CN106699901A - Production technology of high viscosity sodium carboxymethyl cellulose - Google Patents
Production technology of high viscosity sodium carboxymethyl cellulose Download PDFInfo
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- CN106699901A CN106699901A CN201611191591.0A CN201611191591A CN106699901A CN 106699901 A CN106699901 A CN 106699901A CN 201611191591 A CN201611191591 A CN 201611191591A CN 106699901 A CN106699901 A CN 106699901A
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- 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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Abstract
The invention relates to a production technology of high viscosity sodium carboxymethyl cellulose. The production technology comprises the steps of washing raw materials; smashing; conducting an alkalization reaction, wherein smashed cotton clothes and cotton fabric are put into an alkalization kneading machine, air in the alkalization kneading machine is pumped out and inert gas is pumped into the alkalization kneading machine, the step is repeated for multiple times until vacuum degree in the alkalization kneading machine reaches 0.005 Mpa, and the alkalization reaction is conducted under the protection of the inert gas; conducting an etherification reaction, wherein the alkalized product is put into an etherification kneading machine to be subjected to the etherification reaction; washing; neutralization; centrifugation; drying; obtaining the product after smashing. According to the production technology of the high viscosity sodium carboxymethyl cellulos, discarded cotton clothes and cotton fabric are adopted as raw materials, waste is turned into wealth, the production cost is drastically reduced, the technology is easy to operate, the side product is less, the quality index of the obtained product reaches viscosity 1% B type (Brookfield Viscosity)>7000 mpa.s, the substituted ratio is bigger than 0.95, and the purity is bigger than 99.5%.
Description
Technical field
The present invention relates to the production field of sodium carboxymethylcellulose, more particularly to a kind of high-viscosity sodium carboxymethyl cellulose
Production technology.
Background technology
Sodium carboxymethylcellulose, abbreviation CMC is the carboxyl methylation derivant of cellulose, also known as cellulose gum, is main
Ionic cellulose element glue.CMC was seen in generation in 1918 by German prepared first and patented in nineteen twenty-one, hereafter
Just in Europe, realization is commercially produced.Only it is at that time crude product, as colloid and binding agent.1936-1941, to CMC industry
The research of application is quite active, and has delivered several with enlightening patent.It is German by CMC during World War II
For synthetic detergent.Hereafter, production technology, production efficiency and product quality progressively have and are significantly improved.Nineteen forty-seven, the U.S.
FDA is proved according to toxicological studies：CMC is acted on physiology nonhazardous, it is allowed to use it for making additive in food processing industry, is risen
Thickening power.CMC is because with many special natures：Its moisture absorption degree is relevant with atmospheric temperature and relative humidity, is balanced when reaching
Afterwards, just no longer moisture absorption；
The CMC aqueous solution has excellent bonding, thickening, emulsification, suspension, film forming, protecting colloid, holding moisture, resistance to enzymolysis
And it is metabolized the performances such as inertia；When the CMC aqueous solution meets with tin, silver, aluminium lead, iron, copper and some heavy metals, it may occur that precipitation is anti-
Should, when the CMC aqueous solution coexists with calcium, magnesium, salt, precipitation will not be produced, but the viscosity of the CMC aqueous solution can be reduced.The CMC aqueous solution
When running into acid, acid CMC precipitations can be separated out.But anti-acid CMC has certain resistance to acid solution；The CMC aqueous solution and water
The aqueous solution such as dissolubility animal glue, glycerine ethylene glycol, sorbierite, Arabic gum, pectin and soluble starch, can mutually mix altogether
It is molten, CMC decorating films, benzene, acetate esters, carbon tetrachloride, castor oil, corn oil, peanut oil, methyl alcohol, ethanol, ether, chloroform,
The things such as trichloroethanes, gasoline, MEK, toluene, dimethylbenzene, turpentine oil are such as thickened, bonded, film forming, water holding, emulsification, suspension,
And be used widely.In recent years, the CMC of different qualities is used in the different field of industry and people's life, extensive use
In industries such as oil, chemical industry, detergent, ceramics, cigarette, printing and dyeing, weaving, food, medicine, welding rods, have " industrial monosodium glutamate " it
Claim.The purposes of CMC widely, it is nontoxic, corrosion-free, harmless, free from environmental pollution, cohesive force is strong, do not go mouldy, do not give birth to
Worm, can be used as emulsifying agent, thickener, stabilizer, sizing agent, film forming agent, binding agent etc..
The common preparation technology of CMC can be divided into water-borne method and the major class of solvent method two.
With water as reaction medium, cellulosic material forms suspension and is sent out with basifier and etherifying agent water-borne method in the reactor
Raw reaction.Its advantage is that equipment is simple, low cost, but because cellulosic material can be gelatinized to form micelle in a large amount of water, reaction
Reagent is difficult to deeply to the crystalline region of cellulose, causes reaction not enough fully, and the carboxy methylation product substitution value of gained is low, salt content
Greatly, moisture content is high, and the product aqueous solution is in that heat resistance and salt tolerance are poor, are low-and-medium-grade products compared with strong basicity.
Solvent method technique is eliminated ripe after the intrinsic caustic dip of water-borne method, squeezing, alkalization with inert organic solvents as medium
The operations such as change, alkalization and etherificate are carried out in kneader, with short production cycle.The uniformity of product, dissolubility, the aqueous solution it is saturating
Lightness is all preferable, belongs to the carboxy methylation product of medium-to-high grade time.Therefore it is many both at home and abroad at present that CMC is produced with solvent method.But it is organic
Solvent it is relatively costly, generally require increases solvent recovering system in solvent method technological process.Further, since using largely having
Machine solvent, also requires to take a series of measure in secure context, just can guarantee that being smoothed out for production.
Two kinds of traditional handicrafts have certain limitation.With developing rapidly for national economy, the day of economic globalization paces
Increasingly fast, the cellulose ether production industry of China faces huge challenge.Under this background, in the urgent need to research and development one kind is produced into
This relatively low, process is simple, is easy to operation, and products obtained therefrom performance preferably new method to prepare CMC.
In terms of raw material, the traditional raw material that China prepares CMC is mainly by short velveteen through boiling, pickling, washing, drift
The cellulose obtained after preprocessing process, referred to as purified cotton such as in vain, roll, dry.The impurity content of purified cotton is relatively low, after refining
Alpha-cellulose content is more than 95% (mass fraction).But in recent years, raw material supply growing tension, cost of material is higher, causes
The production cost of CMC is higher, therefore in addition to the innovation of preparation method, is also necessary to seek cheap novel cellulose
Resource replaces purified cotton to prepare CMC.
Therefore, in order to overcome these problems, it is desirable to provide one kind can reduce the cost of raw material, obtain viscosity it is high, substitution
The preparation technology of the sodium carboxymethylcellulose that degree is high, purity is good.
The content of the invention
The purpose of the present invention is directed to not enough present in production sodium carboxymethylcellulose technique at present, there is provided one kind can
The cost of raw material is reduced, the preparation technology of the sodium carboxymethylcellulose that viscosity is high, substitution value is high, purity is good is obtained.
The technical scheme is that：A kind of production technology of high-viscosity sodium carboxymethyl cellulose, it is characterised in that including
Following steps：
(1) raw material washing：The waste and old cotton dress cotton that will be purchased by salvage station is rinsed in being put into initial feed kitchen sink
Washing；
(2) crush：The cotton dress cotton obtained by step (1) is put into pulverizer to be crushed；
(3) quaternization：To will be alkalized by the cotton dress cotton input alkalization kneader after the crushing that step (2) obtain
Air in kneader is extracted out and is filled with inert gas, is repeated several times until being at least up to vacuum in alkalization kneader
0.005MPa, carries out quaternization under inert gas shielding, and reaction temperature is 0 DEG C~4 DEG C, and the reaction time is 30~50min；
(4) etherification reaction：Product input etherificate kneader after the alkalization that step (3) is obtained, carries out etherification reaction, instead
It is 78 DEG C~80 DEG C to answer temperature, and the reaction time is 50~70min；
(5) wash：Product after the etherificate that will be obtained in step (4) is put into washing in kitchen sink, product capacity and washing
Liquid capacity ratio is 1：4；
(6) neutralize：The product obtained in step (5) is carried out into acid-base neutralization, is 7~8 to PH；
(7) it is centrifuged：The product obtained in step (6) is centrifuged, wherein, centrifuge speed be 2100~2200 turns/
Point, press speed is 8m3/h；
(8) dry：The product obtained in step (7) is dried；
(9) crush：The product obtained in step (8) is crushed, finished product is obtained after packaging.
It is pointed out that the cleaning solution part by weight in initial feed kitchen sink in the step (1) is：Alcohol
60%th, sodium hypochlorite 30%, hydrogen peroxide 10%.
It is pointed out that the quaternization alkaline solution part by weight in the step (3)：Alcohol 82.5%, liquid caustic soda
12.4%th, solid sodium hydroxide 5.1%.
It is pointed out that the concentration of the liquid caustic soda is 30-32% or 40-42%.
It is pointed out that ether-based liquid is 78% alcohol and monoxone in the step (4), wherein, alcohol and monoxone
Ratio be 4:1.
It is pointed out that the cleaning solution in the step (5) in kitchen sink is alcohol and hydrogen peroxide, its part by weight is
9:1。
It is pointed out that the alcohol in the step (5) in kitchen sink is 78% alcohol.
For further, can also consider in the present invention, the filtrate obtained after centrifugation in the step (7) can be through dividing
Ethanol solution is reclaimed after evaporating, and is recycled as cleaning solution component in step (5).
The beneficial effects of the present invention are：
A kind of production technology of high-viscosity sodium carboxymethyl cellulose of the invention, with waste and old cotton dress cotton as raw material, becomes useless
It is treasured, greatly reduces production cost, technique is easy to operate, and accessory substance is few, and the product quality indicator for obtaining can reach viscosity
1%B types (Brookfield Viscosity) ＞ 7000mpa.s, substitution value>0.95, purity ＞ 99.5%.
Specific embodiment
Embodiment 1
A kind of production technology of high-viscosity sodium carboxymethyl cellulose, comprises the following steps：
(1) raw material washing：The waste and old cotton dress cotton that will be purchased by salvage station is rinsed in being put into initial feed kitchen sink
Wash, cleaning solution part by weight is：Alcohol 60%, sodium hypochlorite 30%, hydrogen peroxide 10%；
(2) crush：The cotton dress cotton obtained by step (1) is put into pulverizer to be crushed；
(3) quaternization：To will be alkalized by the cotton dress cotton input alkalization kneader after the crushing that step (2) obtain
Air in kneader is extracted out and is filled with inert gas, is repeated several times until being at least up to vacuum in alkalization kneader
0.005MPa, carries out quaternization under inert gas shielding, and reaction temperature is 2 DEG C, and the reaction time is 40min, quaternization
Alkaline solution part by weight：Alcohol 82.5%, liquid caustic soda 12.4%, solid sodium hydroxide 5.1%；
(4) etherification reaction：Product input etherificate kneader after the alkalization that step (3) is obtained, carries out etherification reaction, instead
Answer temperature for 79 DEG C, the reaction time is 60, ether-based liquid is 78% alcohol and monoxone, wherein, alcohol and chloroacetic ratio are
4:1；
(5) wash：Product after the etherificate that will be obtained in step (4) is put into washing in kitchen sink, product capacity and washing
Liquid capacity ratio is 1：4, cleaning solution is alcohol and hydrogen peroxide, and its part by weight is 9:1；
(6) neutralize：The product obtained in step (5) is carried out into acid-base neutralization, is 7 to PH；
(7) it is centrifuged：The product obtained in step (6) is centrifuged, wherein, centrifuge speed be 2100~2200 turns/
Point, press speed is 8m3/h；
(8) dry：The product obtained in step (7) is dried；
(9) crush：The product obtained in step (8) is crushed, finished product is obtained after packaging.
The viscosity of finished product is 7500mpa.s, and substitution value is 0.96, and purity is 99.7.
Embodiment 2
A kind of production technology of high-viscosity sodium carboxymethyl cellulose, comprises the following steps：
(1) raw material washing：The waste and old cotton dress cotton that will be purchased by salvage station is rinsed in being put into initial feed kitchen sink
Wash, cleaning solution part by weight is：Alcohol 60%, sodium hypochlorite 30%, hydrogen peroxide 10%；
(2) crush：The cotton dress cotton obtained by step (1) is put into pulverizer to be crushed；
(3) quaternization：To will be alkalized by the cotton dress cotton input alkalization kneader after the crushing that step (2) obtain
Air in kneader is extracted out and is filled with inert gas, is repeated several times until being at least up to vacuum in alkalization kneader
0.005MPa, carries out quaternization under inert gas shielding, and reaction temperature is 4 DEG C, and the reaction time is 50min, quaternization
Alkaline solution part by weight：Alcohol 82.5%, liquid caustic soda 12.4%, solid sodium hydroxide 5.1%；
(4) etherification reaction：Product input etherificate kneader after the alkalization that step (3) is obtained, carries out etherification reaction, instead
Answer temperature for 80 DEG C, the reaction time is 70, ether-based liquid is 78% alcohol and monoxone, wherein, alcohol and chloroacetic ratio are
4:1；
(5) wash：Product after the etherificate that will be obtained in step (4) is put into washing in kitchen sink, product capacity and washing
Liquid capacity ratio is 1：4, cleaning solution is alcohol and hydrogen peroxide, and its part by weight is 9:1；
(6) neutralize：The product obtained in step (5) is carried out into acid-base neutralization, is 8 to PH；
(7) it is centrifuged：The product obtained in step (6) is centrifuged, wherein, centrifuge speed be 2100~2200 turns/
Point, press speed is 8m3/h；
(8) dry：The product obtained in step (7) is dried；
(9) crush：The product obtained in step (8) is crushed, finished product is obtained after packaging.
The viscosity of finished product is 7100mpa.s, and substitution value is 0.98, and purity is 99.6.
Two embodiments of the invention have been described in detail above, but the content is only preferable implementation of the invention
Example, it is impossible to be considered as limiting practical range of the invention.All impartial changes made according to the present patent application scope and improvement
Deng all should still belong within patent covering scope of the invention.
Claims (8)
1. a kind of production technology of high-viscosity sodium carboxymethyl cellulose, it is characterised in that comprise the following steps：
(1) raw material washing：The waste and old cotton dress cotton that will be purchased by salvage station rinses washing in being put into initial feed kitchen sink；
(2) crush：The cotton dress cotton obtained by step (1) is put into pulverizer to be crushed；
(3) quaternization：Alkalization will be mediated by the cotton dress cotton input alkalization kneader after the crushing that step (2) obtain
Air in machine is extracted out and is filled with inert gas, is repeated several times until being at least up to vacuum in alkalization kneader
0.005MPa, carries out quaternization under inert gas shielding, and reaction temperature is 0 DEG C~4 DEG C, and the reaction time is 30~50min；
(4) etherification reaction：Product input etherificate kneader after the alkalization that step (3) is obtained, carries out etherification reaction, reaction temperature
It is 78 DEG C~80 DEG C to spend, and the reaction time is 50~70min；
(5) wash：Product after the etherificate that will be obtained in step (4) is washed in being put into kitchen sink, and product capacity is held with cleaning solution
Amount ratio is 1：4；
(6) neutralize：The product obtained in step (5) is carried out into acid-base neutralization, is 7~8 to PH；
(7) it is centrifuged：The product obtained in step (6) is centrifuged, wherein, centrifuge speed is 2100~2200 revs/min, pressure
Squeezing speed is 8m3/h；
(8) dry：The product obtained in step (7) is dried；
(9) crush：The product obtained in step (8) is crushed, finished product is obtained after packaging.
2. the production technology of a kind of high-viscosity sodium carboxymethyl cellulose according to claim 1, it is characterised in that：The step
Suddenly the cleaning solution part by weight in the initial feed kitchen sink in (1) is：Alcohol 60%, sodium hypochlorite 30%, hydrogen peroxide 10%.
3. the production technology of a kind of high-viscosity sodium carboxymethyl cellulose according to claim 1, it is characterised in that：The step
Suddenly the quaternization alkaline solution part by weight in (3)：Alcohol 82.5%, liquid caustic soda 12.4%, solid sodium hydroxide 5.1%.
4. the production technology of a kind of high-viscosity sodium carboxymethyl cellulose according to claim 3, it is characterised in that：The liquid
The concentration of alkali is 30-32% or 40-42%.
5. the production technology of a kind of high-viscosity sodium carboxymethyl cellulose according to claim 1, it is characterised in that：The step
Suddenly ether-based liquid is 78% alcohol and monoxone in (4), wherein, alcohol and chloroacetic ratio are 4:1.
6. the production technology of a kind of high-viscosity sodium carboxymethyl cellulose according to claim 1, it is characterised in that：The step
Suddenly the cleaning solution in (5) in kitchen sink is alcohol and hydrogen peroxide, and its part by weight is 9:1.
7. the production technology of a kind of high-viscosity sodium carboxymethyl cellulose according to claim 6, it is characterised in that：The step
Suddenly the alcohol in (5) in kitchen sink is 78% alcohol.
8. the production technology of a kind of high-viscosity sodium carboxymethyl cellulose according to claim 1, it is characterised in that：The step
Suddenly the filtrate for being obtained after centrifugation in (7) reclaims ethanol solution after being fractionated into, and makes as cleaning solution component circulation in step (5)
With.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107419579A (en) * | 2017-08-02 | 2017-12-01 | 新乡化纤股份有限公司 | The method for reclaiming waste cotton fabric biomass fiber manufacture dissolving pulp |
| CN109666077A (en) * | 2018-12-28 | 2019-04-23 | 陕西师范大学 | A method of high-viscosity sodium carboxymethyl cellulose is prepared using ramee element as raw material |
| CN111148451A (en) * | 2017-12-14 | 2020-05-12 | 株式会社Lg化学 | Method for manufacturing mask for adsorbing heavy metals and mask manufactured thereby |
| CN112679620A (en) * | 2020-12-28 | 2021-04-20 | 江苏派克斯特纤维素有限公司 | Preparation method of instant 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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| CN101220099A (en) * | 2008-01-31 | 2008-07-16 | 重庆力宏精细化工有限公司 | Production method for high viscosity sodium carboxymethylcellulose |
| 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 |
| CN105801710A (en) * | 2016-05-24 | 2016-07-27 | 江苏泰利达新材料股份有限公司 | Production process of ultralow-viscosity sodium carboxymethylcellulose |
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| CN101220099A (en) * | 2008-01-31 | 2008-07-16 | 重庆力宏精细化工有限公司 | Production method for high viscosity sodium carboxymethylcellulose |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107419579A (en) * | 2017-08-02 | 2017-12-01 | 新乡化纤股份有限公司 | The method for reclaiming waste cotton fabric biomass fiber manufacture dissolving pulp |
| CN111148451A (en) * | 2017-12-14 | 2020-05-12 | 株式会社Lg化学 | Method for manufacturing mask for adsorbing heavy metals and mask manufactured thereby |
| US11771204B2 (en) | 2017-12-14 | 2023-10-03 | Lg Chem, Ltd. | Method for manufacturing mask pack for adsorbing heavy metals, and mask pack manufactured thereby |
| CN109666077A (en) * | 2018-12-28 | 2019-04-23 | 陕西师范大学 | A method of high-viscosity sodium carboxymethyl cellulose is prepared using ramee element as raw material |
| CN112679620A (en) * | 2020-12-28 | 2021-04-20 | 江苏派克斯特纤维素有限公司 | Preparation method of instant 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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Application publication date: 20170524 |