CN104098703A - Preparation method of CMC (carboxymethyl cellulose) - Google Patents
Preparation method of CMC (carboxymethyl cellulose) Download PDFInfo
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- CN104098703A CN104098703A CN201410324681.7A CN201410324681A CN104098703A CN 104098703 A CN104098703 A CN 104098703A CN 201410324681 A CN201410324681 A CN 201410324681A CN 104098703 A CN104098703 A CN 104098703A
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Abstract
The invention provides a preparation method of CMC (carboxymethyl cellulose). The preparation method comprises specific operation steps that as follows: cotton is taken and broken into 2-6-cm cotton pieces, and then the cotton pieces, a sodium hydroxide aqueous solution and ethanol water solution are fed into a kneader reactor to finish batch charging; after the batch charging ends, air in the kneader reactor is exhausted, inert gas is injected, and then materials in the kneader reactor perform an alkalization reaction under the protection of the inert gas; after the alkalization reaction ends, the materials in the kneader reactor are transferred to an etherification tank for an etherification reaction for 55-70 min, a dispersing agent for the etherification reaction is 95% ethanol, and an etherifying agent is an ethanol solution containing 50%-80% chloroacetic acid; and after the etherification ends, the materials are washed, neutralized, centrifugalized, dried, smashed and screened sequentially to obtain CMC. The preparation method is simple to operate and low in cost, and prepared CMC has higher viscosity.
Description
[technical field]
The invention belongs to material preparation method, be specifically related to a kind of preparation method of Xylo-Mucine.
[background technology]
Xylo-Mucine claims again sodium carboxymethyl-cellulose, carboxymethyl cellulose, is the widest, the maximum Mierocrystalline cellulose kind of consumption of use range in the world today; It 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 transparent colloidal solution, insoluble in the organic solvents such as ethanol.1% aqueous solution pH is 6.5～8.5, and in the time of pH>10 or <5, rubber cement viscosity significantly reduces, performance the best in the time of pH=7.To thermally-stabilised, rise rapidly 20 DEG C of following viscosity, 45 DEG C time, change slowlyer, 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 facile hydrolysis, pH value there will be precipitation during for 2-3, meets polyvalent metal salt and also can react appearance and precipitate.
At present, many about pertinent literature how to prepare Xylo-Mucine, but conventionally all exist the problem that viscosity is lower and cost is high.
[summary of the invention]
Technical problem to be solved by this invention is to provide a kind of preparation method of Xylo-Mucine, simple to operate, with low cost, and prepared Xylo-Mucine has higher viscosity.
The present invention solves the problems of the technologies described above by the following technical programs:
A preparation method for Xylo-Mucine, comprises following concrete operation step:
(1) get cotton and be broken into the small pieces cotton of 2-6cm size, the aqueous ethanolic solution that the aqueous sodium hydroxide solution that is 30-55% by small pieces cotton, concentration afterwards and concentration are 70-95% drops into together in kneader and feeds intake to complete, wherein, the mass ratio of small pieces cotton and aqueous sodium hydroxide solution is 1:1.75-4.2, and the quality of aqueous ethanolic solution is 0.5-8 times of small pieces cotton;
(2) feed intake after end, the air of discharging in kneader is also filled with rare gas element, and the material in kneader carries out quaternization under the protection of rare gas element afterwards, and alkalization temperature is controlled at 10-35 DEG C, and the reaction times is 40-100 minute;
(3) after alkalization finishes, the material in kneader is gone to and in etherificate tank, carries out etherification reaction, and the dispersion agent of etherification reaction is that 95% ethanol, etherifying agent are that the chloroacetic ethanolic soln of 50-80%, time are 55-70 minute;
(4) after etherificate finishes, by material wash successively, neutralization, centrifugal, be dried, pulverize and sieve, obtain described Xylo-Mucine.
The preparation method's of Xylo-Mucine of the present invention beneficial effect is: the method is simple to operate, with low cost, is convenient to large-scale suitability for industrialized production, and prepared Xylo-Mucine has higher viscosity.
[embodiment]
The preparation method of a kind of Xylo-Mucine of the present invention, comprise following concrete operation step: (1) is got cotton and is broken into the small pieces cotton of 2-6cm size, the aqueous ethanolic solution that the aqueous sodium hydroxide solution that is 30-55% by small pieces cotton, concentration afterwards and concentration are 70-95% drops into together in kneader and feeds intake to complete, wherein, the mass ratio of small pieces cotton and aqueous sodium hydroxide solution is 1:1.75-4.2, and the quality of aqueous ethanolic solution is 0.5-8 times of small pieces cotton; (2) feed intake after end, the air of discharging in kneader is also filled with rare gas element, and the material in kneader carries out quaternization under the protection of rare gas element afterwards, and alkalization temperature is controlled at 10-35 DEG C, and the reaction times is 40-100 minute; 3) after alkalization finishes, the material in kneader is gone to and in etherificate tank, carries out etherification reaction, and the dispersion agent of etherification reaction is that 95% ethanol, etherifying agent are that the chloroacetic ethanolic soln of 50-80%, time are 55-70 minute; (4) after etherificate finishes, by material wash successively, neutralization, centrifugal, be dried, pulverize and sieve, obtain described Xylo-Mucine.
In order further to set forth the preparation method's of Xylo-Mucine of the present invention specific operation process, applicant has exemplified following several embodiment.
Embodiment 1
Get cotton and be broken into the small pieces cotton of 2-6cm size, the aqueous ethanolic solution that the aqueous sodium hydroxide solution that is 30% by small pieces cotton, concentration afterwards and concentration are 95% drops into together in kneader and feeds intake to complete, wherein, the mass ratio of small pieces cotton and aqueous sodium hydroxide solution is 1:1.75, and the quality of aqueous ethanolic solution is 5 times of small pieces cotton; Then discharge the air in kneader and be filled with rare gas element, then the material in kneader carries out quaternization under the protection of rare gas element, and alkalization temperature is controlled at 35 DEG C, and the reaction times is 70 minutes; After alkalization finishes, the material in kneader is gone to and in etherificate tank, carries out etherification reaction, and the dispersion agent of etherification reaction is that 95% ethanol, etherifying agent are that 80% chloroacetic ethanolic soln, time are 60 minutes; Finally material is washed successively, neutralization, centrifugal, be dried, pulverize and sieve, obtain described Xylo-Mucine.
Embodiment 2
Get cotton and be broken into the small pieces cotton of 2-6cm size, the aqueous ethanolic solution that the aqueous sodium hydroxide solution that is 45% by small pieces cotton, concentration afterwards and concentration are 85% drops into together in kneader and feeds intake to complete, wherein, the mass ratio of small pieces cotton and aqueous sodium hydroxide solution is 1:4.2, and the quality of aqueous ethanolic solution is 8 times of small pieces cotton; Then discharge the air in kneader and be filled with rare gas element, then the material in kneader carries out quaternization under the protection of rare gas element, and alkalization temperature is controlled at 25 DEG C, and the reaction times is 100 minutes; After alkalization finishes, the material in kneader is gone to and in etherificate tank, carries out etherification reaction, and the dispersion agent of etherification reaction is that 95% ethanol, etherifying agent are that 65% chloroacetic ethanolic soln, time are 55 minutes; Finally material is washed successively, neutralization, centrifugal, be dried, pulverize and sieve, obtain described Xylo-Mucine.
Embodiment 3
Get cotton and be broken into the small pieces cotton of 2-6cm size, the aqueous ethanolic solution that the aqueous sodium hydroxide solution that is 55% by small pieces cotton, concentration afterwards and concentration are 70% drops into together in kneader and feeds intake to complete, wherein, the mass ratio of small pieces cotton and aqueous sodium hydroxide solution is 1:3.75, and the quality of aqueous ethanolic solution is 0.5 times of small pieces cotton; Then discharge the air in kneader and be filled with rare gas element, the material in kneader carries out quaternization under the protection of rare gas element afterwards, and alkalization temperature is controlled at 10 DEG C, and the reaction times is 40 minutes; After alkalization finishes, the material in kneader is gone to and in etherificate tank, carries out etherification reaction, and the dispersion agent of etherification reaction is that 95% ethanol, etherifying agent are that 50% chloroacetic ethanolic soln, time are 70 minutes; Finally material is washed successively, neutralization, centrifugal, be dried, pulverize and sieve, obtain described Xylo-Mucine.
To sum up, preparation method of the present invention is simple to operate, with low cost, is convenient to large-scale suitability for industrialized production, and prepared Xylo-Mucine has higher viscosity.
Claims (1)
1. a preparation method for Xylo-Mucine, is characterized in that: comprise following concrete operation step:
(1) get cotton and be broken into the small pieces cotton of 2-6cm size, the aqueous ethanolic solution that the aqueous sodium hydroxide solution that is 30-55% by small pieces cotton, concentration afterwards and concentration are 70-95% drops into together in kneader and feeds intake to complete, wherein, the mass ratio of small pieces cotton and aqueous sodium hydroxide solution is 1:1.75-4.2, and the quality of aqueous ethanolic solution is 0.5-8 times of small pieces cotton;
(2) feed intake after end, the air of discharging in kneader is also filled with rare gas element, and the material in kneader carries out quaternization under the protection of rare gas element afterwards, and alkalization temperature is controlled at 10-35 DEG C, and the reaction times is 40-100 minute;
(3) after alkalization finishes, the material in kneader is gone to and in etherificate tank, carries out etherification reaction, and the dispersion agent of etherification reaction is that 95% ethanol, etherifying agent are that the chloroacetic ethanolic soln of 50-80%, time are 55-70 minute;
(4) after etherificate finishes, by material wash successively, neutralization, centrifugal, be dried, pulverize and sieve, obtain described Xylo-Mucine.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410324681.7A CN104098703A (en) | 2014-07-09 | 2014-07-09 | Preparation method of CMC (carboxymethyl cellulose) |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410324681.7A CN104098703A (en) | 2014-07-09 | 2014-07-09 | Preparation method of CMC (carboxymethyl cellulose) |
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| CN104098703A true CN104098703A (en) | 2014-10-15 |
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| CN201410324681.7A Pending CN104098703A (en) | 2014-07-09 | 2014-07-09 | Preparation method of CMC (carboxymethyl cellulose) |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106008201A (en) * | 2016-05-24 | 2016-10-12 | 江苏泰利达新材料股份有限公司 | Method for extracting sodium glycollate from CMC wastewater |
| CN110079327A (en) * | 2019-05-30 | 2019-08-02 | 北京理工大学 | The preparation method and application of stalk sodium water conservation and conditioning materials |
| 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 |
-
2014
- 2014-07-09 CN CN201410324681.7A patent/CN104098703A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106008201A (en) * | 2016-05-24 | 2016-10-12 | 江苏泰利达新材料股份有限公司 | Method for extracting sodium glycollate from CMC wastewater |
| 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 |
| CN110079327A (en) * | 2019-05-30 | 2019-08-02 | 北京理工大学 | The preparation method and application of stalk sodium water conservation and conditioning materials |
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Application publication date: 20141015 |