CN104448009A - Preparation method of food-grade acid-resisting sodium carboxymethyl cellulose - Google Patents
Preparation method of food-grade acid-resisting sodium carboxymethyl cellulose Download PDFInfo
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Abstract
The invention relates to a preparation method of food-grade acid-resisting sodium carboxymethyl cellulose and belongs to the technical field of the production of sodium carboxymethyl cellulose. The invention aims at providing a preparation method for producing high-purity food-grade acid-resisting sodium carboxymethyl cellulose which is medium in viscosity and substitution degree by virtue of two kneading machines. The preparation method comprises the following steps: preparing cotton fiber and wood pulp fiber according to certain proportions, adding ethanol and caustic soda liquid with a high concentration to cellulose in accordance with a specially designed formula and carrying out an alkalization reaction; then adding an etherifying agent and carrying out an etherification reaction; and after the etherification reaction is ended, neutralizing and washing, removing liquid, drying and grinding to obtain the food-grade CMC. The product disclosed by the invention is not only good in solubility, but also relatively strong in acid resistance and salt resistance; and the preparation method is simple in production process, short in reaction cycle, free from extra equipment investment and low in raw material consumption.
Description
Technical field
The present invention relates to a kind of preparation method of food grade acid-resistant sodium carboxymethylcellulose, belong to Xylo-Mucine production technical field.
Background technology
Xylo-Mucine is the sodium salt of carboxymethyl cellulose ether, belongs to anionic ether of cellulose, is white or oyster white fibrous powder or particle, density 0.5-0.7 gram/cc, all odorlesses, tasteless, tool water absorbability.Be easy to be dispersed in water into clear gum solution, insoluble in the organic solvents such as ethanol.1% aqueous solution pH is 6.5-8.5, and as pH > 10 or < 5, cement viscosity significantly reduces, and when pH=7, performance is best.To thermally-stabilised, below 20 DEG C, viscosity rises rapidly, and when 45 DEG C, change is comparatively slow, and more than 80 DEG C long-time heating can make its colloid sex change and viscosity and performance obviously decline.Soluble in water, solution is transparent; Very stable in basic solution, meet acid then facile hydrolysis, when pH value is 2-3, there will be precipitation, meet polyvalent metal salt and also can react appearance precipitation.
Pure CMC is used for food by FAO and WHO approved, and it just gets the Green Light after being through very strict biology, toxicologic study and test, and the safe intake (ADI) of international standard is 25mg/ (kgd), i.e. everyone 1.59/d about.Once it was reported that, someone tests intake and reaches 10kg also not toxic reaction.CMC is not only good emulsifying stablizer, thickening material in food applications, and has and excellent to freeze, melt stability, and can improve the local flavor of product, prolongation storage time.Consumption in soymilk, ice-creams, ice cream, jelly, beverage, can is about 1%-1.5%.CMC also can be stable with forming property such as vinegar, soy sauce, vegetables oil, fruit juice, gravy, vegetables juice emulsified dispersed liquid, its consumption is 0.2%-0.5%.Particularly very excellent to the emulsifying property of animal and vegetable oil, protein and the aqueous solution, the homogeneous milk sap that its forming property is stable can be made.Because it is safe and reliable, therefore, its consumption does not limit by national food hygienic standard ADI.CMC is constantly developed at field of food.
Yogurt drink is sour-sweet moderate, smooth good to eat, not only remains the flavour of Yoghourt, has also possessed most of nutrition and the function of Yoghourt.And moderate, be thus deeply subject to the favor, particularly children of consumers in general in China, China's liquid milk market occupies rapidly suitable share, and the rate of rise of annual guarantor about 20%.Yogurt drink is a kind of with fresh milk, recovery milk and soymilk are main raw material, add other sweeting agents, stablizer, the auxiliary material such as essence and pigment, active bacteria is utilized to carry out lactic fermentation or directly add fruit juice, the pH that the auxiliary material allotments such as food acids obtain is between 3.8 to 4.2, the milk-contained drink that protein content is greater than 1%. in order to meet human consumer's demand growing to yogurt drink, dairy enterprises is devoted to the yogurt drink product produced and Development Finance is various, but fat floating and protein precipitation govern production and the exploitation of yogurt drink product always.Because the casein in yogurt drink easily coagulation sedimentation occurs in acid condition, and milk-contained drink is a kind of suspensoid, a kind of Unstable Systems of emulsoil and true solution mixing, therefore aborning, quality product is difficult to control, easy appearance is cotton-shaped, layering, the phenomenons such as precipitation, and shelf-lives is short, having a strong impact on the development of yogurt drink. the additive playing food stability effect has thickening material and the large class of emulsifying agent two, by the viscosity using stablizer to increase yogurt drink dispersion medium, reduce protein settling speed, prevent the generation of protein precipitation, thus improve the stability of yogurt drink.
CMC, as a kind of stablizer, is applied to yogurt drink, in the products such as Yoghourt, requires higher to acid resistance.Low acid is sticky replaces lack of homogeneity than CMC, and acid resistance is poor, can make Yoghourt, milky-drinks generation layering, and the phenomenons such as precipitation, obviously can not meet the demand of user.For this reason, exploitation and research are prepared anti-acid CMC and are had realistic meaning and application prospect widely.The present invention, by the adjustment to composition and engineering, makes the existing better solvability of CMC of producing, has again higher acidproof, can be widely used in Yoghourt, in the products such as yogurt drink.
Application number is 200810069337.2, and the preparation method of a kind of acid-resistant sodium carboxymethylcellulose of Chinese invention patent of publication number CN101280023A discloses a kind of method adopting kneading method industrial production high viscosity, high substitution value acid-resistant sodium carboxymethylcellulose.It is before alkalinization, first gets rid of the air in kneader, when vacuum tightness reaches at least after 0.002MPa, is filled with by rare gas element in kneader, makes pressure be greater than 0.1MPa.Whole alkalinization carries out under protection of inert gas, first cook etherifying agent with the chloroacetic ethanolic soln of 50-80%, the mass values of cotton fibre and etherifying agent is 1:0.8-2.0, sprays etherifying agent in kneader equably, carry out carboxymethylation reaction in 60 minutes; Then modified-reaction is carried out with another kind of etherifying agent, another kind of etherifying agent selects chloropropane, propylene glycol of chlorine, propylene oxide or epoxy chloropropane, be 0.15-0.35:1 with the mass ratio of cotton fibre, adopting vacuum to inhale the mode added adds in kneader, temperature is increased to 60-90 DEG C, continues reaction 50-100 minute; Through washing, neutralization, centrifugal, dry, pulverizing after, obtain acid-resistant sodium carboxymethylcellulose finished product.The method adopts linking agent epoxy chloropropane to CMC modification, improves acid resistance and salt resistant character, Be very effective, but can affect the food safety of CMC due to the toxicity of linking agent, generally can only be applied to industrial circle, as oil production etc.And improve the acid resistance of CMC, so do not affect the food safety of CMC, can field of food be widely used in.
Application number is 200910175262.0, the preparation method of the Chinese invention patent high acid resistance sodium carboxymethyl cellulose for foods of publication number CN101724076A discloses a kind of preparation method of high acid resistance sodium carboxymethyl cellulose for foods, continuously air lift, drying and pulverize each operation successively carry out and make product refining by the quaternization of quaternization device, colter reactor etherification reaction, neutralization washing three times.This patent, mainly by transformation conversion unit, adopts plough coulter type reactor to carry out etherification reaction to improve acid resistance.Although food safety is no problem, plough coulter type reactor price is more expensive, and facility investment is higher, concerning domestic CMC producer, have certain difficulty.And the present invention still uses traditional coventional type biaxial kneader, but improved the acid resistance of CMC by the adjustment of technique and formula.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of food grade acid-resistant sodium carboxymethylcellulose, the particularly preparation method of the acid-resistant sodium carboxymethylcellulose of a kind of medium-viscosity and substitution value.
The technical solution adopted for the present invention to solve the technical problems is:
A preparation method for food grade acid-resistant sodium carboxymethylcellulose, comprises the steps:
A. alkalize
A certain proportion of cellulosic material, mass concentration 40-50% aqueous sodium hydroxide solution and mass concentration 85-95% ethanolic soln are added in alkalization kneader simultaneously and stir (aqueous sodium hydroxide solution and ethanolic soln are pre-mixed evenly), process temperature controls at 20-50 DEG C, and the time is 40-80 minute;
Wherein cellulosic material comprises exquisite gossypin and wood pulp cellulose, and cotton fibre accounts for the 20-60% of cellulosic material quality; Wherein the mass ratio of mass concentration 40-50% aqueous sodium hydroxide solution and cellulosic material is 1-1.5:1; Wherein the mass ratio of 85-95% ethanolic soln and cellulosic material is 1.5-2:1.
B. etherificate
Material is entered etherificate kneader from alkalization kneader, etherifying agent sprayed equably on material in 20-40 minute, etherifying agent is the Mono Chloro Acetic Acid ethanolic soln (the Mono Chloro Acetic Acid ethanolic soln of mass concentration 50-80% and cellulosic material mass ratio are 0.8-1.2:1) of quality of chloroacetic acid concentration 50-80%, the temperature of etherification reaction progressively raises, control at 40-80 DEG C, reaction 30-120 minute, is then cooled to 40-60 DEG C.In the whole process of steps A and B, constantly pass into nitrogen protection makes viscosity not be destroyed, and nitrogen pressure remains on 0.3 to 0.4MPa.
C. washing and drying
Cooling discharge, through neutralization, washing, de-liquid, then obtain food grade acid-resistant sodium carboxymethylcellulose finished product after dried, crushed.
Wherein in steps A, the mean polymerisation degree of wood pulp cellulose is 1000-1100DP, and the mean polymerisation degree of gossypin is 2500-2800DP.
Alkalization and etherificate kneader are coventional type CMC biaxial kneader.
Wherein wood pulp cellulose is Chilean silver-colored star wood pulp, and model is M-950, and cotton fibre is Nantong Yao Hua Mierocrystalline cellulose company limited, and model is M-1000.
The medium substitution value CMC of indication of the present invention refers to that CMC substitution value is within the scope of 0.85-0.95; Medium-viscosity refers to CMC Brookfield viscometer (Brookfield) 1%200-500cps; Anti-acid CMC refers to that CMC acid is sticky and compares >0.65.
The invention has the beneficial effects as follows:
1, preparation method is simple.Also do not use linking agent, safety non-toxic, product meets the requirement that pure CMC is used for food by FAO and WHO approved;
2, by the adjustment (ratio of adjustment cotton fibre and wood pulp cellulose of composition and engineering, the ratio of liquid caustic soda and cellulosic material, the ratio of etherifying agent and cellulosic material) the food-class high-purity acid-resistant sodium carboxymethylcellulose produced has medium substitution value, medium-viscosity, Brookfield viscometer (Brookfield) 1% is 200-400CPS, purity more than 99.5%, acid resistance is good, and acid is sticky than the feature being greater than 70%.
The food-class high-purity acid-resistant sodium carboxymethylcellulose good water solubility of 3, producing, solution is limpid, stable viscosity, be specially adapted to Yoghourt, liquid state milk, soymilk, and in the acidic drinks such as fruit juice, and adapt to the conventional sterilization process such as overtemperature sterilizing (UHT) and pasteurize (pasteurized).
Embodiment
Below by specific embodiment, technical scheme of the present invention is described in further detail.
Embodiment 1
By 1kg cotton fibre and wood pulp cellulose, (wherein wood pulp cellulose is Chilean silver-colored star wood pulp, model is M-950, cotton fibre is Nantong Yao Hua Mierocrystalline cellulose company limited, model is M-100) mixture (mass ratio of cotton fibre and wood pulp cellulose is 3:2, the mean polymerisation degree of wood pulp cellulose is 1000DP, the mean polymerisation degree of gossypin is 2600DP) add in kneader with the ethanol of 1.25kg 50% aqueous sodium hydroxide solution and 1.7kg 95% simultaneously, under stirring, be warmed up to 20-40 DEG C, stir 60 minutes.Chloroacetic for 0.9kg mass concentration 70% ethanolic soln (chloroacetic mass concentration 70%) is sprayed in kneader equably; then etherification reaction is carried out; progressively heat up; 70-80 DEG C of reaction 30 minutes; in whole process, constantly pass into the viscosity that nitrogen protection makes be not destroyed, nitrogen pressure remains on 0.3-0.4MPa.Be cooled to 50 DEG C of dischargings, neutralization, washing, de-liquid, oven dry, pulverizing obtain food grade acid-resistant sodium carboxymethylcellulose.Substitution value 0.89, Type B (Brookfield) 1% viscosity 325cps, purity 99.8%, acid is sticky than 0.84.
Embodiment 2
By 1kg cotton fibre and wood pulp cellulose, (wherein wood pulp cellulose is Chilean silver-colored star wood pulp, model is M-950, cotton fibre is Nantong Yao Hua Mierocrystalline cellulose company limited, model is M-100) mixture (mass ratio of cotton fibre and wood pulp cellulose is 2:3, the mean polymerisation degree of wood pulp cellulose is 1050DP, the mean polymerisation degree of gossypin is 2550DP) add in kneader with the ethanol of 1.3kg 50% aqueous sodium hydroxide solution and 1.7kg 95% simultaneously, under stirring, be warmed up to 20-40 DEG C, stir 60 minutes.Chloroacetic for 1.0kg mass concentration 70% ethanolic soln (chloroacetic mass concentration 70%) is sprayed in kneader equably; then etherification reaction is carried out; progressively heat up; 70-80 DEG C of reaction 30 minutes; in whole process, constantly pass into the viscosity that nitrogen protection makes be not destroyed, nitrogen pressure remains on 0.3-0.4M.pa.Be cooled to 50 DEG C of dischargings, neutralization, washing, de-liquid, oven dry, pulverizing obtain food grade acid-resistant sodium carboxymethylcellulose.Substitution value 0.90, Type B (Brookfield) 1% viscosity 285cps, purity 99.7%, acid is sticky than 0.72.
Embodiment 3
By 1kg cotton fibre and wood pulp cellulose, (wherein wood pulp cellulose is Chilean silver-colored star wood pulp, model is M-950, cotton fibre is Nantong Yao Hua Mierocrystalline cellulose company limited, model is M-100) mixture (mass ratio of cotton fibre and wood pulp cellulose is l:4, the mean polymerisation degree of wood pulp cellulose is 1100DP, the mean polymerisation degree of gossypin is 2650DP) add in kneader with the ethanol of 1.28kg 50% aqueous sodium hydroxide solution and 1.7kg 95% simultaneously, under stirring, be warmed up to 20-40 DEG C, stir 60 minutes.The chloroacetic ethanolic soln (chloroacetic mass concentration 70%) of 0.95kg mass concentration 70% is sprayed in kneader equably; then etherification reaction is carried out; progressively heat up; 70-80 DEG C of reaction 30 minutes; in whole process, constantly pass into the viscosity that nitrogen protection makes be not destroyed, nitrogen pressure remains on 0.3-0.4M.pa.Be cooled to 50 DEG C of dischargings, neutralization, washing, de-liquid, oven dry, pulverizing obtain food grade acid-resistant sodium carboxymethylcellulose.Substitution value 0.91, Type B (Brookfield) 1% viscosity 302cps, purity 99.6%, acid is sticky than 0.67.
Embodiment 4
By 1kg cotton fibre and wood pulp cellulose, (wherein wood pulp cellulose is Chilean silver-colored star wood pulp, model is M-950, cotton fibre is Nantong Yao Hua Mierocrystalline cellulose company limited, model is M-100) mixture (mass ratio of cotton fibre and wood pulp cellulose is 1:4, the mean polymerisation degree of wood pulp cellulose is 1000DP, the mean polymerisation degree of gossypin is 2500DP) add in kneader with the ethanol of 1.4kg 50% aqueous sodium hydroxide solution and 1.7kg 95% simultaneously, under stirring, be warmed up to 20-40 DEG C, stir 60 minutes.The chloroacetic ethanolic soln (chloroacetic mass concentration 70%) of 1.1kg mass concentration 70% is sprayed in kneader equably; then etherification reaction is carried out; progressively heat up; 70-80 DEG C of reaction 30 minutes; in whole process, constantly pass into the viscosity that nitrogen protection makes be not destroyed, nitrogen pressure remains on 0.3-0.4MPa.Be cooled to 50 DEG C of dischargings, neutralization, washing, de-liquid, oven dry, pulverizing obtain food grade acid-resistant sodium carboxymethylcellulose.Substitution value 0.94, Type B (Brookfield) 1% viscosity 278cps, purity 99.5%, acid is sticky than 0.68.
Embodiment 5
By 1kg cotton fibre and wood pulp cellulose, (wherein wood pulp cellulose is Chilean silver-colored star wood pulp, model is M-950, cotton fibre is Nantong Yao Hua Mierocrystalline cellulose company limited, model is M-100) mixture (mass ratio of cotton fibre and wood pulp cellulose is 1:4, the mean polymerisation degree of wood pulp cellulose is 1000DP, the mean polymerisation degree of gossypin is 2500DP) add in kneader with the ethanol of 1kg 40% aqueous sodium hydroxide solution and 1.5kg85% simultaneously, under stirring, be warmed up to 20-30 DEG C, stir 40 minutes.The chloroacetic ethanolic soln (chloroacetic mass concentration 50%) of 0.8kg mass concentration 50% is sprayed in kneader equably; then etherification reaction is carried out; progressively heat up; 40-70 DEG C of reaction 60 minutes; in whole process, constantly pass into the viscosity that nitrogen protection makes be not destroyed, nitrogen pressure remains on 0.3-0.4MPa.Be cooled to 40 DEG C of dischargings, neutralization, washing, de-liquid, oven dry, pulverizing obtain food grade acid-resistant sodium carboxymethylcellulose.Substitution value 0.85, Type B (Brookfield) 1% viscosity 310cps, purity 99.8%, acid is sticky than 0.66.
Embodiment 6
By 1kg cotton fibre and wood pulp cellulose, (wherein wood pulp cellulose is Chilean silver-colored star wood pulp, model is M-950, cotton fibre is Nantong Yao Hua Mierocrystalline cellulose company limited, model is M-100) mixture (mass ratio of cotton fibre and wood pulp cellulose is 1:4, the mean polymerisation degree of wood pulp cellulose is 1100DP, the mean polymerisation degree of gossypin is 2800DP) add in kneader with the ethanol of 1.5kg 50% aqueous sodium hydroxide solution and 2kg95% simultaneously, under stirring, be warmed up to 40-50 DEG C, stir 80 minutes.The chloroacetic ethanolic soln (chloroacetic mass concentration 80%) of 1.2kg mass concentration 80% is sprayed in kneader equably; then etherification reaction is carried out; progressively heat up; 70-80 DEG C of reaction 120 minutes; in whole process, constantly pass into the viscosity that nitrogen protection makes be not destroyed, nitrogen pressure remains on 0.3-0.4MPa.Be cooled to 60 DEG C of dischargings, neutralization, washing, de-liquid, oven dry, pulverizing obtain food grade acid-resistant sodium carboxymethylcellulose.Substitution value 0.95, Type B (Brookfield) 1% viscosity 255cps, purity 99.3%, acid is sticky than 0.65.
Comparative example 1
In reference background technology, application number is 200810069337.2, embodiment 1 in the preparation method of a kind of acid-resistant sodium carboxymethylcellulose of Chinese invention patent of publication number CN101280023A:
By the cotton fibre that 1 times is torn up, 1.3 times of 30% aqueous sodium hydroxide solution and 1.5 times of 90% ethanolic soln drop in kneader simultaneously, get rid of air in kneader, vacuum tightness is made to reach 0.002MPa, rare gas element is filled with in kneader, pressure reaches 0.1MPa, and repeat above vacuumizing, filling with inert gas operation 2-3 time, stir alkalization after 40 minutes, chloroacetic ethanolic soln (strength of solution 50-80%) relative to cotton quality 0.9 times is evenly sprayed in kneader, carries out carboxymethylation reaction.Adopting vacuum to inhale the mode added adds in kneader by the another kind of etherifying agent epoxy chloropropane of cotton quality 0.15 times, temperature is increased to 60-90 DEG C, continue reaction 50 minutes, obtain rough modified carboxy methyl cellulose sodium, through washing, neutralization, centrifugal, dry, exquisite Xylo-Mucine finished product is obtained after pulverizing, substitution value is 0.94, purity is 98%, 2% solution viscosity of NDJ-79 type viscosity meter is 1700mPaS, being mixed with 2% citric acid (0.1mol/L) soltion viscosity is 1600mPaS, acid is sticky than being 0.94, preparation 2%NaCl solution, viscosity is 1740mPaS, salt is sticky than being 1.02.
Comparative example 2
In reference background technology, application number is 200910175262.0, the embodiment 1 in the preparation method of the Chinese invention patent high acid resistance sodium carboxymethyl cellulose for foods of publication number CN101724076A:
Preparation method of the present invention is by the quaternization of quaternization device, colter reactor etherification reaction, neutralization washing is refined for three times, continuous stripping, dry and pulverize each operation (step) and carry out successively and make high acid resistance sodium carboxymethyl cellulose product, the method specifically comprises the steps: (1) by parts by weight be first 100 cellulosic material (be 50 containing parts by weight, mean polymerisation degree is the wood pulp cellulose smashed of 1000DP, and parts by weight are 50, mean polymerisation degree is the exquisite gossypin torn up with hand of 2300DP), be 400 with parts by weight, concentration of volume percent be 94% alcohol solvent and parts by weight be 130, weight percent concentration is the mixed solution of the aqueous sodium hydroxide solution of 48%, be added to quaternization device simultaneously and carry out quaternization, its joining day can be controlled in 21-25 minute.Quaternization 80 minutes, alkalization temperature is 16 DEG C.After quaternization terminates, adding parts by weight is 90, and weight percent concentration is 78%, and temperature is the Mono Chloro Acetic Acid ethanolic soln of 10 DEG C, feed time is 80 minutes, and churning time is 15 minutes, and then blowing is in colter reactor.(2) in colter reactor, carry out etherification reaction, in 30 minutes, be slowly warmed up to 78 DEG C, and keep this temperature under agitation, make material carry out etherification reaction 30 minutes.(insulation terminates rear) material cools to 50 DEG C of dischargings, i.e. obtained Xylo-Mucine raw product.(3) then carry out neutralization washing three times to refine, continuous air lift, dry and pulverize each operation.Obtain high purity, high acid resistance sodium carboxymethyl cellulose product.
By above-mentioned obtained product physical and chemical index by " foodstuff additive Xylo-Mucine " GB1904-2005 standard test, viscosity presses massfraction 1% aqueous solution, with Brookfield type viscometer viscosimetric, another acid adding is sticky than detecting, detection method is with to survey solution viscosity method in GB 1904-2005 national standard identical, just distilled water changes 0.1N aqueous citric acid solution into, then the viscosity number of the CMC measured in acid solution is gone than the viscosity number of CMC in distilled water, namely acid is sticky than (AVR), result and quality product as shown in the table:
| Viscosity mpa.s | Substitution value | Purity % | PH value | Moisture % | The sticky ratio of acid | |
| Embodiment 1 | 350 | 0.95 | 99.7 | 7.0 | 8 | 0.78 |
Test example
Acid is sticky than detecting, detection method is with to survey solution viscosity method in GB 1904-2005 national standard identical, just distilled water changes 0.1N aqueous citric acid solution into, then go than the viscosity number of CMC in distilled water by the viscosity number of the CMC measured in acid solution, namely acid is sticky than (AVR).
Viscosity: 1% aqueous solution, Brookfield type viscosity apparatus, detects under 25 DEG C of conditions.
Substitution value (DS): detect according to 5.5 methods in GB 1904-2005 " foodstuff additive Xylo-Mucine ".
Purity: detect sodium-chlor and sodium glycolate content according to 5.8 methods in ASTM D1439-03 standard or GB 1904-2005 " foodstuff additive Xylo-Mucine ", then obtain with minusing.
Product standard: according to GB 1904-2005 " foodstuff additive Xylo-Mucine ".
The contrast of the common CMC of embodiments of the invention CMC and existing food grade sees the following form 1:
The testing data of table 1 Embodiment C MC and existing food grade CMC
The present invention and 2 two commercially available CMC FH9 are at medium substitution value as can be seen from the table, but when optimum proportioning of the present invention acid sticky than reaching that 0.84 is obviously better than two commercially available CMC FH9 0.60, have better result of use at milk preparation.Although it is substantially identical that the present invention and comparative example 2 compare data, the equipment that we use in whole making processes is more generally general, and the reaction times significantly shortens, and respectively has advantage.
Above-described embodiment is one of the present invention preferably scheme, not does any pro forma restriction to the present invention, also has other variant and remodeling under the prerequisite not exceeding the technical scheme described in claim.
Claims (3)
1. a preparation method for food grade acid-resistant sodium carboxymethylcellulose, carries out according to following step:
A. alkalize
Cellulosic material, mass concentration 40-50% aqueous sodium hydroxide solution and mass concentration 85-95% ethanolic soln are added in alkalization kneader simultaneously and stir, aqueous sodium hydroxide solution and ethanolic soln are pre-mixed evenly, process temperature controls at 20-50 DEG C, and the time is 40-80 minute;
Wherein cellulosic material comprises exquisite gossypin and wood pulp cellulose, and cotton fibre accounts for the 20-60% of cellulosic material quality; Wherein the mass ratio of mass concentration 40-50% aqueous sodium hydroxide solution and cellulosic material is 1-2.5:1; Wherein the mass ratio of 85-95% ethanolic soln and cellulosic material is 1.5-2:1;
B. etherificate
Material is entered etherificate kneader from alkalization kneader, etherifying agent sprayed equably on material in 20-40 minute, etherifying agent is the Mono Chloro Acetic Acid ethanolic soln of quality of chloroacetic acid concentration 50-80%, wherein the Mono Chloro Acetic Acid ethanolic soln of mass concentration 50-80% and cellulosic material mass ratio are 0.8-2.0:1, the temperature of etherification reaction progressively raises, control at 40-80 DEG C, reaction 30-120 minute, is then cooled to 40-60 DEG C; In the whole process of steps A and B, constantly pass into nitrogen protection, nitrogen pressure remains on 0.3 to 0.4MPa;
C. washing and drying
Cooling discharge, through neutralization, washing, de-liquid, then obtain food grade acid-resistant sodium carboxymethylcellulose finished product after dried, crushed.
2. the preparation method of a kind of food grade acid-resistant sodium carboxymethylcellulose according to claim 1, is characterized in that, wherein in steps A, the mean polymerisation degree of wood pulp cellulose is 1000-1100DP, and the mean polymerisation degree of gossypin is 1500-2800DP.
3. the preparation method of a kind of food grade acid-resistant sodium carboxymethylcellulose according to claim 1, is characterized in that, wherein alkalization and etherificate kneader are coventional type CMC biaxial kneader.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110128553A (en) * | 2019-05-15 | 2019-08-16 | 上海长光企业发展有限公司 | A kind of cellulose gum and its preparation method and application |
| CN112679620A (en) * | 2020-12-28 | 2021-04-20 | 江苏派克斯特纤维素有限公司 | Preparation method of instant sodium carboxymethylcellulose |
| CN112707969A (en) * | 2020-12-28 | 2021-04-27 | 常熟威怡科技有限公司 | Production process of sodium carboxymethylcellulose by self-esterification reaction |
-
2014
- 2014-12-05 CN CN201410741883.1A patent/CN104448009A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110128553A (en) * | 2019-05-15 | 2019-08-16 | 上海长光企业发展有限公司 | A kind of cellulose gum and its preparation method and application |
| CN112679620A (en) * | 2020-12-28 | 2021-04-20 | 江苏派克斯特纤维素有限公司 | Preparation method of instant sodium carboxymethylcellulose |
| CN112707969A (en) * | 2020-12-28 | 2021-04-27 | 常熟威怡科技有限公司 | Production process of sodium carboxymethylcellulose by self-esterification reaction |
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