CN103059144A - Preparation method of high-viscosity pelletizing sodium carboxymethylcellulose - Google Patents
Preparation method of high-viscosity pelletizing sodium carboxymethylcellulose Download PDFInfo
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- CN103059144A CN103059144A CN201310043058XA CN201310043058A CN103059144A CN 103059144 A CN103059144 A CN 103059144A CN 201310043058X A CN201310043058X A CN 201310043058XA CN 201310043058 A CN201310043058 A CN 201310043058A CN 103059144 A CN103059144 A CN 103059144A
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Abstract
The invention belongs to the field of chemical modification of a natural high polymer material, and relates to a preparation method of high-viscosity pelletizing sodium carboxymethylcellulose. The sodium carboxymethylcellulose is industrially produced by a kneading method; the obtained sodium carboxymethylcellulose product is added to a steam stripper to carry out partial hydrolyzing in the presence of inert gases after alkalization and etherification reaction, so that the particle morphology of the product can be well controlled in a crushing process so as to play a cross-linking role by adding aluminum chloride, and the granular sodium carboxymethylcellulose with high viscosity is finally obtained. The method disclosed by the invention is simple in technical process of production, short in reaction period, less in equipment investment, low in material consumption, small in dust pollution in the entire process, and environmentally-friendly, and the body health hazard to an operator is reduced to the minimal extent.
Description
Technical field
The invention belongs to natural macromolecular material chemical modification field, relate to a kind of preparation method of high viscosity granulation type Xylo-Mucine.
Background technology
Xylo-Mucine (CMC) is a kind of ionic ether of cellulose; it is water-soluble salt; it is the macromolecular compound that the hydrogen atom on the anhydrous grape sugar unit in the Mierocrystalline cellulose is replaced by carboxymethyl group; it is as main raw material take purified cotton; take ethanol as medium; through alkalization; etherificate; washing; rake is done; oven dry; the operations such as pulverizing are refining to be formed; the CMC aqueous solution has thickening; bonding; film forming; protection glue; keep moisture; the effect such as emulsification and suspension; be widely used in food; toothpaste; pottery; petroleum drilling; papermaking; medicine; weaving; printing and dyeing; coating; the industrial circles such as makeup; be commonly called as " industrial monosodium glutamate "; countries in the world have been produced the CMC of more than 250 kind of different model at present, are applied to different industry and manufacture field.
The carboxymethyl cellulose of present domestic utilization traditional technology preparation is difficult for disperseing in the aqueous solution, and dissolution rate is slow, needs to stir for a long time could dispersing and dissolving even, generally needs 2～4 hours, have in addition need 16～24 hours, comparatively inconvenience during use.Simultaneously, conventional carboxymethyl cellulose is pulverous fine particle in the market, and 80 order sieving rates are generally greater than 95%, produce and use procedure in dust pollution larger, cause detrimentally affect to environment and operative employee healthy.
Summary of the invention
The purpose of this invention is to provide a kind of being convenient to and in water, disperse, simultaneously to the preparation method of environment and the healthy close friend's of operative employee high viscosity granulation type Xylo-Mucine.
Technical scheme of the present invention may further comprise the steps:
A, cotton fibre torn up after, join in the kneader with the mixing solutions of 30～55% aqueous sodium hydroxide solutions together with 90～98% ethanolic solns; Wherein, the quality of aqueous sodium hydroxide solution is 1.20～1.30 times of purified cotton, and the quality of ethanolic soln is 1.50～2.00 times of purified cotton;
After b, the end that feeds intake, get rid of the air in the kneader, make vacuum tightness reach at least 0.06MPa;
C, rare gas element is filled with in the kneader, makes the kneader internal pressure greater than 0.02MPa;
D, carry out the quaternization process under protection of inert gas, the quaternization time is 40～70 minutes, and the quaternization temperature is 10～40 ℃;
After e, quaternization finish, add etherifying agent in the product that obtains in the steps d, the quality of etherifying agent is 1.20～1.30 times of purified cotton.Described etherifying agent is chloroacetic ethanolic soln, and wherein, chloroacetic mass percent concentration is 50 ~ 80%;
Air in f, the eliminating kneader makes vacuum tightness reach at least 0.06MPa;
G, again rare gas element is filled with in the kneader, makes the kneader internal pressure greater than 0.02MPa;
H, carry out the etherification reaction process under protection of inert gas, the etherification reaction time is 50～70 minutes, and etherification reaction temperature is 60～90 ℃;
I, with the product that obtains among the step h through washing, neutralization, centrifugal;
J, will be in the product that obtains after centrifugal add in the steam stripper, add simultaneously the spirituous solution of aluminum chloride; Wherein, the mass percent concentration of alcohol is 30～50%, and the mass percent concentration of aluminum chloride is 0.5～1.5%.The spirituous solution of aluminum chloride and the mass ratio of purified cotton are 1.0～1.5:1, and the reaction times is 20～40 minutes, and temperature of reaction is 70～90 ℃
K, at last with the product among the step j through super-dry, pulverizing.
The innovative point of present method is, the Xylo-Mucine product that employing will be washed after centrifugal joins when carrying out rising temperature reclamation alcohol in the steam stripper, added spirituous solution, can allow like this product partial hydrolysis in steam stripper, so that the back can fine control product when pulverizing particle form, descend for product inner quality behind the precaution of hydrolysis simultaneously and the sticking ratio reduction of salt, in spirituous solution, added certain aluminum chloride, play crosslinked action, prevent the structure considerable damage that product causes because of hydrolysis.
The inventive method production process technology is simple, and reaction time is short, and facility investment is few, and raw material consumption is low, and whole process dust pollution is little.The Xylo-Mucine that adopts the method preparation to produce when having viscosity higher and granularity, has again the preferably sticking ratio of salt.1%NDJ-79 type viscosity reaches more than the 550mps, and the sticking specific energy of 1%NDJ-79 type salt reaches more than 0.75 simultaneously, and 40 order sieving rates reach below 40%.
Description of drawings
Fig. 1 is FB(flow block) of the present invention.
Specific embodiment
The present invention is further illustrated below in conjunction with embodiment.
Embodiment 1:
With a certain amount of purified cotton that tears up, with 2.00 times of quality (namely take the amount of purified cotton as the basis, below identical) ethanolic soln and the mixed solution of the sodium hydroxide solution of 1.25 times of quality put in the kneader, feed intake finish after, get rid of the air in the kneader, make vacuum tightness reach at least 0.06MPa, rare gas element is filled with in the kneader, make the kneader internal pressure greater than 0.02MPa, stir alkalization after 60 minutes, the chloroacetic ethanolic soln of 1.23 times of quality is sprayed equably to kneader, get rid of the air in the kneader, make vacuum tightness reach at least 0.06MPa, again rare gas element is filled with in the kneader, make the kneader internal pressure greater than 0.02MPa, then carry out etherification reaction, temperature is increased to 60-90 ℃, sustained reaction 50 minutes obtains rough Xylo-Mucine product, through washing, neutralization, after centrifugal, the concentration that adds 1.0 times in the time of the product introduction steam stripper is the spirituous solution of 1.3% aluminum chloride, stripping reaction 30 minutes is at last by dry, obtain refining Xylo-Mucine finished product after the pulverizing, 1%NDJ-79 type viscosity 590mPa..s, 1%NDJ-79 type salt is sticking than being that 0.83,40 order sieving rate is 38%.If do not add aluminum chloride in the stripping reaction, sample 1%NDJ-79 type viscosity 575mPa..s, 1%NDJ-79 type salt is sticking than being 0.62.
Embodiment 2:
With a certain amount of purified cotton that tears up, put in the kneader with the mixed solution of the sodium hydroxide solution of the ethanolic soln of 1.80 times of quality and 1.30 times of quality, feed intake finish after, get rid of the air in the kneader, make vacuum tightness reach at least 0.06MPa, rare gas element is filled with in the kneader, make the kneader internal pressure greater than 0.02MPa, stir alkalization after 50 minutes, the chloroacetic ethanolic soln of 1.30 times of quality is sprayed equably to kneader, get rid of the air in the kneader, make vacuum tightness reach at least 0.06MPa, again rare gas element is filled with in the kneader, make the kneader internal pressure greater than 0.02MPa, then carry out etherification reaction, temperature is increased to 60-90 ℃, sustained reaction 60 minutes, obtain rough Xylo-Mucine product, through washing, neutralization, after centrifugal, the concentration that adds 1.5 times in the time of the product introduction steam stripper is the spirituous solution of 1.5% aluminum chloride, stripping reaction 30 minutes, at last by dry, obtain refining Xylo-Mucine finished product after the pulverizing, 1%NDJ-79 type viscosity 595mPa..s, 1%NDJ-79 type salt is sticking than being that 0.88,40 order sieving rate is 36%.If do not add aluminum chloride in the stripping reaction, sample 1%NDJ-79 type viscosity 567mPa..s, 1%NDJ-79 type salt is sticking than being 0.65.
Embodiment 3:
With a certain amount of purified cotton that tears up, put in the kneader with the mixed solution of the sodium hydroxide solution of the ethanolic soln of 1.50 times of quality and 1.20 times of quality, feed intake finish after, get rid of the air in the kneader, make vacuum tightness reach at least 0.06MPa, rare gas element is filled with in the kneader, make the kneader internal pressure greater than 0.02MPa, stir alkalization after 70 minutes, the chloroacetic ethanolic soln of 1.20 times of quality is sprayed equably to kneader, get rid of the air in the kneader, make vacuum tightness reach at least 0.06MPa, again rare gas element is filled with in the kneader, make the kneader internal pressure greater than 0.02MPa, then carry out etherification reaction, temperature is increased to 60-90 ℃, sustained reaction 70 minutes, obtain rough Xylo-Mucine product, through washing, neutralization, after centrifugal, the concentration that adds 1.3 times in the time of the product introduction steam stripper is the spirituous solution of 0.8% aluminum chloride, stripping reaction 40 minutes, at last by dry, obtain refining Xylo-Mucine finished product after the pulverizing, 1%NDJ-79 type viscosity 580mPa..s, 1%NDJ-79 type salt is sticking than being that 0.77,40 order sieving rate is 34%.If do not add aluminum chloride in the stripping reaction, sample 1%NDJ-79 type viscosity 550mPa..s, 1%NDJ-79 type salt is sticking than being 0.59.
Embodiment 4:
With a certain amount of purified cotton that tears up, put in the kneader with the mixed solution of the sodium hydroxide solution of the ethanolic soln of 2.0 times of quality and 1.25 times of quality, feed intake finish after, get rid of the air in the kneader, make vacuum tightness reach at least 0.06MPa, rare gas element is filled with in the kneader, make the kneader internal pressure greater than 0.02MPa, stir alkalization after 60 minutes, the chloroacetic ethanolic soln of 1.25 times of quality is sprayed equably to kneader, get rid of the air in the kneader, make vacuum tightness reach at least 0.06MPa, again rare gas element is filled with in the kneader, make the kneader internal pressure greater than 0.02MPa, then carry out etherification reaction, temperature is increased to 60-90 ℃, sustained reaction 50 minutes, obtain rough Xylo-Mucine product, through washing, neutralization, after centrifugal, the concentration that adds 1.0 times in the time of the product introduction steam stripper is the spirituous solution of 1.0% aluminum chloride, stripping reaction 30 minutes, at last by dry, obtain refining Xylo-Mucine finished product after the pulverizing, 1%NDJ-79 type viscosity 600mPa..s, 1%NDJ-79 type salt is sticking than being that 0.85,40 order sieving rate is 36%.If do not add aluminum chloride in the stripping reaction, sample 1%NDJ-79 type viscosity 570mPa..s, 1%NDJ-79 type salt is sticking than being 0.61.
Embodiment 5:
With a certain amount of purified cotton that tears up, put in the kneader with the mixed solution of the sodium hydroxide solution of the ethanolic soln of 1.8 times of quality and 1.28 times of quality, feed intake finish after, get rid of the air in the kneader, make vacuum tightness reach at least 0.06MPa, rare gas element is filled with in the kneader, make the kneader internal pressure greater than 0.02MPa, stir alkalization after 60 minutes, the chloroacetic ethanolic soln of 1.28 times of quality is sprayed equably to kneader, get rid of the air in the kneader, make vacuum tightness reach at least 0.06MPa, again rare gas element is filled with in the kneader, make the kneader internal pressure greater than 0.02MPa, then carry out etherification reaction, temperature is increased to 60-90 ℃, sustained reaction 50 minutes, obtain rough Xylo-Mucine product, through washing, neutralization, after centrifugal, the concentration that adds 1.2 times in the time of the product introduction steam stripper is the spirituous solution of 1.0% aluminum chloride, stripping reaction 20 minutes, at last by dry, obtain refining Xylo-Mucine finished product after the pulverizing, 1%NDJ-79 type viscosity 573mPa..s, 1%NDJ-79 type salt is sticking than being that 0.76,40 order sieving rate is 35%.If do not add aluminum chloride in the stripping reaction, sample 1%NDJ-79 type viscosity 545mPa..s, 1%NDJ-79 type salt is sticking than being 0.62.
Term:
Viscosity: 1% aqueous solution, NDJ-79 type viscosity apparatus detects under 25 ℃ of conditions.
The sticking ratio of salt: (1% solution viscosity)/(1% salt brine solution viscosity), wherein salt brine solution is 4% sodium chloride aqueous solution, NDJ-79 type viscosity apparatus detects under 25 ℃ of conditions.
Claims (6)
1. the preparation method of a high viscosity granulation type Xylo-Mucine is characterized in that may further comprise the steps:
A, cotton fibre torn up after, join in the kneader together with the mixing solutions of sodium hydroxide solution and ethanolic soln, wherein, the quality of aqueous sodium hydroxide solution is 1.20～1.30 times of purified cotton, the quality of ethanolic soln is 1.50～2.00 times of purified cotton;
After b, the end that feeds intake, get rid of the air in the kneader, make vacuum tightness reach at least 0.06MPa;
C, rare gas element is filled with in the kneader, makes the kneader internal pressure greater than 0.02MPa;
D, under protection of inert gas, carry out quaternization;
E, quaternization add etherifying agent in the product that obtains after finishing in steps d, wherein, the quality of etherifying agent is 1.20～1.30 times of quality of purified cotton;
Air in f, the eliminating kneader makes vacuum tightness reach at least 0.06MPa;
G, again rare gas element is filled with in the kneader, makes the kneader internal pressure greater than 0.02MPa;
H, under protection of inert gas, carry out the etherification reaction process;
I, with the product that obtains among the step h through washing, neutralization, centrifugal;
J, will be in the product that obtains after centrifugal add in the steam stripper, add simultaneously the spirituous solution of aluminum chloride, the spirituous solution of aluminum chloride and the mass ratio of purified cotton are 1.0～1.5:1;
K, at last with the product among the step j through super-dry, pulverizing.
2. the preparation method of high viscosity granulation type Xylo-Mucine according to claim 1, it is characterized in that: among the step a, the mass percent concentration of aqueous sodium hydroxide solution is 30～55%, and the mass percentage concentration of described aqueous ethanolic solution is 90～98%.
3. the method for preparing high viscosity granulation type Xylo-Mucine according to claim 1, it is characterized in that: the quaternization time is 40～70 minutes in the steps d, and temperature of reaction is 10～40 ℃.
4. the method for high viscosity granulation type Xylo-Mucine according to claim 1, it is characterized in that: among the step e, etherifying agent is chloroacetic ethanolic soln, wherein, chloroacetic mass percent concentration is 50～80%.
5. the method for high viscosity granulation type Xylo-Mucine according to claim 1, it is characterized in that: among the step h, the etherification reaction time is 50～70 minutes, and temperature of reaction is 60～90 ℃.
6. the method for high viscosity granulation type Xylo-Mucine according to claim 1, it is characterized in that: among the step j, the mass percent concentration of alcohol is 30～50%, the mass percent 0.5～1.5% of aluminum chloride, reaction times is 20～40 minutes, and temperature of reaction is 70～90 ℃.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105330751A (en) * | 2015-11-05 | 2016-02-17 | 重庆力宏精细化工有限公司 | Continuous production method of carboxymethylcellulose lithium for lithium batteries |
| CN105566500A (en) * | 2016-02-02 | 2016-05-11 | 上海长光企业发展有限公司 | Preparation method of granule-type polyanionic cellulose |
| CN117960020A (en) * | 2024-03-28 | 2024-05-03 | 鞍山天雨发展有限公司 | Preparation method of filter aid for solid-liquid separation of iron concentrate |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101724076A (en) * | 2009-11-27 | 2010-06-09 | 鹰特化工(石家庄)有限公司 | Preparation method of high acid resistance sodium carboxymethyl cellulose for foods |
| CN102675474A (en) * | 2012-05-23 | 2012-09-19 | 重庆力宏精细化工有限公司 | Preparation method of ultrahigh-viscosity sodium carboxymethyl cellulose |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101724076A (en) * | 2009-11-27 | 2010-06-09 | 鹰特化工(石家庄)有限公司 | Preparation method of high acid resistance sodium carboxymethyl cellulose for foods |
| CN102675474A (en) * | 2012-05-23 | 2012-09-19 | 重庆力宏精细化工有限公司 | Preparation method of ultrahigh-viscosity sodium carboxymethyl cellulose |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105330751A (en) * | 2015-11-05 | 2016-02-17 | 重庆力宏精细化工有限公司 | Continuous production method of carboxymethylcellulose lithium for lithium batteries |
| CN105566500A (en) * | 2016-02-02 | 2016-05-11 | 上海长光企业发展有限公司 | Preparation method of granule-type polyanionic cellulose |
| CN117960020A (en) * | 2024-03-28 | 2024-05-03 | 鞍山天雨发展有限公司 | Preparation method of filter aid for solid-liquid separation of iron concentrate |
| CN117960020B (en) * | 2024-03-28 | 2024-05-28 | 鞍山天雨发展有限公司 | Preparation method of filter aid for solid-liquid separation of iron concentrate |
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