SU1208040A1 - Method of producing carboxymethylcellulose - Google Patents

Description

The invention relates to the production of cellulose ethers, in particular, carboxymethyl cellulose (KS), which is widely used in the oil, gas and geological and exploration industries in the drilling of oil and gas wells, in the production of synthetic detergents, mining, chemical, mining, textile, construction and other industrial areas.

The purpose of the invention is to reduce the consumption of sodium monochloroacetate, and to obtain a water-soluble target product.

According to the proposed method, wood pulp is treated with either an alkaline solution containing 100-400 g / l of sodium sulphite or thiosulfate and 150-350 g / l of sodium hydroxide, squeezed to 2.6-3.6-cels in relation to the mass of ishona pulp and mixed with o-alkylation reagent at a ratio of cellulose: sodium mono-poroacetate 1: 0.8-1.8, or alkaline cellulose is obtained by any known method and further it is treated with sodium mono-chloroacetate at the indicated ratio.

Example 1 (prototype). 500 g of wood pulp (9 l of alkaline solution of bottom liquid containing 250 g / l of salts (130 g / l of sodium chloride, 50 g / l of sodium glycolate and 30 g / l of acetates, carbonates and other salts are treated) and 300 g / l caustic soda at for 30 minutes, then alkaline cellulose squeeze up to 2.8 times the mass relative to the mass of the original cellulose, crushed for 90 minutes Crushed alkaline cellulose, having the composition,%: cellulose 33; caustic soda 15; 7.0; water 44, mixed for 60 minutes with 603 g of sodium monochloroacetate, which corresponds to the ratio of cellulose for: sodium monochloro acetate, 1: 1.6 and more vscherzhivayut 2.0 hours at 80 C to complete the reaction of o-alkilirova audio.

The resulting product has the following indicators:

Substitution rate 88.1

Content of the main substance,% 53,0

Solubility,% 97.8 Dissolution rate, h 6.5 O-alkylation reaction efficiency,% 52.0 PRI me R 2 (prototype). 500 g of cellulose are treated with 9.0 l of an aqueous solution of sodium hydroxide at a concentration of 250 g / l, squeezed to a degree of pressing 2.8, after which the alkaline cellulose is ground in a grinder for 60 minutes. The crushed alkali cellulose, and the following composition,%: A-cellulose 32,4; caustic soda 16.9; water 50.7; mixed with 555 g ms5 sodium chloroacetate, which corresponds to a cellulose: sodium monochloroacetate ratio of 1: 1.7 and 165 g of the bottom residue of the carboxymethylcellulose purification step and then held for 2.0 hours at 80 ° C until the completion of the apicalization reaction.

I The resulting product has the following {indicators:

I Degree of substitution 87.9 Content of the main substance,% 52.9

Solubility 98.0 Dissolution rate, h7.0 Efficiency re-. o-alkylation,% 51.7

Example 3. 500 g of wood pulp are treated with 9 liters of sodium sulfite cellulose solution containing 400 g / l of sodium sulfite and 350 g / l of sodium hydroxide for 30 minutes. At the end of the treatment, the alkaline cellulose is squeezed to a spin degree of 2.8 and ground in

for 60 minutes Crushed alkali cellulose, having the composition,%: cellulose 34.2%, caustic soda 16.9; sodium sulfite 12.8; water 36.1, is mixed for 60 minutes with 551 g of sodium monochloroacetate, which corresponds to the K-cellulose: sodium monochloroacetate ratio of 1: 1.6, and the sodium monochloroacetate: sodium sulfite ratio of 1: 0.32, is maintained at 80 ° C for 2 h and dried.

The resulting product has the following indicators:

Substitution degree 86.6 Content of the main substance,% 54.0 Solubility,% 99.8 Dissolution rate, h3.5 Efficiency of the o-alkylation reaction,% 54.1 Example 4. Same as in Example 3, but used sulphate sodium thiosulfate

The resulting product has the following characteristics:

Degree of substitution 87.2 Content of the main substance,% 55.1 Solubility,% 99.8 Dissolution rate, h3.0 Efficiency of the o-alkylating reaction,% 54.5 PRI me R 5. 500 g of wood pulp is treated with 9 l an alkaline solution of sodium sulfite containing 200 g / l of sodium sulfite and 250 g / l of sodium hydroxide at 20 ° C for 30 minutes, then squeezed to 2.7 times the weight relative to the weight of the original cellulose, and crushed for 60 minutes The crushed alkaline cellulose having a composition,%: cellulose 33.2; caustic soda 16.1 sodium sulfite 6.3; water 44.4, is mixed for 60 minutes with 516 g of sodium mono-chloroacetate, which corresponds to the ratio of v-cellulose: sodium monochloroacetate, equal to 1: 1.6, and the ratio of sodium monochloroacetate: sodium sulfite, equal to 1: 0.16 , vydezhivayut when for 2 h and dried.

The resulting product has the following characteristics:

The degree of substitution is .88.0 Content of the main substance,% 56.7 Solubility,% 99.6 Dissolution rate, h3.5 Efficiency of the o-alkylation reaction,% 55.0 Pmimer 6. Same as for example, sodium thiosulfate is used.

The resulting product has the following characteristics:

Degree of Substitution 88.6 The content of the basic substance a,% 57.1

Solubility,% 99.8 Dissolution rate, h3.0 Reaction efficiency of o-alkyl

Vani% 55.5

Example 7. Same as example 3, but using an alkaline sodium sulfite resistor containing 100 g / l sodium sulfite and 150 g / l sodium hydroxide.

380 g of sodium monochloroacetate is added, which corresponds to oi-cellulose: sodium monochloroacetate, equal to 1: 1.2, and the ratio to sodium monochloroacetate: sodium sulfite is 1: 0.33.

The resulting product has the following characteristics:

Degree of Substitution 71 Content of the basic substance,% 61.4 Solubility,% 99.8 Dissolution rate, h4.0.

Reaction efficiency of o-apylicrobi,% 59.2 Example 8 Same as example 7, but using sodium thiosulfate.

The resulting product has the following characteristics:

Substitution degree 72 Content of the main substance,% 61.8 Solubility,% 99.7 Dissolution rate, h4.0 Efficiency of the o-alkylation reaction,% 59.0

Example 9. 500 g of wood pulp is treated with 9.0 l of an aqueous solution of caustic soda with a concentration of 250 g / l. At the end of the treatment, the alkaline cellulose is squeezed to the degree of extraction of 2.8 and crushed for 60 minutes. The crushed alkaline cellulose having a composition,%: cellulose 32.4; caustic soda 16.9; water 48.7, mixed for 60 minutes with 522 g sodium monochloroacetate, which corresponds to the ratio A-cellulose: sodium monochloroacetate 1: 1.6, and 156 g sodium sulfite, which corresponds to the ratio: sodium monochloroacetate: sodium sulfite , 1: 0.3, then left at e for 2 h and dried.

The resulting product has the following indicators:

Degree of substitution 88

Content of the main substance,% 55, I Solubility,% 99.1 Dissolution rate, h3.0 Efficiency of o-alkylation reaction,% 55 Example 10. Same as example 5, but alkaline cellulose is treated with sodium monochloroacetate in the amount of 258 g , which corresponds to the sodium mono-chloroacetate: od-cellulose ratio of 0.8-1.0.

The resulting product has the following characteristics:

Degree of substitution 52

Content of the main substance,% 61.8 Solubility,% 99.1 Dissolution rate, h, .4.5 Efficiency of o-alkylation reaction,% 65 Example 11. Same as example 10, but using sodium thiosulfate.

The resulting product has the following characteristics:

Substitution degree 54

Content of the main substance,% 62,4

Solubility,% 99.3

Dissolution rate, h5.0 O-alkylation reaction efficiency,% 67.5

Example 12. Same as example 9, but using nios thiosulfate.

The resulting product has the following indicators:

Substitution rate 87

Content of the main substance,% 55.8 Solubility,% 99.4 Dissolution rate, h3.0 h Effectiveness of the reaction of o-alcryl1,% 54.4 Example 13. Same as example 9, but using 26.1 g sodium sulfite, which corresponds to co080406

relative to sodium monohporacetate: sul-. sodium fit, equal to 1: 0.05.

The resulting product has the following characteristics:

5 Degree of Substitution 87.5

The content of the basic substance.% 57, I Solubility,% 98.2 Dissolution rate, 10 hours, 3.5 hours. The efficiency of the o-alkylation reaction is 54.7. Example 14. Same as example 9, but using 52 g of sodium sulfite 15, which corresponds to a sodium mono-chloroacetate: sodium sulfite ratio of 1: 1.

The resulting product has the following characteristics:

20 degree of substitution 92

Content of the main substance,% 50.8

Solubility,% 99.9

Dissolution rate - 25 n, h3.0

O-alkylation reaction efficiency,% 57.6

Example 15. Same as example 13, but using sodium thiosulfate.

The resulting product has the following characteristics:

Substitution degree 89.0

Content of the main substance,% 58,4

Solubility,% 98,9

Dissolution rate, h3.0 O-alkylation reaction efficiency,% 55.6 Example 16. Same as Example 14, but using sodium thiosulfate.

I The resulting product has the following characteristics:

Degree of substitution 93

Content of the main substance,% 51,6

Solubility,% 99.9

Dissolution rate,, 0 O-alkylation reaction efficiency,% 58.0

Example 17. Same as example 9, but alkaline cellulose is treated with sodium monochloroacetate in

The amount of 261 g, which corresponds to the ratio of sodium monohporacetate: ei-cellulose, is 0.6: 1.

The resulting product has cmsflyw indicators:

Substitution ratio 58 Main content

substances,% 64.6

 Solubility,% 98.2

Dissolution rate, h4.5 Reaction efficiency

o-apylation,% 72.5

12080408

EXAMPLE 18. Same as example 17, but using thiosulfate sodium.

The resulting product has the following indicators:

5 Degree of substitution 58 Content of the main substance,% 64.6

Solubility,% 98.2 Dissolution rate

Efficiency of reac-1CSh o-alkylation,%

4.0

72.5

Claims (2)

1. METHOD FOR PRODUCING CARBOXYMETHEL CELLULOSE by mercerization of cellulose with a solution of caustic soda followed by squeezing, grinding, 0-alkylation with sodium monochloracetate in the presence of a modifying additive, characterized in that, in order to reduce the consumption of sodium monochloracetate and to obtain the desired product in water-soluble mode, , citing additives use sodium sulfite or thiosulfate, and o-alkylation is carried out at a ratio of sodium monochloracetate - sulfite or sodium thiosulfate 1: 0.05-1.00. 2. The method of pop. 1, characterized in that the mercerization is carried out in the presence of sodium sulfite or sodium thiosulfate with a sodium hydroxide content of 150-350 g / l, sodium sulfite or thiosulfate Ί00400 g / l. SU a "_1208040