CN104761646A - Preparation method of sodium carboxymethylcellulose with long shelf life - Google Patents
Preparation method of sodium carboxymethylcellulose with long shelf life Download PDFInfo
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- CN104761646A CN104761646A CN201510152113.8A CN201510152113A CN104761646A CN 104761646 A CN104761646 A CN 104761646A CN 201510152113 A CN201510152113 A CN 201510152113A CN 104761646 A CN104761646 A CN 104761646A
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Abstract
The invention discloses a preparation method of sodium carboxymethylcellulose with a long shelf life. The preparation method comprises the following steps: alkalifying: alkalifying under nitrogen protection; etherifying: carrying out etherifying reaction for 45-55 minutes in an etherifying device, wherein the temperature is maintained at 75-80 DEG C; washing: transferring the etherified materials into a washing device, washing the materials twice by using an alcohol solution and adding bleaching liquid for bleaching; harrowing and drying: transferring the washed materials into a harrowing and drying device for harrowing and drying; and drying and crushing: controlling the temperature at 60-65 DEG C and drying and crushing the harrowed and dried materials. The product prepared by the invention is long in shelf life in an aqueous solution, viscosity reduction is hardly caused as a result of storage, and the sodium carboxymethylcellulose has the advantages of being simple in process, convenient to use, low in production cost, good in product quality, long in shelf life and the like.
Description
Technical field
The present invention relates to the preparing technical field of macromolecular compound, be specifically related to a kind of preparation method of long quality guaranteed period Xylo-Mucine.
Background technology
Xylo-Mucine (sodium carboxymethylcellulose, CMC), is cellulosic carboxyl methylation derivant, has another name called cellulose gum, is the water miscible ionic ether of one obtained through chemical modification.Its aqueous solution has thickening, bonding film forming, protecting glue, maintenance moisture, emulsification and suspension effect, is topmost ionic cellulose element glue.CMC is obtained after normally being reacted by natural cellulose and caustic alkali and monochloroacetic acid, is a kind of anionic macromolecular compound, and compound molecular weight from several thousand to 1,000,000 is not etc.CMC belongs to natural cellulose modification, and current Food and Argriculture OrganizationFAO (FAO) and the World Health Organization (WHO) formally claim it to be " modified-cellulose ".The synthetic method of CMC, and in nineteen twenty-one issued patents and be seen in generation, is after this just realized in Europe commercially producing in invention in 1918 by fritz E.Jansen.CMC was only thick product at that time, did colloid and binding agent use.1936-1941, CMC industrial applied research is quite active, has delivered the patent of several suitable enlightenment.World War II, Germany using CMC for the synthesis of in washing composition as anti redeposition agent, and as the surrogate of some natural gum (as gelatin, gum arabic), make CMC industry obtain very large development.Hercules company of the U.S. starts industrial production CMC in nineteen forty-three, and produces refining CMC product in nineteen forty-six, and this product is recognized as safety food additive.CMC is because having many special propertys, as thickening, bonding, film forming, water holding, emulsification, suspension etc., and itself is nontoxic, odorless, the not easily feature such as fermentation, Heat stability is good and be widely used in the industries such as oil, geology, daily use chemicals, food, medicine, is described as " industrial monosodium glutamate ".
At present, CMC industrial production, divides solvent method and hydrophily method substantially; With alcohol (also can use Virahol, acetone), for solvent, product forms through desalination, purifying for the former, quality is high, quality better, in neutral; The latter's water is medium, and sodium chloroacetate effective rate of utilization is low, product saltiness is large, moisture is high, in alkalescence, be crude product.The two is all that Mierocrystalline cellulose is through alkalizing, forming with Mono Chloro Acetic Acid or its sodium salt etherificate.Main raw material: linters, caustic soda, soda ash, Mono Chloro Acetic Acid etc.
Summary of the invention
The object of this invention is to provide a kind of preparation method of long quality guaranteed period Xylo-Mucine, the product long quality-guarantee period in aqueous of preparation, not easily cause viscosity reduction because of placing, there is the advantages such as technique is simple, easy-to-use, production cost is low, superior product quality, long quality-guarantee period.
To achieve these goals, the technical solution used in the present invention is as follows:
A preparation method for long quality guaranteed period Xylo-Mucine, comprises the steps:
1) alkalize:
A) preparation needed for liquid caustic soda and alcohol mixt, to alkalization device in drop into sheet alkali and 20% liquid caustic soda and alcohol mixt;
B) cotton liquid caustic soda and the alcohol mixt with remaining 80% of industry is successively added;
C) in alkalization device, be filled with nitrogen as shielding gas, carry out quaternization under agitation 45 ~ 55 minutes;
D) add a certain amount of Mono Chloro Acetic Acid alcohol blend under agitation, add rear reverse agitating function 2 minutes, then forward stirs discharging after 5 minutes;
2) etherificate:
Material after alkalization is added ether-based device, is warming up to 75 ~ 80 degree and carries out etherification reaction, and keep constant temperature 45 ~ 55 minutes in 15 ~ 20 minutes, recovered alcohol, is then cooled to 55 degree, discharging simultaneously;
3) wash:
Material after etherificate is proceeded to washing device, washes twice with the ethanol aqueous solution that mass concentration is 72% and 73% respectively; Adjusted to ph is 7.0 ~ 7.5, adds sodium hypochlorite solution and bleaches, then discharging;
4) rake is dry:
Material after washing is proceeded to rake equipment for drying, is cooled to 40 degree after charging completes, stirs 20 minutes; Be warming up to 78 ~ 80 degree again, recovered alcohol under constant temperature; After treating alcohol recycle, continue to be warmed up to 95 degree with top discharge;
5) pulverizing is dried:
Control temperature is 60 ~ 65 degree, the drying materials after rake is dry, pulverizing.
According to above scheme, the quaternization time in described step 1 is 50 minutes, stirs to comprise forward and stir and reverse agitating function, and except the reverse agitating function 2 minutes when reaction 20 ~ 30 minutes, all the other times are forward and stir; Acid addition time is 50 minutes.
According to above scheme, described step 2) in etherification reaction temperature be 78 degree.
According to above scheme, when drying in described step 5), the mass concentration of material moisture controls 6 ~ 8%, and during pulverizing, the aperture of sieve board of grinder is 0.35 mm, and during packaging, the precision of packaging vibrating screen is 80 orders.
The invention has the beneficial effects as follows: the product utilizing the present invention to prepare long quality-guarantee period in aqueous, not easily cause viscosity reduction because of placing, there is the advantages such as technique is simple, easy-to-use, production cost is low, superior product quality, long quality-guarantee period.
Embodiment
Below in conjunction with embodiment, technical scheme of the present invention is described.
Raw material and specification: essence cotton (polymerization degree is 2400 ~ 2600), alcohol (ethanol content is 95%), liquid caustic soda (NaOH content 50%), sheet alkali (technical grade), Mono Chloro Acetic Acid (>=95%), hydrochloric acid (content 36 ~ 37%).
embodiment 1:
A preparation method for long quality guaranteed period Xylo-Mucine, comprises the steps:
1) alkalize:
A) preparation needed for liquid caustic soda and alcohol mixt, to alkalization device in drop into sheet alkali and 20% liquid caustic soda and alcohol mixt;
B) cotton liquid caustic soda and the alcohol mixt with remaining 80% of industry is successively added;
C) in alkalization device, be filled with nitrogen as shielding gas, carry out quaternization under agitation 50 minutes, the reverse agitating function 2 minutes when reaction 25 minutes;
D) in 50 minutes, add Mono Chloro Acetic Acid alcohol blend under agitation, add rear reverse agitating function 2 minutes, then forward stirs discharging after 5 minutes;
2) etherificate:
Material after alkalization is added ether-based device, is warming up to 78 degree and carries out etherification reaction, and keep constant temperature 50 minutes in 17 minutes, recovered alcohol, is then cooled to 55 degree, discharging simultaneously;
3) wash:
Material after etherificate is proceeded to washing device, washes twice with the ethanol aqueous solution that mass concentration is 72% and 73% respectively; Adjusted to ph is 7.0 ~ 7.5, adds sodium hypochlorite solution and bleaches, then discharging;
4) rake is dry:
Material after washing is proceeded to rake equipment for drying, is cooled to 40 degree after charging completes, stirs 20 minutes; Be warming up to 79 degree again, recovered alcohol under constant temperature; After treating alcohol recycle, discharging after continuing to be warmed up to 95 degree;
5) pulverizing is dried:
Control temperature is 63 degree, and the drying materials after rake is dry, pulverizing, during oven dry, the mass concentration of material moisture controls 7%, and during pulverizing, the aperture of sieve board of grinder is 0.35 mm, and during packaging, the precision of packaging vibrating screen is 80 orders.
embodiment 2:
A preparation method for long quality guaranteed period Xylo-Mucine, comprises the steps:
1) alkalize:
A) preparation needed for liquid caustic soda and alcohol mixt, to alkalization device in drop into sheet alkali and 20% liquid caustic soda and alcohol mixt;
B) cotton liquid caustic soda and the alcohol mixt with remaining 80% of industry is successively added;
C) in alkalization device, be filled with nitrogen as shielding gas, carry out quaternization under agitation 45 minutes, the reverse agitating function 2 minutes when reaction 20 minutes;
D) in 50 minutes, add Mono Chloro Acetic Acid alcohol blend under agitation, add rear reverse agitating function 2 minutes, then forward stirs discharging after 5 minutes;
2) etherificate:
Material after alkalization is added ether-based device, is warming up to 80 degree and carries out etherification reaction, and keep constant temperature 45 minutes in 20 minutes, recovered alcohol, is then cooled to 55 degree, discharging simultaneously;
3) wash:
Material after etherificate is proceeded to washing device, washes twice with the ethanol aqueous solution that mass concentration is 72% and 73% respectively; Adjusted to ph is 7.0 ~ 7.5, adds sodium hypochlorite solution and bleaches, then discharging;
4) rake is dry:
Material after washing is proceeded to rake equipment for drying, is cooled to 40 degree after charging completes, stirs 20 minutes; Be warming up to 80 degree again, recovered alcohol under constant temperature; After treating alcohol recycle, discharging after continuing to be warmed up to 100 degree;
5) pulverizing is dried:
Control temperature is 60 degree, and the drying materials after rake is dry, pulverizing, during oven dry, the mass concentration of material moisture controls 6%, and during pulverizing, the aperture of sieve board of grinder is 0.35 mm, and during packaging, the precision of packaging vibrating screen is 80 orders.
embodiment 3:
A preparation method for long quality guaranteed period Xylo-Mucine, comprises the steps:
1) alkalize:
A) preparation needed for liquid caustic soda and alcohol mixt, to alkalization device in drop into sheet alkali and 20% liquid caustic soda and alcohol mixt;
B) cotton liquid caustic soda and the alcohol mixt with remaining 80% of industry is successively added;
C) in alkalization device, be filled with nitrogen as shielding gas, carry out quaternization under agitation 55 minutes, the reverse agitating function 2 minutes when reaction 30 minutes;
D) in 50 minutes, add Mono Chloro Acetic Acid alcohol blend under agitation, add rear reverse agitating function 2 minutes, then forward stirs discharging after 5 minutes;
2) etherificate:
Material after alkalization is added ether-based device, is warming up to 75 degree and carries out etherification reaction, and keep constant temperature 50 minutes in 15 minutes, recovered alcohol, is then cooled to 55 degree, discharging simultaneously;
3) wash:
Material after etherificate is proceeded to washing device, washes twice with the ethanol aqueous solution that mass concentration is 72% and 73% respectively; Adjusted to ph is 7.0 ~ 7.5, adds sodium hypochlorite solution and bleaches, then discharging;
4) rake is dry:
Material after washing is proceeded to rake equipment for drying, is cooled to 40 degree after charging completes, stirs 20 minutes; Be warming up to 78 degree again, recovered alcohol under constant temperature; After treating alcohol recycle, discharging after continuing to be warmed up to 110 degree;
5) pulverizing is dried:
Control temperature is 65 degree, and the drying materials after rake is dry, pulverizing, during oven dry, the mass concentration of material moisture controls 8%, and during pulverizing, the aperture of sieve board of grinder is 0.35 mm, and during packaging, the precision of packaging vibrating screen is 80 orders.
Above embodiment is the unrestricted technical scheme of the present invention in order to explanation only, although above-described embodiment is to invention has been detailed description, the person skilled of this area is to be understood that: can modify to the present invention or replace on an equal basis, but any amendment not departing from spirit and scope of the invention all should be encompassed in right of the present invention with local replacement.
Claims (4)
1. a preparation method for long quality guaranteed period Xylo-Mucine, is characterized in that, comprise the steps:
1) alkalize:
A) preparation needed for liquid caustic soda and alcohol mixt, to alkalization device in drop into sheet alkali and 20% liquid caustic soda and alcohol mixt;
B) cotton liquid caustic soda and the alcohol mixt with remaining 80% of industry is successively added;
C) in alkalization device, be filled with nitrogen as shielding gas, carry out quaternization under agitation 45 ~ 55 minutes;
D) add a certain amount of Mono Chloro Acetic Acid alcohol blend under agitation, add rear reverse agitating function 2 minutes, then forward stirs discharging after 5 minutes;
2) etherificate:
Material after alkalization is added ether-based device, is warming up to 75 ~ 80 degree and carries out etherification reaction, and keep constant temperature 45 ~ 55 minutes in 15 ~ 20 minutes, recovered alcohol, is then cooled to 55 degree, discharging simultaneously;
3) wash:
Material after etherificate is proceeded to washing device, washes twice with the ethanol aqueous solution that mass concentration is 72% and 73% respectively; Adjusted to ph is 7.0 ~ 7.5, adds sodium hypochlorite solution and bleaches, then discharging;
4) rake is dry:
Material after washing is proceeded to rake equipment for drying, is cooled to 40 degree after charging completes, stirs 20 minutes; Be warming up to 78 ~ 80 degree again, recovered alcohol under constant temperature; After treating alcohol recycle, continue to be warmed up to 95 degree with top discharge;
5) pulverizing is dried:
Control temperature is 60 ~ 65 degree, the drying materials after rake is dry, pulverizing.
2. the preparation method of long quality guaranteed period Xylo-Mucine according to claim 1, it is characterized in that, the quaternization time in described step 1 is 50 minutes, stirring comprises forward and stirs and reverse agitating function, except the reverse agitating function 2 minutes when reaction 20 ~ 30 minutes, all the other times are forward and stir; Acid addition time is 50 minutes.
3. the preparation method of long quality guaranteed period Xylo-Mucine according to claim 1, is characterized in that, described step 2) in etherification reaction temperature be 78 degree.
4. the preparation method of long quality guaranteed period Xylo-Mucine according to claim 1, it is characterized in that, when drying in described step 5), the mass concentration of material moisture controls 6 ~ 8%, and during pulverizing, the aperture of sieve board of grinder is 0.35 mm, and during packaging, the precision of packaging vibrating screen is 80 orders.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107417798A (en) * | 2017-09-04 | 2017-12-01 | 江苏泰利达新材料股份有限公司 | A kind of special CMC of ceramics production technology |
| WO2022162133A1 (en) | 2021-01-29 | 2022-08-04 | Nutrition & Biosciences Usa 1, Llc | Method of preparation of carboxymethyl cellulose having improved storage stability |
Citations (7)
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|---|---|---|---|---|
| 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 |
| CN102093481A (en) * | 2009-12-10 | 2011-06-15 | 上海长光企业发展有限公司 | Method for preparing instant carboxymethylcellulose |
| CN102268095A (en) * | 2011-07-28 | 2011-12-07 | 郑玉庆 | Preparation method of carboxymethyl cellulose |
| 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 |
| 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 |
| CN104387476A (en) * | 2014-12-05 | 2015-03-04 | 上海申光食用化学品有限公司 | Preparation method of food-grade sodium carboxymethyl cellulose (CMC) with high purity and relatively-high viscosity |
-
2015
- 2015-04-02 CN CN201510152113.8A patent/CN104761646A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102093481A (en) * | 2009-12-10 | 2011-06-15 | 上海长光企业发展有限公司 | Method for preparing instant carboxymethylcellulose |
| 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 |
| 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 |
| 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 |
| CN104387476A (en) * | 2014-12-05 | 2015-03-04 | 上海申光食用化学品有限公司 | Preparation method of food-grade sodium carboxymethyl cellulose (CMC) with high purity and relatively-high viscosity |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107417798A (en) * | 2017-09-04 | 2017-12-01 | 江苏泰利达新材料股份有限公司 | A kind of special CMC of ceramics production technology |
| WO2022162133A1 (en) | 2021-01-29 | 2022-08-04 | Nutrition & Biosciences Usa 1, Llc | Method of preparation of carboxymethyl cellulose having improved storage stability |
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Application publication date: 20150708 |