CN104774273A - Method for preparing phosphate ester starch slurry - Google Patents
Method for preparing phosphate ester starch slurry Download PDFInfo
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- CN104774273A CN104774273A CN201510173689.2A CN201510173689A CN104774273A CN 104774273 A CN104774273 A CN 104774273A CN 201510173689 A CN201510173689 A CN 201510173689A CN 104774273 A CN104774273 A CN 104774273A
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Abstract
The invention discloses a method for preparing phosphate ester starch slurry. The method comprises the following steps: adding water and native starch into a reactor, preparing starch milk of which the mass percentage concentration of the native starch is 10-15%, adding a phosphate esterification reagent which accounts for 5-15% of the mass of the native starch relatively and a composite catalyst which is equal to 2-5% of the weight of the starch into the starch milk under stirring conditions, adjusting a pH value to be 6.0-8.5, starting heating, controlling the temperature of the reactor to be 0-50 DEG C higher than the complete gelatinization temperature of corresponding native starch, and completing reaction to obtain slurry namely the phosphate ester starch slurry. The slurry disclosed by the invention can be directly used for warp sizing, ensures that a process of specifically producing phosphate ester starch in a starch factory can be removed, and ensures that the production cost can be greatly saved, production procedures can be simplified, and the pollution to the environment caused by wastewater discharged in a phosphate ester starch production process can be reduced.
Description
Technical field
The present invention relates to a kind of preparation method of starch ester derivative, especially a kind of method preparing phosphate ester starch slurry.
Background technology
In current textile industry, the phosphate ester starch that starch plants is produced normally directly bought by phosphate ester starch slurry, adds water and is mixed with certain density starch milk, after Heat Gelatinization, obtain the phosphate ester starch slurry that may be used for sizing technique.And starch plants can as adopted dry method or wet processing when producing phosphate ester starch, conventional wet processing is: in the starch milk of 35%-42%, add the urea of 15% phosphoric acid salt mixed thing of starch quality and 2% of starch quality as catalyzer, and reactant is mixed, at temperature 30-60 DEG C, pH value is under the condition of 5.0-6.5, reaction 3-10 hour, by reaction product solid-liquid separation, the abundant dispersed with stirring of sodium chloride aqueous solution adding 2.5% of 2 times amount in solid becomes emulsus, leave standstill again and soak 30min, solid-liquid separation again, solid repeats this process at least 6 times, finally use distilled water rinsing 3 times, phosphate ester starch is obtained after the solid drying finally obtained.This production process, production stage is loaded down with trivial details, and production cost is higher, and energy consumption is large, especially can discharge more acid-bearing wastewater, to environment in the last handling process of phosphoric acid acid esters starch.And phosphate ester starch prepares under lower than the gelatinization point of ative starch, during preparation, starch is graininess, and esterifying agent can be hindered to be diffused into starch granules inside, affects the reaction efficiency of esterifying agent and the substitution value of phosphate ester starch.
Summary of the invention
For above-mentioned prior art Problems existing, technical problem to be solved by this invention is to provide a kind of method preparing phosphate ester starch slurry.
For solving the problems of the technologies described above, the technical solution used in the present invention is: a kind of method preparing phosphate ester starch slurry, comprises the following steps:
A () adds water and ative starch (its chemical structure is identical with when being present in raw material with character) in the reactor, preparation ative starch mass percentage concentration is the starch milk of 10%-15%, and described ative starch is at least one in W-Gum, yam starch, tapioca (flour);
B () under agitation, the Phosphation reagent relative to ative starch quality 5%-15% and the composite catalyst being equivalent to starch weight 2%-5% is added in starch milk, described Phosphation reagent is at least one of tripoly phosphate sodium STPP, Trisodium trimetaphosphate or trisodium phosphate, described composite catalyst is urea and inferior sodium phosphate, and wherein the quality of urea is 0.5-2 times of inferior sodium phosphate quality;
C () adds acid for adjusting pH value between 6.0-8.5, open heating, controls temperature of reactor than the gelatinization of corresponding ative starch complete temperature height 0-50 DEG C, and maintains this temperature to reacting end.
In order to make to improve further the substitution value of the high and phosphate ester starch of reaction efficiency, the technical scheme further that the present invention adopts is: a kind of method preparing phosphate ester starch slurry, comprises the following steps:
A () adds water and ative starch (its chemical structure is identical with when being present in raw material with character) in the reactor, preparation ative starch mass percentage concentration is the starch milk of 12%-14%, and described ative starch is at least one in W-Gum, yam starch, tapioca (flour);
B () under agitation, the Phosphation reagent relative to ative starch quality 7%-10% and the composite catalyst being equivalent to starch weight 3%-4% is added in starch milk, described Phosphation reagent is at least one of tripoly phosphate sodium STPP, Trisodium trimetaphosphate or trisodium phosphate, described composite catalyst is urea and inferior sodium phosphate, and wherein the quality of urea is 1-1.5 times of inferior sodium phosphate quality;
C () adds dilute hydrochloric acid or dilute sulphuric acid adjust ph between 6.5-7.5, open heating, controls temperature of reactor than the gelatinization of corresponding ative starch complete temperature height 10-30 DEG C, and maintains this temperature to reacting end.
The inventive method compared with prior art, has following beneficial effect:
(1) sizing mixing of starch size to combine with the production of phosphate ester starch slurry by the present invention, achieve starch size size mixing and the one kettle way of production of phosphate ester starch slurry carries out the online production with phosphate ester starch slurry, the phosphate ester starch slurry obtained can be directly used in warp sizing, eliminate phosphate ester starch and carry out special process of producing at starch factory or slurry factory, significantly save production cost, simplify production process, alleviate the waste water that discharges in phosphate ester starch production process to the pollution of environment.
(2) because starch size is when phosphating reaction occurs, starch is in gelatinization state, and molecular chain fully stretches, and fully can contact with Phosphation reagent, improve the homogeneity of reaction, significantly improve the reaction efficiency of Phosphation reagent and the substitution value of phosphate ester starch.
Embodiment
Below by specific embodiment, the present invention is described in further detail, and the following stated is only the preferred embodiment of the present invention, is not limited to the present invention.
Embodiment 1
Take 100kg tapioca (flour) (the complete temperature of gelatinization is 70 DEG C), add 900kg water and make the starch milk that mass percentage concentration is 10%, start stirrer and stir.Adding 5kg trisodium phosphate, 0.67kg urea, 1.33kg inferior sodium phosphate, stir, is then 7.5-8.5 by the pH value of the dilute hydrochloric acid solution regulation system of 5%.Open heating while stirring, after the temperature of system reaches 70 DEG C, control heating, remain on 70 DEG C, and isothermal reaction 120min at this temperature.Turn off heating, the slurries obtained are the phosphate ester starch slurries of living broadcast.
Get the phosphate ester starch slurries of appropriate above-mentioned preparation, fully wash farinaceous size with the alcohol of 65%-70%, pyrophosphate salt unreacted in slurries is washed away, and phosphate ester starch Precipitation.Unreacted pyrophosphate salt is checked whether thoroughly to wash away with ammonium molybdate solution.By the phosphate ester starch vacuum dehydrating at lower temperature of precipitation to constant weight.Take the phosphate ester starch sample being dried to constant weight in right amount, the substitution value recording sample is 0.009, and the reaction efficiency calculating trisodium phosphate is 50%.
Get the phosphate ester starch slurries of appropriate above-mentioned preparation, adjusting its mass concentration is 6.0%, and recording its viscosity by NDJ-79 type Rotary Viscosimeter is 15.6mPa.s, and thermoviscosity stability is 88.5%.
Get the phosphate ester starch slurries of appropriate above-mentioned preparation, adjusting its mass concentration is 6.0%, under fixed temperature and humidity condition, be prepared into serous coat, and the breaking tenacity recording serous coat is 22.5N/mm
2, elongation at break is 3.8%, and serous coat rate of moisture absorption is 25.6%.
Get the phosphate ester starch slurries of appropriate above-mentioned preparation, adjusting its mass concentration is 1.0%, and recording it to the adhesion of the textile rove of 14.5tex is 65.9N, is 115.8N to the adhesion of 13tex63/35 polyester-cotton blend rove.
Embodiment 2
Take 150kg W-Gum (the complete temperature of gelatinization is 72 DEG C), add 850kg water and make the starch milk that mass percentage concentration is 15%, start stirrer and stir.Adding 22.5kg Trisodium trimetaphosphate, 3.33kg urea, 1.67kg inferior sodium phosphate, stir, is then 6.0-7.0 by the pH value of the dilute hydrochloric acid solution regulation system of 5%.Open heating while stirring, after the temperature of system reaches 122 DEG C, control heating, remain on 122 DEG C, and isothermal reaction 30min at this temperature.Turn off heating, the slurries obtained are the phosphate ester starch slurries of living broadcast.
According to the method for embodiment 1, the substitution value recording sample is 0.022, and the reaction efficiency calculating Trisodium trimetaphosphate is 28%; Viscosity is 16.7mPa.s, and thermoviscosity stability is 91.0%.The breaking tenacity of serous coat is 23.2N/mm
2, elongation at break is 3.2%, and serous coat rate of moisture absorption is 25.4%; Being 68.0N to the adhesion of the textile rove of 14.5tex, is 121.3N to the adhesion of 13tex63/35 polyester-cotton blend rove.
Embodiment 3
Take 120kg yam starch (the complete temperature of gelatinization is 67 DEG C), add 880kg water and make the starch milk that mass percentage concentration is 12%, start stirrer and stir.Adding 8.4kg tripoly phosphate sodium STPP, 1.5kg urea, 1.5kg inferior sodium phosphate, stir, is then 6.5-7.5 by the pH value of the dilution heat of sulfuric acid regulation system of 5%.Open heating while stirring, after the temperature of system reaches 77 DEG C, control heating, remain on 77 DEG C, and isothermal reaction 90min at this temperature.Turn off heating, the slurries obtained are the phosphate ester starch slurries of living broadcast.
According to the method for embodiment 1, the substitution value recording sample is 0.017, and the reaction efficiency calculating tripoly phosphate sodium STPP is 55%; Viscosity is 17.3mPa.s, and thermoviscosity stability is 87.3%.The breaking tenacity of serous coat is 19.5N/mm
2, elongation at break is 4.2%, and serous coat rate of moisture absorption is 23.7%.Being 68.3N to the adhesion of the textile rove of 14.5tex, is 110.7N to the adhesion of 13tex63/35 polyester-cotton blend rove.
Embodiment 4
Take 140kg yam starch (the complete temperature of gelatinization is 67 DEG C), add 860kg water and make the starch milk that mass percentage concentration is 14%, start stirrer and stir.Adding 14kg tripoly phosphate sodium STPP, 3.36kg urea, 2.24kg inferior sodium phosphate, stir, is then 6.5-7.5 by the pH value of the dilution heat of sulfuric acid regulation system of 5%.Open heating while stirring, after the temperature of system reaches 97 DEG C, control heating, remain on 97 DEG C, and isothermal reaction 90min at this temperature.Turn off heating, the slurries obtained are the phosphate ester starch slurries of living broadcast.
According to the method for embodiment 1, the substitution value recording sample is 0.025, and the reaction efficiency calculating tripoly phosphate sodium STPP is 57%; Viscosity is 17.8mPa.s, and thermoviscosity stability is 84.7%.The breaking tenacity of serous coat is 19.8N/mm
2, elongation at break is 4.0%, and serous coat rate of moisture absorption is 23.8%.Being 65.3N to the adhesion of the textile rove of 14.5tex, is 107.6N to the adhesion of 13tex63/35 polyester-cotton blend rove.
Claims (2)
1. prepare a method for phosphate ester starch slurry, comprise the following steps:
A () adds water and ative starch (its chemical structure is identical with when being present in raw material with character) in a reservoir, preparation ative starch mass percentage concentration is the starch milk of 10%-15%, and described ative starch is at least one in W-Gum, yam starch, tapioca (flour).
B () under agitation, the Phosphation reagent relative to ative starch quality 5%-15% and the composite catalyst being equivalent to ative starch weight 2%-5% is added in starch milk, described Phosphation reagent is at least one of tripoly phosphate sodium STPP, Trisodium trimetaphosphate or trisodium phosphate, described composite catalyst is urea and sodium hypophosphite, and wherein the quality of urea is 0.5-2 times of inferior sodium phosphate quality;
C () adds acid for adjusting pH value between 6.0-8.5, heat, and controls temperature of reaction than the gelatinization of corresponding ative starch complete temperature height 0-50 DEG C, and maintains this temperature to reacting end.
2. the method preparing phosphate ester starch slurry according to claim 1, comprises the following steps:
A () adds water and ative starch (its chemical structure is identical with when being present in raw material with character) in a reservoir, preparation ative starch mass percentage concentration is the starch milk of 12%-14%, and described ative starch is at least one in W-Gum, yam starch, tapioca (flour).
B () under agitation, the Phosphation reagent relative to ative starch quality 7%-10% and the composite catalyst being equivalent to ative starch weight 3%-4% is added in starch milk, described Phosphation reagent is at least one of tripoly phosphate sodium STPP, Trisodium trimetaphosphate or trisodium phosphate, described composite catalyst is urea and sodium hypophosphite, and wherein the quality of urea is 1-1.5 times of inferior sodium phosphate quality;
C () adds dilute hydrochloric acid or dilute sulphuric acid adjust ph between 6.5-7.5, heat, and controls temperature of reaction than the gelatinization of corresponding ative starch complete temperature height 10-30 DEG C, and maintains this temperature to reacting end.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105105335A (en) * | 2015-09-16 | 2015-12-02 | 安徽农业大学 | Phosphate-modified porous starch quantitative embedding tea polyphenol compound and preparation method and application thereof |
| CN107815917A (en) * | 2017-10-27 | 2018-03-20 | 吉林中粮生化有限公司 | A kind of starch composites being used in paper industry |
| CN109468089A (en) * | 2018-09-21 | 2019-03-15 | 安溪县斯马拓科技发展有限公司 | A kind of corrugated paper adhesive preparation method |
| CN112877382A (en) * | 2021-01-18 | 2021-06-01 | 江南大学 | Method for preparing phosphate starch by enzyme method |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3838149A (en) * | 1973-03-28 | 1974-09-24 | Nat Starch Chem Corp | Starch phosphate esters |
| CN101033262A (en) * | 2006-03-10 | 2007-09-12 | 四平帝达变性淀粉有限公司 | Method of preparing starch phosphate |
| CN101508738A (en) * | 2009-03-17 | 2009-08-19 | 闫怀义 | Phosphoric acid ester amylase, derivative and preparation method thereof |
| CN101544702A (en) * | 2009-05-06 | 2009-09-30 | 中南林业科技大学 | Preparation method of phosphate rice starch |
-
2015
- 2015-04-13 CN CN201510173689.2A patent/CN104774273B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3838149A (en) * | 1973-03-28 | 1974-09-24 | Nat Starch Chem Corp | Starch phosphate esters |
| CN101033262A (en) * | 2006-03-10 | 2007-09-12 | 四平帝达变性淀粉有限公司 | Method of preparing starch phosphate |
| CN101508738A (en) * | 2009-03-17 | 2009-08-19 | 闫怀义 | Phosphoric acid ester amylase, derivative and preparation method thereof |
| CN101544702A (en) * | 2009-05-06 | 2009-09-30 | 中南林业科技大学 | Preparation method of phosphate rice starch |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105105335A (en) * | 2015-09-16 | 2015-12-02 | 安徽农业大学 | Phosphate-modified porous starch quantitative embedding tea polyphenol compound and preparation method and application thereof |
| CN107815917A (en) * | 2017-10-27 | 2018-03-20 | 吉林中粮生化有限公司 | A kind of starch composites being used in paper industry |
| CN109468089A (en) * | 2018-09-21 | 2019-03-15 | 安溪县斯马拓科技发展有限公司 | A kind of corrugated paper adhesive preparation method |
| CN112877382A (en) * | 2021-01-18 | 2021-06-01 | 江南大学 | Method for preparing phosphate starch by enzyme method |
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Effective date of registration: 20161031 Address after: 214101, Wuxi Xishan Economic Development Zone, Jiangsu, Wuxi No. 128, No. 1, Furong new textile Limited by Share Ltd Patentee after: Wuxi Association of Limited by Share Ltd Address before: 214122 Jiangsu Province, Wuxi City Lake Road No. 1800, Jiangnan University School of textile and clothing Patentee before: Jiangnan University |