high (about 20:1 )
[0020] In summary, the preparation of CMC from non-cotton raw materials at home and abroad mostly uses inert organic solvents as the reaction medium, and the production cost is relatively high.
Although there are individual application examples of the lower-cost water-based method, the performance of the obtained product is not satisfactory, and it is difficult to meet the needs of various industries.

Method used

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  • Preparation method of sodium carboxymethylcellulose

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0087] In this example, a qualified low-viscosity sodium carboxymethylcellulose for drilling fluid was prepared by semi-dry method using wood pulp block as raw material.

[0088] (1) Preparation: Put the wood pulp block into a pulverizer and pulverize until the raw material changes from block to fluffy floc without hard core. Put the floc raw materials into an oven to dry.

[0089] Add 10 g of dried flocculent wood pulp raw material, 6.03 g of granular solid sodium hydroxide into the pulverizer, and then add 15.46 g of a 25% sodium hydroxide aqueous solution in the form of spraying. Start the pulverizer for 2min. After the pulverization is completed, put the pulverizer at room temperature for 20 minutes to complete an alkalization cycle. Then carry out the crushing-standstill alkalization process again, and repeat 3 cycles in total. The whole alkalization reaction time is 1.1h.

[0090] Add 13.5 g of solid monochloroacetic acid to the pulverizer at one time, and then start...

Embodiment 2

[0102] In this example, a qualified medium-viscosity sodium carboxymethylcellulose for drilling fluid was prepared by semi-dry method using wood pulp block as raw material. The main difference between this example and Example 1 is that: during the alkalization reaction, the amount of solid sodium hydroxide and sodium hydroxide solution is different; the time for a single operation of the pulverizer is different; the time for alkalization reaction and etherification reaction is different ; Chloroacetic acid was added twice in a ratio of 1:1.

[0103] (1) Preparation: Put the wood pulp block into a pulverizer and pulverize until the raw material changes from block to fluffy floc without hard core. Put the floc raw materials into an oven to dry.

[0104] Add 10 g of dried floc wood pulp raw material, 5.3 g of flaky solid sodium hydroxide into the pulverizer, and then add 17.85 g of a 25% sodium hydroxide aqueous solution in the form of dropwise addition. Start the pulverizer fo...

Embodiment 3

[0114] In this example, a qualified high-viscosity sodium carboxymethyl cellulose for drilling fluid was prepared by semi-dry method using wood pulp block as raw material. The main differences between this example and Example 1 are: in the alkalization process, the amount of solid sodium hydroxide and sodium hydroxide solution is different; the concentration of sodium hydroxide solution is different; the time of a single operation of the pulverizer is different; etherification The ambient temperature of the reaction is different; the total time of the etherification reaction is different; monochloroacetic acid is added twice in a ratio of 1:2.

[0115] (1) Preparation: Put the wood pulp block into a pulverizer and pulverize until the raw material changes from block to fluffy floc without hard core. Put the floc raw materials into an oven to dry.

[0116] Add 10 g of dried flocculent wood pulp raw material, 5.78 g of granular solid sodium hydroxide into the pulverizer, and the...

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Abstract

The invention provides a preparation method of sodium carboxymethylcellulose. The sodium carboxymethylcellulose is prepared from wood pulp or paper pulp through a semidry method without use of an organic solvent, and the preparation method comprises the steps of alkaline reaction: carrying out alkaline reaction on sodium hydroxide by taking water as a medium to obtain alkali cellulose; etherification reaction: implementing etherification reaction on alkali cellulose and monochloro acetic acid to obtain a crude sodium carboxymethylcellulose product; neutralization and washing: neutralizing the crude sodium carboxymethylcellulose product in an aqueous solution of alcohol and washing in alcohol; and drying treatment: drying, grinding and sieving obtained solid material to obtain sodium carboxymethylcellulose. The method disclosed by the invention has the advantages that raw materials are abundant, waste paper pulp is used as raw material and little water in the sodium hydroxide solution serves as a reaction medium in a preparation process; the preparation cost is low because of no use of organic solvents; and the product performances are controllable. The method disclosed by the invention can finish the entire preparation process in a grinder, so as to realize efficient utilization of equipment.

Description

technical field [0001] The invention relates to a method for preparing sodium carboxymethyl cellulose, in particular to a method for preparing sodium carboxymethyl cellulose with different viscosities and degrees of substitution by using wood pulp or waste paper pulp as raw materials through a semi-dry method, which belongs to natural polymers field of chemical modification. Background technique [0002] Sodium carboxymethylcellulose (Na-CMC) is a product obtained from cellulose substances as raw materials and modified by carboxymethylation reaction, which is customarily called CMC. Its molecular formula is shown in figure 1 . CMC is one of the most important cellulose ethers. It can form a colloidal solution with a certain viscosity after being dissolved in water. It has the functions of thickening, bonding, film forming, water retention, colloid protection, emulsification and suspension, etc. Oil drilling, printing and dyeing textiles, papermaking, ceramics, constructio...

Claims

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Application Information

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IPC IPC(8): C08B11/12
Inventor 赵雄虎李外季一辉赵武顾岳
Owner CHINA UNIV OF PETROLEUM (BEIJING)
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