CN103059144B - Preparation method of high-viscosity pelletizing sodium carboxymethylcellulose - Google Patents
Preparation method of high-viscosity pelletizing sodium carboxymethylcellulose Download PDFInfo
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- CN103059144B CN103059144B CN201310043058.XA CN201310043058A CN103059144B CN 103059144 B CN103059144 B CN 103059144B CN 201310043058 A CN201310043058 A CN 201310043058A CN 103059144 B CN103059144 B CN 103059144B
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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 field of chemical modification, relate to a kind of preparation method of high viscosity granulation type Xylo-Mucine.
Background technology
Xylo-Mucine (CMC) is a kind of ionic cellulose ethers, it is water-soluble salt, it is the macromolecular compound that the hydrogen atom on the anhydrous grape sugar unit in Mierocrystalline cellulose is replaced by carboxymethyl group, it take purified cotton as main raw material, take ethanol as medium, through alkalization, etherificate, washing, rake is dry, dry, the operations such as pulverizing are refining to be formed, the CMC aqueous solution has thickening, bonding, film forming, protecting 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 ", current countries in the world have produced the CMC of more than 250 kind of different model, be applied to different industry and manufacture field.
Carboxymethyl cellulose prepared by current domestic utilization traditional technology not easily disperses in aqueous, and dissolution rate is slow, and need to stir ability dispersing and dissolving for a long time even, generally need 2 ~ 4 hours, what have even needs 16 ~ 24 hours, comparatively inconvenient during use.Meanwhile, carboxymethyl cellulose conventional is in the market pulverous fine particle, and 80 order sieving rates are generally greater than 95%, produce and dust pollution in use procedure comparatively greatly, cause detrimentally affect to environment and the healthy of operative employee.
Summary of the invention
The object of this invention is to provide one to be convenient to disperse in water, simultaneously to the preparation method of the high viscosity granulation type Xylo-Mucine of environment and the healthy close friend of operative employee.
Technical scheme of the present invention comprises the following steps:
A, cotton fibre is torn up after, join in kneader with 30 ~ 55% aqueous sodium hydroxide solutions together with the mixing solutions of 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 kneader, make vacuum tightness reach at least 0.06MPa;
C, rare gas element is filled with in kneader, makes kneader internal pressure be greater than 0.02MPa;
D, under protection of inert gas, carry out quaternization process, the quaternization time is 40 ~ 70 minutes, and quaternization temperature is 10 ~ 40 DEG C;
After e, quaternization terminate, add etherifying agent in the product obtained in 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%;
F, the air got rid of in kneader, make vacuum tightness reach at least 0.06MPa;
G, again rare gas element is filled with in kneader, makes kneader internal pressure be greater than 0.02MPa;
H, under protection of inert gas, carry out etherification reaction process, the etherification reaction time is 50 ~ 70 minutes, and etherification reaction temperature is 60 ~ 90 DEG C;
I, by the product that obtains in step h through washing, neutralization, centrifugal;
J, by adding in steam stripper in the product obtained after centrifugal, add the spirituous solution of aluminum chloride simultaneously; 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 DEG C
K, finally by the product in step j through super-dry, pulverizing.
The innovative point of present method is, adopt while the Xylo-Mucine product after centrifugal for washing is joined and carries out rising temperature reclamation alcohol in steam stripper, add spirituous solution, product can be allowed like this at steam stripper Partial hydrolysis, the particle form of product can be controlled very well when pulverizing after making, simultaneously in order to product inner quality after precaution of hydrolysis declines and salt is sticky than reducing, certain aluminum chloride is added in spirituous solution, 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.Adopt the Xylo-Mucine that the method preparation is produced, while there is viscosity higher and granularity, there is again the sticky ratio of good salt.1%NDJ-79 type viscosity reaches more than 550mps, and 1%NDJ-79 type salt is sticky simultaneously reaches less than 40% than reaching more than 0.75,40 order sieving rates.
Accompanying drawing explanation
Fig. 1 is FB(flow block) of the present invention.
Specific embodiment
Below in conjunction with embodiment, the present invention is further illustrated.
Embodiment 1:
By a certain amount of purified cotton torn up, with 2.00 times of quality (namely based on the amount of purified cotton, identical below) ethanolic soln and the mixed solution of sodium hydroxide solution of 1.25 times of quality put in kneader, feed intake after terminating, get rid of the air in kneader, vacuum tightness is made to reach at least 0.06MPa, rare gas element is filled with in kneader, kneader internal pressure is made to be greater than 0.02MPa, stir alkalization after 60 minutes, the chloroacetic ethanolic soln of 1.23 times of quality is sprayed in kneader equably, get rid of the air in kneader, vacuum tightness is made to reach at least 0.06MPa, again rare gas element is filled with in kneader, kneader internal pressure is made to be greater than 0.02MPa, then etherification reaction is carried out, temperature is increased to 60-90 DEG C, sustained reaction 50 minutes, obtain rough Xylo-Mucine product, through washing, neutralization, after centrifugal, the concentration adding 1.0 times while product introduction steam stripper is the spirituous solution of the aluminum chloride of 1.3%, stripping reacts 30 minutes, finally by drying, refining Xylo-Mucine finished product is obtained after pulverizing, 1%NDJ-79 type viscosity 590mPa..s, 1%NDJ-79 type salt is sticky than being 0.83, 40 order sieving rates are 38%.If do not add aluminum chloride, sample 1%NDJ-79 type viscosity 575mPa..s in stripping reaction, 1%NDJ-79 type salt is sticky than being 0.62.
Embodiment 2:
By a certain amount of purified cotton torn up, put in kneader with the mixed solution of the ethanolic soln of 1.80 times of quality and the sodium hydroxide solution of 1.30 times of quality, feed intake after terminating, get rid of the air in kneader, vacuum tightness is made to reach at least 0.06MPa, rare gas element is filled with in kneader, kneader internal pressure is made to be greater than 0.02MPa, stir alkalization after 50 minutes, the chloroacetic ethanolic soln of 1.30 times of quality is sprayed in kneader equably, get rid of the air in kneader, vacuum tightness is made to reach at least 0.06MPa, again rare gas element is filled with in kneader, kneader internal pressure is made to be greater than 0.02MPa, then etherification reaction is carried out, temperature is increased to 60-90 DEG C, sustained reaction 60 minutes, obtain rough Xylo-Mucine product, through washing, neutralization, after centrifugal, the concentration adding 1.5 times while product introduction steam stripper is the spirituous solution of the aluminum chloride of 1.5%, stripping reacts 30 minutes, finally by drying, refining Xylo-Mucine finished product is obtained after pulverizing, 1%NDJ-79 type viscosity 595mPa..s, 1%NDJ-79 type salt is sticky than being 0.88, 40 order sieving rates are 36%.If do not add aluminum chloride, sample 1%NDJ-79 type viscosity 567mPa..s in stripping reaction, 1%NDJ-79 type salt is sticky than being 0.65.
Embodiment 3:
By a certain amount of purified cotton torn up, put in kneader with the mixed solution of the ethanolic soln of 1.50 times of quality and the sodium hydroxide solution of 1.20 times of quality, feed intake after terminating, get rid of the air in kneader, vacuum tightness is made to reach at least 0.06MPa, rare gas element is filled with in kneader, kneader internal pressure is made to be greater than 0.02MPa, stir alkalization after 70 minutes, the chloroacetic ethanolic soln of 1.20 times of quality is sprayed in kneader equably, get rid of the air in kneader, vacuum tightness is made to reach at least 0.06MPa, again rare gas element is filled with in kneader, kneader internal pressure is made to be greater than 0.02MPa, then etherification reaction is carried out, temperature is increased to 60-90 DEG C, sustained reaction 70 minutes, obtain rough Xylo-Mucine product, through washing, neutralization, after centrifugal, the concentration adding 1.3 times while product introduction steam stripper is the spirituous solution of the aluminum chloride of 0.8%, stripping reacts 40 minutes, finally by drying, refining Xylo-Mucine finished product is obtained after pulverizing, 1%NDJ-79 type viscosity 580mPa..s, 1%NDJ-79 type salt is sticky than being 0.77, 40 order sieving rates are 34%.If do not add aluminum chloride, sample 1%NDJ-79 type viscosity 550mPa..s in stripping reaction, 1%NDJ-79 type salt is sticky than being 0.59.
Embodiment 4:
By a certain amount of purified cotton torn up, put in kneader with the mixed solution of the ethanolic soln of 2.0 times of quality and the sodium hydroxide solution of 1.25 times of quality, feed intake after terminating, get rid of the air in kneader, vacuum tightness is made to reach at least 0.06MPa, rare gas element is filled with in kneader, kneader internal pressure is made to be greater than 0.02MPa, stir alkalization after 60 minutes, the chloroacetic ethanolic soln of 1.25 times of quality is sprayed in kneader equably, get rid of the air in kneader, vacuum tightness is made to reach at least 0.06MPa, again rare gas element is filled with in kneader, kneader internal pressure is made to be greater than 0.02MPa, then etherification reaction is carried out, temperature is increased to 60-90 DEG C, sustained reaction 50 minutes, obtain rough Xylo-Mucine product, through washing, neutralization, after centrifugal, the concentration adding 1.0 times while product introduction steam stripper is the spirituous solution of the aluminum chloride of 1.0%, stripping reacts 30 minutes, finally by drying, refining Xylo-Mucine finished product is obtained after pulverizing, 1%NDJ-79 type viscosity 600mPa..s, 1%NDJ-79 type salt is sticky than being 0.85, 40 order sieving rates are 36%.If do not add aluminum chloride, sample 1%NDJ-79 type viscosity 570mPa..s in stripping reaction, 1%NDJ-79 type salt is sticky than being 0.61.
Embodiment 5:
By a certain amount of purified cotton torn up, put in kneader with the mixed solution of the ethanolic soln of 1.8 times of quality and the sodium hydroxide solution of 1.28 times of quality, feed intake after terminating, get rid of the air in kneader, vacuum tightness is made to reach at least 0.06MPa, rare gas element is filled with in kneader, kneader internal pressure is made to be greater than 0.02MPa, stir alkalization after 60 minutes, the chloroacetic ethanolic soln of 1.28 times of quality is sprayed in kneader equably, get rid of the air in kneader, vacuum tightness is made to reach at least 0.06MPa, again rare gas element is filled with in kneader, kneader internal pressure is made to be greater than 0.02MPa, then etherification reaction is carried out, temperature is increased to 60-90 DEG C, sustained reaction 50 minutes, obtain rough Xylo-Mucine product, through washing, neutralization, after centrifugal, the concentration adding 1.2 times while product introduction steam stripper is the spirituous solution of the aluminum chloride of 1.0%, stripping reacts 20 minutes, finally by drying, refining Xylo-Mucine finished product is obtained after pulverizing, 1%NDJ-79 type viscosity 573mPa..s, 1%NDJ-79 type salt is sticky than being 0.76, 40 order sieving rates are 35%.If do not add aluminum chloride, sample 1%NDJ-79 type viscosity 545mPa..s in stripping reaction, 1%NDJ-79 type salt is sticky than being 0.62.
Term:
Viscosity: 1% aqueous solution, NDJ-79 type viscosity apparatus, detects under 25 DEG C of conditions.
The sticky 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 DEG C of conditions.
Claims (5)
1. a preparation method for high viscosity granulation type Xylo-Mucine, is characterized in that comprising the following steps:
A, cotton fibre is torn up after, the mixing solutions together with sodium hydroxide solution and ethanolic soln joins in kneader, and 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 kneader, make vacuum tightness reach at least 0.06MPa;
C, rare gas element is filled with in kneader, makes kneader internal pressure be greater than 0.02MPa;
D, under protection of inert gas, carry out quaternization;
After e, quaternization terminate, add etherifying agent in the product obtained in steps d, wherein, the quality of etherifying agent is 1.20 ~ 1.30 times of the quality of purified cotton;
F, the air got rid of in kneader, make vacuum tightness reach at least 0.06MPa;
G, again rare gas element is filled with in kneader, makes kneader internal pressure be greater than 0.02MPa;
H, under protection of inert gas, carry out etherification reaction process;
I, by the product that obtains in step h through washing, neutralization, centrifugal;
J, will add in steam stripper in the product obtained after centrifugal, add the spirituous solution of aluminum chloride, the spirituous solution of aluminum chloride and the mass ratio of purified cotton be 1.0 ~ 1.5:1 simultaneously; The mass percent concentration of alcohol is 30 ~ 50%, the mass percent 0.5 ~ 1.5% of aluminum chloride, and the reaction times is 20 ~ 40 minutes, and temperature of reaction is 70 ~ 90 DEG C;
K, finally by the product in step j through super-dry, pulverizing.
2. the preparation method of high viscosity granulation type Xylo-Mucine according to claim 1, is characterized in that: in step a, and 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 preparing high viscosity granulation type Xylo-Mucine according to claim 1, is characterized in that: in steps d, the quaternization time is 40 ~ 70 minutes, and temperature of reaction is 10 ~ 40 DEG C.
4. the preparation method of high viscosity granulation type Xylo-Mucine according to claim 1, is characterized in that: in step e, and etherifying agent is chloroacetic ethanolic soln, and wherein, chloroacetic mass percent concentration is 50 ~ 80%.
5. the preparation method of high viscosity granulation type Xylo-Mucine according to claim 1, is characterized in that: in step h, and the etherification reaction time is 50 ~ 70 minutes, and temperature of reaction is 60 ~ 90 DEG C.
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