CN102153662A - Method for producing low-sodium sodium carboxymethylcellulose by microwaves - Google Patents
Method for producing low-sodium sodium carboxymethylcellulose by microwaves Download PDFInfo
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- CN102153662A CN102153662A CN 201110041598 CN201110041598A CN102153662A CN 102153662 A CN102153662 A CN 102153662A CN 201110041598 CN201110041598 CN 201110041598 CN 201110041598 A CN201110041598 A CN 201110041598A CN 102153662 A CN102153662 A CN 102153662A
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Abstract
The invention discloses a method for producing low-sodium sodium carboxymethylcellulose by microwaves. The method comprises the following steps of: puffing a raw material, adding acid solution, processing by microwaves, reacting at a certain temperature, separating to remove centrifugate, adding alkali, processing by microwaves, dehydrating, drying and crushing to obtain a product. By the method, the high-quality low-sodium sodium carboxymethylcellulose can be obtained. The method is energy-saving, time-saving and easy and convenient to operate, and the obtained product has the characteristics of high performance and stable quality among batches.
Description
Technical field
The present invention relates to the production method of low CMC (Sodium Carboxymethyl Cellulose) BP/USP sodium, specifically is the method that a kind of microwave is used to produce 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, simultaneously 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 beverage, milk preparation, ice-creams, soy sauce, jelly, jam, instant noodles of modern food industry.Standard GB 2760-2007 classifies it as: can need an amount of additive list (A3,53) that uses by producing in varieties of food items, 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.
Human body is not only taken in sodium ion by salt, and additive (as Sodium Benzoate, Sodium Glutamate, Xylo-Mucine, sodium alginate etc.) contains a large amount of sodium ions equally and also absorbed by human body.Effective way is suitably to reduce the intake of sodium salt on the one hand; Increase the amount of sylvite in the food on the other hand, thereby reduce 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.
CMC is a weak polyelectrolyte, one of feature 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.
Summary of the invention
The objective of the invention is at the deficiencies in the prior art, provide a kind of microwave to be used to produce the method for low CMC (Sodium Carboxymethyl Cellulose) BP/USP sodium, can effectively improve the production efficiency of low CMC (Sodium Carboxymethyl Cellulose) BP/USP sodium, have energy-conservation, save time, its ratio of viscosities of product simple, convenient, that obtain contains same potassium amount (raw material CMC+KCl) height, has the performance height, stay-in-grade characteristics between batch.
A kind of microwave is used to produce the method for low CMC (Sodium Carboxymethyl Cellulose) BP/USP sodium, comprises the steps:
The first step raw material adding mass concentration is 10-40% H
2SO
4The aqueous solution, H
2SO
4The amount ratio of the aqueous solution and raw material is the 4-16 liter: 1 kilogram, described raw material is food grade Xylo-Mucine or purifying food grade Xylo-Mucine not;
The second step batch microwave was handled 1～5 minute, and the microwave treatment power density is 0.1～0.5 kW/m
3, handled 0.5～5 minute at every turn, in 10 ~ 40 ℃ of insulations 0.5 ~ 1 hour, separate after the microwave treatment, solid separates obtaining solid with pH=1～3,0～30 ℃ water washing;
The solid that second step of the 3rd step obtains, microwave treatment 0.1～3 minute, microwave treatment power density are 0.1～0.5 kW/m
3, adding the ground caustic end, pH=7.5 ~ 8 again neutralize; Carry out, separate;
The 4th step solid that obtains of the 3rd step dewater, dry, pulverize product.
Above-mentioned microwave is used to produce the method for low CMC (Sodium Carboxymethyl Cellulose) BP/USP sodium, and in the first step, add and carry out protection of inert gas before the acid and handle, be to outgas 5 ~ 20 minutes 0.05 ~ 0.10 MPa under in vacuum tightness, charge into rare gas element.
Above-mentioned microwave is used to produce the method for low CMC (Sodium Carboxymethyl Cellulose) BP/USP sodium, and the described intermittent time in second step is 1 ~ 3 minute, and the moisture massfraction of solid that the last separation of second step obtains is 55 ~ 65%.
Above-mentioned microwave is used to produce the method for low CMC (Sodium Carboxymethyl Cellulose) BP/USP sodium, carries out described microwave treatment in the 3rd step under protection of inert gas, and 25 ~ 35 ℃ of insulations of temperature are 0.1 ~ 0.5 hour after the microwave treatment, and described ground caustic end is by Na according to parts by weight
2CO
385 ~ 98 parts, K
2CO
31.5 ~ 14 parts, (NH
4)
2CO
30.5 the mixture of ~ 1.5 parts of compositions, the mol ratio of carboxymethyl is 1:2 in alkali and the raw material.
Above-mentioned microwave is used to produce the method for low CMC (Sodium Carboxymethyl Cellulose) BP/USP sodium, and described food grade Xylo-Mucine is FH6 type, FH9 type, FVH9 type or FM9 type, and microwave frequency is that national Specification uses.Prepared product viscosity is greater than the KCl that directly adds same amount in its raw material.
Above-mentioned microwave is used to produce the method for low CMC (Sodium Carboxymethyl Cellulose) BP/USP sodium, and described rare gas element is nitrogen, helium or argon gas.Be applicable to that same batch raw material of the present invention is little to the quality influence of the finished product, the raw material of different batches produces considerable influence to the quality of the finished product.The microwave treatment technology that the present invention adopts is the no gradient-heated effect that has of utilizing microwave, the protection of inert gas technology of employing, and make that under the processing condition that limited product has the performance height, steady quality between batch.
Generally speaking, the present invention compared with prior art has following advantage:
1 obtain batch between steady quality, low CMC (Sodium Carboxymethyl Cellulose) BP/USP sodium that quality is high, its viscosity is greater than the KCl that directly adds same amount in its raw material (food grade Xylo-Mucine or not purifying food grade Xylo-Mucine);
2 because use microwave treatment technology is energy-conservation, saves time;
3 equipment washing and simple, convenient.
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%) 65g, and vacuum tightness is that 0.05 MPa outgased 5 minutes down, charges into nitrogen, adds the H of mass concentration 10%
2SO
4Aqueous solution 1040mL;
The second step microwave treatment 1 minute, the microwave treatment power density is 0.5 kW/m
3, 3 minutes intermittences, microwave treatment was 2 times, each 0.5 minute; 10 ℃ are incubated 1 hour, separate, and solid pH=1,0 ℃ of water washing separates, and obtains the solid that water content is 55%wt;
The solid that second step of the 3rd step obtains carries out under nitrogen protection, and microwave treatment 0.1 minute, microwave treatment power density are 0.5 kW/m
3, 25 ℃ of temperature of reaction add Na
2CO
385 parts, K
2CO
314 parts, (NH
4)
2CO
31.5 part alkali mix powder 10.7g(alkali of forming: the carboxymethyl in the raw material is the 1:2(mol ratio)), be incubated 0.5 hour pH=7.5, separate;
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% aqueous solution viscosity (Brookfield) 360mPa, purity 99.8%.In the same time, there is not the not dissolving fully of product of microwave treatment, can't carry out viscosity measurement.Raw material CMC(FH6 type, DS=0.62,1% 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 that 0.10 MPa outgased 20 minutes down, charges into nitrogen, adds the H of mass concentration 40%
2SO
4Aqueous solution 260mL;
The second step microwave treatment 5 minutes, the microwave treatment power density is 0.1kW/m
3Intermittently 1 minute microwave treatment is 5 times, and each 1 minute, 40 ℃ of insulations 0.5 hour separated, solid pH=3, and 30 ℃ of water washings, separation obtains water content and is 65% solid;
The solid that second step of the 3rd step obtains carries out under nitrogen protection, and microwave treatment 3 minutes, microwave treatment power density are 0.1 kW/m
3, 35 ℃ of temperature of reaction add Na
2CO
385 parts, K
2CO
314 parts, (NH
4)
2CO
31.5 part alkali mix powder 9.5g(alkali of forming: the carboxymethyl in the raw material is the 1:2(mol ratio)), be incubated 0.5 hour, pH=8.0 separates;
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) 355mPa, purity 98.9% in the same time, does not have the not dissolving fully of product of microwave treatment, can't carry out viscosity measurement.Raw material CMC(FH6 type, DS=0.62,2% aqueous solution viscosity (Brookfield) 50mPa, purity 85.0%) contain 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 0.05 MPa outgased 10 minutes down, charges into argon gas, adds the H of mass concentration 15%
2SO
4Aqueous solution 300mL;
The second step microwave treatment 4 minutes, the microwave treatment power density is 0.25 kW/m
3Intermittently 1.5 minutes microwave treatment are 4 times, and each 1 minute, 10 ℃ of insulations 1 hour separated, solid pH=1, and 10 ℃ of water washings, separation obtains water content and is 60% solid;
The solid that second step of the 3rd step obtains carries out under argon shield, and microwave treatment 2 minutes, microwave treatment power density are 0.25 kW/m
3, 30 ℃ of temperature of reaction add Na
2CO
398 parts, K
2CO
31.5 part, (NH
4)
2CO
30.5 part alkali mix powder 8.7g(alkali of forming: the carboxymethyl in the raw material is the 1:2(mol ratio)), be incubated 0.5 hour, pH=8.0 separates;
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) 480mPa, purity 99.8% in the same time, does not have the not dissolving fully of product of microwave treatment, can't carry out viscosity measurement.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 0.09 MPa outgased 15 minutes down, charges into argon gas, adds the H of mass concentration 15%
2SO
4Aqueous solution 500mL;
The second step microwave treatment 3 minutes, the microwave treatment power density is 0.2 kW/m
3Intermittently 1 minute microwave treatment is 3 times, and each 1 minute, 20 ℃ of insulations 0.7 hour separated, solid pH=1, and 20 ℃ of water washings, separation obtains water content and is 65% solid;
The solid that second step of the 3rd step obtains carries out under argon shield, and microwave treatment 3 minutes, microwave treatment power density are 0.1 kW/m
3, 20 ℃ of temperature of reaction add Na
2CO
390 parts, K
2CO
39.5 part, (NH
4)
2CO
30.5 part alkali mix powder 8.4g(alkali of forming: the carboxymethyl in the raw material is the 1:2(mol ratio)), be incubated 0.5 hour, pH=8.0 separates;
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) 960mPa, purity 99.8% in the same time, does not have the not dissolving fully of product of microwave treatment, can't carry out viscosity measurement.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 0.09 MPa outgased 15 minutes down, charges into argon gas, adds the H of mass concentration 15%
2SO
4Aqueous solution 500mL;
The second step microwave treatment 2 minutes, microwave treatment, power density are 0.4 kW/m
32 minutes microwave treatment intermittently, each 1 minute, 20 ℃ of insulations 0.5 hour separated, solid pH=1,20 ℃ of water washings, separation obtains water content and is 65% solid;
The solid that second step of the 3rd step obtains carries out under argon shield, and microwave treatment 2 minutes, microwave treatment power density are 0.1 kW/m
3, 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 of forming: the carboxymethyl in the raw material is the 1:2(mol ratio)), be incubated 0.1 hour, pH=8.0 separates;
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) 970mPa, purity 99.8% in the same time, does not have the not dissolving fully of product of microwave treatment, can't carry out viscosity measurement.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 (6)
1. the method that microwave is used to produce low CMC (Sodium Carboxymethyl Cellulose) BP/USP sodium is characterized in that comprising the steps:
The first step raw material adding mass concentration is 10-40% H
2SO
4The aqueous solution, H
2SO
4The amount ratio of the aqueous solution and raw material is the 4-16 liter: 1 kilogram, described raw material is food grade Xylo-Mucine or purifying food grade Xylo-Mucine not;
The second step batch microwave was handled 1～5 minute, and the microwave treatment power density is 0.1～0.5 kW/m
3, handled 0.5～5 minute at every turn, in 10 ~ 40 ℃ of insulations 0.5 ~ 1 hour, separate after the microwave treatment, solid separates with pH=1～3,0～30 ℃ water washing;
The solid that second step of the 3rd step obtains, microwave treatment 0.1～3 minute, microwave treatment power density are 0.1～0.5 kW/m
3, adding the ground caustic end, pH=7.5 ~ 8 again neutralize; Carry out, separate;
The 4th step solid that obtains of the 3rd step dewater, dry, pulverize product.
2. method according to claim 1 is characterized in that in the first step, adds to carry out protection of inert gas before the acid and handle, and be to outgas 5 ~ 20 minutes 0.05 ~ 0.10 MPa under in vacuum tightness, charge into rare gas element.
3. method according to claim 2 is characterized in that, the described intermittent time in second step is 1 ~ 3 minute, and the moisture massfraction of solid that the last separation of second step obtains is 55 ~ 65%.
4. method according to claim 3 is characterized in that, carries out described microwave treatment in the 3rd step under protection of inert gas, and 25 ~ 35 ℃ of insulations of temperature are 0.1 ~ 0.5 hour after the microwave treatment, and described ground caustic end is by Na according to parts by weight
2CO
385 ~ 98 parts, K
2CO
31.5 ~ 14 parts, (NH
4)
2CO
30.5 the mixture of ~ 1.5 parts of compositions, the mol ratio of carboxymethyl is 1:2 in alkali and the raw material.
5. method according to claim 4 is characterized in that described food grade Xylo-Mucine is FH6 type, FH9 type, FVH9 type or FM9 type.
6. according to each described method of claim 1 ~ 5, it is characterized in that described rare gas element is nitrogen, helium or argon gas.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN109836506A (en) * | 2017-11-29 | 2019-06-04 | 上海长光企业发展有限公司 | A kind of food-grade cellulose element glue and preparation method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2008247927A (en) * | 2007-03-02 | 2008-10-16 | Dai Ichi Kogyo Seiyaku Co Ltd | Carboxymethyl cellulose sodium salt having high yield value |
| CN101838349A (en) * | 2010-05-18 | 2010-09-22 | 华南理工大学 | Method for preparing carboxymethyl hemicellulose by microwave radiation |
| CN101942027A (en) * | 2010-09-30 | 2011-01-12 | 华南理工大学 | Method for producing sodium carboxymethyl cellulose (CMC) with low sodium by utilizing ultraphonic |
| CN101967233A (en) * | 2010-09-30 | 2011-02-09 | 华南理工大学 | Method for producing potassium carboxymethylcellulose by using ultrasonic |
-
2011
- 2011-02-21 CN CN2011100415985A patent/CN102153662B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2008247927A (en) * | 2007-03-02 | 2008-10-16 | Dai Ichi Kogyo Seiyaku Co Ltd | Carboxymethyl cellulose sodium salt having high yield value |
| CN101838349A (en) * | 2010-05-18 | 2010-09-22 | 华南理工大学 | Method for preparing carboxymethyl hemicellulose by microwave radiation |
| CN101942027A (en) * | 2010-09-30 | 2011-01-12 | 华南理工大学 | Method for producing sodium carboxymethyl cellulose (CMC) with low sodium by utilizing ultraphonic |
| CN101967233A (en) * | 2010-09-30 | 2011-02-09 | 华南理工大学 | Method for producing potassium carboxymethylcellulose by using ultrasonic |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN109836506A (en) * | 2017-11-29 | 2019-06-04 | 上海长光企业发展有限公司 | A kind of food-grade cellulose element glue and preparation method thereof |
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| CN102153662B (en) | 2012-10-31 |
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Application publication date: 20110817 Assignee: Shanghai Everest Fine Chemicals Co., Ltd. Assignor: South China University of Technology Contract record no.: 2014440000355 Denomination of invention: Method for producing low-sodium sodium carboxymethylcellulose by microwaves Granted publication date: 20121031 License type: Exclusive License Record date: 20140723 |
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