CN105330752B - A kind of method for preparing carboxymethyl cellulose with high degree sodium - Google Patents
A kind of method for preparing carboxymethyl cellulose with high degree sodium Download PDFInfo
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- CN105330752B CN105330752B CN201510827053.5A CN201510827053A CN105330752B CN 105330752 B CN105330752 B CN 105330752B CN 201510827053 A CN201510827053 A CN 201510827053A CN 105330752 B CN105330752 B CN 105330752B
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- C—CHEMISTRY; METALLURGY
- 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]
Abstract
The invention belongs to chemical fields, and in particular to a kind of method for preparing carboxymethyl cellulose with high degree sodium.The technical problems to be solved by the invention are to provide a kind of method for preparing carboxymethyl cellulose with high degree sodium, include the following steps：A, alcohol and sodium hydrate aqueous solution are configured to mixed liquor；B, the mixed liquor of step a and cellulosic material, sodium hydrate solid mixing are subjected to quaternization；C, etherification reaction is carried out in the material for adding in etherifying agent after step b reactions；D, etherifying agent is added in the materials of step c after reaction and carries out etherification reaction again；E, alcohol and sodium hydrate aqueous solution are configured to mixed liquor；F, the mixed liquor of step e and the material mixings of step d after reaction are subjected to quaternization again；E, it post-processes.The sodium carboxymethylcellulose that degree of substitution is up to more than 1.35 can be prepared in the method for the present invention.
Description
Technical field
The invention belongs to chemical fields, and in particular to a kind of method for preparing carboxymethyl cellulose with high degree sodium.
Background technology
Sodium carboxymethylcellulose is a kind of important cellulose ether, be that natural fiber is obtained after chemical modification one
The polyanionic compound of kind good water solubility, is soluble in hot and cold water.It has emulsifying dispersant, solid dispersibility, be not easy corruption,
Physiologically harmless etc. unusual and extremely valuable comprehensive physical, chemical property, are a kind of widely used natural polymers
Sub- derivative.The leading indicator for weighing sodium carboxymethylcellulose quality is degree of substitution (DS) and viscosity, degree of substitution difference then carboxylic first
The property of base sodium cellulosate is also different；In general degree of substitution is bigger, and the stability of solution is also better.
Invention content
The goal of the invention of the present invention is to provide for a kind of method for the sodium carboxymethylcellulose for preparing high substituted degree.The party
The degree of substitution for the sodium carboxymethylcellulose that method can be prepared is up to more than 1.35.
The technical problems to be solved by the invention are to provide a kind of method for the sodium carboxymethylcellulose for preparing high substituted degree.
This method includes the following steps：
A, mixed liquor is prepared：By 220~270 parts of alcohol and 95~125 parts of sodium hydrate aqueous solution mixings, mixed liquor is controlled
Temperature is 20~45 DEG C, obtains mixed liquor；
B, it alkalizes：The temperature of reaction unit is controlled less than 40 DEG C, added in into reaction unit 40~60 parts of cellulosic materials,
The mixed liquor progress quaternization of 45~65 parts of solid sodium hydroxides, step a；It is 20 that charging, which starts to alkalization finishing control temperature,
~50 DEG C, it is 50~80min that charging, which started to the time that alkalization terminates,；
C, it is etherified：65~90 parts of etherifying agent is added in the materials of step b after reaction and carries out etherification reaction；Add
It is 35~60 DEG C that material, which starts to etherificate finishing control temperature, and it is 20~40min that charging, which started to the time that etherificate terminates,；The ether
Agent is the monoxone alcoholic solution of concentration 73.0~75.0% (w/w)；
D, it is etherified again：25~40 portions of etherifying agents are added in the materials of step c after reaction and are etherified again
Reaction；It is 35~60 DEG C that charging, which starts to etherificate finishing control temperature, the time that charging starts to etherificate to terminate for 10~
25min；The etherifying agent is the monoxone alcoholic solution of concentration 73.0~75.0% (w/w)；
E, mixed liquor is prepared again：By 85~110 parts of alcohol and 35~60 parts of sodium hydrate aqueous solution mixings, temperature is controlled
It is 20~45 DEG C, obtains mixed liquor；
F, it alkalizes again：The mixed liquor of step e, 15~25 parts of solid sodium hydroxides are added to step d after reaction
Material in carry out quaternization again；It feeds before terminating controlled at 40~60 DEG C；After charging controlled at
50~60 DEG C of 5~10min of stirring；It is warming up to 30~40min of constant temperature at 75~80 DEG C again；It is cooled to less than 50 DEG C again；
G, neutralization, the materials of washing step f after reaction are dried after separation of solid and liquid, are crushed, packed and taken up to height
The sodium carboxymethylcellulose of Dai Du；
Above-mentioned number represents the mole of each raw material；If the raw material is solution, number if, represents the mole of its solute.
Preferably, in the method and step a of above-mentioned preparation carboxymethyl cellulose with high degree sodium, a concentration of the 90 of the alcohol
~95% (v/v)；A concentration of 48.0~50.0% (w/w) of the sodium hydrate aqueous solution.
Preferably, in the method and step b of above-mentioned preparation carboxymethyl cellulose with high degree sodium, the cellulosic material is
Any one in purified cotton, wood pulp or bamboo pulp.
Preferably, in the method and step b of above-mentioned preparation carboxymethyl cellulose with high degree sodium, the charging starts to charging
End time is 8~12min.
Preferably, in the method and step c of above-mentioned preparation carboxymethyl cellulose with high degree sodium, the etherifying agent is with quality
The monoxone of score >=97.5% is that solute, 90~95% (v/v) alcohol are formulated for solvent.
Preferably, in the method and step c of above-mentioned preparation carboxymethyl cellulose with high degree sodium, the charging starts to charging
End time is 15~25min.
Preferably, in the method and step d of above-mentioned preparation carboxymethyl cellulose with high degree sodium, the etherifying agent is with quality
The monoxone of score >=97.5% is that solute, 90~95% (v/v) alcohol are formulated for solvent.
Preferably, in the method and step d of above-mentioned preparation carboxymethyl cellulose with high degree sodium, the charging starts to charging
End time is 5~15min.
Preferably, in the method and step e of above-mentioned preparation carboxymethyl cellulose with high degree sodium, a concentration of the 90 of the alcohol
~95% (v/v)；A concentration of 48.0~50.0% (w/w) of the sodium hydrate aqueous solution.
Preferably, in the method and step f of above-mentioned preparation carboxymethyl cellulose with high degree sodium, the charging starts to charging
End time is 5~15min.
Preferably, in the method and step g of above-mentioned preparation carboxymethyl cellulose with high degree sodium, the alcohol of the washing use
A concentration of 75~85 (v/v) %.
The method of the present invention is by controlling suitable feeding quantity, feed time, reaction time and etherificate and twice alkali twice
The sodium carboxymethylcellulose that degree of substitution is up to more than 1.35 has been prepared in change, so as to the system for high substituted carboxymethyl sodium cellulosate
It is standby to provide a more efficient way.
Specific embodiment
A kind of method for the sodium carboxymethylcellulose for preparing high substituted degree, includes the following steps：
A, mixed liquor is prepared：By a concentration of 90~95% (v/v) 220~270 parts of alcohol and a concentration of 48.0~50.0%
(w/w) 95~125 parts of sodium hydrate aqueous solution mixings, control mixeding liquid temperature is 20~45 DEG C, obtains mixed liquor；
B, it alkalizes：The temperature of reaction unit is controlled to add in 40~60 into reaction unit in 8~12min less than 40 DEG C
The mixed liquor progress quaternization of part cellulosic material, 45~65 parts of solid sodium hydroxides, step a；Charging starts to alkalization to tie
For beam controlled at 20~50 DEG C, it is 50~80min that charging, which started to the time that alkalization terminates,；
C, it is etherified：By 65~90 parts of etherifying agent be added in 15~25min in the materials of step b after reaction into
Row etherification reaction；It is 35~60 DEG C that charging, which starts to etherificate finishing control temperature, and it is 20 that charging, which started to the time that etherificate terminates,
~40min；The etherifying agent is matched using the monoxone of mass fraction >=97.5% as solute, 90~95% (v/v) alcohol for solvent
Make the monoxone alcoholic solution of a concentration of 73.0~75.0% (w/w) formed；
D, it is etherified again：25~40 portions of etherifying agents are added in 5~15min in the materials of step c after reaction
Etherification reaction is carried out again；Charging start to etherificate finishing control temperature be 35~60 DEG C, charging start to etherificate terminate when
Between be 10~25min；The etherifying agent is using the monoxone of mass fraction >=97.5% as solute, 90~95% (v/v) alcohol
The monoxone alcoholic solution of a concentration of 73.0~75.0% (w/w) that solvent is formulated；
E, mixed liquor is prepared again：By a concentration of 90~95% (v/v) 85~110 parts of alcohol and a concentration of 48.0~
50.0% 35~60 parts of (w/w) sodium hydrate aqueous solution mixing, controlled at 20~45 DEG C, obtains mixed liquor；
F, it alkalizes again：The mixed liquor of step e, 15~25 parts of solid sodium hydroxides are added to step in 5~15min
Quaternization is carried out again in the materials of d after reaction；It feeds before terminating controlled at 40~60 DEG C；After charging
Controlled at 50~60 DEG C of 5~10min of stirring；It is warming up to 30~40min of constant temperature at 75~80 DEG C again；Be cooled to again 50 DEG C with
Under；
G, neutralization, the materials of washing step f after reaction are dried after separation of solid and liquid, are crushed, packed and taken up to height
The sodium carboxymethylcellulose of Dai Du；
Above-mentioned number represents the mole of each raw material；If the raw material is solution, number if, represents the mole of its solute.
Such as：1) when raw material is solution, such as 95~125 parts of sodium hydrate aqueous solutions in step a, represent that purity is
The mole of 100% sodium hydrate solid is 95~125 parts, if used solid sodium hydroxide purity is not 100%,
It so just weighs, is then added in corresponding water, the sodium hydroxide for being configured to respective concentration is water-soluble again after being converted
Liquid；
2) when raw material is solid, such as 45~65 parts of solid sodium hydroxides in step b, the hydrogen that purity is 100% is represented
Sodium oxide molybdena mole is 45~65 parts, if used solid sodium hydroxide purity is not 100%, then with regard to being changed
It is weighed again after calculation.
The degree of substitution for the sodium carboxymethylcellulose that the method for the present invention is prepared is the method analysis according to GB1904-2005
It detects obtained.
Embodiment 1
(1), mixed liquor is prepared：By 227 parts of a concentration of 90% (v/v) alcohol and 112 parts of a concentration of 48.0% (w/w) liquid caustic soda
Mixed liquor is mixed to obtain, control mixeding liquid temperature is 45 DEG C；
(2), it alkalizes：Control mediates built-in temperature less than 40 DEG C, in 10min that 55 parts of wood pulp cellulose raw material are equal
In even addition kneader, during feeding intake, 60 parts of piece alkali are added three times, while mixed liquor prepared by step (1) is passed through into spray
Shower pipe is added in kneader, and mixed liquor adds in time 12min, and the quaternization time (including charging time) is 50min, is controlled
30 DEG C~50 DEG C of quaternization temperature；
(3), etherifying agent is prepared：Using the monoxone of mass fraction >=97.5% as solute, 90% (v/v) alcohol is matched for solvent
Make the etherifying agent of a concentration of 74.0% (w/w)；
(4), it is etherified：The etherifying agent of 70 parts of steps (3) is added to the material of step (2) after reaction by spray tube
In, time 20min is added in, stirs 10min later, temperature is controlled at 40 DEG C~60 DEG C；
(5), it is etherified again：The monoxone alcoholic solution of 28 parts of a concentration of 74.0% (w/w) is added to by spray tube
In material after step (4) reaction, time 10min is added in, then stirs 5min, temperature is controlled at 40 DEG C~60 DEG C, using
10min slowly heats up, until 58 DEG C~60 DEG C constant temperature 20min；
(6), mixed liquor is prepared：89 parts of a concentration of 90% (v/v) alcohol and 54 parts of a concentration of 48.0% (w/w) liquid caustic soda are stirred
It mixes and mixes to obtain mixed liquor, control mixeding liquid temperature is 35 DEG C~45 DEG C；
(7), it alkalizes again：The mixed liquor of step (6) is added in by spray tube in the material of step (5), adds in the time
10min, with 2 additions of time-division, 25 parts of piece alkali；After stirring 10min, then 10min heatings are passed slowly, until 75 DEG C~78 DEG C constant temperature
35min is cooled to less than 50 DEG C and enters washing kettle；
(8) it washs：It washs for the first time：The alcohol of 1800 parts of a concentration of 80% (v/v) is got in washing kettle ready, by step (7)
Material is put into washing kettle, adds in 1 part of bleaching liquid, is stirred and is added in hydrochloric acid adjusting pH value, hydrochloric acid dosage after being spaced at least 10min
9 parts, 10min or so is then stirred, starts to centrifuge；Second of washing：Get 1800 parts of a concentration of 80% (v/v's) in washing kettle ready
Alcohol, the material after once washing centrifugation enter in washing kettle, and stirring at least starts to centrifuge after twenty minutes.
(9), drying and last handling process：High substitution is dried, crushed, packing and to be obtained to product process after step (8) has centrifuged
Spend sodium carboxymethylcellulose.
Embodiment 1 and the 7 batches of same periods require with all achievement datas of technique productions product according to GB 1904-2005
Method analysis obtain, as shown in table 1：
Table 1
| Lot number | Viscosity (mpa.s) | PH | Degree of substitution | CI- (%) | Moisture content (%) |
| Standard | ≤40 | 6.5-8.0 | ≥1.35 | ≤2 | ≤10 |
| Embodiment 1 | 27.5 | 7.05 | 1.39 | 1.57 | 7.45 |
| 12-13-4 | 23.8 | 7.12 | 1.38 | 1.64 | 7.59 |
| 12-14-4 | 24.6 | 7.08 | 1.41 | 1.61 | 6.75 |
| 12-14-5 | 23.0 | 7.07 | 1.40 | 1.57 | 7.65 |
| 12-15-4 | 22.1 | 7.03 | 1.41 | 1.55 | 6.56 |
| 12-15-5 | 23.9 | 7.06 | 1.39 | 1.53 | 5.83 |
| 12-16-4 | 23.0 | 7.08 | 1.38 | 1.58 | 5.54 |
| 12-16-5 | 26.5 | 7.01 | 1.41 | 1.62 | 6.40 |
Comparative example 1
(1), first time Compound mixed solution：By 300 parts of a concentration of 90% (v/v) alcohol and 166 parts of a concentration of 48.0% (w/
W) mixed liquor is mixed to obtain in liquid caustic soda, and control mixeding liquid temperature is 45 DEG C；
(2), it alkalizes for the first time：Control mediates built-in temperature control at 40 DEG C, by 55 parts of wood pulp cellulose in 10min
Raw material are uniformly added into kneader, during feeding intake, point 5 additions, 85 parts of piece alkali, while will be mixed prepared by step (1)
Liquid is added to by spray tube in kneader, and mixed liquor adds in time 12min, and the quaternization time is (including charging time)
50min, 30 DEG C~55 DEG C of control quaternization temperature；
(3), etherifying agent is prepared：Using the monoxone of mass fraction >=97.5% as solute, 90% (v/v) alcohol is matched for solvent
Make the etherificate of 74.0% (w/w)；
(4), it is etherified for the first time：Material after first time is alkalized adds in a concentration of 74.0% (w/ by spray tube
W) 70 parts of monoxone alcoholic solution adds in time 20min, stirs 10min later, and temperature is controlled at 40 DEG C~60 DEG C；
(5), it is etherified for second：Material after first time etherification reaction is added in into a concentration of 74.0% (w/ by spray tube
W) 28 parts of monoxone alcoholic solution adds in time 10min, then stirs 5min, and temperature is controlled at 40 DEG C~60 DEG C, then slowly
Heat up by 15min, until 75 DEG C of -78 DEG C of constant temperature 35min, after be cooled to less than 50 DEG C and enter washing kettle；
(6) it washs for the first time：It gets the alcohol of 1800 parts of a concentration of 70% (v/v) in washing kettle ready, step (7) material is put
Enter in washing kettle, add in 1 part of bleaching liquid, stir and add in hydrochloric acid adjusting pH value, hydrochloric acid dosage≤10 after being spaced at least 10min
Part, 10min or so is then stirred, starts to centrifuge；Second of washing：Get 1800 parts of a concentration of 70% (v/v's) in washing kettle ready
Alcohol, the material after a washing centrifugation enter in washing kettle, and stirring at least starts to centrifuge after twenty minutes.
(7), drying and last handling process：High substitution is dried, crushed, packing and to be obtained to product process after step (6) has centrifuged
Spend sodium carboxymethylcellulose.
Comparative example 1 and the 7 batches of same periods require with all achievement datas of technique productions product according to GB 1904-2005
Method analysis obtain, as shown in table 2：
Table 2
| Lot number | Viscosity (mpa.s) | PH | Degree of substitution | CI- (%) | Moisture content (%) |
| Standard | ≤40 | 6.5-8.0 | ≥1.35 | ≤2 | ≤10 |
| Comparative example 1 | 25.5 | 7.10 | 0.94 | 1.67 | 8.45 |
| 10-13-12 | 24.0 | 7.09 | 0.95 | 1.60 | 7.50 |
| 10-14-11 | 25.0 | 7.00 | 0.93 | 1.60 | 6.79 |
| 10-14-12 | 24.0 | 7.12 | 0.95 | 1.59 | 7.66 |
| 10-15-10 | 23.0 | 7.04 | 0.94 | 1.55 | 6.66 |
| 10-15-11 | 24.0 | 7.08 | 0.95 | 1.53 | 6.83 |
| 10-16-10 | 23.6 | 7.08 | 0.93 | 1.58 | 6.59 |
| 10-16-11 | 24.5 | 7.01 | 0.94 | 1.62 | 7.60 |
From the comparison of table 1,2 as can be seen that the degree of substitution of sodium carboxymethylcellulose that is prepared of the method for the present invention is significantly high
It is prepared in conventional method, while also meets the requirement of standard, illustrate that the method for the present invention can effectively prepare height
The sodium carboxymethylcellulose of degree of substitution.
Claims (6)
- A kind of 1. method for preparing carboxymethyl cellulose with high degree sodium, it is characterised in that：Include the following steps：A, mixed liquor is prepared：By 220~270 parts of alcohol and 95~125 parts of sodium hydrate aqueous solution mixings, mixeding liquid temperature is controlled It is 20~45 DEG C, obtains mixed liquor；B, it alkalizes：The temperature of reaction unit is controlled less than 40 DEG C, added in into reaction unit 40~60 parts of cellulosic materials, 45~ The mixed liquor progress quaternization of 65 parts of solid sodium hydroxides, step a；It is 20~50 that charging, which starts to alkalization finishing control temperature, DEG C, it is 50~80min that charging, which started to the time that alkalization terminates,；It is 8~12min that charging, which started to the charging end time,；C, it is etherified：65~90 parts of etherifying agent is added in the materials of step b after reaction and carries out etherification reaction；Charging is opened It is 35~60 DEG C to begin to etherificate finishing control temperature, and it is 20~40min that charging, which started to the time that etherificate terminates,；The etherifying agent Monoxone alcoholic solution for mass concentration 73.0~75.0%；It is 15~25min that charging, which started to the charging end time,；D, it is etherified again：25~40 portions of etherifying agents are added in the materials of step c after reaction and carry out etherification reaction again； It is 35~60 DEG C that charging, which starts to etherificate finishing control temperature, and it is 10~25min that charging, which started to the time that etherificate terminates,；It is described Etherifying agent is the monoxone alcoholic solution of mass concentration 73.0~75.0%；Charging start to the charging end time for 5~ 15min；E, mixed liquor is prepared again：By 85~110 parts of alcohol and 35~60 parts of sodium hydrate aqueous solution mixings, controlled at 20 ~45 DEG C, obtain mixed liquor；F, it alkalizes again：The mixed liquor of step e, 15~25 parts of sodium hydroxides are added in the materials of step d after reaction Quaternization is carried out again；It feeds before terminating controlled at 40~60 DEG C；Controlled at 50~60 DEG C after charging Stir 5~10min；It is warming up to 30~40min of constant temperature at 75~80 DEG C again；It is cooled to less than 50 DEG C again；Charging starts to charging End time is 5~15min；G, neutralization, the materials of washing step f after reaction are dried after separation of solid and liquid, are crushed, being packed up to high substituted degree Sodium carboxymethylcellulose；Above-mentioned number represents the mole of each raw material；If the raw material is solution, number if, represents the mole of its solute.
- 2. the method according to claim 1 for preparing carboxymethyl cellulose with high degree sodium, it is characterised in that：Step a or e In, the volumetric concentration of the alcohol is 90~95%；The mass concentration of the sodium hydrate aqueous solution is 48.0~50.0%.
- 3. the method according to claim 1 for preparing carboxymethyl cellulose with high degree sodium, it is characterised in that：In step b, The cellulosic material is any one in purified cotton, wood pulp or bamboo pulp.
- 4. the method according to claim 1 for preparing carboxymethyl cellulose with high degree sodium, it is characterised in that：In step c, The etherifying agent using the monoxone of mass fraction >=97.5% as solute, 90~95% alcohol of volumetric concentration be solvent prepare and Into.
- 5. the method according to claim 1 for preparing carboxymethyl cellulose with high degree sodium, it is characterised in that：In step d, The etherifying agent using the monoxone of mass fraction >=97.5% as solute, 90~95% alcohol of volumetric concentration be solvent prepare and Into.
- 6. the method according to claim 1 for preparing carboxymethyl cellulose with high degree sodium, it is characterised in that：In step g, The alcohol by volume a concentration of 75~85% that the washing uses.
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| CN106496335A (en) * | 2016-11-24 | 2017-03-15 | 泸州北方化学工业有限公司 | A kind of method for preparing carboxymethyl cellulose lithium |
| CN109988244B (en) * | 2017-12-29 | 2022-09-20 | 上海长光企业发展有限公司 | Sodium carboxymethylcellulose and preparation method and application thereof |
| CN114957492A (en) * | 2021-12-28 | 2022-08-30 | 常熟威怡科技有限公司 | Preparation method of low-insoluble substance fast-dispersing carboxymethyl cellulose ether |
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| JPS6037121B2 (en) * | 1982-10-04 | 1985-08-24 | ダイセル化学工業株式会社 | Carboxymethylcellulose sodium salt |
| CN101240035B (en) * | 2008-03-14 | 2010-05-12 | 山东一滕化工有限公司 | Ultra-high substitution carboxymethyl cellulose sodium and its preparation method and application |
| CN102286108B (en) * | 2011-07-12 | 2012-11-28 | 重庆力宏精细化工有限公司 | Method for preparing potassium carboxymethylcellulose |
| CN103554273B (en) * | 2013-10-31 | 2016-06-08 | 泸州北方化学工业有限公司 | The production method of technology level sodium carboxymethylcellulose |
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Effective date of registration: 20210702 Address after: 646003 Gaoba Luzhou North cellulose Co., Ltd., Longmatan District, Luzhou City, Sichuan Province Patentee after: LUZHOU BEIFANG CELLULOSE Co.,Ltd. Address before: 646003 Sichuan Luzhou high dam Luzhou North Chemical Industry Co., Ltd. Patentee before: LUZHOU NORTH CHEMICAL INDUSTRY Co.,Ltd. |