CN101585883A - High-purity sodium carboxymethyl starch, preparation method thereof and application thereof - Google Patents
High-purity sodium carboxymethyl starch, preparation method thereof and application thereof Download PDFInfo
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Abstract
The invention discloses high-purity sodium carboxymethyl starch, a preparation method thereof and application thereof. Mainly during basification and etherification of starch in a reaction kettle, the stable reaction temperature, stirring time and stirring speed are strictly kept; and after an organic solvent is added into the starch, a semi-powder semi-grain product is completely stirred and fully dispersed in the organic solvent, and the solvent is removed to form a powder product. The purity of the prepared sodium carboxymethyl starch is as high as 90 to 99 percent, the substitution value is as high as 1.3 to 1.9, and the application fields of dye printing, spinning, food, papermaking, ceramics, petroleum and the like are enlarged.
Description
Technical field
The invention belongs to the macromolecular material field of fine chemical, especially relate to the preparation and the application of high-purity sodium carboxymethyl starch.
Background technology
Along with the development of Chinese national economy, the purposes of sodium starch glycolate is more and more wider, and annual requirement constantly increases.Can be used as emulsifying agent, thickening material, dispersion agent, stablizer, sizing agent, membrane-forming agent, water-holding agent etc., be applied in industrial circles such as oil, weaving, daily use chemicals, cigarette, papermaking, building, food, medicine.
Traditional Preparation of sodium carboxymethy starch technology generally is that disposable the putting into fully of NaOH made sodium hydroxide solution in the solvent, again starch is dropped in the NaOH solution earlier through the alkalization process, and then adding etherifying agent-Mono Chloro Acetic Acid carries out the reaction of carboxymethyl chemical combination, add acetic acid at last and neutralize, obtain product after the drying treatment.According to solvent medium difference used in the alkalization process, be divided into water-soluble matchmaker's method, organic solvent method, half method such as method, solid method admittedly.
All there is weak point in the whole bag of tricks of above-mentioned preparation Xylo-Mucine, particularly mainly shows the following aspects:
(1) water-soluble matchmaker's method
,, then add sodium hydroxide and alkalize during at water owing to add starch aborning earlier as reaction medium, and add Mono Chloro Acetic Acid and carry out etherification reaction, there is not washing process, so the product saltiness height that obtains, and trivial operations, the etherifying agent utilization ratio is low, and productive rate is not high yet.
(2) organic solvent method
Because starch all uses low-carbon alcohol as solvent and media in alkalization and etherification reaction, be particulate state so make product, and solvent-oil ratio is big, drying time is long, material color Huang, production cost height.
(3) half consolidates method
As reaction medium, starch and the alcohol back that stirs is added alkali lye with a small amount of alcohol, add Mono Chloro Acetic Acid then and react, reacted postcooling, after vacuum-drying, make product.The crude product that this method produces is more, reacts inhomogeneous, unstable properties.
(4) solid method
Liquid caustic soda is sprayed in starch by the prescription requirement, in kneader, mediate evenly, obtain the starch that alkalizes, with Mono Chloro Acetic Acid generation etherification reaction, make product again.This method technological process is simple, reacts not really even, and substitution value is low, and product produces bigger consumption in crushing process, increases cost.
By the purity of the Xylo-Mucine of above-mentioned prepared be about 75%, substitution value is about 1.0, the product yield ratio of the sodium starch glycolate product that goes out (amount of starch of knocking down with) 0.85, Xylo-Mucine per ton consume about solvent 75KG.Because purity is low, so application industry is restricted, just can't use as industries such as printing and dyeing, oil.
Summary of the invention
One of purpose of the present invention is the deficiency that overcomes above-mentioned sodium starch glycolate preparation technology, improves on traditional sodium starch glycolate preparation technology's basis, and a kind of permanent formula graded response production method of high-purity sodium carboxymethyl starch is provided.
Another object of the present invention provides a kind of high-purity sodium carboxymethyl starch by this prepared.
The present invention provides the application of this high-purity sodium carboxymethyl starch simultaneously.
For achieving the above object, the preparation technology of high-purity sodium carboxymethyl starch of the present invention is as follows: comprise traditional alkalization, etherificate and N-process, it is characterized in that, adopted permanent formula graded response technology method in said process.
So-called permanent formula graded response technology method is, starch in reactor, alkalize and etherification procedure in, strictly keep stable temperature of reaction, churning time and stirring velocity; After adding organic solvent, half powder, half granular product fully stirred be scattered in fully in the organic solvent, slough solvent and form powder-like product.
Concrete steps of the present invention are as follows:
The first step: implantation concentration is 160～180 parts of 90% ethanol in reactor, drops into NaOH40～45 part simultaneously, is warming up to 30～40 ℃, and continuously stirring 15～30min makes sodium hydroxide solution under the constant temperature;
Second step: get 120-130 part starch and drop in the aforesaid reaction vessel with the moistening back of soft water, continuously stirring 60min under 30～40 ℃ of constant temperatures alkalizes;
The 3rd step: after having alkalized, vacuumizing and drop into concentration in reactor is 30～40 parts of 95% Mono Chloro Acetic Acids, continuously stirring 20min, be warmed up to 54 ± 1 ℃ of constant temperature continuously stirring 30～40min then and carry out etherification reaction one time, be warming up to 65 ± 1 ℃ again, constant temperature continuously stirring 50～60min carries out the secondary etherification reaction;
The 4th step: after etherification reaction is intact, when being cooled to 30～40 ℃, add concentration again and be acetic acid 5-8 part of 50%, stir 15-25min and carry out neutralization reaction, make the pH value reach 6.5～7.5, discharging is then sloughed solvent by whizzer after the discharging and is obtained half powder, half granular material;
The 5th step: the 4th half powder, half granular material that obtain of step is dropped into another, and to be marked with 170～190 parts of concentration be in the 80% alcoholic acid reactor, agitator treating 30～45min, half powder, half granular material is scattered in the ethanol fully, sloughs solvent through whizzer then, oven dry obtains finished product.
Above-mentioned umber all refers to parts by weight.
The preferred version of above-mentioned preparation high-purity sodium carboxymethyl starch production method is:
The first step: implantation concentration is 170 parts of 90% ethanol in reactor, drops into 42 parts of NaOH simultaneously, is warming up to 40 ℃, and continuously stirring 15min makes NaOH solution under the constant temperature;
Second step: get 125 parts of starch and drop in the reactor with the moistening back of soft water, continuously stirring 60min under 30 ℃ of constant temperatures alkalizes;
The 3rd step: after having alkalized, vacuumizing and drop into concentration in reactor is 35 parts of 95% Mono Chloro Acetic Acids, and continuously stirring 20min is warmed up to 54 ± 1 ℃ of constant temperature continuously stirring 40min then and carries out etherification reaction one time, be warming up to 65 ± 1 ℃ again, constant temperature continuously stirring 55min carries out the secondary etherification reaction;
The 4th step: after etherification reaction is intact, when being cooled to 30 ℃, add concentration again and be 5.5 parts of 50% acetic acid, stir 20min and carry out neutralization reaction, make the pH value reach 7.0, discharging is then sloughed solvent by whizzer after the discharging and is obtained granular material;
The 5th step: the 4th half powder, half granular material that obtain of step is dropped into another, and to be marked with 190 parts of concentration be in the 80% alcoholic acid reactor, agitator treating 45min, half powder, half granular material is scattered in the ethanol fully, sloughs solvent through whizzer then, oven dry obtains finished product.
Two above-mentioned reactors are plough formula reactor, and the reaction stirring velocity is 120 rev/mins.
Up to 90-99%, substitution value is up to 1.3-1.9 by the sodium starch glycolate purity of above-mentioned prepared.Be applied in fields such as printing and dyeing, weaving, food, papermaking, pottery, oil.
Advantage of the present invention is:
(1) on the basis that traditional technology is produced with organic solvent, adopt plough formula reactor to react, be provided with the fly cutter that runs up in this reactor, have crushing effect, the granular material that is produced is carried out high-speed stirring, make material fully stirred with grinding dispersion in organic solvent, centrifugal drying directly obtains powder-like product, has improved reaction efficiency, reduce the pulverizing process link, greatly reduced production cost.
(2) starch that is adopted reacts more abundant in advance with the moistening pulpous state that is mixed with of soft water in alkalization and etherification procedure, has avoided particulate to produce in a large number.
(3) alkalization and etherification reaction process are to carry out in a reactor, and the workman is simple to operate.
(4) increased advanced desolventizing equipment (G-500 whizzer) and carried out precipitation, dry again behind the precipitation, the production time is short, has improved working efficiency.And the organic solvent of not participating in reaction in the production process can recycle, has reduced solvent consumption, and energy consumption is low, does not have the discharging of " three wastes ".
(5) reacted slough solvent after, increased washing step, remove byproduct of reaction sodium-chlor, sodium-acetate etc., improved the purity of product greatly, enlarged Application Areas, such as printing and dyeing, food etc.
Advantages such as the high-purity methyl Starch Sodium that technical solution of the present invention is produced is by detecting, and up to 1.3-1.9, product yield is up to about 2.0 up to 90-99%, substitution value for purity, and consumption solvent per ton is only about 40KG, and application industry is wider.
The high-purity sodium carboxymethyl starch that the present invention produces is the water-soluble ionic-type functional polymer that starch is made through etherification reaction, has multiple functions such as chelating, ion-exchange, flocculation, thickening, emulsification, suction, adhesion.Use and test through too much tame unit, verify that this product has multiple functions such as thickening, emulsification, chelating and flocculation, is widely used in fields such as oil, coating, washing composition, building materials, weaving, papermaking, medicine, food, pottery, printing and dyeing.
Embodiment
Below in conjunction with embodiment the present invention is done more detailed description, but be not limited thereto.
Embodiment 1
Carry out the preparation that following step is carried out high-purity sodium carboxymethyl starch successively:
The first step: implantation concentration is 160 parts of 90% ethanol in reactor, drops into 40 parts of NaOH simultaneously, is warming up to 35 ℃, and continuously stirring 15min makes NaOH solution under the constant temperature;
Second step: get 120 parts of starch and drop in the reactor with the moistening back of soft water, continuously stirring 60min under 35 ℃ of constant temperatures alkalizes;
The 3rd step: after having alkalized, vacuumizing and drop into concentration in reactor is 30 parts of 95% Mono Chloro Acetic Acids, and continuously stirring 20min is warmed up to 54 ± 1 ℃ of constant temperature continuously stirring 35min then and carries out etherification reaction one time, be warming up to 65 ± 1 ℃ again, constant temperature continuously stirring 50min carries out the secondary etherification reaction;
The 4th step: after etherification reaction is intact, when being cooled to 30 ℃, add concentration again and be 5 parts of 50% acetic acid, stir 15min and carry out neutralization reaction, making the pH value is discharging in 7.5 o'clock, sloughs solvent by whizzer after the discharging and obtains half powder, half granular material;
The 5th step: the 4th half powder, half granular material that obtain of step is dropped into another, and to be marked with 170 parts of concentration be in the 80% alcoholic acid reactor, agitator treating 30min, half powder, half granular material is scattered in the ethanol fully, sloughs solvent through whizzer then, oven dry obtains finished product.
Embodiment 2
Carry out the preparation that following step is carried out high-purity sodium carboxymethyl starch successively:
The first step: implantation concentration is 170 parts of 90% ethanol in reactor, drops into 43 parts of NaOH simultaneously, is warming up to 35 ℃, and continuously stirring 18min makes NaOH solution under the constant temperature;
Second step: get 125 parts of starch and drop in the reactor with the moistening back of soft water, continuously stirring 60min under 34 ℃ of constant temperatures alkalizes;
The 3rd step: after having alkalized, vacuumizing and drop into concentration in reactor is 35 parts of 95% Mono Chloro Acetic Acids, and continuously stirring 20min is warmed up to 54 ± 1 ℃ of constant temperature continuously stirring 40min then and carries out etherification reaction one time, be warming up to 65 ± 1 ℃ again, constant temperature continuously stirring 52min carries out the secondary etherification reaction;
The 4th step: after etherification reaction is intact, when being cooled to 35 ℃, add concentration again and be 6 parts of 50% acetic acid, stir 15min and carry out neutralization reaction, making the pH value is 6.8, and discharging is then sloughed solvent by whizzer after the discharging and obtained half powder, half granular material;
The 5th step: the 4th half powder, half granular material that obtain of step is dropped into another, and to be marked with 180 parts of concentration be in the 80% alcoholic acid reactor, agitator treating 45min, half powder, half granular material is dissolved in the ethanol fully, sloughs solvent through whizzer then, oven dry obtains finished product.
Embodiment 3
Carry out the preparation that following step is carried out high-purity sodium carboxymethyl starch successively:
The first step: implantation concentration is 175 parts of 90% ethanol in reactor, drops into 45 parts of NaOH simultaneously, is warming up to 30 ℃, and continuously stirring 25min makes NaOH solution under the constant temperature;
Second step: get 130 parts of starch and drop in the reactor with the moistening back of soft water, continuously stirring 60min under 40 ℃ of constant temperatures alkalizes;
The 3rd step: after having alkalized, vacuumizing and drop into concentration in reactor is 40 parts of 95% Mono Chloro Acetic Acids, and continuously stirring 20min is warmed up to 54 ± 1 ℃ of constant temperature continuously stirring 40min then and carries out etherification reaction one time, be warming up to 65 ± 1 ℃ again, constant temperature continuously stirring 60min carries out the secondary etherification reaction;
The 4th step: after etherification reaction is intact, when being cooled to 30 ℃, add concentration again and be 7 parts of 50% acetic acid, stir 20min and carry out neutralization reaction, making the pH value is 6.5, and discharging is then sloughed solvent by whizzer after the discharging and obtained half powder, half granular material;
The 5th step: the 4th half powder, half granular material that obtain of step is dropped into another, and to be marked with 190 parts of concentration be in the 80% alcoholic acid reactor, agitator treating 45min, half powder, half granular material is scattered in the ethanol fully, sloughs solvent through whizzer then, oven dry obtains finished product.
Embodiment 4
Carry out the preparation that following step is carried out high-purity sodium carboxymethyl starch successively:
The first step: implantation concentration is 180 parts of 90% ethanol in reactor, drops into 45 parts of NaOH simultaneously, is warming up to 30 ℃, and continuously stirring 15min makes NaOH solution under the constant temperature;
Second step: get 128 parts of starch and drop in the reactor with the moistening back of soft water, continuously stirring 60min under 40 ℃ of constant temperatures alkalizes;
The 3rd step: after having alkalized, vacuumizing and drop into concentration in reactor is 38 parts of 95% Mono Chloro Acetic Acids, and continuously stirring 20min is warmed up to 54 ± 1 ℃ of constant temperature continuously stirring 40min then and carries out etherification reaction one time, be warming up to 65 ± 1 ℃ again, constant temperature continuously stirring 55min carries out the secondary etherification reaction;
The 4th step: after etherification reaction is intact, when being cooled to 32 ℃, add 7 parts of the acetic acid of concentration 50% again, stir 25min and carry out neutralization reaction, making the pH value is 6.5, and discharging is then sloughed solvent by whizzer after the discharging and obtained half powder, half granular material;
The 5th step: the 4th half powder, half granular material that obtain of step is dropped into another, and to be marked with 190 parts of concentration be in the 80% alcoholic acid reactor, agitator treating 30min, granular material is scattered in the ethanol fully, sloughs solvent through whizzer then, oven dry obtains finished product.
Claims (6)
1, a kind of preparation method of high-purity sodium carboxymethyl starch, it comprises alkalization, etherificate and N-process, it is characterized in that, has adopted permanent formula graded response technology in said process.
2, the preparation method of high-purity sodium carboxymethyl starch as claimed in claim 1, it is characterized in that, described permanent formula graded response technology is, starch in reactor, alkalize and etherification procedure in, strictly keep stable temperature of reaction, churning time and stirring velocity; After adding organic solvent, half powder, half granular product fully stirred be scattered in fully in the organic solvent, slough solvent and form powder-like product.
3, the preparation method of high-purity sodium carboxymethyl starch as claimed in claim 1 or 2 is characterized in that, this method may further comprise the steps:
The first step: implantation concentration is 160～180 parts of 90% ethanol in reactor, drops into NaOH40～45 part simultaneously, is warming up to 30～40 ℃, and continuously stirring 15～30min makes sodium hydroxide solution under the constant temperature;
Second step: get 120-130 part starch and drop in the aforesaid reaction vessel with the moistening back of soft water, continuously stirring 60min under 30～40 ℃ of constant temperatures alkalizes;
The 3rd step: after having alkalized, vacuumizing and drop into concentration in reactor is 30～40 parts of 95% Mono Chloro Acetic Acids, continuously stirring 20min, be warmed up to 54 ± 1 ℃ of constant temperature continuously stirring 30～40min then and carry out etherification reaction one time, be warming up to 65 ± 1 ℃ again, constant temperature continuously stirring 50～60min carries out the secondary etherification reaction;
The 4th step: after etherification reaction is intact, when being cooled to 30～40 ℃, add concentration again and be acetic acid 5-8 part of 50%, stir 15-25min and carry out neutralization reaction, make the pH value reach 6.5～7.5, discharging is then sloughed solvent by whizzer after the discharging and is obtained half powder, half granular material;
The 5th step: the 4th half powder, half granular material that obtain of step is dropped into another, and to be marked with 170～190 parts of concentration be in the 80% alcoholic acid reactor, agitator treating 30～45min, half powder, half granular material is scattered in the ethanol fully, sloughs solvent through whizzer then, oven dry obtains finished product;
Above-mentioned umber all refers to parts by weight;
Above-mentioned two reactors are plough formula reactor, and the reaction stirring velocity is 120 rev/mins.
4, the preparation method of high-purity sodium carboxymethyl starch as claimed in claim 3 is characterized in that, this method may further comprise the steps:
The first step: implantation concentration is 170 parts of 90% ethanol in reactor, drops into 42 parts of NaOH simultaneously, is warming up to 40 ℃, and continuously stirring 15min makes NaOH solution under the constant temperature;
Second step: get 125 parts of starch and drop in the reactor with the moistening back of soft water, continuously stirring 60min under 30 ℃ of constant temperatures alkalizes;
The 3rd step: after having alkalized, vacuumizing and drop into concentration in reactor is 35 parts of 95% Mono Chloro Acetic Acids, and continuously stirring 20min is warmed up to 54 ± 1 ℃ of constant temperature continuously stirring 40min then and carries out etherification reaction one time, be warming up to 65 ± 1 ℃ again, constant temperature continuously stirring 55min carries out the secondary etherification reaction;
The 4th step: after etherification reaction is intact, when being cooled to 30 ℃, add concentration again and be 5.5 parts of 50% acetic acid, stir 20min and carry out neutralization reaction, make the pH value reach 7.0, discharging is then sloughed solvent by whizzer after the discharging and is obtained granular material;
The 5th step: the 4th half powder, half granular material that obtain of step is dropped into another, and to be marked with 190 parts of concentration be in the 80% alcoholic acid reactor, agitator treating 45min, half powder, half granular material is scattered in the ethanol fully, sloughs solvent through whizzer then, oven dry obtains finished product;
Above-mentioned umber all refers to parts by weight;
Two above-mentioned reactors are plough formula reactor, and the reaction stirring velocity is 120 rev/mins.
5, a kind of high-purity sodium carboxymethyl starch by the preparation of claim 1 method is characterized in that its purity is 90-99%, and substitution value is 1.3-1.9.
6, by the high-purity sodium carboxymethyl starch of claim 1 method preparation in the application in printing and dyeing, weaving, food, papermaking, pottery and oil field.
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| CN102153664A (en) * | 2011-01-17 | 2011-08-17 | 温州大学 | Method for preparing nanometer lamellar sodium carboxymethyl starch |
| CN102229675A (en) * | 2011-05-19 | 2011-11-02 | 湖北达雅化工技术发展有限公司 | Preparation method of food grade high viscosity sodium carboxymethyl starch |
| CN102311507A (en) * | 2011-06-28 | 2012-01-11 | 郑桂富 | Preparation method of pharmaceutical adjuvant sodium carboxymethyl starch |
| CN102746409A (en) * | 2012-06-18 | 2012-10-24 | 新疆光大山河化工科技有限公司 | Preparation method of super sodium carboxymethyl starch |
| CN103450364A (en) * | 2013-09-03 | 2013-12-18 | 华中农业大学 | High-substitution-degree carboxymethyl starch and composite hydrogel thereof, and preparation method and application of carboxymethyl starch and composite hydrogel thereof |
| CN103554282A (en) * | 2012-12-07 | 2014-02-05 | 新疆光大山河化工科技有限公司 | Highly substituted carboxymethyl starch sodium preparation method |
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| CN110330572A (en) * | 2019-08-12 | 2019-10-15 | 山东六佳药用辅料股份有限公司 | A kind of production technology of low spot rapid disintegrating agent carboxymethyl sodium starch |
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| CN102153664B (en) * | 2011-01-17 | 2013-11-06 | 温州大学 | Method for preparing nanometer lamellar sodium carboxymethyl starch |
| CN102153664A (en) * | 2011-01-17 | 2011-08-17 | 温州大学 | Method for preparing nanometer lamellar sodium carboxymethyl starch |
| CN102229675B (en) * | 2011-05-19 | 2012-11-28 | 湖北达雅化工技术发展有限公司 | Preparation method of food grade high viscosity sodium carboxymethyl starch |
| CN102229675A (en) * | 2011-05-19 | 2011-11-02 | 湖北达雅化工技术发展有限公司 | Preparation method of food grade high viscosity sodium carboxymethyl starch |
| CN102311507B (en) * | 2011-06-28 | 2012-10-24 | 郑桂富 | Preparation method of pharmaceutical adjuvant sodium carboxymethyl starch |
| CN102311507A (en) * | 2011-06-28 | 2012-01-11 | 郑桂富 | Preparation method of pharmaceutical adjuvant sodium carboxymethyl starch |
| CN102746409A (en) * | 2012-06-18 | 2012-10-24 | 新疆光大山河化工科技有限公司 | Preparation method of super sodium carboxymethyl starch |
| CN103554282A (en) * | 2012-12-07 | 2014-02-05 | 新疆光大山河化工科技有限公司 | Highly substituted carboxymethyl starch sodium preparation method |
| CN103554282B (en) * | 2012-12-07 | 2017-06-30 | 新疆光大山河化工科技有限公司 | The preparation method of substituted carboxymethyl starch sodium high |
| CN103450364A (en) * | 2013-09-03 | 2013-12-18 | 华中农业大学 | High-substitution-degree carboxymethyl starch and composite hydrogel thereof, and preparation method and application of carboxymethyl starch and composite hydrogel thereof |
| CN103450364B (en) * | 2013-09-03 | 2016-03-16 | 华中农业大学 | Carboxymethyl starch with high substitution degree and composite aquogel, preparation method and application |
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| CN110330572A (en) * | 2019-08-12 | 2019-10-15 | 山东六佳药用辅料股份有限公司 | A kind of production technology of low spot rapid disintegrating agent carboxymethyl sodium starch |
| CN112029486A (en) * | 2020-11-03 | 2020-12-04 | 胜利油田钻井飞龙泥浆技术服务有限公司 | Preparation method of environment-friendly degradable high-temperature-resistant salt-resistant anti-collapse filtrate reducer |
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|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C56 | Change in the name or address of the patentee |
Owner name: SHANDONG YITENG NEW MATERIAL STOCK CO., LTD. Free format text: FORMER NAME: SHANDONG YITENG CHEMICAL CO. LTD. |
|
| CP01 | Change in the name or title of a patent holder |
Address after: 271600, Shandong Feicheng hi tech Development Zone Industrial two West Road, the first Shandong Teng Chemical Co., Ltd. Patentee after: Shandong Yiteng New Material Stock Co., Ltd. Address before: 271600, Shandong Feicheng hi tech Development Zone Industrial two West Road, the first Shandong Teng Chemical Co., Ltd. Patentee before: Shandong Yiteng Chemicals Co., Ltd. |