CN105330752A - Method for preparing sodium carboxymethyl cellulose with high degree of substitution - Google Patents
Method for preparing sodium carboxymethyl cellulose with high degree of substitution Download PDFInfo
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- C08B11/04—Alkyl or cycloalkyl ethers with substituted hydrocarbon radicals
- C08B11/10—Alkyl or cycloalkyl ethers with substituted hydrocarbon radicals substituted with acid radicals
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Abstract
The invention belongs to the field of chemical industry, in particular relates to a method for preparing sodium carboxymethyl cellulose with a high degree of substitution, and aims to solve the technical problem about provision of the method for preparing the sodium carboxymethyl cellulose with the high degree of substitution. The method comprises the following steps: a, preparing ethyl alcohol and an aqueous solution of sodium hydroxide into a mixed solution; b, mixing the mixed solution of the step a, cellulose serving as a raw material, and solid sodium hydroxide uniformly to perform an alkalization reaction; c, adding an etherifying agent into the material which is obtained after the reaction of the step b to perform an etherifying reaction; d, adding the etherifying agent into the material after the reaction of the step c to perform the etherifying reaction again; e, preparing the ethyl alcohol and the aqueous solution of the sodium hydroxide into the mixed solution; f, mixing the mixed solution of the step e and the material after the reaction of the step d uniformly to perform the alkalization reaction again; g, performing post-processing. By the method, the sodium carboxymethyl cellulose with the high degree of substitution of over 1.35 can be prepared.
Description
Technical field
The invention belongs to chemical field, be specifically related to a kind of method preparing carboxymethyl cellulose with high degree sodium.
Background technology
Xylo-Mucine is a kind of important ether of cellulose, is the polyanionic compound of a kind of good water solubility that natural fiber obtains after chemical modification, is soluble in cold and hot water.It has on emulsifying dispersant, solid dispersal, not easily corrupt, physiology harmless etc. unusual with extremely valuable comprehensive physical, chemical property, is a kind of broad-spectrum modified natural polymer.The leading indicator weighing Xylo-Mucine quality is substitution value (DS) and viscosity, and the character of the different then Xylo-Mucine of substitution value is also different; In general substitution value is larger, and the stability of solution is also better.
Summary of the invention
Goal of the invention of the present invention is to provide a kind of method preparing the Xylo-Mucine of high substitution value.The substitution value of the Xylo-Mucine that the method can prepare reaches more than 1.35.
Technical problem to be solved by this invention is to provide a kind of method preparing the Xylo-Mucine of high substitution value.The method comprises the following steps:
A, preparation mixed solution: by 220 ~ 270 parts of alcohol and 95 ~ 125 parts of aqueous sodium hydroxide solution mixings, controlling mixeding liquid temperature is 20 ~ 45 DEG C, obtains mixed solution;
B, alkalization: control the temperature of reaction unit lower than 40 DEG C, add in reaction unit 40 ~ 60 parts of cellulosic materials, 45 ~ 65 parts of solid sodium hydroxides, step a mixed solution carry out quaternization; Reinforced to start to alkalization finishing control temperature be 20 ~ 50 DEG C, and the reinforced time starting to terminate to alkalization is 50 ~ 80min;
C, etherificate: the etherifying agent of 65 ~ 90 parts is joined step b reaction terminate after material in carry out etherification reaction; Reinforced to start to etherificate finishing control temperature be 35 ~ 60 DEG C, and the reinforced time starting to terminate to etherificate is 20 ~ 40min; Described etherifying agent is the Mono Chloro Acetic Acid spirituous solution of concentration 73.0 ~ 75.0% (w/w);
D, again etherificate: 25 ~ 40 portions of etherifying agents are joined step c reaction terminate after material in again carry out etherification reaction; Reinforced to start to etherificate finishing control temperature be 35 ~ 60 DEG C, and the reinforced time starting to terminate to etherificate is 10 ~ 25min; Described etherifying agent is the Mono Chloro Acetic Acid spirituous solution of concentration 73.0 ~ 75.0% (w/w);
E, again prepare mixed solution: by 85 ~ 110 parts of alcohol and 35 ~ 60 parts of aqueous sodium hydroxide solutions mixings, control temperature is 20 ~ 45 DEG C, obtains mixed solution;
F, again to alkalize: the mixed solution of step e, 15 ~ 25 parts of solid sodium hydroxides are joined steps d reaction terminate after material in again carry out quaternization; Before reinforced end, control temperature is 40 ~ 60 DEG C; After reinforced end, control temperature is 50 ~ 60 DEG C of stirring 5 ~ 10min; Constant temperature 30 ~ 40min at being warming up to 75 ~ 80 DEG C again; Be cooled to less than 50 DEG C again;
Material after g, neutralization, washing step f reaction terminate, carries out the Xylo-Mucine drying, pulverize, pack and obtain high substitution value after solid-liquid separation;
Above-mentioned number represents the molar weight of each raw material; If this raw material is solution, number then represents the molar weight of its solute.
Preferably, in the method steps a of above-mentioned preparation carboxymethyl cellulose with high degree sodium, the concentration of described alcohol is 90 ~ 95% (v/v); The concentration of described aqueous sodium hydroxide solution is 48.0 ~ 50.0% (w/w).
Preferably, in the method steps b of above-mentioned preparation carboxymethyl cellulose with high degree sodium, described cellulosic material is any one in purified cotton, wood pulp or bamboo pulp.
Preferably, in the method steps b of above-mentioned preparation carboxymethyl cellulose with high degree sodium, described reinforced start to the reinforced end time be 8 ~ 12min.
Preferably, in the method steps c of above-mentioned preparation carboxymethyl cellulose with high degree sodium, described etherifying agent with massfraction >=97.5% Mono Chloro Acetic Acid be solute, 90 ~ 95% (v/v) alcohol is that solvent is formulated.
Preferably, in the method steps c of above-mentioned preparation carboxymethyl cellulose with high degree sodium, described reinforced start to the reinforced end time be 15 ~ 25min.
Preferably, in the method steps d of above-mentioned preparation carboxymethyl cellulose with high degree sodium, described etherifying agent with massfraction >=97.5% Mono Chloro Acetic Acid be solute, 90 ~ 95% (v/v) alcohol is that solvent is formulated.
Preferably, in the method steps d of above-mentioned preparation carboxymethyl cellulose with high degree sodium, described reinforced start to the reinforced end time be 5 ~ 15min.
Preferably, in the method steps e of above-mentioned preparation carboxymethyl cellulose with high degree sodium, the concentration of described alcohol is 90 ~ 95% (v/v); The concentration of described aqueous sodium hydroxide solution is 48.0 ~ 50.0% (w/w).
Preferably, in the method steps f of above-mentioned preparation carboxymethyl cellulose with high degree sodium, described reinforced start to the reinforced end time be 5 ~ 15min.
Preferably, in the method steps g of above-mentioned preparation carboxymethyl cellulose with high degree sodium, the ethanol concn that described washing adopts is 75 ~ 85 (v/v) %.
The inventive method is by controlling suitable feeding quantity, feed time, reaction times, and twice etherificate and twice alkalization have prepared substitution value up to the Xylo-Mucine of more than 1.35, thus provide a more efficiently method for the preparation of high substituted carboxymethyl sodium cellulosate.
Embodiment
Prepare a method for the Xylo-Mucine of high substitution value, comprise the following steps:
A, preparation mixed solution: 95 ~ 125 parts of aqueous sodium hydroxide solutions mixings that to be 90 ~ 95% (v/v) 220 ~ 270 parts of alcohol and concentration by concentration be 48.0 ~ 50.0% (w/w), controlling mixeding liquid temperature is 20 ~ 45 DEG C, obtains mixed solution;
B, alkalization: control the temperature of reaction unit lower than 40 DEG C, add in reaction unit in 8 ~ 12min 40 ~ 60 parts of cellulosic materials, 45 ~ 65 parts of solid sodium hydroxides, step a mixed solution carry out quaternization; Reinforced to start to alkalization finishing control temperature be 20 ~ 50 DEG C, and the reinforced time starting to terminate to alkalization is 50 ~ 80min;
C, etherificate: the etherifying agent of 65 ~ 90 parts is joined in 15 ~ 25min step b reaction terminate after material in carry out etherification reaction; Reinforced to start to etherificate finishing control temperature be 35 ~ 60 DEG C, and the reinforced time starting to terminate to etherificate is 20 ~ 40min; Described etherifying agent with massfraction >=97.5% Mono Chloro Acetic Acid be solute, the Mono Chloro Acetic Acid spirituous solution of 90 ~ 95% (v/v) alcohol to be the formulated concentration of solvent be 73.0 ~ 75.0% (w/w);
D, again etherificate: 25 ~ 40 portions of etherifying agents are joined in 5 ~ 15min step c reaction terminate after material in again carry out etherification reaction; Reinforced to start to etherificate finishing control temperature be 35 ~ 60 DEG C, and the reinforced time starting to terminate to etherificate is 10 ~ 25min; Described etherifying agent with massfraction >=97.5% Mono Chloro Acetic Acid be solute, the Mono Chloro Acetic Acid spirituous solution of 90 ~ 95% (v/v) alcohol to be the formulated concentration of solvent be 73.0 ~ 75.0% (w/w);
E, again prepare mixed solution: be 90 ~ 95% (v/v) 85 ~ 110 parts of alcohol and concentration by concentration be 48.0 ~ 50.0% (w/w) 35 ~ 60 parts of aqueous sodium hydroxide solutions mixings, control temperature is 20 ~ 45 DEG C, obtains mixed solution;
F, again to alkalize: the mixed solution of step e, 15 ~ 25 parts of solid sodium hydroxides are joined in 5 ~ 15min steps d reaction terminate after material in again carry out quaternization; Before reinforced end, control temperature is 40 ~ 60 DEG C; After reinforced end, control temperature is 50 ~ 60 DEG C of stirring 5 ~ 10min; Constant temperature 30 ~ 40min at being warming up to 75 ~ 80 DEG C again; Be cooled to less than 50 DEG C again;
Material after g, neutralization, washing step f reaction terminate, carries out the Xylo-Mucine drying, pulverize, pack and obtain high substitution value after solid-liquid separation;
Above-mentioned number represents the molar weight of each raw material; If this raw material is solution, number then represents the molar weight of its solute.
Such as: 1) when raw material is solution, as part aqueous sodium hydroxide solution of 95 ~ 125 in step a, expression purity is the molar weight of the sodium hydrate solid of 100% is 95 ~ 125 parts, if the solid sodium hydroxide purity adopted is not 100%, take again after so converting with regard to needs, then join in corresponding water, be mixed with the aqueous sodium hydroxide solution of respective concentration;
2) when raw material is solid, as part solid sodium hydroxide of 45 ~ 65 in step b, represent purity be 100% sodium hydroxide molar weight be 45 ~ 65 parts, if the solid sodium hydroxide purity adopted is not 100%, take again after so converting with regard to needs.
The substitution value of the Xylo-Mucine that the inventive method prepares detects according to the methods analyst of GB1904-2005 to obtain.
Embodiment 1
(1), preparation mixed solution: be 90% (v/v) alcohol and 112 parts of concentration by 227 parts of concentration be that 48.0% (w/w) liquid caustic soda mix and blend obtains mixed solution, controlling mixeding liquid temperature is 45 DEG C;
(2), alkalize: control to mediate built-in temperature and be less than 40 DEG C, in 10min, the wood pulp cellulose starting material of 55 parts are evenly added in kneader, in the process of feeding intake, divide and add 60 parts of sheet alkali for 3 times, prepared for step (1) mixed solution is joined in kneader by shower simultaneously, mixed solution joining day 12min, the quaternization time (comprising charging time) is 50min, controls quaternization temperature 30 DEG C ~ 50 DEG C;
(3), preparation etherifying agent: with the Mono Chloro Acetic Acid of massfraction >=97.5% for solute, the etherifying agent of 90% (v/v) alcohol to be solvent compound concentration be 74.0% (w/w);
(4), etherificate: the etherifying agent of 70 parts of steps (3) is joined step (2) by shower and reacts in the material after terminating, joining day 20min, stirs 10min afterwards, and temperature controls at 40 DEG C ~ 60 DEG C;
(5), etherificate again: be that the Mono Chloro Acetic Acid spirituous solution of 74.0% (w/w) joins in step (4) reacted material by shower by 28 parts of concentration, joining day 10min, then 5min is stirred, temperature controls at 40 DEG C ~ 60 DEG C, slowly heat up through 10min again, to 58 DEG C ~ 60 DEG C constant temperature 20min;
(6), preparation mixed solution: be 90% (v/v) alcohol and 54 parts of concentration by 89 parts of concentration be that 48.0% (w/w) liquid caustic soda is uniformly mixed to obtain mixed solution, controlling mixeding liquid temperature is 35 DEG C ~ 45 DEG C;
(7), again alkalize: the mixed solution of step (6) is added in the material of step (5) by shower, joining day 10min, add 25 parts of sheet alkali for 2 times with the time-division; After stirring 10min, then pass slowly 10min intensification, to 75 DEG C ~ 78 DEG C constant temperature 35min, be cooled to less than 50 DEG C and enter washing kettle;
(8) wash: first time washing: get the alcohol that 1800 parts of concentration are 80% (v/v) in washing kettle ready, step (7) material is put into washing kettle, add sodium hypochlorite solution 1 part, to stir and interval at least adds hydrochloric acid after 10min regulates pH value, hydrochloric acid dosage 9 parts, then stir about 10min, start centrifugal; Second time washing: get the alcohol that 1800 parts of concentration are 80% (v/v) in washing kettle ready, the material after once washing is centrifugal enters in washing kettle, stir start after at least 20 minutes centrifugal.
(9), to dry and last handling process: step (8) centrifugal complete after product through drying, pulverize, pack to obtain carboxymethyl cellulose with high degree sodium.
The methods analyst that embodiment 1 and 7 batch same period all requires according to GB1904-2005 with all achievement datas of explained hereafter product draws, as shown in table 1:
Table 1
| Lot number | Viscosity (mpa.s) | PH | Substitution value | 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: be 90% (v/v) alcohol and 166 parts of concentration by 300 parts of concentration be that 48.0% (w/w) liquid caustic soda mix and blend obtains mixed solution, controlling mixeding liquid temperature is 45 DEG C;
(2), first time alkalization: control to mediate built-in temperature and control at 40 DEG C, in 10min, the wood pulp cellulose starting material of 55 parts are evenly added in kneader, in the process of feeding intake, divide and add 85 parts of sheet alkali for 5 times, prepared for step (1) mixed solution is joined in kneader by shower simultaneously, mixed solution joining day 12min, the quaternization time (comprising charging time) is 50min, controls quaternization temperature 30 DEG C ~ 55 DEG C;
(3), etherifying agent preparation: with the Mono Chloro Acetic Acid of massfraction >=97.5% for solute, 90% (v/v) alcohol is the etherificate of solvent preparation 74.0% (w/w);
(4), first time etherificate: by first time alkalization terminate after material add by shower the Mono Chloro Acetic Acid spirituous solution 70 parts that concentration is 74.0% (w/w), joining day 20min, stirs 10min afterwards, and temperature controls at 40 DEG C ~ 60 DEG C;
(5), second time etherificate: the material after first time etherification reaction is added by shower the Mono Chloro Acetic Acid spirituous solution 28 parts that concentration is 74.0% (w/w), joining day 10min, then 5min is stirred, temperature controls at 40 DEG C ~ 60 DEG C, pass slowly 15min again to heat up, to 75 DEG C-78 DEG C constant temperature 35min, after be cooled to less than 50 DEG C and enter washing kettle;
(6) first time washing: get the alcohol that 1800 parts of concentration are 70% (v/v) in washing kettle ready, step (7) material is put into washing kettle, add sodium hypochlorite solution 1 part, to stir and interval at least adds hydrochloric acid after 10min regulates pH value, hydrochloric acid dosage≤10 part, then stir about 10min, start centrifugal; Second time washing: get the alcohol that 1800 parts of concentration are 70% (v/v) in washing kettle ready, one washing centrifugal after material enter in washing kettle, stir start after at least 20 minutes centrifugal.
(7), to dry and last handling process: step (6) centrifugal complete after product through drying, pulverize, pack to obtain carboxymethyl cellulose with high degree sodium.
The methods analyst that comparative example 1 and 7 batch same period all requires according to GB1904-2005 with all achievement datas of explained hereafter product draws, as shown in table 2:
Table 2
| Lot number | Viscosity (mpa.s) | PH | Substitution value | 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 |
As can be seen from table 1,2 contrasts, the substitution value of the Xylo-Mucine that the inventive method prepares prepares apparently higher than ordinary method, also meet the requirement of standard simultaneously, describe the Xylo-Mucine that the inventive method can prepare high substitution value effectively.
Claims (10)
1. prepare a method for carboxymethyl cellulose with high degree sodium, it is characterized in that: comprise the following steps:
A, preparation mixed solution: by 220 ~ 270 parts of alcohol and 95 ~ 125 parts of aqueous sodium hydroxide solution mixings, controlling mixeding liquid temperature is 20 ~ 45 DEG C, obtains mixed solution;
B, alkalization: control the temperature of reaction unit lower than 40 DEG C, add in reaction unit 40 ~ 60 parts of cellulosic materials, 45 ~ 65 parts of solid sodium hydroxides, step a mixed solution carry out quaternization; Reinforced to start to alkalization finishing control temperature be 20 ~ 50 DEG C, and the reinforced time starting to terminate to alkalization is 50 ~ 80min;
C, etherificate: the etherifying agent of 65 ~ 90 parts is joined step b reaction terminate after material in carry out etherification reaction; Reinforced to start to etherificate finishing control temperature be 35 ~ 60 DEG C, and the reinforced time starting to terminate to etherificate is 20 ~ 40min; Described etherifying agent is the Mono Chloro Acetic Acid spirituous solution of concentration 73.0 ~ 75.0% (w/w);
D, again etherificate: 25 ~ 40 portions of etherifying agents are joined step c reaction terminate after material in again carry out etherification reaction; Reinforced to start to etherificate finishing control temperature be 35 ~ 60 DEG C, and the reinforced time starting to terminate to etherificate is 10 ~ 25min; Described etherifying agent is the Mono Chloro Acetic Acid spirituous solution of concentration 73.0 ~ 75.0% (w/w);
E, again prepare mixed solution: by 85 ~ 110 parts of alcohol and 35 ~ 60 parts of aqueous sodium hydroxide solutions mixings, control temperature is 20 ~ 45 DEG C, obtains mixed solution;
F, again to alkalize: the mixed solution of step e, 15 ~ 25 parts of sodium hydroxide are joined steps d reaction terminate after material in again carry out quaternization; Before reinforced end, control temperature is 40 ~ 60 DEG C; After reinforced end, control temperature is 50 ~ 60 DEG C of stirring 5 ~ 10min; Constant temperature 30 ~ 40min at being warming up to 75 ~ 80 DEG C again; Be cooled to less than 50 DEG C again;
Material after g, neutralization, washing step f reaction terminate, carries out the Xylo-Mucine drying, pulverize, pack and obtain high substitution value after solid-liquid separation;
Above-mentioned number represents the molar weight of each raw material; If this raw material is solution, number then represents the molar weight of its solute.
2. the method preparing carboxymethyl cellulose with high degree sodium according to claim 1, is characterized in that: in step a or d, and the concentration of described alcohol is 90 ~ 95% (v/v); The concentration of described aqueous sodium hydroxide solution is 48.0 ~ 50.0% (w/w).
3. the method preparing carboxymethyl cellulose with high degree sodium according to claim 1, is characterized in that: in step b, and described cellulosic material is any one in purified cotton, wood pulp or bamboo pulp.
4. the method preparing carboxymethyl cellulose with high degree sodium according to claim 1, is characterized in that: in step b, described reinforced start to the reinforced end time be 8 ~ 12min.
5. the method preparing carboxymethyl cellulose with high degree sodium according to claim 1, it is characterized in that: in step c, described etherifying agent with massfraction >=97.5% Mono Chloro Acetic Acid be solute, 90 ~ 95% (v/v) alcohol is that solvent is formulated.
6. the method preparing carboxymethyl cellulose with high degree sodium according to claim 1, is characterized in that: in step c, described reinforced start to the reinforced end time be 15 ~ 25min.
7. the method preparing carboxymethyl cellulose with high degree sodium according to claim 1, is characterized in that: in steps d, described reinforced start to the reinforced end time be 5 ~ 15min.
8. the method preparing carboxymethyl cellulose with high degree sodium according to claim 1, it is characterized in that: in steps d, described etherifying agent with massfraction >=97.5% Mono Chloro Acetic Acid be solute, 90 ~ 95% (v/v) alcohol is that solvent is formulated.
9. the method preparing carboxymethyl cellulose with high degree sodium according to claim 1, is characterized in that: in step f, described reinforced start to the reinforced end time be 5 ~ 15min.
10. the method preparing carboxymethyl cellulose with high degree sodium according to claim 1, is characterized in that: in step g, and the ethanol concn that described washing adopts is 75 ~ 85% (v/v).
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN109988244A (en) * | 2017-12-29 | 2019-07-09 | 上海长光企业发展有限公司 | A kind of sodium carboxymethylcellulose and its preparation method and application |
| 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 |
| CN116462774A (en) * | 2023-05-06 | 2023-07-21 | 绿能纤材(重庆)科技有限公司 | Preparation method of lithium battery grade carboxymethyl cellulose potassium |
| CN116478305A (en) * | 2023-04-19 | 2023-07-25 | 绿能纤材(重庆)科技有限公司 | Synthetic preparation method of high-purity lithium battery-grade sodium carboxymethyl cellulose |
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| CN101240035A (en) * | 2008-03-14 | 2008-08-13 | 山东一滕化工有限公司 | Ultra-high substitution carboxymethyl cellulose sodium and its preparation method and application |
| CN102286108A (en) * | 2011-07-12 | 2011-12-21 | 重庆力宏精细化工有限公司 | Method for preparing potassium carboxymethylcellulose |
| 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 |
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| EP0106228A1 (en) * | 1982-10-04 | 1984-04-25 | Daicel Chemical Industries, Ltd. | Sodium carboxymethylcellulose |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN109988244A (en) * | 2017-12-29 | 2019-07-09 | 上海长光企业发展有限公司 | A kind of sodium carboxymethylcellulose and its preparation method and application |
| 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 |
| CN116478305A (en) * | 2023-04-19 | 2023-07-25 | 绿能纤材(重庆)科技有限公司 | Synthetic preparation method of high-purity lithium battery-grade sodium carboxymethyl cellulose |
| CN116462774A (en) * | 2023-05-06 | 2023-07-21 | 绿能纤材(重庆)科技有限公司 | Preparation method of lithium battery grade carboxymethyl cellulose potassium |
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