CN101440132A - Preparation of technology level sodium carboxymethylcellulose - Google Patents
Preparation of technology level sodium carboxymethylcellulose Download PDFInfo
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- CN101440132A CN101440132A CNA2008101772174A CN200810177217A CN101440132A CN 101440132 A CN101440132 A CN 101440132A CN A2008101772174 A CNA2008101772174 A CN A2008101772174A CN 200810177217 A CN200810177217 A CN 200810177217A CN 101440132 A CN101440132 A CN 101440132A
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Abstract
The invention discloses a method for preparing a technical grade sodium carboxymethyl cellulose with higher purity and not producing exhaust affecting the environment during production, which comprises the following steps: 1) pre-mixing a certain amount of sodium hydroxide water solution with ethanol water proportionately, cooling the mixed liquid to the indoor temperature, and loosening refined cotton into flocs; 2) adding the refined cotton and the mixed liquid into a kneader in sequence for quaternization, wherein the time of adding cotton is controlled to be 5 to 20 minutes and the time of adding the mixed liquid is controlled to be 10 to 30 minutes; 3) performing etherification reaction after the quaternization, wherein time of adding etherifying agent is controlled to be about 30 to 60 minutes and the temperature is controlled between 20 and 40 DEG C; and then heating for reclaiming alcohol and continuing heating to between 75 and 80 DEG C for etherification reaction for 40 to 80 minutes; and 4) after the completion of etherification reaction, adjusting the PH value of material between 7.0 and 8.5, drying, crushing and screening so as to obtain the technical grade sodium carboxymethyl cellulose product.
Description
Technical field
The invention discloses a kind of preparation method of technology level sodium carboxymethylcellulose.
Background technology
Carboxymethyl cellulose obtains natural cellulose through chemical modification, be one of industrial most important water-soluble polymers, develops rapidly at present.Carboxymethyl cellulose is the most representative ionic ether of cellulose, and normally used is its sodium salt.Xylo-Mucine (be called for short Na-CMC) be natural cellulose (being raw material with velveteen or wood pulp usually) under alkaline condition with Mono Chloro Acetic Acid generation etherification reaction, different by the situation that carboxymethyl replaced according to the raw material specification difference with the hydroxyl hydrogen in the Mierocrystalline cellulose D-glucose unit, the water-soluble high-molecular compound that different degree of substitution that obtains and different molecular weight distribute.Xylo-Mucine has the advantageous property of many uniquenesses, is widely used in industrial production such as building, cement, oil, food, weaving, washing composition, coating, medicine, papermaking and electronic devices and components.
The hydrophily method is to produce a kind of common technology of Na-CMC, and its production process is that soda cellulose and etherifying agent are reacted under the condition of free alkali and water.Do not exist organic solvent such as alcohol to make reaction medium in alkalization and the etherification procedure; hydrophily method equipment is relatively simple, less investment, cost are low; in mainly producing, low-grade technology level sodium carboxymethylcellulose; but the product purity that the hydrophily method obtains is lower; usually also to pass through treating process; just can be used for fields such as washing composition, textile sizing, binding agent, mosquito-repellent incense and petroleum industry, cause the production cost height, energy consumption is bigger.The solvent method is to produce the another kind of common technology of Na-CMC, and it is to do to alkalize and etherification reaction under reaction medium (thinner) condition at organic solvent.The product purity that the solvent method obtains is higher relatively, and the discharge of environment causes environmental pollution but this processing method can exert an influence.
Summary of the invention
Technical problem to be solved by this invention is: will provide that a kind of product purity is higher, the preparation method of the technology level sodium carboxymethylcellulose of the discharge of the environment that do not exert an influence in the production process.
For addressing the above problem, the technical solution used in the present invention is: the preparation method of described technology level sodium carboxymethylcellulose comprises the steps:
1. be weight concentration that 40～50% aqueous sodium hydroxide solution is 70～98% aqueous ethanolic solution with weight concentration by weight 1: 0.5～3 mixed in advance, the mixed solution that obtains is cooled to room temperature, again the purified cotton shredding is become cotton-shaped, the mol ratio of purified cotton and sodium hydroxide is controlled at 1: 2.2～6.0, and the amount of aqueous ethanolic solution is 1～10 times of purified cotton;
2. in order purified cotton and mixed solution are joined in the kneader and alkalize, throwing the cotton time was controlled at 5-20 minute, was controlled at 10-30 minute with the mixed solution time, fed intake to close the kneader dog-house after finishing, alkalization temperature is controlled between 20～30 ℃, and the reaction times is 30～60 minutes;
3. alkalization is carried out etherification reaction after finishing, and the mol ratio of purified cotton and etherifying agent is controlled at 1: 1.0～2.8; During adding etherifying agent, the time was controlled at 30～60 minutes, and temperature is controlled between 20～40 ℃; Begin after etherifying agent adds to heat up, after temperature is raised to 70 ℃, reduce quantity of steam, allow it be warming up to 75～80 ℃ naturally, high temperature etherification reaction 40～80 minutes; Heat up again subsequently and carry out the alcohol recovery, after temperature rises to more than 84 ℃, can cool off, finish etherification reaction;
4. after etherification reaction finished, the pH value of adjusting material drying, was pulverized and is sieved between 7.0-8.5, obtains the technology level sodium carboxymethylcellulose product.
Etherifying agent recited above is chloroacetic spirituous solution, and wherein chloroacetic weight accounts for 50～80%.
The invention has the beneficial effects as follows: use above-mentioned method have that product performance are stable, technology simple,, advantages such as convenient solvent reclaiming.The product purity that obtains does not need treating process between 70-75%, saved cost, consumes lowly, and does not produce the discharge of environmental pollution, has optimized environmental health.Raw material sources can be selected other purified cotton of difference level or towel suede for use in addition, can utilization of waste material, belong to a kind of renewable resource.When using method for preparing mosquito-repellent incense material, than saving 20-30% with the hydrophily method through the cost of the refining product that obtains, economic benefit is considerable.
Embodiment
The invention will be further described below in conjunction with specific embodiment.The umber of each raw material and ratio are all by weight among the embodiment.
Embodiment 1:
In advance 2.5 parts of 48.0% aqueous sodium hydroxide solutions with 3.0 parts of mixing of aqueous ethanolic solution of 92.5%, mixed solution is cooled to room temperature, again 1 part of purified cotton shredding is become cotton-shaped, in order purified cotton and mixed solution are joined in the kneader and alkalize, throwing the cotton time was controlled at 5-20 minute, was controlled at 10-30 minute with the mixed solution time, fed intake to close the kneader dog-house after finishing, alkalization temperature is controlled between 20-30 ℃, and the reaction times is 30-60 minute.Alkalization is carried out etherification reaction after finishing, 1.3 parts of the Mono Chloro Acetic Acid spirituous solutions of etherifying agent employing 50-80%, and during adding etherifying agent, the time was controlled at 30-60 minute, and temperature is controlled between 20-40 ℃, the not overtemperature of trying one's best.Begin after etherifying agent adds to heat up, after temperature is raised to 70 ℃, reduce quantity of steam, allow it be warming up to 75～80 ℃ naturally, high temperature etherification reaction 40～80 minutes; Heat up again subsequently and carry out the alcohol recovery, after temperature rises to more than 84 ℃, can cool off, finish etherification reaction;
Insulation finishes, and adjusts the pH value of material, and the PH of control material is 7.0---and 8.5, drying and pulverizing, sieve, obtain the technology level sodium carboxymethylcellulose product, NShi viscosity 990, substitution value 0.789 purity 73.46%.
Embodiment 2:
In advance 2.6 parts of 47.5% aqueous sodium hydroxide solutions with 3.2 parts of mixing of aqueous ethanolic solution of 92.0%, mixed solution is cooled to room temperature, again 1 part of purified cotton shredding is become cotton-shaped, in order purified cotton and mixed solution are joined in the kneader and alkalize, throwing the cotton time was controlled at 5-20 minute, was controlled at 10-30 minute with the mixed solution time, fed intake to close the kneader dog-house after finishing, alkalization temperature is controlled between 20-30 ℃, and the reaction times is 30-60 minute.Alkalization is carried out etherification reaction after finishing, 1.28 parts of the Mono Chloro Acetic Acid spirituous solutions of etherifying agent employing 50-80%, and during adding etherifying agent, the time was controlled at 30-60 minute, and temperature is controlled between 20-40 ℃, the not overtemperature of trying one's best.Begin after etherifying agent adds to heat up, after temperature is raised to 70 ℃, reduce quantity of steam, allow it be warming up to 75～80 ℃ naturally, high temperature etherification reaction 40～80 minutes; Heat up again subsequently and carry out the alcohol recovery, after temperature rises to more than 84 ℃, can cool off, finish etherification reaction;
Insulation finishes, and adjusts the pH value of material, and the PH of control material is 7.0-8.5, drying and pulverizing, sieves, and obtains the technology level sodium carboxymethylcellulose product, NShi viscosity 1030, substitution value 0.802 purity 72.16%.
Embodiment 3:
In advance 2.4 parts of 47.5% aqueous sodium hydroxide solutions with 2.8 parts of mixing of aqueous ethanolic solution of 93.0%, mixed solution is cooled to room temperature, again 1 part of purified cotton shredding is become cotton-shaped, in order purified cotton and mixed solution are joined in the kneader and alkalize, throwing the cotton time was controlled at 5-20 minute, was controlled at 10-30 minute with the mixed solution time, fed intake to close the kneader dog-house after finishing, alkalization temperature is controlled between 20-30 ℃, and the reaction times is 30-60 minute.Alkalization is carried out etherification reaction after finishing, 1.32 parts of the Mono Chloro Acetic Acid spirituous solutions of etherifying agent employing 50-80%, and during adding etherifying agent, the time was controlled at 30-60 minute, and temperature is controlled between 20-40 ℃, the not overtemperature of trying one's best.Begin after etherifying agent adds to heat up, after temperature is raised to 70 ℃, reduce quantity of steam, allow it be warming up to 75～80 ℃ naturally, high temperature etherification reaction 40～80 minutes; Heat up again subsequently and carry out the alcohol recovery, after temperature rises to more than 84 ℃, can cool off, finish etherification reaction;
Insulation finishes, and adjusts the pH value of material, and the PH of control material is 7.0-8.5, drying and pulverizing, sieves, and obtains the technology level sodium carboxymethylcellulose product, NShi viscosity 996, substitution value 0.812 purity 71.98%.
Claims (2)
1, the preparation method of technology level sodium carboxymethylcellulose comprises the steps:
1. be weight concentration that 40～50% aqueous sodium hydroxide solution is 70～98% aqueous ethanolic solution with weight concentration by weight 1: 0.5～3 mixed in advance, the mixed solution that obtains is cooled to room temperature, again the purified cotton shredding is become cotton-shaped, the mol ratio of purified cotton and sodium hydroxide is controlled at 1: 2.2～6.0, and the amount of aqueous ethanolic solution is 1～10 times of purified cotton;
2. in order purified cotton and mixed solution are joined in the kneader and alkalize, throwing the cotton time was controlled at 5-20 minute, was controlled at 10-30 minute with the mixed solution time, fed intake to close the kneader dog-house after finishing, alkalization temperature is controlled between 20～30 ℃, and the reaction times is 30～60 minutes;
3. alkalization is carried out etherification reaction after finishing, and the mol ratio of purified cotton and etherifying agent is controlled at 1: 1.0～2.8; During adding etherifying agent, the time was controlled at 30～60 minutes, and temperature is controlled between 20～40 ℃; Begin after etherifying agent adds to heat up, after temperature is raised to 70 ℃, reduce quantity of steam, allow it be warming up to 75～80 ℃ naturally, high temperature etherification reaction 40～80 minutes; Heat up again subsequently and carry out the alcohol recovery, after temperature rises to more than 84 ℃, can cool off, finish etherification reaction;
4. after etherification reaction finished, the pH value of adjusting material drying, was pulverized and is sieved between 7.0-8.5, obtains the technology level sodium carboxymethylcellulose product.
2, preparation method according to claim 1 is characterized in that: described etherifying agent is chloroacetic spirituous solution, and wherein chloroacetic weight accounts for 50～80%.
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| Application Number | Priority Date | Filing Date | Title |
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| CNA2008101772174A CN101440132A (en) | 2008-12-09 | 2008-12-09 | Preparation of technology level sodium carboxymethylcellulose |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101830991A (en) * | 2010-06-04 | 2010-09-15 | 淄博联技化工有限公司 | Rapid production technology for carboxymethyl cellulose by aqueous medium process |
| 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 |
| CN111187355A (en) * | 2018-11-14 | 2020-05-22 | 河南正弘药用辅料股份有限公司 | Production method of sodium carboxymethylcellulose |
-
2008
- 2008-12-09 CN CNA2008101772174A patent/CN101440132A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101830991A (en) * | 2010-06-04 | 2010-09-15 | 淄博联技化工有限公司 | Rapid production technology for carboxymethyl cellulose by aqueous medium process |
| 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 |
| CN111187355A (en) * | 2018-11-14 | 2020-05-22 | 河南正弘药用辅料股份有限公司 | Production method of sodium carboxymethylcellulose |
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Open date: 20090527 |