CN104761647B - Preparation method of quick-dissolving sodium carboxymethyl celluloses - Google Patents
Preparation method of quick-dissolving sodium carboxymethyl celluloses Download PDFInfo
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Abstract
The invention provides a preparation method of quick-dissolving sodium carboxymethyl celluloses, which comprises the following steps: alkalization: carrying out alkalization under the protection of nitrogen; etherification: in an etherification device, carrying out an etherification reaction for 45-55 minutes under the condition that the temperature is controlled at 75-80 DEG C; washing: transferring an etherified material into a washing device, washing for two time by using an alcohol aqueous solution, adding bleaching liquid to bleach; harrowed drying: transferring the washed material into a harrowed drying device to dry by harrowing; and drying and crushing: drying and crushing the material dried by harrowing under the condition that the temperature is controlled at 60-65 DEG C. According to the invention, products are endowed with a characteristic of quick dissolving by taking diethyl ether as a surfactant, so that the problem that sodium carboxymethyl celluloses are easily huddled in the process of application, so that the dissolution time is long is solved; and the preparation method has the advantages of simple process, convenience in use, low production cost, good product quality, and rapid dissolving speed, and the like.
Description
Technical field
The present invention relates to the preparing technical field of macromolecular compound is and in particular to a kind of instant level sodium carboxymethylcellulose
Preparation method.
Background technology
Sodium carboxymethyl cellulose (sodium carboxymethylcellulose, cmc), is the carboxy methylation of cellulose
Derivant, also known as cellulose gum, are the chemically modified a kind of water miscible ion-type ether obtaining.Its aqueous solution have thickening,
Bonding film forming, Protection glue, holding moisture, emulsifying and suspension effect, are topmost ionic cellulose element glue.Cmc typically by
Native cellulose is obtained after being reacted with caustic alkali and monochloroacetic acid, is a kind of anionic macromolecular compound, compound molecule
Amount is from thousand of to million.Cmc belongs to native cellulose modification, current FAO (Food and Agriculture Organization of the United Nation) (fao) and world health group
Formally it is called " modified cellulose " to knit (who).The synthetic method of cmc is to be invented in 1918 by German e.jansen
, and it is seen in generation in nineteen twenty-one issued patents, hereafter just in Europe, realization is commercially produced.Cmc was only crude product at that time,
Make colloid and binding agent uses.1936-1941, cmc industrial applied research is quite active, has delivered several suitable enlightenments
Patent.During World War II, cmc is used for as anti redeposition agent in synthetic detergent for Germany, and as some
The succedaneum of natural gum (such as gelatin, arabic gum), makes cmc industry obtain very big development.Hercules company of the U.S. in
Nineteen forty-three starts commercial production cmc, and produces refined cmc product in nineteen forty-six, and this product is recognized as safety food additive.
Cmc because having many special natures, such as thickening, bonding, film forming, water holding, emulsifying, suspension etc., and in itself nontoxic, odorless, be difficult
Fermentation, heat stability good the features such as and be widely used in the industries such as oil, geology, daily use chemicals, food, medicine, be described as " industry
Monosodium glutamate ".
At present, cmc commercial production, substantially divides solvent method and hydrophily method；The former is with ethanol (also can use isopropanol, acetone)
For solvent, product forms through desalination, purification, quality height, quality better, in neutrality；The latter's water is medium, sodium chloroacetate effectively utilizes
Rate is low, product salinity is big, moisture is high, in alkalescence, be crude product.The two be all cellulose through alkalization, again with monoxone or its sodium
Salt etherificate forms.Primary raw material: cotton linter, Caustic soda, soda, monoxone etc..
Content of the invention
It is an object of the invention to provide a kind of preparation method of instant level sodium carboxymethylcellulose, second diether is used as table
Face activating agent gives product instant characteristic, solves sodium carboxymethyl cellulose and easily unites in use so that dissolving
The problem of time length, has the advantages that process is simple, easy-to-use, low production cost, superior product quality, dissolution velocity are fast.
To achieve these goals, the technical solution used in the present invention is as follows:
A kind of preparation method of instant level sodium carboxymethylcellulose, comprises the steps:
1) alkalize:
A) prepare required liquid caustic soda and crude alcohol mixture, put into piece alkali and 20% liquid caustic soda in alkalization device and ethanol mixes
Compound；
B) liquid caustic soda of the industrial cotton of successively addition and residue 80% and crude alcohol mixture；
C) it is filled with nitrogen as protective gas in alkalization device, carry out 45～55 points of quaternization under agitation
Clock；
D) add a certain amount of monoxone alcohol blend under agitation, add rear reverse agitating function 2 minutes, more positive
Discharging after stirring 5 minutes；
2) it is etherified:
Material after alkalization is added ether-based device, is warming up to 75～80 DEG C in 15～20 minutes and carries out etherification reaction,
And keep constant temperature 45～55 minutes, and recovered alcohol simultaneously, then it is cooled to 55 DEG C, discharging；
3) wash:
Material after etherificate is proceeded to wash mill, is 72% to wash with 73% alcohol water blend with mass concentration respectively
Twice；Adjustment ph value is 7.0～7.5, adds bleaching liquid to be bleached, then discharging；
4) harrow and do:
Material after washing is proceeded to rake equipment for drying, after the completion of charging, is cooled to 40 DEG C, spray adds second diether ethanol to mix
Compound, stirs 20 minutes；It is warming up to 78～80 DEG C again, recovered alcohol under constant temperature, discharging after alcohol recycle finishes；
5) dries pulverizing:
Temperature is controlled to be 60～65 DEG C, the drying materials after rake is done, pulverizing.
According to above scheme, the quaternization time in described step 1 is 50 minutes, and stirring includes positive stirring and reverse
Stirring, except when reacting 20～30 minutes, reverse agitating function 2 minutes is outer, remaining time is positive stirring；Acid addition time is 50
Minute.
According to above scheme, described step 2) in etherification reaction temperature be 78 DEG C.
According to above scheme, described step 5) in when drying the mass concentration of material moisture control 6～8%, during pulverizing
The aperture of sieve board of grinder is 0.35mm, and during packaging, the precision of packaging vibrating screen is 80 mesh.
The invention has the beneficial effects as follows: it is used second diether to give product instant characteristic as surfactant, solve
Sodium carboxymethyl cellulose is easily united in use so that the problem of dissolution time length, and product is in neutrality, has work
The advantages of skill is simple, easy-to-use, low production cost, superior product quality, dissolution velocity are fast.
Specific embodiment
With reference to embodiment, technical scheme is illustrated.
Raw material and specification: smart cotton (degree of polymerization is 2400～2600), ethanol (ethanol content is 95%), (naoh contains liquid caustic soda
Amount 50%), piece alkali (technical grade), monoxone (>=95%), hydrochloric acid (content 36～37%).
Embodiment 1:
A kind of preparation method of instant level sodium carboxymethylcellulose, comprises the steps:
1) alkalize:
A) prepare required liquid caustic soda and crude alcohol mixture, put into piece alkali and 20% liquid caustic soda in alkalization device and ethanol mixes
Compound；
B) liquid caustic soda of the industrial cotton of successively addition and residue 80% and crude alcohol mixture；
C) it is filled with nitrogen as protective gas in alkalization device, carry out quaternization 50 minutes under agitation,
Reverse agitating function 2 minutes when reacting 25 minutes；
D) add monoxone alcohol blend in 50 minutes under agitation, add rear reverse agitating function 2 minutes, more just
The discharging to after stir 5 minutes；
2) it is etherified:
Material after alkalization is added ether-based device, is warming up to 78 DEG C in 17 minutes and carries out etherification reaction, and keep permanent
Temperature 50 minutes, recovered alcohol simultaneously, then it is cooled to 55 DEG C, discharging；
3) wash:
Material after etherificate is proceeded to wash mill, is 72% to wash with 73% alcohol water blend with mass concentration respectively
Twice；Adjustment ph value is 7.0～7.5, adds bleaching liquid to be bleached, then discharging；
4) harrow and do:
Material after washing is proceeded to rake equipment for drying, after the completion of charging, is cooled to 40 DEG C, spray adds second diether ethanol to mix
Compound, stirs 20 minutes；It is warming up to 79 DEG C again, recovered alcohol under constant temperature, discharging after alcohol recycle finishes；
5) dries pulverizing:
Temperature is controlled to be 63 DEG C, the drying materials after rake is done, pulverizing, during drying, the mass concentration of material moisture controls
7%, during pulverizing, the aperture of sieve board of grinder is 0.35mm, and during packaging, the precision of packaging vibrating screen is 80 mesh.
Embodiment 2:
A kind of preparation method of instant level sodium carboxymethylcellulose, comprises the steps:
1) alkalize:
A) prepare required liquid caustic soda and crude alcohol mixture, put into piece alkali and 20% liquid caustic soda in alkalization device and ethanol mixes
Compound；
B) liquid caustic soda of the industrial cotton of successively addition and residue 80% and crude alcohol mixture；
C) it is filled with nitrogen as protective gas in alkalization device, carry out quaternization 45 minutes under agitation,
Reverse agitating function 2 minutes when reacting 20 minutes；
D) add monoxone alcohol blend in 50 minutes under agitation, add rear reverse agitating function 2 minutes, more just
The discharging to after stir 5 minutes；
2) it is etherified:
Material after alkalization is added ether-based device, is warming up to 80 DEG C in 20 minutes and carries out etherification reaction, and keep permanent
Temperature 45 minutes, recovered alcohol simultaneously, then it is cooled to 55 DEG C, discharging；
3) wash:
Material after etherificate is proceeded to wash mill, is 72% to wash with 73% alcohol water blend with mass concentration respectively
Twice；Adjustment ph value is 7.0～7.5, adds bleaching liquid to be bleached, then discharging；
4) harrow and do:
Material after washing is proceeded to rake equipment for drying, after the completion of charging, is cooled to 40 DEG C, spray adds second diether ethanol to mix
Compound, stirs 20 minutes；It is warming up to 80 DEG C again, recovered alcohol under constant temperature, discharging after alcohol recycle finishes；
5) dries pulverizing:
Temperature is controlled to be 60 DEG C, the drying materials after rake is done, pulverizing, during drying, the mass concentration of material moisture controls
6%, during pulverizing, the aperture of sieve board of grinder is 0.35mm, and during packaging, the precision of packaging vibrating screen is 80 mesh.
Embodiment 3:
A kind of preparation method of instant level sodium carboxymethylcellulose, comprises the steps:
1) alkalize:
A) prepare required liquid caustic soda and crude alcohol mixture, put into piece alkali and 20% liquid caustic soda in alkalization device and ethanol mixes
Compound；
B) liquid caustic soda of the industrial cotton of successively addition and residue 80% and crude alcohol mixture；
C) it is filled with nitrogen as protective gas in alkalization device, carry out quaternization 55 minutes under agitation,
Reverse agitating function 2 minutes when reacting 30 minutes；
D) add monoxone alcohol blend in 50 minutes under agitation, add rear reverse agitating function 2 minutes, more just
The discharging to after stir 5 minutes；
2) it is etherified:
Material after alkalization is added ether-based device, is warming up to 75 DEG C in 15 minutes and carries out etherification reaction, and keep permanent
Temperature 50 minutes, recovered alcohol simultaneously, then it is cooled to 55 DEG C, discharging；
3) wash:
Material after etherificate is proceeded to wash mill, is 72% to wash with 73% alcohol water blend with mass concentration respectively
Twice；Adjustment ph value is 7.0～7.5, adds bleaching liquid to be bleached, then discharging；
4) harrow and do:
Material after washing is proceeded to rake equipment for drying, after the completion of charging, is cooled to 40 DEG C, spray adds second diether ethanol to mix
Compound, stirs 20 minutes；It is warming up to 78 DEG C again, recovered alcohol under constant temperature, discharging after alcohol recycle finishes；
5) dries pulverizing:
Temperature is controlled to be 65 DEG C, the drying materials after rake is done, pulverizing, during drying, the mass concentration of material moisture controls
8%, during pulverizing, the aperture of sieve board of grinder is 0.35mm, and during packaging, the precision of packaging vibrating screen is 80 mesh.
Above example only in order to illustrative and not limiting technical scheme, although above-described embodiment enters to the present invention
Gone detailed description, the person skilled of this area it is understood that the present invention being modified or replacing on an equal basis, but
Any modification without departing from spirit and scope of the invention and local are replaced and all should be covered in scope of the presently claimed invention.
Claims (4)
1. a kind of preparation method of instant level sodium carboxymethylcellulose is it is characterised in that comprise the steps:
1) alkalize:
A) prepare required liquid caustic soda and crude alcohol mixture, put into piece alkali in alkalization device and 20% liquid caustic soda is mixed with ethanol
Thing；
B) liquid caustic soda of the industrial cotton of successively addition and residue 80% and crude alcohol mixture；
C) it is filled with nitrogen as protective gas in alkalization device, carry out quaternization 45～55 minutes under agitation；
D) add a certain amount of monoxone alcohol blend under agitation, add rear reverse agitating function 2 minutes, more positive stirring
Discharging after 5 minutes；
Described stirring condition stirring includes positive stirring and reverse agitating function, except 2 points of the reverse agitating function when reacting 20～30 minutes
Outside clock, remaining time is positive stirring；
2) it is etherified:
Material after alkalization is added ether-based device, is warming up to 75～80 DEG C in 15～20 minutes and carries out etherification reaction, and protect
Hold constant temperature 45～55 minutes, simultaneously recovered alcohol, be then cooled to 55 DEG C, discharging；
3) wash:
Material after etherificate is proceeded to wash mill, washs two with the alcohol water blend that mass concentration is 72% and 73% respectively
Secondary；Adjustment ph value is 7.0～7.5, adds bleaching liquid to be bleached, then discharging；
4) harrow and do:
Material after washing is proceeded to rake equipment for drying, after the completion of charging, is cooled to 40 DEG C, spray adds second diether crude alcohol mixture,
Stirring 20 minutes；It is warming up to 78～80 DEG C again, recovered alcohol under constant temperature, discharging after alcohol recycle finishes；
5) dries pulverizing:
Temperature is controlled to be 60～65 DEG C, the drying materials after rake is done, pulverizing.
2. the preparation method of instant level sodium carboxymethylcellulose according to claim 1 is it is characterised in that described step 1
In the quaternization time be 50 minutes, acid addition time be 50 minutes.
3. the preparation method of instant level sodium carboxymethylcellulose according to claim 1 is it is characterised in that described step 2)
Middle etherification reaction temperature is 78 DEG C.
4. the preparation method of instant level sodium carboxymethylcellulose according to claim 1 is it is characterised in that described step 5)
The mass concentration of middle material moisture when drying controls 6～8%, and during pulverizing, the aperture of sieve board of grinder is 0.35mm, during packaging
The precision of packaging vibrating screen is 80 mesh.
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| CN109836506B (en) * | 2017-11-29 | 2021-08-20 | 上海长光企业发展有限公司 | Food-grade cellulose gum and preparation method thereof |
| CN114276461B (en) * | 2021-12-27 | 2023-03-28 | 重庆力宏精细化工有限公司 | Sodium carboxymethylcellulose and preparation method thereof, and battery cathode slurry and preparation method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101830989A (en) * | 2010-04-14 | 2010-09-15 | 兰州大学 | Method for preparing high-viscosity sodium carboxymethyl cellulose by utilizing potato starch residues |
| CN102268095A (en) * | 2011-07-28 | 2011-12-07 | 郑玉庆 | Preparation method of carboxymethyl cellulose |
| CN103554273A (en) * | 2013-10-31 | 2014-02-05 | 泸州北方化学工业有限公司 | Production method of technical-grade sodium carboxymethylcellulose |
| CN103865077A (en) * | 2014-03-17 | 2014-06-18 | 山东润峰集团新能源科技有限公司 | Method for rapidly dissolving sodium carboxymethylcellulose |
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- 2015-04-02 CN CN201510152478.0A patent/CN104761647B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101830989A (en) * | 2010-04-14 | 2010-09-15 | 兰州大学 | Method for preparing high-viscosity sodium carboxymethyl cellulose by utilizing potato starch residues |
| CN102268095A (en) * | 2011-07-28 | 2011-12-07 | 郑玉庆 | Preparation method of carboxymethyl cellulose |
| CN103554273A (en) * | 2013-10-31 | 2014-02-05 | 泸州北方化学工业有限公司 | Production method of technical-grade sodium carboxymethylcellulose |
| CN103865077A (en) * | 2014-03-17 | 2014-06-18 | 山东润峰集团新能源科技有限公司 | Method for rapidly dissolving sodium carboxymethylcellulose |
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