CN101942028B - Method for producing potassium carboxymethylcellulose - Google Patents
Method for producing potassium carboxymethylcellulose Download PDFInfo
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- CN101942028B CN101942028B CN2010102997134A CN201010299713A CN101942028B CN 101942028 B CN101942028 B CN 101942028B CN 2010102997134 A CN2010102997134 A CN 2010102997134A CN 201010299713 A CN201010299713 A CN 201010299713A CN 101942028 B CN101942028 B CN 101942028B
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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 working method of CMC 99.5 potassium, specifically is a kind of working method of CMC 99.5 potassium.
Background technology
National standard foodstuff additive GB2760-2007 standard is classified Xylo-Mucine (CMC) as: can in varieties of food items, need an amount of additive list (A3 that uses by production; 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, the research proof, diseases such as mellitus, 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.Like 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 makes in the alkalization process much larger than the alkalescence of NaOH; 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 property 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 CMC 99.5 potassium with the process method of producing CMC, resulting product substitution value is low, and viscosity is low, is difficult for dissolving, and Na+ content is high, and production cost is high, has seriously limited the use of CMC 99.5 potassium.
The working method of a kind of CMC 99.5 potassium of the present invention; Can obtain the high purity CMC 99.5 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 reduced cost, had important and profound significance the sustainable fast development of ether of cellulose industry.
Summary of the invention
The objective of the invention is to the deficiency to prior art, provide that a kind of cost is low, efficient is high, the high (working method of the CMC 99.5 potassium of Na salt≤0.5%wt) of the quality of product.The present invention realizes through following technical scheme.
A kind of working method of CMC 99.5 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; Said 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 working method of above-mentioned CMC 99.5 potassium, the first step are carried out the protection of inert gas processing before adding acid, are to outgas 5～20 minutes under 0.05～0.10MPa in vacuum tightness, charge into rare gas element.
Adopt the aqueous solution of water or alcohol when the working method of above-mentioned CMC 99.5 potassium, second step said water washing, the moisture massfraction of the solid that obtains is 55～65%.
The working method of above-mentioned CMC 99.5 potassium, the aqueous solution of said alcohol are methyl alcohol, ethanol or aqueous isopropanol.
The working method of above-mentioned CMC 99.5 potassium, the 3rd step was under protection of inert gas, to carry out, 25～35 ℃ of insulations of temperature 1～6 hour, said 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 ethyloic mol ratio in alkali and the raw material is 1: 2.
The working method of above-mentioned CMC 99.5 potassium, said 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 under the processing condition that limited, obtains has the CMC 99.5 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; Enlarge the use range of modified-cellulose, effectively reduced cost, can directly on existing installation, realize the present invention.
Embodiment
Below in conjunction with embodiment, detailed description is further done in practical implementation 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, and solid use pH=1,0 ℃ of water washing, and separation obtains water cut 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 ethyloic 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, and solid use pH=3, and 30 ℃, 80% ethanol water washing, separation obtains water cut 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 ethyloic 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, and solid use pH=1, and 10 ℃, the washing of 80% methanol-water, separation obtains water cut 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 ethyloic 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, and solid use pH=1, and 20 ℃, the washing of 80% isopropanol water, separation obtains water cut 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 ethyloic 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, and solid use pH=1, and 20 ℃, the washing of 85% isopropanol water, separation obtains water cut 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 ethyloic 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 (5)
1. the working method of a CMC 99.5 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; Said 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 is with the solution washing of pH=1～3,0～30 ℃ water or alcohol, and separating the moisture massfraction of solid that obtains is 55～65%;
The 3rd step carried out under protection of inert gas, added pH=7.5～8 that neutralize, ground caustic end to the last solid that obtains that separates of second step, and 25～35 ℃ of insulations of temperature 1～6 hour, said ground caustic end was by parts by weight K
2CO
399.0～99.5 parts, (NH
4)
2CO
3The mixture of 1～1.5 part of composition, the ethyloic mol ratio in alkali and the raw material is 1: 2;
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 5～20 minutes under 0.05～0.10MPa in vacuum tightness, charges into rare gas element.
3. method according to claim 1 is characterized in that, the aqueous solution of said alcohol is methyl alcohol, ethanol or aqueous isopropanol.
4. according to each described method of claim 1～3, it is characterized in that said rare gas element is nitrogen or argon gas.
5. method according to claim 4 is characterized in that, Na salt≤0.5%wt in the resultant the finished product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010102997134A CN101942028B (en) | 2010-09-30 | 2010-09-30 | Method for producing potassium carboxymethylcellulose |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010102997134A CN101942028B (en) | 2010-09-30 | 2010-09-30 | Method for producing potassium carboxymethylcellulose |
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|---|---|
| CN101942028A CN101942028A (en) | 2011-01-12 |
| CN101942028B true CN101942028B (en) | 2012-02-01 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
| CN114605562B (en) * | 2022-02-21 | 2023-05-16 | 浙江隆腾医用新材料有限公司 | Desalting method in sodium carboxymethylcellulose fiber production process |
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| FI71750C (en) * | 1981-09-10 | 1987-02-09 | Daicel Chem | Process for producing an alkali salt of carboxymethyl cellulose ether. |
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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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