CN101942028A - Method for producing potassium carboxymethylcellulose - Google Patents
Method for producing potassium carboxymethylcellulose Download PDFInfo
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- CN101942028A CN101942028A CN 201010299713 CN201010299713A CN101942028A CN 101942028 A CN101942028 A CN 101942028A CN 201010299713 CN201010299713 CN 201010299713 CN 201010299713 A CN201010299713 A CN 201010299713A CN 101942028 A CN101942028 A CN 101942028A
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Abstract
The invention discloses a method for producing potassium carboxymethylcellulose, which comprises the following steps of: adding acidic solution into a raw material of sodium carboxymethylcellulose, and performing reaction at the set temperature; and separating to remove centrifugate, adding alkali, dehydrating, drying and crushing to prepare the product. The method for producing the potassium carboxymethylcellulose has the advantages of capacity of preparing high-quality potassium carboxymethylcellulose, simple and convenient operation, high-purity product, high performance, stable batch quality, and direct implementation on conventional equipment for producing the sodium carboxymethylcellulose.
Description
Technical field
The present invention relates to a kind of production method of carboxymethyl cellulose potassium, specifically is a kind of production method of carboxymethyl cellulose potassium.
Background technology
National standard foodstuff additive GB2760-2007 standard is classified Xylo-Mucine (CMC) as: can need an amount of additive list (A3 that uses by producing in varieties of food items, 53), be widely used in the foodstuffs industry such as beverage, milk preparation, ice-creams, soy sauce, jelly, jam, instant noodles.This just means that in foodstuff production, CMC can heavy addition.Yet, studies have shown that diseases such as diabetes, hypertension, cardiovascular diseases all have close getting in touch with the sodium ion Excessive Intake.
Reduce human body and take in the total amount of sodium ion.Suitably reduce the intake of sodium salt on the one hand, effective way is the amount that increases sylvite in the food, thereby reduces the total amount of sodium ion in the human body.As the product that has all occurred Cardia Salt on the market is exactly to add the salt that a certain amount of Repone K replaces sodium-chlor.
The CMC production technique is that refined stock and NaOH generate soda cellulose according to certain ratio reaction, and soda cellulose and Mono Chloro Acetic Acid carry out etherification reaction according to certain ratio, neutralization, and purifying, drying is pulverized.Because, the alkalescence of KOH is much larger than the alkalescence of NaOH, make in the alkalization process, cellulose degradation is serious, can't obtain full-bodied product, the etherifying agent utilization ratio is low in etherification procedure, and by product increases, the water-absorbent of KOH, suction carbonic acid gas and price are higher than NaOH far away, and contain a certain amount of Na among the KOH
+(analytical pure Na salt≤2%, GB/T2306), the usage quantity of KCl is big less than NaCl, and use range is wide less than NaCl.Therefore, produce carboxymethyl cellulose potassium with the processing method of producing CMC, resulting product substitution value is low, and viscosity is low, is difficult for dissolving, Na+ content height, and the production cost height has seriously limited the use of carboxymethyl cellulose potassium.
The production method of a kind of carboxymethyl cellulose potassium of the present invention, can obtain the high purity carboxymethyl cellulose potassium (Na salt≤0.5%) of different degree of substitution and viscosity, increased the kind of modified-cellulose, enlarged the use range of modified-cellulose, effectively reduce cost, have important and profound significance the sustainable fast development of ether of cellulose industry.
Summary of the invention
The objective of the invention is at the deficiencies in the prior art, provide that a kind of cost is low, efficient is high, the quality height of the product (production method of the carboxymethyl cellulose potassium of Na salt≤0.5%wt).The present invention is achieved through the following technical solutions.
A kind of production method of carboxymethyl cellulose potassium comprises the steps:
The first step adds the H of mass concentration 10～40% to raw material
2SO
4The aqueous solution, H
2SO
4The amount ratio of the aqueous solution and raw material is 4～16 liters: 1 kilogram; Described raw material is food grade Xylo-Mucine finished product or purifying food grade Xylo-Mucine not;
Second step, 10～40 ℃ of insulations 2～10 hours separate, and the solid that obtains separates with pH=1～3,0～30 ℃ water washing;
Second step of the 3rd step is last separates the solid that obtains and adds pH=7.5～8 that neutralize, ground caustic end;
The 4th step solid that obtains of the 3rd step dewater, dry, pulverize product.
The production method of above-mentioned carboxymethyl cellulose potassium, the first step are carried out the protection of inert gas processing before adding acid, are to outgas under 0.05～0.10MPa 5～20 minutes in vacuum tightness, charge into rare gas element.
Adopt the aqueous solution of water or alcohol when the production method of above-mentioned carboxymethyl cellulose potassium, second step described water washing, the moisture massfraction of the solid that obtains is 55～65%.
The production method of above-mentioned carboxymethyl cellulose potassium, the aqueous solution of described alcohol are methyl alcohol, ethanol or aqueous isopropanol.
The production method of above-mentioned carboxymethyl cellulose potassium, the 3rd step was to carry out under protection of inert gas, 25～35 ℃ of insulations of temperature 1～6 hour, described ground caustic end is by parts by weight K
2CO
399.0～99.5 parts, (NH
4)
2CO
3The mixture of 1～1.5 part of composition, the carboxymethyl mol ratio in alkali and the raw material is 1: 2.
The production method of above-mentioned carboxymethyl cellulose potassium, described rare gas element is nitrogen or argon gas, obtains product Na salt≤0.5%.
Compared with prior art; the protection of inert gas technology that the present invention adopts; utilize food grade Xylo-Mucine finished product or not purifying food grade Xylo-Mucine be raw material; and the product that obtains under the processing condition that limited has the carboxymethyl cellulose potassium of high substitution value, high viscosity, Na salt≤0.5%; steady quality between batch; the present invention has increased the kind of modified-cellulose; enlarged the use range of modified-cellulose; effectively reduce cost, can directly on existing installation, realize the present invention.
Embodiment
Below in conjunction with embodiment, detailed description is further done in concrete enforcement of the present invention, but enforcement of the present invention and protection domain are not limited thereto.
The contriver has carried out in depth creative research and test to the present invention, and many successful embodiment are arranged, and enumerates five embodiment below.
Embodiment 1
The first step is with food grade Xylo-Mucine (FH6 type, DS=0.62,1% aqueous solution viscosity (Brookfield) 250mPa, purity 98.8%) 51g, and vacuum tightness is that 0.05MPa outgased 5 minutes down, charges into nitrogen, adds the H of mass concentration 10%
2SO
4Aqueous solution 816mL;
Second step, 10 ℃ of insulations 10 hours separate, solid pH=1, and 0 ℃ of water washing, separation obtains water content and is 55% solid;
The solid that second step of the 3rd step obtains carries out under nitrogen protection, and 25 ℃ of temperature add K
2CO
399 parts, (NH
4)
2CO
31.5 part alkali mix powder 7.3g (alkali: the carboxymethyl in the raw material is 1: 2 (mol ratio)) that forms is incubated 6 hours pH=7.5;
The 3rd step of the 4th step obtains solid and dewaters, dries, pulverizes, gets product.
Products obtained therefrom DS=0.62,1% aqueous solution viscosity (Brookfield) 320mPa, purity 99.8%, Na salt≤0.15%wt.
Embodiment 2
The first step will be produced does not have the food grade of purifying Xylo-Mucine (FH6 type, DS=0.62,2% aqueous solution viscosity (Brookfield) 50mPa, purity 85.0%) 65g, vacuum tightness is that 0.10MPa outgased 20 minutes down, charges into nitrogen, adds the H of mass concentration 40%
2SO
4Aqueous solution 260mL;
Second step, 40 ℃ of insulations 2 hours separate, solid pH=3, and 30 ℃, 80% ethanol water washing, separation obtains water content and is 65% solid;
The solid that second step of the 3rd step obtains carries out under nitrogen protection, and 35 ℃ of temperature add K
2CO
399.5 part, (NH
4)
2CO
3The alkali mix powder 8.1g of 1 part of composition (alkali: the carboxymethyl in the raw material is 1: 2 (mol ratio)) is incubated 1 hour, pH=8.0;
The 3rd step of the 4th step obtains solid and dewaters, dries, pulverizes, gets product.
Products obtained therefrom DS=0.60,1% aqueous solution viscosity (Brookfield) 330mPa, purity 98.9%, Na salt≤0.5%wt.
Embodiment 3
The first step is with food grade Xylo-Mucine (FH9 type, DS=1.0,1% aqueous solution viscosity (Brookfield) 400mPa, purity 98.8%) 40g, and vacuum tightness is that 0.05MPa outgased 10 minutes down, charges into argon gas, adds the H of mass concentration 15%
2SO
4Aqueous solution 300mL;
Second step, 10 ℃ of insulations 4 hours separate, solid pH=1, and 10 ℃, the washing of 80% methanol-water, separation obtains water content and is 60% solid;
The solid that second step of the 3rd step obtains carries out 30 ℃ of temperature, adding, K under argon shield
2CO
399.5 part, (NH
4)
2CO
3The alkali mix powder 8.4g of 1 part of composition (alkali: the carboxymethyl in the raw material is 1: 2 (mol ratio)) is incubated 3 hours, pH=8.0;
The 3rd step of the 4th step obtains solid and dewaters, dries, pulverizes, gets product.
Products obtained therefrom DS=0.99,1% aqueous solution viscosity (Brookfield) 460mPa, purity 99.8%, Na salt≤0.17%.
Embodiment 4
The first step is with food grade Xylo-Mucine (FVH9 type, DS=0.90,1% aqueous solution viscosity (Brookfield) 800mPa, purity 98.8%) 40g, and vacuum tightness is that 0.09MPa outgased 15 minutes down, charges into argon gas, adds the H of mass concentration 15%
2SO
4Aqueous solution 500mL;
Second step, 20 ℃ of insulations 3 hours separate, solid pH=1, and 20 ℃, the washing of 80% isopropanol water, separation obtains water content and is 65% solid;
The solid that second step of the 3rd step obtains carries out under argon shield, and 20 ℃ of temperature add K
2CO
399.5 part, (NH
4)
2CO
3The alkali mix powder 7.5g of 1 part of composition (alkali: the carboxymethyl in the raw material is 1: 2 (mol ratio)) is incubated 5 hours, pH=8.0;
The 3rd step of the 4th step obtains solid and dewaters, dries, pulverizes, gets product.
Products obtained therefrom DS=0.90,1% aqueous solution viscosity (Brookfield) 950mPa, purity 99.8%, Na salt≤0.15%wt.
Embodiment 5
The first step is with food grade Xylo-Mucine (FM9 type, DS=0.90,2% aqueous solution viscosity (Brookfield) 800mPa, purity 98.8%) 40g, and vacuum tightness is that 0.09MPa outgased 15 minutes down, charges into argon gas, adds the H of mass concentration 15%
2SO
4Aqueous solution 500mL;
Second step, 20 ℃ of insulations 3 hours separate, solid pH=1, and 20 ℃, the washing of 85% isopropanol water, separation obtains water content and is 65% solid;
The solid that second step of the 3rd step obtains carries out under argon shield, and 20 ℃ of temperature add K
2CO
399.5 part, (NH
4)
2CO
3The alkali mix powder 7.5g of 1 part of composition (alkali: the carboxymethyl in the raw material is 1: 2 (mol ratio)) is incubated 5 hours, pH=8.0;
The 3rd step of the 4th step obtains solid and dewaters, dries, pulverizes, gets product.
Products obtained therefrom DS=0.90,2% aqueous solution viscosity (Brookfield) 950mPa, purity 99.8%, Na salt≤0.15%wt.
Claims (7)
1. the production method of a carboxymethyl cellulose potassium is characterized in that comprising the steps:
The first step adds the H of mass concentration 10～40% to raw material
2SO
4The aqueous solution, H
2SO
4The amount ratio of the aqueous solution and raw material is 4～16 liters: 1 kilogram; Described raw material is food grade Xylo-Mucine finished product or purifying food grade Xylo-Mucine not;
Second step, 10～40 ℃ of insulations 2～10 hours separate, and the solid that obtains separates with pH=1～3,0～30 ℃ water washing;
Second step of the 3rd step is last separates the solid that obtains and adds pH=7.5～8 that neutralize, ground caustic end;
The 4th step solid that obtains of the 3rd step dewater, dry, pulverize product.
2. method according to claim 1 is characterized in that, the first step is carried out the protection of inert gas processing before adding acid, is to outgas under 0.05～0.10MPa 5～20 minutes in vacuum tightness, charges into rare gas element.
3. method according to claim 1 is characterized in that, adopts the aqueous solution of water or alcohol during second step described water washing, and the moisture massfraction of the solid that obtains is 55～65%.
4. method according to claim 1 is characterized in that, the aqueous solution of described alcohol is methyl alcohol, ethanol or aqueous isopropanol.
5. method according to claim 1 is characterized in that, the 3rd step was to carry out under protection of inert gas, 25～35 ℃ of insulations of temperature 1～6 hour, and described ground caustic end is by parts by weight K
2CO
399.0～99.5 parts, (NH
4)
2CO
3The mixture of 1～1.5 part of composition, the carboxymethyl mol ratio in alkali and the raw material is 1: 2.
6. according to each described method of claim 1～5, it is characterized in that described rare gas element is nitrogen or argon gas.
7. method according to claim 6 is characterized in that, Na salt≤0.5%wt in the resultant the finished product.
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|---|---|---|---|
| CN2010102997134A CN101942028B (en) | 2010-09-30 | 2010-09-30 | Method for producing potassium carboxymethylcellulose |
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|---|---|---|---|
| CN2010102997134A CN101942028B (en) | 2010-09-30 | 2010-09-30 | Method for producing potassium carboxymethylcellulose |
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| CN101942028A true CN101942028A (en) | 2011-01-12 |
| CN101942028B CN101942028B (en) | 2012-02-01 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101967231A (en) * | 2010-09-30 | 2011-02-09 | 华南理工大学 | Production method of sodium carboxymethyl cellulose with low sodium content |
| CN106336462A (en) * | 2016-10-13 | 2017-01-18 | 重庆力宏精细化工有限公司 | Method for preparing carboxymethyl cellulose |
| CN108330724A (en) * | 2018-01-17 | 2018-07-27 | 太原理工大学 | A method of using waste and old cotton for water-soluble cellulose |
| CN114605562A (en) * | 2022-02-21 | 2022-06-10 | 浙江隆腾医用新材料有限公司 | Desalting method in production process of sodium carboxymethylcellulose fibers |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4426518A (en) * | 1981-09-10 | 1984-01-17 | Daicel Chemical Industries, Ltd. | Process for producing an alkali salt of a carboxymethylcellulose ether |
-
2010
- 2010-09-30 CN CN2010102997134A patent/CN101942028B/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4426518A (en) * | 1981-09-10 | 1984-01-17 | Daicel Chemical Industries, Ltd. | Process for producing an alkali salt of a carboxymethylcellulose ether |
Non-Patent Citations (3)
| Title |
|---|
| 《应用化工》 20080831 吕少等 "不同碱金属氢氧化物对纤维素羧甲基化的影响" 921-929 1-7 第37卷, 第8期 2 * |
| 《纤维素科学与技术》 19951231 张黎明等 "水溶性改性纤维素对粘土水化的抑制作用" 20-27 1-7 第3卷, 第4期 2 * |
| 《纤维素醚工业》 20011231 杨之礼 "纤维素醚的其它品种介绍" 61-63 1-7 第9卷, 第4期 2 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101967231A (en) * | 2010-09-30 | 2011-02-09 | 华南理工大学 | Production method of sodium carboxymethyl cellulose with low sodium content |
| CN101967231B (en) * | 2010-09-30 | 2012-06-20 | 华南理工大学 | Production method of sodium carboxymethyl cellulose with low sodium content |
| CN106336462A (en) * | 2016-10-13 | 2017-01-18 | 重庆力宏精细化工有限公司 | Method for preparing carboxymethyl cellulose |
| CN108330724A (en) * | 2018-01-17 | 2018-07-27 | 太原理工大学 | A method of using waste and old cotton for water-soluble cellulose |
| CN114605562A (en) * | 2022-02-21 | 2022-06-10 | 浙江隆腾医用新材料有限公司 | Desalting method in production process of sodium carboxymethylcellulose fibers |
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| CN101942028B (en) | 2012-02-01 |
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Application publication date: 20110112 Assignee: Shanghai Everest Fine Chemicals Co., Ltd. Assignor: South China University of Technology Contract record no.: 2014440000355 Denomination of invention: Method for producing potassium carboxymethylcellulose Granted publication date: 20120201 License type: Exclusive License Record date: 20140723 |
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