CN106432515B - A kind of preparation method and applications of carboxymethyl cellulose with high degree sodium - Google Patents
A kind of preparation method and applications of carboxymethyl cellulose with high degree sodium Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B11/00—Preparation of cellulose ethers
- C08B11/02—Alkyl or cycloalkyl ethers
- C08B11/04—Alkyl or cycloalkyl ethers with substituted hydrocarbon radicals
- C08B11/10—Alkyl or cycloalkyl ethers with substituted hydrocarbon radicals substituted with acid radicals
- C08B11/12—Alkyl or cycloalkyl ethers with substituted hydrocarbon radicals substituted with acid radicals substituted with carboxylic radicals, e.g. carboxymethylcellulose [CMC]
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
- D06P1/44—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders
- D06P1/46—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders using compositions containing natural macromolecular substances or derivatives thereof
- D06P1/48—Derivatives of carbohydrates
- D06P1/50—Derivatives of cellulose
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Abstract
The present invention relates to a kind of preparation method of carboxymethyl cellulose with high degree sodium, comprise the following steps：（1）Pre- alkaline wine mixed solution is stand-by；（2）Alkalized again using sodium carboxymethylcellulose as raw material；（3）Carry out etherification reaction；（4）Carry out washing centrifugation and solvent recovery；（5）Carry out dries pulverizing and batch mixing packaging；Present invention also offers the application of the preparation method, and it is applied in reactive printing gum.The preparation technology of the present invention is easy and effective, is etherified efficiency high, salinity removal efficiency is high, is easy to dries pulverizing, the production capacity of production line obtains to be played to the limit, and the sodium carboxymethylcellulose produced has extra-high substitution degree（DS1.7 2.2), the higher viscosity (15000mpas of 2% aqueous solution Brookfield types 3000）And purity（90‑98%）, suitable for reactive printing gum.
Description
Technical field
The invention belongs to the production field of sodium carboxymethylcellulose, and in particular to a kind of carboxymethyl cellulose with high degree sodium
Preparation method and its application in reactive printing gum.
Background technology
Sodium carboxymethylcellulose（Na-CMC）Be native cellulose it is chemically modified obtain a kind of there is ethers structure
Derivative.It is a kind of important industrial water soluble polymer, traditionally referred to as CMC.CMC is formed with certain after being dissolved in water
The colloidal solution of viscosity, there is thickening, bonding, film forming, Protection glue, keep the effect such as moisture, emulsification and suspension, be widely used in more
Kind industrial circle.
Printing gum is the high-molecular compound that thickening power is played in print paste, and traditional printing gum is mainly using sea
Mosanom, but sodium alginate electrolyte resistance is poor, easily goes mouldy, and Storage period is short, and paste making rate is low, and use cost is high；It is high in recent years
Substitution degree, high-viscosity sodium carboxymethyl cellulose substitution sodium alginate are widely used as reactive printing gum, mesh
Before be commonly used in reactive printing gum CMC substitution value be about 1.1-1.7.With the continuous development of dyeing, especially
It is that fabric feeling, color yield, definition etc. are required to improve, the CMC of this substitution value can not meet reactive printing
The needs of thickener.Higher substitution degree, as DS1.7-2.4 sodium carboxymethylcellulose product is developed.
Preparing the method for the CMC product of high degree of substitution and high viscosity has a lot, such as with wadding fibrous plain for original after shredding
Material, by the kneading method technique of the low range solvent for the etherificate that repeatedly alkalizes, substep improves CMC of the substitution value acquisition compared with high substituted degree
Product；Or using the cellulose powder of certain fineness as raw material, using the aq slurry process of big multiplying power solvent, it is etherified by improving
Efficiency, obtain the CMC product compared with high substituted degree.
The CMC product that high substituted degree is prepared using these processes is usually constructed with some drawbacks：Repeatedly alkalization is etherified
The technical process of kneading method is unfavorable for improving the viscosity of product, while the heating down cycles of continuous several times are tight to device damage
Weight；The easy aquation caking of product, salinity are not easy to remove in washing process；CMC cakings are serious after ethanol is reclaimed and dried, and crush tired
It is difficult；Particularly repeatedly the kneading method technique of alkalization etherificate is set by consersion unit, washing centrifugation apparatus, distillation equipment and freezing
Standby limitation, when producing extra-high substitution value CMC product (DS1.7-2.2), the production capacity of production line is reduced to conventional substitution
Spend CMC product（DS0.8-1.0）The 35 ~ 45% of product, the cost of product is caused to improve by a larger margin.Aq slurry process is using different
Propyl alcohol is solvent, and the ratio of fibrillation and isopropanol is about 1:8 ~ 30, therefore solvent-oil ratio is big, process time length, production capacity is low,
Valuable product；Most importantly, due to aq slurry process does not possess cost performance, therefore slurry in conventional CMC productions are manufactured
Method technique is not yet popularized at home, and aq slurry process and the equipment of kneading method technique is not general, is set for existing kneading method
For standby, aq slurry process does not apply to.
Patent 201210582442.2 is to prepare extra low viscose degree carboxymethyl cellulose using low-viscosity sodium carboxymethyl cellulose
Sodium, belong to CMC post-processing, CMC viscosity is changed by adding thinner, due to not carrying out alkalization etherification reaction, no
The substitution value for being related to CMC changes；But the method involved by the patent can not be carried out using existing equipment, it is necessary to additionally increase anti-
Answer equipment, production cost is higher.
The content of the invention
Problem to be solved by this invention is to overcome that current extra-high substitution value CMC's is low, viscous into efficiency is etherified during production
Spend the shortcomings that low, desalination is difficult, production capacity is inexpensive high, there is provided a kind of height substitutes and substitution value stabilization, high viscosity, purity are high, de-
Salt effect is good, production cost is low, can be widely applied for the preparation method of industrial carboxymethyl cellulose with high degree sodium,
Present invention simultaneously provides its application in reactive printing gum.
The technical solution adopted by the present invention is：
A kind of preparation method of carboxymethyl cellulose with high degree sodium, including alkalization etherificate, washing centrifugation, dries pulverizing and
Batch mixing packaging process, sodium carboxymethylcellulose is used as raw material；Specifically comprise the following steps：
（1）By the sodium hydrate aqueous solution and 160-250 parts by weight volume fractions that 80-150 parts by weight mass fraction is 50%
Mixed for 85-93% ethanol water, be cooled to 18-30 DEG C, obtain alkali wine；
（2）By the sodium carboxymethylcellulose raw material and step that 100 parts by weight substitution values are 0.6-1.4（1）Gained alkali wine is equal
Even mixing carries out quaternization；
（3）By the monoxone ethanol that 0-0.5 parts by weight epoxy chloropropane and 100-200 parts by weight mass fraction are 70-75%
The aqueous solution mix, then with step（2）Product uniformly mix, 20-40 DEG C of controlling reaction temperature；Then 20-30 points are stirred
Clock, 25-40 DEG C of controlling reaction temperature；Mixture is delivered into methyltertiarvbutyl ether reactor, 75-80 DEG C of controlling reaction temperature, reaction time 60-
120 minutes；
（4）Step（3）It is after end, gains are water-soluble in the ethanol that 1800-2500 parts by weight volume fraction is 75-85%
Liquid washs, and centrifugation, reclaims ethanol；
（5）Drying, crush, packaging, produce.
It is further to improve, step（2）The quaternization is carried out in reactor is mediated；
Step（2）Quaternization is specially：Sodium carboxymethylcellulose raw material and alkali wine are uniformly added into and mediated in reactor,
The addition time of sodium carboxymethylcellulose raw material is 15-25 minutes, and alkali wine mixed solution sprays minute time 20-30；Alkali wine sprays
After leaching, 0-35 parts by weight solids sodium hydroxides are added, uniform stirring 30-40 minutes, carry out quaternization, quaternization temperature
Degree control is at 15-25 DEG C.
It is further to improve, step（2）Middle sodium carboxymethylcellulose raw material is powdery or cotton-shaped, preferably cotton-shaped.
It is further to improve, step（2）The substitution value of middle sodium carboxymethylcellulose raw material is 0.8-1.2, preferably 0.9-
1.0。
It is further to improve, step（2）The moisture of middle sodium carboxymethylcellulose raw material is 3-12%, preferably 5-10%,
More preferably 6-8%.
It is further to improve, step（2）The input quality of middle sodium carboxymethylcellulose raw material and the ratio of kneader volume
For 1.6-15, preferably 1:8-12, more preferably 1:9-11.
It is further to improve, when being consersion unit from kneader, step（3）Specially：After the completion of alkalization, by 0-
0.5 parts by weight epoxy chloropropane and the monoxone ethanol water that 100-200 parts by weight mass fraction is 70-75% mix, and
It is even to be sprayed to containing step（2）In the kneading reactor of reactant, spray time 30-40 minutes, controlling reaction temperature 20-40
℃；After the completion of spray, 20-30 minutes, 25-40 DEG C of controlling reaction temperature are stirred；Mixture is delivered into methyltertiarvbutyl ether reactor, controlled
75-80 DEG C of reaction temperature processed, minute in reaction time 60-120；
Further improve, the washing in step (4) is 78-85% with the concentration of ethanol solution, more preferably 78-82%.
It is further to improve, step（4）The material that centrifugation is completed reclaims ethanol by steam stripper.
Invention also provides application of the preparation method in reactive printing gum.
The present invention uses the carboxymethyl cellulose raw material of fixed substitution value as reaction raw materials, in later basification and etherification procedure
In greatly reduce the side reaction of reaction and accessory substance produces, and improve the efficiency of quaternization and etherification reaction, only pass through
The operation of finite number of time, so that it may reach high substituted degree and high viscosity, there are the incomparable properties of product of prior art.
Conventionally employed cellulosic material is carried out in alkalization etherification procedure, and repeatedly alkalization can produce substantial amounts of accessory substance and pair is anti-
Answer product（It is referred to as by-product salt）, with gathering for by-product salt, the etherificate efficiency of reaction can decline.It is typically repeated operation 3-4
Secondary, substitution degree can just reach the substitution degree of the application, but be etherified efficiency and there was only 30-40%, and the application alkalizes equivalent to repetition
Etherificate 2 times, for etherificate efficiency up to 55-65%, this means very high efficiency in this area, can be brought to production a series of favourable
Condition.
The application uses substitution degree 0.6-1.4 CMC as raw material, mainly take into account etherificate efficiency, viscosity and production
The equalization problem of energy.The substitution value of raw material is too low, and viscosity easily improves, but substitution value is not easy to improve；Raw material substitution value is too high, takes
Easily improved for degree, viscosity is not easy to improve；Meanwhile the problem of being both related to yield, only by creative work,
Trial dare to be challenged, the substitution value scope in could selecting preferably, just easily existing equipment is utilized, production capacity is improved to highest.
The preparation method of the present invention does not need specific process equipment, mainly relies on existing kneader to can be achieved, and
Loss to production equipment is low, reduces production cost.
In quaternization, spray alkali carries out the addition of solid sodium hydroxide again after drinking, is advantageous to improve the substitution of product
Degree.
Any chemical manufacturing process can all run into the problem of new in industrial production is applied to.The preparation of the present invention
Method is particularly directed to industrial production, it is contemplated that the problems such as efficiency, production capacity in production, cost, optimized from parameters,
The program that suitable industrial production is promoted has been finally given, has been that inventor tests repeatedly in the line of industrial production one for many years, is created
The result drawn after the property made work, it is significant in actual production.
In the industrial production, the final substitution value that obtains is 1.7-2.2 to the present invention, purity 90-95%, 2%Brookfield water
The sodium carboxymethylcellulose product of solution viscosity 3000-15000mpas extra-high degree of substitution and high viscosity, so superior performance are
Prior art is incomparable.
The preparation method of the present invention is applied in reactive printing gum, is advantageous to improve feel, the color yield of dyeing and printing products
And definition.
Embodiment
Embodiment 1
(1) liquid caustic soda of 80 part of 50% mass fraction is mixed with 160 part of 93% volume fraction ethanol, and is cooled to 20 DEG C
Alkali wine mixed solution is stand-by；
(2) the cotton-shaped sodium carboxymethylcellulose of 100 parts of substitution values 0.9 is uniformly added into above-mentioned alkali wine mixed solution and pinched
Close in reactor, the 15 minutes addition time of sodium carboxymethylcellulose raw material, the alkali wine mixed solution 20 minutes time of spray；Alkali wine
35 parts of solid sodium hydroxides are added after spray and stir progress quaternization in 40 minutes, quaternization 25 DEG C of temperature of control；
(3) after the completion of alkalizing, the monoxone ethanol water of 120 part of 70% mass fraction is uniformly sprayed to kneading reaction
In device, spray time 40 minutes, 30 DEG C of controlling reaction temperature；After the completion of monoxone ethanol water spray, continue 20 points of mixing
Clock, 30 DEG C of controlling reaction temperature；
(4) said mixture is delivered in methyltertiarvbutyl ether reactor and carries out etherification reaction, 78 DEG C of controlling reaction temperature, reaction
100 minutes time；
(5) after etherification reaction terminates, by reaction mass with being washed in the ethanol solution of 2000 part of 82% volume fraction
Twice and centrifuge, the material for centrifuging completion reclaims ethanol by steam stripper；
(6) dries pulverizing and packaging are carried out after the completion of ethanol recovery, the final substitution value that obtains is 1.75, purity 95%, 2%
The sodium carboxymethylcellulose product of Brookfield solution viscosities 10000mpas extra-high degree of substitution and high viscosity.
Embodiment 2
(1) liquid caustic soda of 85 part of 50% mass fraction is mixed with 200 part of 93% volume fraction ethanol, and is cooled to 25 DEG C
Alkali wine mixed solution is stand-by；
(2) the powdery sodium carboxymethylcellulose of 100 parts of substitution values 1.0 is uniformly added into above-mentioned alkali wine mixed solution and pinched
Close in reactor, the 20 minutes addition time of sodium carboxymethylcellulose raw material, the alkali wine mixed solution 30 minutes time of spray；Alkali wine
20 parts of solid sodium hydroxides are added after spray and stir progress quaternization in 35 minutes, quaternization 25 DEG C of temperature of control；
(3) after the completion of alkalizing, by 0.5 part of epoxychloropropane and the monoxone ethanol water of 100 part of 70% mass fraction
Mixing, and be uniformly sprayed to and mediate in reactor, spray time 30 minutes, 40 DEG C of controlling reaction temperature；Monoxone ethanol is water-soluble
After the completion of liquid spray, continue mixing 20 minutes, 30 DEG C of controlling reaction temperature；
(4) said mixture is delivered in methyltertiarvbutyl ether reactor and carries out etherification reaction, 75 DEG C of controlling reaction temperature, reaction
100 minutes time；
(5) after etherification reaction terminates, by reaction mass with being washed in the ethanol solution of 2100 part of 78% volume fraction
Twice and centrifuge, the material for centrifuging completion reclaims ethanol by steam stripper；
(6) dries pulverizing and packaging are carried out after the completion of ethanol recovery, the final substitution value that obtains is 1.9 purity 92%, 2%
The sodium carboxymethylcellulose product of Brookfield solution viscosities 6700mpas extra-high degree of substitution and high viscosity.
Embodiment 3
(1) liquid caustic soda of 150 part of 50% mass fraction is mixed with 200 part of 90% volume fraction ethanol, and is cooled to 18 DEG C
Alkali wine mixed solution is stand-by；
(2) sodium carboxymethylcellulose that 100 parts of substitution values are 0.8 is uniformly added into kneading with above-mentioned alkali wine mixed solution
In reactor, the 20 minutes addition time of sodium carboxymethylcellulose raw material, the alkali wine mixed solution 25 minutes time of spray；Alkali wine sprays
25 parts of solid sodium hydroxides are added after leaching and stir progress quaternization in 30 minutes, quaternization 20 DEG C of temperature of control；
(3) after the completion of alkalizing, by 0.1 part of epoxychloropropane and the monoxone ethanol water of 150 part of 75% mass fraction
Mixing, and be uniformly sprayed to and mediate in reactor, spray time 30 minutes, 35 DEG C of controlling reaction temperature；Monoxone ethanol is water-soluble
After the completion of liquid spray, continue mixing 20 minutes, 35 DEG C of controlling reaction temperature；
(4) said mixture is delivered in methyltertiarvbutyl ether reactor and carries out etherification reaction, 78 DEG C of controlling reaction temperature, reaction
100 minutes time；
(5) after etherification reaction terminates, by reaction mass with being washed in the ethanol solution of 1800 part of 80% volume fraction
Twice and centrifuge, the material for centrifuging completion reclaims ethanol by steam stripper；
(6) dries pulverizing and packaging are carried out after the completion of ethanol recovery, the final substitution value that obtains is 1.75 purity 95%, 2%
The sodium carboxymethylcellulose product of Brookfield solution viscosities 8000mpas extra-high degree of substitution and high viscosity.
Embodiment 4
(1) liquid caustic soda of 100 part of 50% mass fraction is mixed with 250 part of 85% volume fraction ethanol, and is cooled to 30 DEG C
Alkali wine mixed solution is stand-by；
(2) sodium carboxymethylcellulose that 100 parts of substitution values are 1.2 is uniformly added into kneading with above-mentioned alkali wine mixed solution
In reactor, the 20 minutes addition time of sodium carboxymethylcellulose raw material, the alkali wine mixed solution 25 minutes time of spray；Alkali wine sprays
15 parts of solid sodium hydroxides are added after leaching and stir progress quaternization in 30 minutes, quaternization 20 DEG C of temperature of control；
(3) after the completion of alkalizing, by 0.25 part of epoxychloropropane and the monoxone ethanol water of 200 part of 72% mass fraction
Mixing, and be uniformly sprayed to and mediate in reactor, spray time 30 minutes, 35 DEG C of controlling reaction temperature；Monoxone ethanol is water-soluble
After the completion of liquid spray, continue mixing 20 minutes, 35 DEG C of controlling reaction temperature；
(4) said mixture is delivered in methyltertiarvbutyl ether reactor and carries out etherification reaction, 78 DEG C of controlling reaction temperature, reaction
100 minutes time；
(5) after etherification reaction terminates, by reaction mass with being washed in the ethanol solution of 2500 part of 75% volume fraction
Twice and centrifuge, the material for centrifuging completion reclaims ethanol by steam stripper；
(6) dries pulverizing and packaging are carried out after the completion of ethanol recovery, the final substitution value that obtains is 1.85, purity 93%, 2%
The sodium carboxymethylcellulose product of Brookfield solution viscosities 6500mpas extra-high degree of substitution and high viscosity.
Embodiment 5
(1) liquid caustic soda of 110 part of 50% mass fraction is mixed with 220 part of 87% volume fraction ethanol, and is cooled to 25 DEG C
Alkali wine mixed solution is stand-by；
(2) sodium carboxymethylcellulose that 100 parts of substitution values are 0.6 is uniformly added into kneading with above-mentioned alkali wine mixed solution
In reactor, the 15 minutes addition time of sodium carboxymethylcellulose raw material, the alkali wine mixed solution 25 minutes time of spray, alkali is carried out
Change reaction, quaternization 25 DEG C of temperature of control；
(3) after the completion of alkalizing, by 0.2 part of epoxychloropropane and the monoxone ethanol water of 125 part of 70% mass fraction
Mixing, and be uniformly sprayed to and mediate in reactor, spray time 40 minutes, 40 DEG C of controlling reaction temperature；Monoxone ethanol is water-soluble
After the completion of liquid spray, continue mixing 20 minutes, 40 DEG C of controlling reaction temperature；
(4) said mixture is delivered in methyltertiarvbutyl ether reactor and carries out etherification reaction, 75 DEG C of controlling reaction temperature, reaction
120 minutes time；
(5) after etherification reaction terminates, by reaction mass with being washed in the ethanol solution of 2500 part of 82% volume fraction
Twice and centrifuge, the material for centrifuging completion reclaims ethanol by steam stripper；
(6) dries pulverizing and packaging are carried out after the completion of ethanol recovery, the final substitution value that obtains is 2.15 purity 91%, 2%
The sodium carboxymethylcellulose product of Brookfield solution viscosities 5000mpas extra-high degree of substitution and high viscosity.
Embodiment 6
(1) liquid caustic soda of 100 part of 50% mass fraction is mixed with 250 part of 85% volume fraction ethanol, and is cooled to 30 DEG C
Alkali wine mixed solution is stand-by；
(2) sodium carboxymethylcellulose that 100 parts of substitution values are 1.4 is uniformly added into kneading with above-mentioned alkali wine mixed solution
In reactor, the 25 minutes addition time of sodium carboxymethylcellulose raw material, the alkali wine mixed solution 25 minutes time of spray；Alkali wine sprays
35 parts of solid sodium hydroxides are added after leaching and stir progress quaternization in 30 minutes, quaternization 15 DEG C of temperature of control；
(3) after the completion of alkalizing, the monoxone ethanol water of 173 part of 70% mass fraction is uniformly sprayed to kneading reaction
In device, spray time 30 minutes, 20 DEG C of controlling reaction temperature；After the completion of monoxone ethanol water spray, continue 30 points of mixing
Clock, 25 DEG C of controlling reaction temperature；
(4) said mixture is delivered in methyltertiarvbutyl ether reactor and carries out etherification reaction, 80 DEG C of controlling reaction temperature, reaction
60 minutes time；
(5) after etherification reaction terminates, by reaction mass with being washed in the ethanol solution of 2200 part of 85% volume fraction
Twice and centrifuge, the material for centrifuging completion reclaims ethanol by steam stripper；
(6) dries pulverizing and packaging are carried out after the completion of ethanol recovery, the final substitution value that obtains is 2.0, purity 92%, 2%
The sodium carboxymethylcellulose product of Brookfield solution viscosities 6000mpas extra-high degree of substitution and high viscosity.
Comparative example 1
The difference from Example 1 of comparative example 1 is, sodium carboxymethylcellulose raw material is replaced with into purified cotton or cotton pulp
The dregs of rice, and repeat to alkalize, be etherified, other operating procedures are identical, are specially：
(1) liquid caustic soda of 80 part of 50% mass fraction is mixed with 150 part of 93% volume fraction ethanol, and is cooled to 20 DEG C
Alkali wine mixed solution is stand-by；
(2) 100 parts of purified cottons or Cotton Pulp are uniformly added into above-mentioned alkali wine mixed solution and mediated in reactor, refined
Cotton or the 15 minutes addition time of Cotton Pulp, alkali wine mixed solution 25 minutes time of spray；Alkali wine adds 35 parts after spraying
Solid sodium hydroxide, which stirs, carries out quaternization for 30 minutes, quaternization 25 DEG C of temperature of control；
(3) after the completion of alkalizing, by 0.1 part of epoxychloropropane and the monoxone ethanol water of 120 part of 70% mass fraction
Mixing, and be uniformly sprayed to and mediate in reactor, spray time 40 minutes, 30 DEG C of controlling reaction temperature；Monoxone ethanol is water-soluble
After the completion of liquid spray, continue mixing 20 minutes, 30 DEG C of controlling reaction temperature；
(4) said mixture is delivered in methyltertiarvbutyl ether reactor and carries out etherification reaction, 78 DEG C of controlling reaction temperature, reaction
100 minutes time；
Step（4）After end, repetition is carried out successively（2）、（3）、（4）Operation, is repeated twice.
(5) reaction mass is centrifuged with being washed twice and being centrifuged in the ethanol solution of 2000 part of 80% volume fraction
The material of completion reclaims ethanol by steam stripper；
(6) dries pulverizing and packaging are carried out after the completion of ethanol recovery, the final substitution value that obtains is 1.5, purity 78%, 2%
Brookfield solution viscosities 3800mpas sodium carboxymethylcellulose product.
Comparative example 2
For the sodium carboxymethylcellulose of commercially available substitution value 1.2, model IH-12,1%Brookfield solution viscosity
1200mpas。
Comparative example 3
For commercially available sodium alginate, model LY1, Qingdao bright moon.
Effect example
Embodiment 1-6 and comparative example 1-3 is subjected to stamp application detection, thickener proportioning is shown in Table 1.
The thickener of table 1 matches（Percentage by weight）
In table 1, thickener dosage and Parameter are shown in Table 2.
The thickener dosage of table 2 and parameter
Dyestuff is in table 2：3% reactive turquoise blue BNC or 3% reactive blue BNC P3R or 3% active black BNC.Per set product
Respectively use three of the above dyestuff.
Found out by table 2, the usage amount of sodium alginate is big, and sodium alginate price is high in practice, therefore the application can have
Effect reduces production cost.
The said goods are subjected to stamp to bafta and spun rayon, stamp process is：
--- --- 100 DEG C of 102 DEG C of decatizes 8 minutes --- flushing --- use detergent Z04 to stamp within 2 minutes for 90 DEG C of dryings
Drying that 2g/L soaps 10 minutes --- flushing ---.
PRINTED FABRIC is detected, testing result is shown in Table 3.
The testing result of table 3
Claims (7)
- A kind of 1. preparation method of carboxymethyl cellulose with high degree sodium, it is characterised in that including alkalization etherificate, washing centrifugation, Drying smashes and batch mixing packaging process, uses sodium carboxymethylcellulose as raw material；Specifically comprise the following steps：(1) it is by the sodium hydrate aqueous solution that 80-150 parts by weight mass fractions are 50% and 160-250 parts by weight volume fractions 85-93% ethanol water mixing, is cooled to 18-30 DEG C, obtains alkali wine；(2) the sodium carboxymethylcellulose raw material that 100 parts by weight substitution values are 0.6-1.4 is uniformly mixed with alkali wine obtained by step (1) Close and carry out quaternization；(3) by monoxone ethanol water that 0-0.5 parts by weight epoxy chloropropane and 100-200 parts by weight mass fraction are 70-75% Solution mixes, then is uniformly mixed with the product of step (2), 20-40 DEG C of controlling reaction temperature；Then 20-30 minutes are stirred, 25-40 DEG C of controlling reaction temperature；Mixture is delivered into methyltertiarvbutyl ether reactor, 75-80 DEG C of controlling reaction temperature, reaction time 60-120 Minute；(4) after step (3) terminates, by gains in the ethanol aqueous wash that 1800-2500 parts by weight volume fraction is 75-85% Wash, centrifuge, reclaim ethanol；(5) dry, crush, packaging, produce.
- A kind of 2. preparation method of carboxymethyl cellulose with high degree sodium according to claim 1, it is characterised in that step (2) quaternization is carried out in reactor is mediated.
- A kind of 3. preparation method of carboxymethyl cellulose with high degree sodium according to claim 2, it is characterised in that step (2) quaternization is specially：Sodium carboxymethylcellulose raw material and alkali wine are uniformly added into and mediated in reactor, while adding carboxymethyl fine Tie up plain sodium side spray alkali wine；After alkali wine spray, 0-35 part solid sodium hydroxides are added, are stirred, carry out quaternization, Quaternization temperature control is at 15-25 DEG C.
- A kind of 4. preparation method of carboxymethyl cellulose with high degree sodium according to claim 1, it is characterised in that step (2) sodium carboxymethylcellulose raw material is powdery or cotton-shaped in.
- A kind of 5. preparation method of carboxymethyl cellulose with high degree sodium according to claim 1, it is characterised in that step (2) substitution value of sodium carboxymethylcellulose raw material is 0.8-1.2 in.
- A kind of 6. preparation method of carboxymethyl cellulose with high degree sodium according to claim 1, it is characterised in that step (2) the moisture 3-12% of sodium carboxymethylcellulose raw material in.
- A kind of 7. preparation method of carboxymethyl cellulose with high degree sodium according to claim 2, it is characterised in that step (2) the input quality of sodium carboxymethylcellulose raw material and the ratio of kneader volume are 1 in：6-15.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610620338.6A CN106432515B (en) | 2016-08-02 | 2016-08-02 | A kind of preparation method and applications of carboxymethyl cellulose with high degree sodium |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610620338.6A CN106432515B (en) | 2016-08-02 | 2016-08-02 | A kind of preparation method and applications of carboxymethyl cellulose with high degree sodium |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106432515A CN106432515A (en) | 2017-02-22 |
| CN106432515B true CN106432515B (en) | 2018-02-16 |
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| CN109988244B (en) * | 2017-12-29 | 2022-09-20 | 上海长光企业发展有限公司 | Sodium carboxymethylcellulose and preparation method and application thereof |
| CN110093792A (en) * | 2019-05-23 | 2019-08-06 | 成都市山马生物科技有限公司 | A kind of high substituted carboxymethyl starch composite reactive printing gum and preparation method |
| CN111574637B (en) * | 2020-06-15 | 2022-02-08 | 昆山京昆油田化学科技有限公司 | Methyl carboxymethyl guar gum and preparation method and application thereof |
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