The method of producing carboxymethyl cellulose

 

(57) Abstract:

The invention relates to the production of cellulose derivatives, in particular to a technology for production of carboxymethyl cellulose, which is widely used in the oil and gas industry for making mud used during drilling. The method comprises conducting the process in two stages in a flow vibratory centrifugal mill - first processing of the original cellulose-containing raw material sodium salt of monochloracetic acid, then adding to the resulting composite aqueous solution of sodium hydroxide at a molar ratio of components cellulose:sodium salt of monochloracetic acid: sodium hydroxide:water= 1:1,7:1,6:0,85-0,90, and maturing during heating. When this process is carried out at the acceleration of milling bodies of 100-200 m/c2within 1-2 minutes the Technical result of the invention is to simplify the technology of production of carboxymethyl cellulose in the form of loose soluble powder.

The invention relates to the production of cellulose derivatives, namely the technology of production of carboxymethyl cellulose (CMC), which is widely used in the oil and gas industry for the preparation of clay process is which the original cellulose raw material is processed in a twin screw reactor-mixer with a mixture of sodium salt of monochloracetic acid and alkali solution at room temperature, and then gradually increase it up to 85-100oC to achieve a homogeneous plastic state of the reaction mixture, which hardens at the outlet of the reactor (ed. St. USSR N 1063803, class C 08 B 11/12, prototype).

The disadvantages of the prototype:

- get the target product in the form of monolith, to give to which the goods form (granules or powder), you need additional equipment for drying and grinding;

- complex technological equipment in the reactor has 8 working zones, each of which is necessary to maintain a specific temperature using a cooling system that creates additional problems;

complex technology of obtaining the target product.

The claimed technical solution solves the problem of obtaining carboxymethylcellulose in the form of loose soluble powder for preparation of clay solutions, as well as the simplification of its receipt.

The problem is solved by the claimed method of producing carboxymethyl cellulose, comprising conducting the process in two stages in the reactor-mixer - first processing of raw cellulose-containing raw material sodium salt of monochloracetic acid, then dobavleniyami use flow vibratory centrifugal mill continuous action (VCM), and the process is carried out at the acceleration of milling bodies of 100-200 m/s2within 1-2 minutes, and the molar ratio of the components: cellulose : sodium salt of monochloracetic acid : sodium hydroxide : water= 1 : 1,7 : 1,6 : 0,85-0,90.

As a source of raw materials used waste paper, straw and other cellulosic products with a particle size of not more than 5 mm. raw Cellulose and sodium salt of monochloracetic acid were loaded into VCM and processed when accelerating particles of 100-200 m/s2within 1-2 minutes After treatment formed the dry bulk composite, semi-finished product to obtain the CMC, which can be stored for a long time.

To obtain the CMC in the reactor with injected composite aqueous solution of alkali, and water should be no more than of 0.85-0.90 moles per 1 mole of the original cellulose. Then the product is sent for ripening at 50oC for 1.5 - 2 h and obtain the target product (CMC) in the form of dry free flowing powder without any additional operations on the ground, as it was known in the technology.

The specified amount of water in relation to the original cellulose completely spent for its intended purpose (for reaction), this prevents the appearance of unwanted problems. Namely, ka is AE also reduce the amount of water (less than 0,85), it is not enough to wetting of the composite, which leads to not complete reaction of the starting components, which target the product reveals the presence of unreacted composite.

The ratio of all initial components: cellulose : sodium salt of monochloracetic acid : sodium hydroxide : water= 1 : 1,7 : 1,6 : 0,85-0,90.

As shredder and reactor-mixer used flow vibratory centrifugal mill of continuous acceleration of small particles of 100-200 m/s2that has significantly simplified the technology (known - 8 working zones, each of which is necessary to accurately maintain the temperature).

Example 1. In the VIC with acceleration of small particles of 100-200 m/s2download the shredded paper with a particle size up to 5 mm and the sodium salt of monochloracetic acid in the ratio of 1 : 1,7, respectively, and treated for 1 min, then enter the aqueous alkali solution is based 1.6 moles of alkali and 0.9 mol of water per 1 mol of cellulose and again powerhaul processing on WCM for 2 minutes After which the resulting product is sent for ripening at 50oC for 1.5 hours Get dry CMC in the form of a loose, fairly small, water soluble powder is added a solution of sodium hydroxide at a molar ratio of cellulose : water = 1 : 0,85, get CMC in the form of a dry powder of good quality.

Example 3. Under the conditions of example 1 at the second stage, introducing the alkali solution at a ratio of cellulose : water = 1 : 0,8. Because of the lack of water for wetting and incomplete interaction between the components in the target product was observed the presence of moistened powder composite (cellulose + sodium salt of monochloracetic acid).

Example 4. Under the conditions of example 1 at the second stage, introducing the alkali solution at a ratio of cellulose : water = 1 : 1. There is a partial formation of a homogeneous mass, from which on cooling formed lumps of up to 3 mm and more.

Example 5. The conditions of example 1 were processed in VCM at each stage for 1 min. the resulting homogeneous powder CMC required quality.

Example 6. Under the conditions of example 1 as the starting cellulose-containing raw material used straw. The resulting homogeneous CMC powder with a particle size less than 0.2 mm

As seen from the above examples, when the stated molar ratio of the components, and also used as a reactor running vibratory centrifugal mill of continuous operation, is achieved plebiscite quality indicators:

The moisture content,% Not more than 5.0

The content of free alkali,% Not more than 1,0

The content of basic substance,% Not less than 25-50

The degree of polymerization,% Not less than 450

The degree of substitution by carboxyl groups,% Not less than 60

Flowability, C - 20

The dissolution rate, min - 5

Low percentage content of the basic substance in a dry product due to the low content of cellulose in the raw materials used (in straw - not more than 40%, in the paper - no more than 70%). While the inventive method is simple in hardware design, requires no additional equipment for operations to maintain the temperature in each of the 8 zones, cutting devices and equipment for the grinding of the cooling at the outlet of the reactor "plastic mass", as stated in the known way.

The method of producing carboxymethyl cellulose, comprising conducting the process in two stages in the reactor-mixer - first processing of raw cellulose-containing raw material sodium salt of monochloracetic acid, then adding to the resulting composite aqueous solution of caustic soda, and maturing by heating, characterized in that as a reactor-mixer used in the covering bodies 100 - 200 m/s2within 1 to 2 min and the molar ratio of components cellulose : sodium salt of monochloracetic acid : sodium hydroxide : water= 1 : 1,7 : 1,6 : 0,85 - 0,90.

 

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[C6H7O2(OH)3-x(OCnH2nCOOMe)x]m,

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< / BR>
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FIELD: method for production of carboxymethyl esters useful as adsorbents.

SUBSTANCE: claimed method includes preliminary removing from air-dry lignocarbohydrate material of extractive and water soluble substances by 3-steps subsequent extraction with alcohol/benzene mixture, hot water and cold water. Then macromolecules are cross-linked by polycondensation of extracted material with formaldehyde in ratio lignocarbohydrate material OH-groups/formaldehyde of 1:3-5 in presence of alkali catalyst. Cross-linked lignocarbohydrate material is washed and carboxymethylated with monochloroacetic acid and alkali in ratio lignocarbohydrate material OH-groups/ClCH2COOH/NaOH of 1:3:27 at 45-65°C for at least 3 h. Obtained product is separated, treated with mineral acid to convert carboxylic groups to H-form; washed with water up to neutral filtrate pH-value, and dried.

EFFECT: product with high content of carboxylic groups, increased change capacity, and stability in aqueous and non-aqueous media.

6 ex, 2 tbl

FIELD: cellulose derivatives production.

SUBSTANCE: object of invention is production of sodium-carboxymethylcellulose product from cellulose-containing vegetable stock without separation cellulose from lignin, lipids, and resinous substances present in plant tissues. Method according to invention comprises treatment of vegetable stock, namely straw, with monochloroacetic acid sodium salt on flow-type vibration-centrifugal mill run in continuous mode at acceleration of elastic grinding bodies 100-200 m/s-1, addition of aqueous sodium hydroxide solution to resulting powder composite, and stirring. Starting components are taken in following molar proportion: cellulose/monochloroacetic acid salt/sodium hydroxide/water = 1:(1.7-2.1):(3.0-3.5):(8-12).

EFFECT: increased viscosity of aqueous suspension prepared from sodium-carboxymethylcellulose product.

1 tbl, 4 ex

FIELD: cellulose derivatives production.

SUBSTANCE: invention relates to production of high-molecular weight substances, in particular carboxymethylcellulose sodium salt with high substitution degrees, which is characterized by uniform distribution of carboxyl groups, that is polyanionic cellulose applicable as thickener and emulsifier in papermaking, textile, and oil and gas producing industries. Process is accomplished through activation of cellulose followed by feeding the same on twin-screw multizone reactor-mixing machine, addition of sodium hydroxide in the form of aqueous solution in amount 0.9-1.2 mole per 1 mole cellulose and sodium monochloroacetate, and finally intensive stirring of resulting product in one or several in series arranged reactor-mixing machines while additionally introducing sodium hydroxide in the form of aqueous solution in amount 0.4-0.6 mole per 1 mole cellulose all in one time or in equal portions. Transfer of into next reactor-mixing machine is accomplished with the aid of transportation means.

EFFECT: increased resistance of aqueous solutions of polyanionic cellulose to polymineral aggression and their biological resistance.

6 cl, 1 tbl

FIELD: production of carboxymethyl cellulose (CMC) sodium salt useful as thickening agent and emulsifier in paper, textile and petroleum industry.

SUBSTANCE: claimed method includes cellulose treatment with sodium hydroxide aqueous solution to produce alkali cellulose, wherein in sodium hydroxide aqueous solution (100 mass pts) low molecular polyether based on ethylene oxide or propylene oxide (1.0-2.5 mass pts) is introduced and for cellulose treatment sodium hydroxide aqueous solution in concentration of 19.5-23.0 % at temperature 50-60°C is used, and process is carried out for 2.5-3.0 h at 30-45°C.

EFFECT: CMC aqueous solutions with decreased viscosity.

4 cl, 1 tbl, 8 ex

FIELD: production of carboxymethyl cellulose (CMC) sodium salt useful as thickening agent and emulsifier in paper, textile and petroleum industry.

SUBSTANCE: claimed method includes cellulose treatment with sodium hydroxide aqueous solution to produce alkali cellulose, addition of carboxymethylating agent, agitation and drying wherein in sodium hydroxide aqueous solution (100 mass pts) low molecular polyether based on ethylene oxide or propylene oxide (1.0-2.5 mass pts) is introduced and for cellulose treatment sodium hydroxide aqueous solution in concentration of 19.5-23.0 % at temperature of 20-25°C is used, and process is carried out for 2.5-3.0 h at 25-35°C.

EFFECT: CMC aqueous solutions with decreased viscosity and increased substitution ratio.

3 cl, 1 tbl, 8 ex

FIELD: chemical technology, polymers.

SUBSTANCE: invention proposes a method for continuous processing derivatives of polysaccharides as a solid substance that involves reaction and/or conditioning in suspension with liquid reactive components by the following steps: (a) preliminary temperature-controlled suspending flow consisting of a solid substance SE and liquid phase LE is added into upper part of column continuously wherein this column is filled almost completely with temperature-controlled similar or other liquid phase L after this process; (b) solid substance SE is converted to solid substance SA by gravitation and reaction of and/or conditioning with liquid phase L and precipitated freely through liquid phase in bottom part of column; (c) if necessary, gases G evolved from column are removed from upper part of column, and (d) solid substance SA is removed from the process continuously through bottom part of column as a suspension flow at constant level of the column filling by addition of liquid phase LR removed early from upper part of column and transporting as a separating compound to bottom part of column and/or by addition of novel liquid phase LN into bottom part of column.

EFFECT: improved processing method.

8 cl, 1 dwg, 2 ex

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