CN101280023B - Preparation of acid-resistant sodium carboxymethylcellulose - Google Patents
Preparation of acid-resistant sodium carboxymethylcellulose Download PDFInfo
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Abstract
The invention provides a method for industrially producing acid-proof sodium carboxymethyl cellulose with high-viscosity and high-degree of substitution through the kneading method. Under the protection of inert gas, cellulose is basified by high-concentration liquid alkali to generate alkali cellulose; after the alkali cellulose is processed in carboxy methylation reaction of chloroacetic acid, cross-linker is added through vacuum suction to modify the alkali cellulose, then the acid-proof sodium carboxymethyl cellulose product with high-viscosity and high-degree of substitution is obtained after being washed, neutralized, centrifugated, dried and crushed. The product not only has good solubility, but also has strong acid-resistant and salt-resistant capacities, which also had simple production process, short reaction period, less investment and low consumption of raw materials.
Description
Technical field
The present invention relates to the preparation method of a kind of high viscosity, high substitution value acid-resistant sodium carboxymethylcellulose.
Background technology
Xylo-Mucine (CMC) is that purified cotton and Mono Chloro Acetic Acid alkalize under alkaline condition, etherification reaction and the water miscible fiber derivative that makes, the brill that it is widely used in synthetic detergent and soapmaking industry, textile and dyeing industry, paper industry, silicate industry, foodstuffs industry, medicine industry, daily chemical industry and the oil and gas industry of digging well.Because every profession and trade requires to differ to the salt resistance of CMC and resistance to acid, the sticking CMC than, the sticking ratio of salt of low acid can not satisfy user's demand, and for this reason, high acidproof, the salt tolerance CMC of exploitation and research preparation has realistic meaning and application prospect widely.The present invention has obtained existing better solvability by the modification of carboxymethyl cellulose is handled, and has the modified carboxy methyl cellulose sodium of higher acidproof, salt resistance ability again.
The main chemical reactions of preparation acid-resistant sodium carboxymethylcellulose is: Mierocrystalline cellulose and alkaline solution reaction generate soda cellulose; Soda cellulose and chloroacetic etherification reaction carry out etherification reaction with other etherifying agent again.
The anti-acid carboxymethyl cellulose has good solvability as thickening material.The feed purification cotton that produces the anti-acid carboxymethyl cellulose contains hydrophilic oh group, but these hydroxyls are in cellulosic molecule and the very strong hydrogen bond of intermolecular formation, and forms crystallization, thereby causes great difficulty for the dissolving of cellulosic molecule in water.And Mierocrystalline cellulose is introduced carboxymethyl and linking agent substituted radical gradually in etherification procedure, and the introducing of these groups makes that adjacent cellulose chain obtains stretching on the one hand, has destroyed the hydrogen bond between them, promptly produces the brilliant effect that disappears.Crystalline reduces or disappearance helps water molecules to whole cellulosic molecule diffusion and infiltration (when etherification procedure began, brilliant the acting on that partly disappear also played in the activation of alkali).On the other hand, because the substituted radical that is imported all is very strong hydrophilic radicals, be easy to make the ether of cellulose dissolving with water molecules generation hydration.
Cellulosic carboxymethylation makes the CMC can be water-soluble and monovalent salt solution, and cellulosic carboxymethylation mixed ether can not only water-soluble and monovalent salt solution, and can be dissolved in the divalent alkaline-earth metal salts solution, even can be dissolved in heavy metal divalence barium salt solution.Three free hydroxyl groups are arranged on each glucose unit in the cellulose macromolecule, and etherification reaction all occurs on this trihydroxy-, and what substitution value and molar substitution were represented is exactly the number that three hydroxyls participate in reaction.Substitution value increases, and it is water-soluble to help the anti-acid carboxymethyl cellulose, and in acid, the salts solution, molar substitution is big more, and then antiacid, the saline-alkaline tolerance of anti-acid carboxymethyl cellulose increase.Under acid solution or metal ion influence, the viscosity of the viscosity ratio of Xylo-Mucine (CMC) in solution in pure water of not passing through modification has decline by a relatively large margin, its reason is that carboxymethyl is electronegative behind dissociation in water among the CMC, the repulsion of identical charges comes the CMC molecular stretching, and its viscosity in aqueous solution increases; When under acid solution or metal ion influence, gegenion makes CMC lose the part water of hydration, and interacts with carboxymethyl, and electric charge is cancelled, and charge repulsion weakens, and the molecular chain kindliness increases, and reels, and viscosity reduces.Through the anti-acid carboxymethyl cellulose after the modification; not only contain a certain amount of carboxymethyl group; and contain a certain amount of nonionic group; when it and electronegative group near the time can form hydrogen bond; carboxymethyl is greatly weakened the gegenion magnetism; add that the nonionic group is bigger; space steric effect also makes carboxymethyl group not be subject to the attack of gegenion; thereby the stable of protection hydration layer is not damaged; therefore; anti-acid carboxymethyl cellulose after the modification, it is acidproof, salt resistance ability obviously strengthens.
Patent US3,448, the 100 step synthesis reaction schemes of introducing are long, and intermediate product need pass through purification process, and the consumption amount of chemicals used is big, and reaction time is long, and product falls that to gather degree big, and viscosity is low.Patent USP2618632 uses Virahol to react, because that Virahol and hydroxyalkylation are the side reaction that takes place between the epoxide is many, the utilization ratio of epoxide is low, and salt tolerance is relatively poor, can not be used for occasions such as petroleum drilling.The clear 62-151402 of patent uses the Virahol of specific concentrations, after alkalizing under given conditions, carries out carboxylation alkylation and hydroxyalkylation again, obtains the good carboxyalkyl hydroxylalkyl fiber of salt tolerance.But above method often uses big liquor ratio or polycomponent blended organic solvent to make thinner in order to obtain to replace uniform product, causes separated from solvent to reclaim difficulty, and economical effectiveness is dissatisfied.
Summary of the invention
It is simple to the purpose of this invention is to provide a kind of production process technology, reaction time is short, facility investment is few, the production that raw material consumption is low has the method for the modified carboxy methyl cellulose sodium of high acidproof, salt tolerant, the modified carboxy methyl cellulose sodium that adopts this method to produce, the good solubility that not only has carboxymethyl cellulose sodium, simultaneously it is antiacid, saline-alkaline tolerance significantly strengthens.
Technical scheme of the present invention is:
A, cotton fibre torn up after, with the aqueous sodium hydroxide solution of 30-55%, drop in the kneader together with the aqueous ethanolic solution of concentration 70-98%; Wherein, the quality ratio of cotton fibre and sodium hydroxide is 1: 1.6-4.2, and the alcoholic acid quality is 0.5-8 a times of cotton fibre;
After b, the end that feeds intake, get rid of the air in the kneader, make vacuum tightness reach 0.002MPa at least;
C, rare gas element is charged in the kneader, make the kneader internal pressure greater than 0.1MPa;
D, vacuumize more than repeating, the operation of filling with inert gas 2-3 time, drain the interior air of reactor as far as possible;
E, carry out quaternization under protection of inert gas, alkalization time is 40-90 minute, and alkalization temperature is 10-40 ℃;
After f, alkalization finish, carry out etherification reaction.Be etherifying agent with the chloroacetic ethanolic soln of 50-80% earlier, the quality ratio of cotton fibre and etherifying agent is 1: 0.8-2.0, in 60 minutes, equably etherifying agent is sprayed to kneader, carry out carboxymethylation reaction, then another kind of etherifying agent being adopted vacuum to inhale the mode that adds adds in the kneader, temperature is increased to 60-90 ℃, continues reaction 50-100 minute.The mass ratio of another kind of etherifying agent and cotton fibre is 0.15-0.35: 1.Another kind of etherifying agent is selected chloropropane, propylene glycol of chlorine, propylene oxide or epoxy chloropropane for use.
G, through after washing, neutralization, centrifugal, dry, the pulverizing, obtain the acid-resistant sodium carboxymethylcellulose finished product.
The inventive method production process technology is simple, and reaction time is short, and facility investment is few, and raw material consumption is low, and the modified carboxy methyl cellulose sodium that adopts this method to produce not only has the good solubility of carboxymethyl cellulose sodium, and it is antiacid simultaneously, saline-alkaline tolerance significantly strengthens.
Description of drawings
Fig. 1 is this preparation method's a process flow sheet;
Embodiment
The present invention is further illustrated below in conjunction with embodiment.
Embodiment 1:
With 1 times of cotton fibre that tears up, 1.3 doubly 30% aqueous sodium hydroxide solution and 1.5 times of 90% ethanolic soln drop in the kneader simultaneously, get rid of air in the kneader, make vacuum tightness reach 0.002MPa, rare gas element is charged in the kneader, pressure reaches 0.1MPa, and vacuumize more than repeating, filling with inert gas operation 2-3 time, stir alkalization after 40 minutes, to spray equably to kneader with respect to the chloroacetic ethanolic soln (strength of solution 50-80%) of 0.9 times of cotton quality, carry out carboxymethylation reaction.The employing vacuum is inhaled in the another kind of etherifying agent chloropropane adding kneader of mode with 0.15 times of cotton quality that adds, temperature is increased to 60-90 ℃, continue reaction 50 minutes, obtain rough modified carboxy methyl cellulose sodium, through washing, neutralization, centrifugal, dry, obtain refining Xylo-Mucine finished product after the pulverizing, substitution value is 0.94, purity is 98%, 2% solution viscosity that NDJ-79 type viscometer is measured is 1700mPaS, is mixed with 2% citric acid (0.1mol/L) solution, and viscosity is 1600mPaS, acid is sticking than being 0.94, be mixed with 2%NaCl solution, viscosity is 1740mPaS, and salt is sticking than 1.02.
Embodiment 2:
With 1 times of cotton fibre that tears up, 1.2 doubly 40% aqueous sodium hydroxide solution and 1.7 times of 90% ethanolic soln drop in the kneader simultaneously, get rid of air in the kneader, make vacuum tightness reach 0.002MPa, rare gas element is charged in the kneader, pressure reaches 0.1MPa, and vacuumize more than repeating, filling with inert gas operation 2-3 time, stir alkalization after 60 minutes, 0.8 times of chloroacetic ethanolic soln (strength of solution 50-80%) is sprayed equably to kneader, carry out carboxymethylation reaction.The employing vacuum is inhaled in the another kind of etherifying agent propylene glycol of chlorine adding kneader of mode with 0.2 times of cotton quality that adds, temperature is increased to 60-90 ℃, continue reaction 60 minutes, obtain rough modified carboxy methyl cellulose sodium, through washing, neutralization, centrifugal, dry, obtain refining Xylo-Mucine finished product after the pulverizing, substitution value is 0.85, purity is 98.5%, 2% solution viscosity that NDJ-79 type viscometer is measured is 1600mPaS, is mixed with 2% citric acid (0.1mol/L) solution, and viscosity is 1470mPaS, acid is sticking than being 0.92, be mixed with 2%NaCl solution, viscosity is 1670mPaS, and salt is sticking than 1.04.
Embodiment 3:
With 1 times of cotton fibre that tears up, 1 times of 40% aqueous sodium hydroxide solution and 2 times of 90% ethanolic soln drop in the kneader simultaneously, get rid of air in the kneader, make vacuum tightness reach 0.002MPa, rare gas element is charged in the kneader, pressure reaches 0.1MPa, and vacuumize more than repeating, filling with inert gas operation 2-3 time, stir alkalization after 60 minutes, 0.7 times of chloroacetic ethanolic soln of cotton quality (strength of solution 50-80%) is sprayed equably to kneader, carry out carboxymethylation reaction.The employing vacuum is inhaled in the another kind of etherifying agent propylene oxide adding kneader of mode with 0.2 times of cotton quality that adds, temperature is increased to 60-90 ℃, continue reaction 60 minutes, obtain rough modified carboxy methyl cellulose sodium, through washing, neutralization, centrifugal, dry, obtain refining Xylo-Mucine finished product after the pulverizing, substitution value is 0.80, purity is 98.5%, 2% solution viscosity that NDJ-79 type viscometer is measured is 1500mPaS, is mixed with 2% citric acid (0.1mol/L) solution, and viscosity is 1335mPaS, acid is sticking than being 0.89, be mixed with 2%NaCl solution, viscosity is 1620mPaS, and salt is sticking than 1.08.
Embodiment 4:
With 1 times of cotton fibre that tears up, 1.3 doubly 40% aqueous sodium hydroxide solution and 1.7 times of 90% ethanolic soln drop in the kneader simultaneously, get rid of air in the kneader, make vacuum tightness reach 0.002MPa, rare gas element is charged in the kneader, pressure reaches 0.1MPa, and vacuumize more than repeating, filling with inert gas operation 2-3 time, stir alkalization after 90 minutes, 0.9 times of chloroacetic ethanolic soln of cotton quality (strength of solution 50-80%) is sprayed equably to kneader, carry out carboxymethylation reaction.The mode that adopts the vacuum suction to add adds 0.2 times of another kind of etherifying agent propylene glycol of chlorine of cotton quality in the kneader, temperature is increased to 60-90 ℃, continue reaction 90 minutes, obtain rough modified carboxy methyl cellulose sodium, through washing, neutralization, centrifugal, dry, obtain refining Xylo-Mucine finished product after the pulverizing, substitution value is 0.96, purity is 98%, 2% solution viscosity that NDJ-79 type viscometer is measured is 1750mPaS, is mixed with 2% citric acid (0.1mol/L) solution, and viscosity is 1680mPaS, acid is sticking than being 0.96, be mixed with 2%NaCl solution, viscosity is 1870mPaS, and salt is sticking than 1.07.
Embodiment 5:
With 1 times of cotton fibre that tears up, 1.2 doubly 40% aqueous sodium hydroxide solution and 2.7 times of 90% ethanolic soln drop in the kneader simultaneously, get rid of air in the kneader, make vacuum tightness reach 0.002MPa, rare gas element is charged in the kneader, pressure reaches 0.1MPa, and vacuumize more than repeating, filling with inert gas operation 2-3 time, stir alkalization after 90 minutes, 0.9 times of chloroacetic ethanolic soln of cotton quality (strength of solution 50-80%) is sprayed equably to kneader, carry out carboxymethylation reaction.The mode that adopts the vacuum suction to add adds 0.3 times of another kind of etherifying agent epoxy chloropropane of cotton quality in the kneader, temperature is increased to 60-90 ℃, continue reaction 100 minutes, obtain rough modified carboxy methyl cellulose sodium, through washing, neutralization, centrifugal, dry, obtain refining Xylo-Mucine finished product after the pulverizing, substitution value is 0.82, purity is 98%, 2% solution viscosity that NDJ-79 type viscometer is measured is 1470mPaS, is mixed with 2% citric acid (0.1mol/L) solution, and viscosity is 1370mPaS, acid is sticking than being 0.93, be mixed with 2%NaCl solution, viscosity is 1620mPaS, and salt is sticking than 1.10.
Term:
Viscosity: 2% aqueous solution, NDJ-79 type rotary viscometer detects under 25 ℃ of conditions
Substitution value (D.S): detect according to 5.5 methods among the GB 1904-2005 " foodstuff additive Xylo-Mucine ".
Purity:, obtain with minusing again according to ASTM D1439-03 standard detection sodium-chlor and sodium glycolate content.
Claims (5)
1. the preparation method of an acid-resistant sodium carboxymethylcellulose, described mode is the cotton fibre that 1 times is torn up, 1.3 doubly 30% aqueous sodium hydroxide solution and 1.5 times of 90% ethanolic soln drop in the kneader simultaneously, get rid of air in the kneader, make vacuum tightness reach 0.002MPa, rare gas element is charged in the kneader, pressure reaches 0.1MPa, and vacuumize more than repeating, filling with inert gas operation 2-3 time, stir alkalization after 40 minutes, to spray equably with respect to the chloroacetic ethanolic soln of 0.9 times of cotton quality to kneader then, ethanolic soln concentration 50-80% carries out carboxymethylation reaction; The mode that adopts vacuum to inhale again to add adds the another kind of etherifying agent chloropropane of 0.15 times of cotton quality in the kneader, and temperature is increased to 60-90 ℃, continues reaction 50 minutes, obtains rough modified carboxy methyl cellulose sodium; Through washing, neutralization, centrifugal, dry, obtain making with extra care the Xylo-Mucine finished product after pulverizing; The substitution value of described finished product is 0.94, purity is 98%, 2% solution viscosity that NDJ-79 type viscometer is measured is 1700mPaS, with concentration is that the citric acid of 0.1mol/L is mixed with 2% citric acid solution, viscosity is 1600mPaS, and acid is sticking than being 0.94, is mixed with 2%NaCl solution, viscosity is 1740mPaS, and salt is sticking than 1.02.
2. the preparation method of an acid-resistant sodium carboxymethylcellulose, described method is the cotton fibre that 1 times is torn up, 1.2 doubly 40% aqueous sodium hydroxide solution and 1.7 times of 90% ethanolic soln drop in the kneader simultaneously, get rid of air in the kneader, make vacuum tightness reach 0.002MPa, rare gas element is charged in the kneader, pressure reaches 0.1MPa, and vacuumize more than repeating, filling with inert gas operation 2-3 time, stir alkalization after 60 minutes, 0.8 times of chloroacetic ethanolic soln is sprayed equably to kneader, and ethanolic soln concentration is 50-80%, carries out carboxymethylation reaction; The mode that adopts vacuum to inhale again to add adds the another kind of etherifying agent propylene glycol of chlorine of 0.2 times of cotton quality in the kneader, and temperature is increased to 60-90 ℃, continues reaction 60 minutes, obtains rough modified carboxy methyl cellulose sodium; Through washing, neutralization, centrifugal, dry, obtain making with extra care the Xylo-Mucine finished product after pulverizing; Substitution value is 0.85, purity is 98.5%, 2% solution viscosity that NDJ-79 type viscometer is measured is 1600mPaS, with concentration is that the citric acid of 0.1mol/L is mixed with 2% citric acid solution, viscosity is 1470mPaS, and acid is sticking than being 0.92, is mixed with 2%NaCl solution, viscosity is 1670mPaS, and salt is sticking than 1.04.
3. the preparation method of an acid-resistant sodium carboxymethylcellulose, described method is the cotton fibre that 1 times is torn up, 1 times of 40% aqueous sodium hydroxide solution and 2 times of 90% ethanolic soln drop in the kneader simultaneously, get rid of air in the kneader, make vacuum tightness reach 0.002MPa, rare gas element is charged in the kneader, pressure reaches 0.1MPa, and vacuumize more than repeating, filling with inert gas operation 2-3 time, stir alkalization after 60 minutes, 0.7 times of chloroacetic ethanolic soln of cotton quality is sprayed equably to kneader, and ethanolic soln concentration is 50-80%, carries out carboxymethylation reaction; The mode that adopts vacuum to inhale again to add adds the another kind of etherifying agent propylene oxide of 0.2 times of cotton quality in the kneader, and temperature is increased to 60-90 ℃, continues reaction 60 minutes, obtains rough modified carboxy methyl cellulose sodium; Through washing, neutralization, centrifugal, dry, obtain making with extra care the Xylo-Mucine finished product after pulverizing; Substitution value is 0.80, purity is 98.5%, 2% solution viscosity that NDJ-79 type viscometer is measured is 1500mPaS, with concentration is that the citric acid of 0.1mol/L is mixed with 2% citric acid solution, viscosity is 1335mPaS, and acid is sticking than being 0.89, is mixed with 2%NaCl solution, viscosity is 1620mPaS, and salt is sticking than 1.08.
4. the preparation method of an acid-resistant sodium carboxymethylcellulose, described method is the cotton fibre that 1 times is torn up, 1.3 doubly 40% aqueous sodium hydroxide solution and 1.7 times of 90% ethanolic soln drop in the kneader simultaneously, get rid of air in the kneader, make vacuum tightness reach 0.002MPa, rare gas element is charged in the kneader, pressure reaches 0.1MPa, and vacuumize more than repeating, filling with inert gas operation 2-3 time, stir alkalization after 90 minutes, 0.9 times of chloroacetic ethanolic soln of cotton quality is sprayed equably to kneader, and ethanolic soln concentration is 50-80%, carries out carboxymethylation reaction; The mode that adopts the vacuum suction to add again adds 0.2 times of another kind of etherifying agent propylene glycol of chlorine of cotton quality in the kneader, and temperature is increased to 60-90 ℃, continues reaction 90 minutes, obtains rough modified carboxy methyl cellulose sodium; Through washing, neutralization, centrifugal, dry, obtain making with extra care the Xylo-Mucine finished product after pulverizing; Substitution value is 0.96, purity is 98%, 2% solution viscosity that NDJ-79 type viscometer is measured is 1750mPaS, with concentration is that the citric acid of 0.1mol/L is mixed with 2% citric acid solution, viscosity is 1680mPaS, and acid is sticking than being 0.96, is mixed with 2%NaCl solution, viscosity is 1870mPaS, and salt is sticking than 1.07.
5. the preparation method of an acid-resistant sodium carboxymethylcellulose, described method is the cotton fibre that 1 times is torn up, 1.2 doubly 40% aqueous sodium hydroxide solution and 2.7 times of 90% ethanolic soln drop in the kneader simultaneously, get rid of air in the kneader, make vacuum tightness reach 0.002MPa, rare gas element is charged in the kneader, pressure reaches 0.1MPa, and vacuumize more than repeating, filling with inert gas operation 2-3 time, stir alkalization after 90 minutes, 0.9 times of chloroacetic ethanolic soln of cotton quality is sprayed equably to kneader, and ethanolic soln concentration is 50-80%, carries out carboxymethylation reaction; The mode that adopts the vacuum suction to add again adds 0.3 times of another kind of etherifying agent epoxy chloropropane of cotton quality in the kneader, and temperature is increased to 60-90 ℃, continues reaction 100 minutes, obtains rough modified carboxy methyl cellulose sodium; Through washing, neutralization, centrifugal, dry, obtain making with extra care the Xylo-Mucine finished product after pulverizing; Substitution value is 0.82, purity is 98%, 2% solution viscosity that NDJ-79 type viscometer is measured is 1470mPaS, with concentration is that the citric acid of 0.1mol/L is mixed with 2% citric acid solution, viscosity is 1370mPaS, and acid is sticking than being 0.93, is mixed with 2%NaCl solution, viscosity is 1620mPaS, and salt is sticking than 1.10.
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