CN101967231B - Production method of sodium carboxymethyl cellulose with low sodium content - Google Patents

Production method of sodium carboxymethyl cellulose with low sodium content Download PDF

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Publication number
CN101967231B
CN101967231B CN2010102997079A CN201010299707A CN101967231B CN 101967231 B CN101967231 B CN 101967231B CN 2010102997079 A CN2010102997079 A CN 2010102997079A CN 201010299707 A CN201010299707 A CN 201010299707A CN 101967231 B CN101967231 B CN 101967231B
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carboxymethyl cellulose
sodium
sodium carboxymethyl
raw material
solid
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CN101967231A (en
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叶君
熊犍
孙润仓
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South China University of Technology SCUT
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South China University of Technology SCUT
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Abstract

The invention provides a production method of sodium carboxymethyl cellulose with low sodium content, which comprises the following steps: firstly, adding an acid solution into the sodium carboxymethyl cellulose raw material for reacting at the set temperature; carrying out separation, and removing the separating solution; adding alkali; and dehydrating, baking and crushing to obtain a product. The invention can obtain high-quality sodium carboxymethyl cellulose with low sodium content and has simple and convenient operation; the obtained product has high performance, high viscosity and stable batch quality; and the invention can be directly realized on the existing equipment.

Description

A kind of working method of low CMC (Sodium Carboxymethyl Cellulose) BP/USP sodium
Technical field
The present invention relates to a kind of working method of low CMC (Sodium Carboxymethyl Cellulose) BP/USP sodium.
Background technology
Xylo-Mucine (CMC) uses as additive in food; Have multiple functions such as thickening, suspension, emulsification, stable, conformal, film forming, expanded, anti-corrosive fresh-keeping, acidproof and health care; Because the price of CMC is cheap than food glue such as gelatin, agar, sodium-alginates, therefore be widely used in the food such as the industrial beverage of modern food, milk preparation, ice-creams, soy sauce, jelly, jam, instant noodles simultaneously.Standard GB 2760-2007 classifies it as: can in varieties of food items, need an amount of additive list (A3,53) that uses by production, 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.
Human body is not only taken in sodium ion through salt, and additive (like Sodium Benzoate, Sodium Glutamate, Xylo-Mucine, sodium-alginate etc.) contains a large amount of sodium ions equally and also absorbed by human body.Exactly because notice, in food processing process, additive also can be brought a certain amount of sodium ion into.China NNFA, it is about 6g/ day that the healthy dose of salt is recommended by how tame authoritative mechanism such as FSA, and World Health Organization's recent proposals: per day for adults is eaten the salt amount and is changed 5g into by 6g.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.
CMC is a weak polyelectrolyte, one of characteristic of polyelectrolyte solution: its solution viscosity size with add the kind of salt and the concentration of salts solution has great dependency.Therefore,, considerable influence will be arranged, and cause solution viscosity to descend significantly the SOLUTION PROPERTIES of CMC if in CMC, directly add sylvite.
The working method of a kind of low CMC (Sodium Carboxymethyl Cellulose) BP/USP sodium of the present invention; Can increase the kind of CMC product; Its ratio of viscosities contains same potassium amount (raw material CMC+KCl) height, enlarges its use range, and reduces the content of its sodium ion; HUMAN HEALTH is had nourishing function, keep the sustainable fast development of CMC industry to have important and profound significance.
Summary of the invention
The objective of the invention is to deficiency, the working method of the low CMC (Sodium Carboxymethyl Cellulose) BP/USP sodium that a kind of cost is low, efficient is high, the quality of product is high is provided to prior art.
A kind of working method of low CMC (Sodium Carboxymethyl Cellulose) BP/USP sodium comprises the steps:
The first step is with the H of mass concentration 10～40% 2SO 4The aqueous solution adds in the raw material, 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;
The 3rd step solid that obtains of second step adds pH=7.5～8 that neutralize, ground caustic end;
The 4th the step the 3rd the step obtain solid dewater, dry, pulverize product.
The working method of above-mentioned low CMC (Sodium Carboxymethyl Cellulose) BP/USP sodium, 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.
The working method of above-mentioned low CMC (Sodium Carboxymethyl Cellulose) BP/USP sodium, the solid water cut quality that second step obtained at last is 55～65%.
The working method of above-mentioned low CMC (Sodium Carboxymethyl Cellulose) BP/USP sodium, reaction is under protection of inert gas, to carry out in the 3rd step, and 25～35 ℃ of temperature are incubated 1～6 hour, and said alkali is according to parts by weight Na 2CO 385～98 parts, K 2CO 31.5～14 parts, (NH 4) 2CO 30.5 the mixture of～1.5 parts of compositions, the ethyloic mol ratio in alkali and the raw material is 1: 2.
The working method of above-mentioned low CMC (Sodium Carboxymethyl Cellulose) BP/USP sodium, said rare gas element are high pure nitrogen, helium or argon gas, and its viscosity is greater than the KCl that directly adds same amount in its raw material.
The working method of above-mentioned low CMC (Sodium Carboxymethyl Cellulose) BP/USP sodium, said food grade Xylo-Mucine are FH6 type, FH9 type, FVH9 type or FM9 type.
Generally speaking, compared with prior art, the present invention has following advantage and beneficial effect: 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 ratio of viscosities that under the processing condition that limited, makes the product that obtains contains same potassium amount (CMC+KCl) height, has the performance height, steady quality between batch; Enlarge its use range; And reduce the content of its sodium ion, and HUMAN HEALTH is had nourishing function, 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%) 65g, and vacuum tightness is that 0.05MPa outgased 5 minutes down, charges into nitrogen, adds the H of mass concentration 10% 2SO 4Aqueous solution 1040mL;
Second step, 10 ℃ of insulations 10 hours separate, and the solid that obtains is used pH=1, and 0 ℃ of water washing separates, and obtains the solid that water cut is 55%wt;
The solid that second step of the 3rd step obtains carries out under nitrogen protection, and 25 ℃ of temperature add Na 2CO 385 parts, K 2CO 314 parts, (NH 4) 2CO 31.5 part alkali mix powder 10.7g (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 (Na:0.53, K:0.09), 1%wt aqueous solution viscosity (Brookfield) 350mPa; Purity 99.8%; Raw material CMC (FH6 type, DS=0.62,1%wt aqueous solution viscosity (Brookfield) 250mPa; Purity 98.8%) contain same K, 1%wt aqueous solution viscosity (Brookfield) 180mPa.
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 the 0.10MPa degassing 20 minutes down, charges into nitrogen, adds 40% H 2SO 4Aqueous solution 260mL;
Second step, 40 ℃ of insulations 2 hours separate, and solid use pH=3,30 ℃ of water washings, and 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 Na2CO 385 parts, K 2CO 314 parts, (NH 4) 2CO 31.5 part alkali mix powder 9.5g (alkali: the ethyloic in the raw material is 1: 2 (mol ratio)) that forms 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 (Na:0.52, K:0.08), 1% aqueous solution viscosity (Brookfield) 350mPa, purity 98.9%.Raw material CMC (FH6 type, DS=0.62,2% aqueous solution viscosity (Brookfield) 50mPa, purity 85.0%) contains same K, 2%wt aqueous solution viscosity (Brookfield) 30mPa.
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 15% H 2SO 4Aqueous solution 300mL;
Second step, 10 ℃ of insulations 4 hours separate, and solid use pH=1,10 ℃ of water washings, and separation obtains water cut and is 60% solid;
The solid that second step of the 3rd step obtains carries out under argon shield, and 30 ℃ of temperature add Na 2CO 398 parts, K 2CO 31.5 part, (NH 4) 2CO 30.5 part alkali mix powder 8.7g (alkali: the ethyloic in the raw material is 1: 2 (mol ratio)) that forms 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 (Na:0.98, K:0.01), 1% aqueous solution viscosity (Brookfield) 450mPa; Purity 99.8%; Raw material CMC (FH9 type, DS=1.0,1% aqueous solution viscosity (Brookfield) 400mPa; Purity 98.8%) contain same K, 1%wt aqueous solution viscosity (Brookfield) 280mPa.
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 15% H 2SO 4Aqueous solution 500mL;
Second step, 20 ℃ of insulations 3 hours separate, and solid use pH=1,20 ℃ of water washings, and 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 Na 2CO 390 parts, K 2CO 39.5 part, (NH 4) 2CO 30.5 part alkali mix powder 8.4g (alkali: the ethyloic in the raw material is 1: 2 (mol ratio)) that forms 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 (Na:0.81, K:0.09), 1% aqueous solution viscosity (Brookfield) 950mPa; Purity 99.8%; Raw material CMC (FVH9 type, DS=0.90,1% aqueous solution viscosity (Brookfield) 800mPa; Purity 98.8%) contain same K, 1%wt aqueous solution viscosity (Brookfield) 680mPa.
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 15% H 2SO 4Aqueous solution 500mL;
Second step, 20 ℃ of insulations 3 hours separate, and solid use pH=1,20 ℃ of water washings, and 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 Na 2CO 390 parts, K 2CO 39.5 part, (NH 4) 2CO 30.5 part alkali mix powder 8.4g (alkali: the ethyloic in the raw material is 1: 2 (mol ratio)) that forms 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 (Na:0.81, K:0.09), 2% aqueous solution viscosity (Brookfield) 950mPa; Purity 99.8%; Raw material CMC (FM9 type, DS=0.90,1% aqueous solution viscosity (Brookfield) 800mPa; Purity 98.8%) contain same K, 1%wt aqueous solution viscosity (Brookfield) 720mPa.

Claims (5)

1. the working method of a low CMC (Sodium Carboxymethyl Cellulose) BP/USP sodium is characterized in that comprising the steps:
The first step is with the H of mass concentration 10～40% 2SO 4The aqueous solution adds in the raw material, H 2SO 4The amount ratio of the aqueous solution and raw material is 4～16 liters: 1 kilogram; Said raw material is a food grade Xylo-Mucine finished product;
Second step, 10～40 ℃ of insulations 2～10 hours separate, and the solid that obtains separates with pH=1～3,0～30 ℃ water washing;
The 3rd step, second solid that obtain of step added pH=7.5～8 that neutralize, ground caustic end under protection of inert gas, and 25～35 ℃ of temperature are incubated 1～6 hour, and said alkali is according to parts by weight Na 2CO 385～98 parts, K 2CO 31.5～14 parts, (NH 4) 2CO 30.5 the mixture of～1.5 parts of compositions, the ethyloic mol ratio in alkali and the raw material is 1: 2;
The 4th the step the 3rd the step obtain solid dewater, dry, pulverize product.
2. the working method of low CMC (Sodium Carboxymethyl Cellulose) BP/USP sodium 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. the working method of low CMC (Sodium Carboxymethyl Cellulose) BP/USP sodium according to claim 2 is characterized in that, the solid water cut quality that second step obtained at last is 55～65%.
4. the working method of low CMC (Sodium Carboxymethyl Cellulose) BP/USP sodium according to claim 3 is characterized in that, said rare gas element is helium or argon gas or adopts high pure nitrogen to replace.
5. according to the working method of each described low CMC (Sodium Carboxymethyl Cellulose) BP/USP sodium of claim 1～4, it is characterized in that said food grade Xylo-Mucine is FH6 type, FH9 type, FVH9 type or FM9 type.
CN2010102997079A 2010-09-30 2010-09-30 Production method of sodium carboxymethyl cellulose with low sodium content Expired - Fee Related CN101967231B (en)

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CN104458610A (en) * 2014-11-27 2015-03-25 华南理工大学 Method for determining degree of substitution of water soluble food grade sodium carboxymethylcellulose by assistance of ultrasonic waves
CN104459014A (en) * 2014-11-27 2015-03-25 华南理工大学 Method for determining degree of substitution of sodium carboxymethylcellulose
CN104459013A (en) * 2014-11-27 2015-03-25 华南理工大学 Method for testing degree of substitution of low-sodium sodium carboxymethylcellulose
CN110214932B (en) * 2019-06-11 2022-02-15 华南理工大学 High-temperature-resistant sodium carboxymethyl cellulose and preparation method thereof

Citations (5)

* Cited by examiner, † Cited by third party
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
CN101280023A (en) * 2008-01-31 2008-10-08 重庆力宏精细化工有限公司 Preparation of acid-resistant sodium carboxymethylcellulose
CN101475696A (en) * 2008-12-09 2009-07-08 丹尼斯克（张家港）亲水胶体有限公司 Process for preparing high viscosity sodium carboxymethylcellulose
CN101548732A (en) * 2008-04-03 2009-10-07 上海长光企业发展有限公司 Preparation method for low-viscosity sodium carboxymethyl cellulose for foodstuff
CN101942028A (en) * 2010-09-30 2011-01-12 华南理工大学 Method for producing potassium carboxymethylcellulose

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1144756A1 (en) * 1998-12-30 2001-10-17 Kimberly-Clark Worldwide, Inc. Kraft wood fibers for carboxyalkyl cellulose

Patent Citations (5)

* Cited by examiner, † Cited by third party
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
CN101280023A (en) * 2008-01-31 2008-10-08 重庆力宏精细化工有限公司 Preparation of acid-resistant sodium carboxymethylcellulose
CN101548732A (en) * 2008-04-03 2009-10-07 上海长光企业发展有限公司 Preparation method for low-viscosity sodium carboxymethyl cellulose for foodstuff
CN101475696A (en) * 2008-12-09 2009-07-08 丹尼斯克（张家港）亲水胶体有限公司 Process for preparing high viscosity sodium carboxymethylcellulose
CN101942028A (en) * 2010-09-30 2011-01-12 华南理工大学 Method for producing potassium carboxymethylcellulose

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