CN103242453A - Method for preparing low-viscosity sodium carboxymethylcellulose - Google Patents
Method for preparing low-viscosity sodium carboxymethylcellulose Download PDFInfo
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- CN103242453A CN103242453A CN2012102892502A CN201210289250A CN103242453A CN 103242453 A CN103242453 A CN 103242453A CN 2012102892502 A CN2012102892502 A CN 2012102892502A CN 201210289250 A CN201210289250 A CN 201210289250A CN 103242453 A CN103242453 A CN 103242453A
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Abstract
The invention discloses a method for preparing low-viscosity sodium carboxymethylcellulose. The method comprises the steps of alkalization of cellulose and etherification of alkali cellulose, and is characterized in that microcrystalline cellulose is taken as a cellulose raw material, wherein the average degree of polymerization of the microcrystalline cellulose ranges from 100 to 250. During preparation, the method provided by the invention takes the microcrystalline cellulose with ultra-low degree of polymerization as the raw material and does not utilize any strong oxidant; and during production, the method is safe and easy to operate; the viscosity of the product is ultralow; measured by BrookfieldLVDV-I+ type viscometer, the viscosity of the aqueous solution having the mass fraction of 15% is below 300 mpa.s, and the viscosity of the aqueous solution having the mass fraction of 30% is below 20000 mpa.s.
Description
Technical field
the present invention relates to a kind of preparation method of Xylo-Mucine, especially a kind of preparation method of low-viscosity sodium carboxymethyl cellulose.
Background technology
microcrystalline Cellulose is a kind of pure Mierocrystalline cellulose depolymerization product.By the natural cellulose preparation, it is the crystalline powder of odorless, tasteless.Be widely used as drug excipient, flow aids, weighting material, disintegrating agent, antisticking agent etc.Press dry product and calculate, cellulose should be 97.0%～102.0%.
the raw material that the domestic production low-viscosity sodium carboxymethyl cellulose is generally used at present is wooden oar, and what prepare the use of ultra low viscosity carboxymethyl cellulose sodium is to add the method that hydrogen peroxide carries out strong oxidation.This method is wayward, and has potential safety hazard, if do not adopt strong oxidation style, the viscosity ratio of product is higher, does not reach ultra-low viscosity, makes Xylo-Mucine be restricted in the application in a lot of fields.
Summary of the invention
the present invention seeks to: the preparation method that a kind of low-viscosity sodium carboxymethyl cellulose product is provided.
technical scheme of the present invention is:
a kind of preparation method of low-viscosity sodium carboxymethyl cellulose, the step comprised has cellulosic alkalization, the etherificate of soda cellulose; It is characterized in that, the method be take Microcrystalline Cellulose as cellulosic material; The mean polymerisation degree of described Microcrystalline Cellulose is 100 ~ 250.
the preferred technical scheme of technique scheme is that the temperature of reaction of described cellulosic alkalization is controlled at 15 ~ 40 ℃; Alkalization time 40 ~ 80min.
the preferred technical scheme of technique scheme is that the reaction process of the etherificate of soda cellulose is divided into two steps:
step 1, add the first etherification reaction 40-70min of chloroacetic acid solution;
step 2, be warming up to 75 ~ 80 ℃, continue etherification reaction 40-80min.
advantage of the present invention is:
the Microcrystalline Cellulose with ultra low polymerization degree of take when prepared by the inventive method is raw material, do not need to use strong oxidizer, safe during production, easy to operate, product viscosity is ultralow, the solution viscosity that the measurement quality mark is 15% on BrookfieldLVDV-I+ type viscometer is below 300mpas, and the solution viscosity that massfraction is 30% is below 20000mpas.
The accompanying drawing explanation
below in conjunction with drawings and Examples, the invention will be further described:
the preparation method's that Fig. 1 is the low-viscosity sodium carboxymethyl cellulose described in embodiment schema.
Embodiment
referring to Fig. 1.The preparation method of the described low-viscosity sodium carboxymethyl cellulose of this embodiment, take Microcrystalline Cellulose as cellulosic material, comprises the following steps:
1), premix: the ethanolic soln that the sodium hydroxide solution that is a certain amount of weight concentration 45-52% in advance is 86-96% with weight concentration mixes in mixing vessel by weight 1:1-3, and is cooled to 10-30 ℃.
2), feed intake: the sodium hydroxide ethanolic soln after premix is joined in the kneader with a pair of serpentine axle along the mutual reverse rotation campaign of axis, then add uniformly Microcrystalline Cellulose, the polymerization degree 100-250 of Microcrystalline Cellulose.The weight ratio of Microcrystalline Cellulose and sodium hydroxide is controlled at 1:1-3, with the weight ratio of ethanolic soln be 1:1.2-5.
3), cellulosic alkalization: 15 ~ 40 ℃ of temperature of reaction, the reaction times is 40-80min.
4), the etherificate of soda cellulose: add the chloroacetic acid solution that weight concentration is 65-78% to carry out etherification reaction, the weight ratio of Microcrystalline Cellulose and chloroacetic acid solution is 1:1-3, first etherificate 40-70 minute, etherificate is warming up to 75-80 ℃ after finishing, and continues etherificate 40-80 minute.Make rough Xylo-Mucine.
5), neutralization: reaction mass is discharged to neutralization bucket after being cooled to 60 ℃, and being neutralized to pH value with the hydrochloric acid soln of 30-40% is 7.0-8.5.
6), washing: the reaction mass after neutralization carries out twice washing with the ethanolic soln of 56-76% to be made with extra care, and press dry recovery ethanol.
7), the aftertreatment of product: make again refining low-viscosity sodium carboxymethyl cellulose after the processes such as super-dry, pulverizing.
the viscosity measurement of products obtained therefrom of the present invention: the aqueous solution that the massfraction of formulated product is 15% and 30%, on BrookfieldLVDV-I+ type viscometer, measure under 25 ℃.Concrete testing method is with reference to GB1904-2005.Substitution value, pH value, purity, moisture are tested according to the GB1904-2005 testing standard.
the invention will be further described in conjunction with specific embodiments.The umber of embodiment Raw and ratio are all by weight.
embodiment mono-:
2.5 parts of ethanolic solns that 1.6 parts of sodium hydroxide solutions that is weight concentration 48% in advance and weight concentration are 90% mix and are cooled to below 25 ℃, join in reactor, then drop into 1 part of Microcrystalline Cellulose, quaternization 40-80 minute, alkalization temperature 15-40 ℃, alkalization adds the chloroacetic acid solution that 1.2 parts of weight concentrations are 65-78%, etherificate 40-70 minute, etherification temperature 25-50 ℃ after finishing.Be warming up to 75-80 ℃ after adding Mono Chloro Acetic Acid, continue etherificate 40-80 minute, after etherificate finishes blowing and in and PH to 7.0-8.5, more refining through washing, reclaim ethanol, dry, as to make ultra-low viscosity after pulverizing, sieving Xylo-Mucine product.Viscosity (15% aqueous solution) 291mpas, viscosity (30% aqueous solution) 16500mpas, substitution value 0.962, purity 92.34%.
?
case study on implementation two:
2.4 parts of ethanolic solns that 1.7 parts of sodium hydroxide solutions that is weight concentration 50% in advance and weight concentration are 92% mix and are cooled to below 25 ℃, join in reactor, then drop into 1 part of Microcrystalline Cellulose, quaternization 40-80 minute, alkalization temperature 15-40 ℃, alkalization adds the chloroacetic acid solution that 1.3 parts of weight concentrations are 65-78%, etherificate 40-70 minute, etherification temperature 25-50 ℃ after finishing.Be warming up to 75-80 ℃ after adding Mono Chloro Acetic Acid, continue etherificate 40-80 minute, after etherificate finishes blowing and in and PH to 7.0-8.5, more refining through washing, reclaim ethanol, dry, as to make ultra-low viscosity after pulverizing, sieving Xylo-Mucine product.Viscosity (15% aqueous solution) 283mpas, viscosity (30% aqueous solution) 14750mpas, substitution value 0.971, purity 91.76%.
?
case study on implementation three:
2.5 parts of ethanolic solns that 1.75 parts of sodium hydroxide solutions that is weight concentration 50% in advance and weight concentration are 94% mix and are cooled to below 25 ℃, join in reactor, then drop into 1 part of Microcrystalline Cellulose, quaternization 40-80 minute, alkalization temperature 15-40 ℃, alkalization adds the chloroacetic acid solution that 1.36 parts of weight concentrations are 65-78%, etherificate 40-70 minute, etherification temperature 25-50 ℃ after finishing.Be warming up to 75-80 ℃ after adding Mono Chloro Acetic Acid, continue etherificate 40-80 minute, after etherificate finishes blowing and in and PH to 7.0-8.5, more refining through washing, reclaim ethanol, dry, as to make ultra-low viscosity after pulverizing, sieving Xylo-Mucine product.Viscosity (15% aqueous solution) 268mpas, viscosity (30% aqueous solution) 13870mpas, substitution value 0.979, purity 90.21%.
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above demonstration and described ultimate principle of the present invention, principal character and advantage of the present invention.The technician of the industry should understand; the present invention is not restricted to the described embodiments; that in above-described embodiment and specification sheets, describes just illustrates principle of the present invention; the present invention also has various changes and modifications without departing from the spirit and scope of the present invention, and these changes and improvements all fall in the claimed scope of the invention.
Claims (3)
1. the preparation method of a low-viscosity sodium carboxymethyl cellulose, the step comprised has cellulosic alkalization, the etherificate of soda cellulose; It is characterized in that, the method be take Microcrystalline Cellulose as cellulosic material; The mean polymerisation degree of described Microcrystalline Cellulose is 100 ~ 250.
2. the preparation method of low-viscosity sodium carboxymethyl cellulose according to claim 1, is characterized in that, the temperature of reaction of described cellulosic alkalization is controlled at 15 ~ 40 ℃; Alkalization time 40 ~ 80min.
3. the preparation method of low-viscosity sodium carboxymethyl cellulose according to claim 1, is characterized in that, the reaction process of the etherificate of soda cellulose is divided into two steps:
Step 1, add the first etherification reaction 40-70min of chloroacetic acid solution;
Step 2, be warming up to 75 ~ 80 ℃, continue etherification reaction 40-80min.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104558205A (en) * | 2014-12-19 | 2015-04-29 | 西安北方惠安化学工业有限公司 | Preparation method of low-viscosity sodium carboxymethyl cellulose |
| CN104877033A (en) * | 2015-06-03 | 2015-09-02 | 西南大学 | Preparation method of carboxymethyl modified nano-crystalline celluloses |
| CN105906724A (en) * | 2016-06-07 | 2016-08-31 | 常熟威怡科技有限公司 | Preparation method of low-turbidity high-performance sodium carboxymethylcellulose |
| CN106749685A (en) * | 2016-12-21 | 2017-05-31 | 天津润圣纤维素科技有限公司 | A kind of production technology of low-viscosity sodium carboxymethyl cellulose |
| CN108659134A (en) * | 2018-06-13 | 2018-10-16 | 常熟威怡科技有限公司 | A kind of preparation method of sodium carboxymethylcellulose as emulsifier |
| CN108822223A (en) * | 2018-06-14 | 2018-11-16 | 恒达亲水胶体泰州有限公司 | It is a kind of for exploiting the preparation method of the sodium carboxymethylcellulose of combustible ice |
| CN113875972A (en) * | 2021-10-29 | 2022-01-04 | 福建农林大学 | Method for preparing modified mushroom particles through carboxymethylation one-step method |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101220099A (en) * | 2008-01-31 | 2008-07-16 | 重庆力宏精细化工有限公司 | Production method for high viscosity sodium carboxymethylcellulose |
| CN101324034A (en) * | 2007-06-11 | 2008-12-17 | 北京盖雅技术中心有限公司 | Method for producing sodium carboxymethylcellulose from waste coated paper |
-
2012
- 2012-08-14 CN CN2012102892502A patent/CN103242453A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101324034A (en) * | 2007-06-11 | 2008-12-17 | 北京盖雅技术中心有限公司 | Method for producing sodium carboxymethylcellulose from waste coated paper |
| CN101220099A (en) * | 2008-01-31 | 2008-07-16 | 重庆力宏精细化工有限公司 | Production method for high viscosity sodium carboxymethylcellulose |
Non-Patent Citations (1)
| Title |
|---|
| 张俊等: "微晶纤维素的羧甲基化反应", 《纤维素科学与技术》 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104558205A (en) * | 2014-12-19 | 2015-04-29 | 西安北方惠安化学工业有限公司 | Preparation method of low-viscosity sodium carboxymethyl cellulose |
| CN104877033A (en) * | 2015-06-03 | 2015-09-02 | 西南大学 | Preparation method of carboxymethyl modified nano-crystalline celluloses |
| CN105906724A (en) * | 2016-06-07 | 2016-08-31 | 常熟威怡科技有限公司 | Preparation method of low-turbidity high-performance sodium carboxymethylcellulose |
| CN106749685A (en) * | 2016-12-21 | 2017-05-31 | 天津润圣纤维素科技有限公司 | A kind of production technology of low-viscosity sodium carboxymethyl cellulose |
| CN108659134A (en) * | 2018-06-13 | 2018-10-16 | 常熟威怡科技有限公司 | A kind of preparation method of sodium carboxymethylcellulose as emulsifier |
| CN108822223A (en) * | 2018-06-14 | 2018-11-16 | 恒达亲水胶体泰州有限公司 | It is a kind of for exploiting the preparation method of the sodium carboxymethylcellulose of combustible ice |
| CN113875972A (en) * | 2021-10-29 | 2022-01-04 | 福建农林大学 | Method for preparing modified mushroom particles through carboxymethylation one-step method |
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Application publication date: 20130814 |