CN104387476A - Preparation method of food-grade sodium carboxymethyl cellulose (CMC) with high purity and relatively-high viscosity - Google Patents

Preparation method of food-grade sodium carboxymethyl cellulose (CMC) with high purity and relatively-high viscosity Download PDF

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CN104387476A
CN104387476A CN201410737763.4A CN201410737763A CN104387476A CN 104387476 A CN104387476 A CN 104387476A CN 201410737763 A CN201410737763 A CN 201410737763A CN 104387476 A CN104387476 A CN 104387476A
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food
viscosity
preparation
purity
xylo
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CN104387476B (en
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蔡银华
乐义华
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SHANGHAI SHENGUANG EDIBLE CHEMICALS Co Ltd
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SHANGHAI SHENGUANG EDIBLE CHEMICALS Co Ltd
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Abstract

The invention relates to a preparation method of food-grade sodium carboxymethyl cellulose (CMC) with high purity and relatively-high viscosity, belonging to the technical field of sodium CMC production. The preparation method comprises the following steps of adding ethanol and liquid caustic soda with high concentration into cotton fibers; then, adding an etherifying agent, and adding concentrated alkaline and the etherifying agent after reacting for a period of time; next, etherifying until ending the etherification reaction; and finally, neutralizing, washing, removing a solution, drying and crushing to obtain the food-grade sodium CMC with relatively-high viscosity. The food-grade sodium CMC disclosed by the invention is relatively-high in substitution degree and viscosity and has the 1% Brookfield viscosity of more than 6000CPS (measured by using a type-B viscometer) and the purity of higher than 99.5%. The CMC is clear in solution and stable in viscosity.

Description

The preparation method of food-class high-purity viscosity higher Xylo-Mucine
Technical field
The present invention relates to a kind of preparation method of food-class high-purity viscosity higher Xylo-Mucine, 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, almost odorless, 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 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 1.5g/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% one 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 animal and vegetable oil, protein and aqueous solution white peony root emulsifying property, 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.
Along with the standard of living of people improves day by day, the food health for oneself is more and more paid attention to.Milk preparation is a wherein indispensable integral part.The CMC of high-quality can make milk preparation prevent point newborn layer and juice layer, adds product protein content.Prevent its aging and expose in high temperature environments, milk preparation occur dehydration or occur that whey is separated, the phenomenon of milk preparation viscosity degradation in sterilizing process can also be prevented.Glutinous sliding sense when milk preparation is drunk can be increased, make it without glutinous sense and stiff sense.And food-class high-purity viscosity higher Xylo-Mucine has more good result of use in this respect.
Application number is 201210161733.4, publication number is the preparation method that the preparation method of a kind of ultrahigh-viscosity sodium carboxymethyl cellulose of Chinese patent application of CN 102675474A discloses a kind of ultrahigh-viscosity sodium carboxymethyl cellulose, it take purified cotton as main raw material, with with the mixing solutions of aqueous ethanolic solution and water for reaction medium, the operations such as, ovens dry dry through alkalization, etherificate, washing, rake, pulverizing are refined and are formed, simultaneously in order to ensure the effect that alkalizes, add a certain amount of alkali while alkalization to improve acid-utilising rate.Only illustrate in patent CN102675474A that viscosity is more than 10000mPa.s, not mentioned substitution value and purity problem.Only mention substitution value at his example 7 and be only 0.57, and substitution value and viscosity are inversely proportional to, in this patent, the viscosity of products obtained therefrom is higher, therefore substitution value is lower; And the purity of ultrahigh-viscosity sodium carboxymethyl cellulose that obtains of above-mentioned preparation method is lower than 98% after measured, in standard GB/T 1904-2005, regulation purity cannot use as food grade lower than 98%.Preparation method needs in patent CN 102675474A repeatedly pour rare gas element and vacuumize, process is loaded down with trivial details.
Application number is 201210287380.2, publication number is the preparation method that the preparation method of the Chinese patent application height salt tolerant high-viscosity sodium carboxymethyl cellulose of CN 102775503A discloses a kind of high salt tolerant high-viscosity sodium carboxymethyl cellulose, the method take purified cotton as cellulosic material, the step comprised has cellulosic alkalization, the etherificate of soda cellulose; It is characterized in that, the mean polymerisation degree of described purified cotton is 3000 ~ 3300.Illustrate in patent CN 102775503A that its product main application is used in oilfield exploitation, be partial to industrial application, this product is not suitable in food.
What be mainly used in food service industry in prior art has high purity (purity >=99.5%), high substitution value (substitution value >=0.9), and 1%Brookfield type glues >=6000mPa.s Xylo-Mucine product.Prior art is prepared in the method for Xylo-Mucine product to be needed repeatedly pour rare gas element and vacuumize, and process is loaded down with trivial details, and the present invention is intended to design the preparation method that only once need pour rare gas element, and process is more simple, more convenient operation.
A preparation method for food-class high-purity viscosity higher Xylo-Mucine, described preparation method comprises the steps:
A. alkalize
Cotton fibre (mean polymerisation degree is at 2600-2700), mass concentration 40-50% aqueous sodium hydroxide solution and mass concentration 85-95% ethanolic soln are added in alkalization kneader (common ' S ' axle kneader) simultaneously and stir (cotton fibre: aqueous sodium hydroxide solution: the mass ratio of ethanolic soln is 1:1.4-2.8:1.5-2.0, aqueous sodium hydroxide solution and ethanolic soln are pre-mixed evenly), process temperature controls at 30-50 DEG C, and the time is 40-80 minute;
B. etherificate
Etherifying agent sprayed equably on material in 20-40 minute, etherifying agent is the Mono Chloro Acetic Acid ethanolic soln (mass ratio of cotton fibre and etherifying agent is 1:0.9-2.0) of mass concentration 60-80%, then material is entered etherificate kneader (common ' S ' axle kneader) from alkalization kneader, the temperature of etherification reaction progressively raises, control at 60-80 DEG C, reaction 60-120 minute.
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
Be cooled to 40-60 DEG C of discharging, through neutralization, 70-80% (volume percent) ethanolic soln is repeatedly used to wash by a certain percentage, cellulosic material and ethanolic soln mass ratio are 1:(10-20), de-liquid, then obtain purity >=99.5% food-grade high-purity food grade viscosity higher Xylo-Mucine after dried, crushed.
In steps A, preferably, cotton fibre: aqueous sodium hydroxide solution: the mass ratio of ethanolic soln is 1:1.8-2.2:1.6-1.7.
In step B, preferably, the mass ratio of cotton fibre and etherifying agent is 1:1.5-1.8.
Alkalization kneader, etherificate kneader are CMC coventional type biaxial kneader, and model is: NH-100, and manufacturer is that machine works is mediated in Nantong banburying.
The high purity of indication of the present invention refers to CMC purity >=98%; Viscosity higher refers to CMC Brookfield viscometer (Brookfield) 1% >=6000cps.
The invention has the beneficial effects as follows:
1. preparation method is simple.
2. by selecting the cotton fibre of high-polymerization degree and producing the method that whole process pours rare gas element, the high-viscosity sodium carboxymethyl cellulose produced has high substitution value, high viscosity, Brookfield viscometer (Brookfield) 1% is the feature of more than 600OCPS, purity more than 99.5%.
3. the viscosity carboxymethyl cellulose sodium good water solubility of producing, solution is bright, stable viscosity, is particularly suitable for dense milk preparation and uses.
What be mainly used in food service industry in prior art has high purity (purity >=99.5%), high substitution value (substitution value >=0.9), and 1%Brookfield type glues >=6000mPa.s Xylo-Mucine product.Need repeatedly pour rare gas element and vacuumize in the method for this product of preparation of prior art, process is loaded down with trivial details, and the present invention is intended to design the preparation method that only once need pour rare gas element, and process is more simple, more convenient operation.
In prior art, the mean polymerisation degree of cotton fiber material used is at 3000-3300, and the starting material cotton fibre mean polymerisation degree selected by the present invention is at 2600-2700, more broad, technically more reasonable on starting material are selected.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of food-class high-purity viscosity higher Xylo-Mucine.
The technical solution adopted in the present invention is:
Embodiment
Below by specific embodiment, technical scheme of the present invention is described in further detail.
Embodiment 1
By 1kg cotton fibre, (Nantong Yao Hua Mierocrystalline cellulose company limited, model are M-1000, the polymerization degree is 2650) add in kneader (aqueous sodium hydroxide solution mixes in advance with ethanol) with 1.8kg 50% aqueous sodium hydroxide solution and the ethanol of 1.6Okg 95% simultaneously, under stirring, be warmed up to 35-45 DEG C, stir 60 minutes.Chloroacetic for 1.5kg ethanolic soln (chloroacetic concentration 70%) is sprayed in kneader equably; then etherification reaction is carried out; progressively be warming up to 70-80 DEG C; etherification reaction 70 minutes; in whole process, constantly pass into the viscosity that nitrogen protection makes be not destroyed, O.3-0.4MPa nitrogen pressure remains on.Be cooled to 40-60 DEG C of discharging, neutralization, washing, de-liquid, oven dry, pulverizing obtain high-purity grade of food grade high-viscosity sodium carboxymethyl cellulose.Substitution value 0.95, Type B (Brookfield) 1% viscosity 7679cps, purity 99.5%, cmc solution is bright.
Embodiment 2
By 1kg cotton fibre, (Nantong Yao Hua Mierocrystalline cellulose company limited, model are M-1000, the polymerization degree is 2650) add in kneader (aqueous sodium hydroxide solution mixes in advance with ethanol) with 2.0kg 45% aqueous sodium hydroxide solution and the ethanol of 1.6kg 95% simultaneously, under stirring, be warmed up to 35-45 DEG C, stir 60 minutes.Chloroacetic for 1.5kg ethanolic soln (chloroacetic concentration 75%) is sprayed in kneader equably; then etherification reaction is carried out; progressively be warming up to 70-80 DEG C; etherification reaction 80 minutes; in whole process, constantly pass into the viscosity that nitrogen protection makes be not destroyed, nitrogen pressure remains on 0.3-O.4MPa.Be cooled to 40-60 DEG C of discharging, neutralization, washing, de-liquid, oven dry, pulverizing obtain high-purity grade of food grade high-viscosity sodium carboxymethyl cellulose.Substitution value 0.97, Type B (Brookfield) 1% viscosity 735Ocps, purity 99.5%, cmc solution is bright.The mensuration of substitution value is carried out with reference to GB 1904-2005 testing standard.
Embodiment 3
By 1kg cotton fibre, (Nantong Yao Hua Mierocrystalline cellulose company limited, model are M-1000, the polymerization degree is 2650) add in kneader (aqueous sodium hydroxide solution mixes in advance with ethanol) with 2.2kg 48% aqueous sodium hydroxide solution and the ethanol of 1.7kg 95% simultaneously, under stirring, be warmed up to 35-45 DEG C, stir 60 minutes.Chloroacetic for 1.8kg ethanolic soln (chloroacetic concentration 70%) is sprayed equably and then carry out etherification reaction to kneader; progressively be warming up to 70-80 DEG C; etherification reaction 80 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 40-60 DEG C of discharging, neutralization, washing, de-liquid, oven dry, pulverizing obtain high-purity grade of food grade high-viscosity sodium carboxymethyl cellulose.Substitution value 0.99, Type B (Brookfield) 1% viscosity 6998cps, purity 99.5%, cmc solution is bright.The mensuration of substitution value is carried out with reference to GB 1904-2005 testing standard.
Embodiment 4
By 1kg cotton fibre, (Nantong Yao Hua Mierocrystalline cellulose company limited, model are M-1000, the polymerization degree is 2700) add in kneader (aqueous sodium hydroxide solution mixes in advance with ethanol) with 1.4kg 40% aqueous sodium hydroxide solution and the ethanol of 1.5kg 85% simultaneously, under stirring, be warmed up to 30-35 DEG C, stir 40 minutes.Chloroacetic for 0.9kg ethanolic soln (chloroacetic concentration 60%) is sprayed in kneader equably; then etherification reaction is carried out; progressively be warming up to 70-80 DEG C; etherification 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.Lower the temperature 40-60 DEG C of discharging, neutralization, washing, de-liquid, oven dry, pulverizing obtains high-purity grade of food grade high-viscosity sodium carboxymethyl cellulose.Substitution value 0.9, Type B (Brookfield) 1% viscosity 8300cps, purity 99.5%, cmc solution is bright.The mensuration of substitution value is carried out with reference to GB 1904-2005 testing standard.
Embodiment 5
By 1kg cotton fibre, (Nantong Yao Hua Mierocrystalline cellulose company limited, model are M-1000, the polymerization degree is 2600) add in kneader (aqueous sodium hydroxide solution mixes in advance with ethanol) with 2.8kg 50% aqueous sodium hydroxide solution and the ethanol of 2.0kg 85% simultaneously, under stirring, be warmed up to 45-50 DEG C, stir 80 minutes.Chloroacetic for 2.0kg ethanolic soln (chloroacetic concentration 80%) is sprayed in kneader equably; then etherification reaction is carried out; progressively be warming up to 65-75 DEG C; etherification 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.Lower the temperature 40-60 DEG C of discharging, neutralization, washing, de-liquid, oven dry, pulverizing obtains high-purity grade of food grade high-viscosity sodium carboxymethyl cellulose.Substitution value 1.05, Type B (Brookfield) 1% viscosity 6013cps, purity 99.5%, cmc solution is bright.The mensuration of substitution value is carried out with reference to GB 1904-2005 testing standard.
Comparative example
By 1kg cotton fibre, (Nantong Yao Hua Mierocrystalline cellulose company limited, model are M-1000, the polymerization degree is 2650) add in kneader (aqueous sodium hydroxide solution mixes in advance with ethanol) with 2.0kg 45% aqueous sodium hydroxide solution and the ethanol of 1.6kg 95% simultaneously, under stirring, be warmed up to 35-45 DEG C, stir 60 minute hands.Spray in kneader equably by chloroacetic for 1.5kg ethanolic soln (chloroacetic concentration 75%), then carry out etherification reaction, be progressively warming up to 70-80 DEG C, etherification reaction 80 minutes, whole process does not pass into rare gas element.Be cooled to 40-60 DEG C of discharging, neutralization, washing, de-liquid, oven dry, pulverizing obtain the high-purity grade of sticky Xylo-Mucine of food grade height.Substitution value 0.97, Type B (Brookfield) 1% viscosity 2564cps, purity 99.5%, cmc solution is bright.
The illogical protection of inert gas of whole process in comparative example, other conditions are identical with example 2, but 1% viscosity results only has 2564cps, differ huge with 1% viscosity 735Ocps in example 2.Viscosity improves fairly obvious.
Above comparative example and embodiment medium 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 ".
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 (5)

1. a preparation method for food-class high-purity viscosity higher Xylo-Mucine, carries out according to following step:
A. alkalize
Mean polymerisation degree is added in alkalization kneader at the cotton fibre of 2600-2700, mass concentration 40-50% aqueous sodium hydroxide solution and mass concentration 85-95% ethanolic soln simultaneously and stirs, wherein cotton fibre: aqueous sodium hydroxide solution: the mass ratio of ethanolic soln is 1:1.4-2.8:1.5-2.0, aqueous sodium hydroxide solution and ethanolic soln are pre-mixed evenly, whipping process temperature controls at 30-50 DEG C, and the time is 40-80 minute;
B. etherificate
Etherifying agent sprayed equably on material in 20-40 minute, etherifying agent is the Mono Chloro Acetic Acid ethanolic soln of mass concentration 60-80%, wherein the mass ratio of cotton fibre and etherifying agent is 1:0.9-2.0, then material is entered etherificate kneader from alkalization kneader, the temperature of etherification reaction progressively raises, control at 60-80 DEG C, reaction 60-120 minute;
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
Be cooled to 40-60 DEG C of discharging, after washing, neutralization, de-liquid, oven dry, pulverizing, obtain the sticky Xylo-Mucine finished product of food-class high-purity height.
2. the preparation method of a kind of food-class high-purity viscosity higher Xylo-Mucine according to claim 1, it is characterized in that, washing step in step C is specially: wash more than 2 times with volume percent 70-80% ethanolic soln, and cellulosic material and ethanolic soln mass ratio are 1:10-20.
3. the preparation method of a kind of food-class high-purity viscosity higher Xylo-Mucine according to claim 1, is characterized in that in steps A, cotton fibre: aqueous sodium hydroxide solution: the mass ratio of ethanolic soln is 1:1.8-2.2:1.6-1.7.
4. the preparation method of a kind of food-class high-purity viscosity higher Xylo-Mucine according to claim 1, is characterized in that in step B, and the mass ratio of cotton fibre and etherifying agent is 1:1.5-1.8.
5. the preparation method of a kind of food-class high-purity viscosity higher Xylo-Mucine according to claim 1, is characterized in that described alkalization kneader, etherificate kneader is CMC coventional type biaxial kneader.
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104761646A (en) * 2015-04-02 2015-07-08 佛山市富实新高分子纤维有限公司 Preparation method of sodium carboxymethylcellulose with long shelf life
CN111187355A (en) * 2018-11-14 2020-05-22 河南正弘药用辅料股份有限公司 Production method of 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

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3574188A (en) * 1969-03-04 1971-04-06 Dai Ichi Kogyo Seiyaku Co Ltd Process for preparing carboxymethyl cellulose or its alkali salt of high viscosity
CN101033256A (en) * 2007-03-09 2007-09-12 北京理工大学 Method of preparing high viscosity carboxymethyl cellulose by slurry method
CN101445561A (en) * 2008-06-20 2009-06-03 淄博宜龙化工有限公司 Preparing method of carboxymethyl cellulose with high viscosity and obtained product

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3574188A (en) * 1969-03-04 1971-04-06 Dai Ichi Kogyo Seiyaku Co Ltd Process for preparing carboxymethyl cellulose or its alkali salt of high viscosity
CN101033256A (en) * 2007-03-09 2007-09-12 北京理工大学 Method of preparing high viscosity carboxymethyl cellulose by slurry method
CN101445561A (en) * 2008-06-20 2009-06-03 淄博宜龙化工有限公司 Preparing method of carboxymethyl cellulose with high viscosity and obtained product

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104761646A (en) * 2015-04-02 2015-07-08 佛山市富实新高分子纤维有限公司 Preparation method of sodium carboxymethylcellulose with long shelf life
CN111187355A (en) * 2018-11-14 2020-05-22 河南正弘药用辅料股份有限公司 Production method of 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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