CN106866829B - preparation method of hydrophobic starch calcium - Google Patents
preparation method of hydrophobic starch calcium Download PDFInfo
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- CN106866829B CN106866829B CN201510919523.0A CN201510919523A CN106866829B CN 106866829 B CN106866829 B CN 106866829B CN 201510919523 A CN201510919523 A CN 201510919523A CN 106866829 B CN106866829 B CN 106866829B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B31/00—Preparation of derivatives of starch
- C08B31/02—Esters
- C08B31/04—Esters of organic acids, e.g. alkenyl-succinated starch
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B31/00—Preparation of derivatives of starch
- C08B31/02—Esters
- C08B31/06—Esters of inorganic acids
- C08B31/066—Starch phosphates, e.g. phosphorylated starch
Abstract
The invention provides a preparation method of hydrophobic starch calcium, which comprises the following steps: 1) stirring raw starch, modified starch or starch derivatives and water at a constant temperature of 25-40 ℃ to form 30-40 wt.% starch emulsion; 2) adjusting the pH value of the emulsion to 7.5-8.5 by using an alkaline solution at the temperature of 25-40 ℃ in a reaction system; 3) adding anhydride into the reaction system at 25-40 ℃; continuously adding an alkaline solution or calcium salt to keep the pH value of the emulsion at 7.5-8.5, and continuously reacting for a certain time; 4) adding acid to adjust the pH value to 6.0 at the temperature of 25-40 ℃ in a reaction system; 5) and then adding water, washing, filtering, drying at 50 ℃, crushing and sieving to obtain white hydrophobic starch calcium. The hydrophobic starch calcium product belongs to modified starch of adsorbent, has good fluidity, good hydrophobicity and good safety, is an excellent adsorbent, and can be widely applied to skin care products such as adsorbent of cold spray products, talcum powder, prickly heat powder and the like.
Description
Technical Field
The invention belongs to the technical field of starch deep processing, and particularly relates to a preparation method of hydrophobic starch calcium.
Background
As is known, the original hydrophobic starch refers to aluminum starch octenyl succinate, which has been deleted from the permitted varieties of food additives according to the regulations of GB2760-2014 national standard for food safety food additive usage. The hydrophobic starch has good fluidity and hydrophobicity, and can be widely applied to skin care products such as an adsorbent in a cold spray product, talcum powder prickly heat powder and the like, and the existing other modified starches cannot meet the requirements of the fluidity and the hydrophobicity of the original hydrophobic starch.
Disclosure of Invention
The invention aims to provide a preparation method of hydrophobic starch calcium to replace original hydrophobic starch, and the hydrophobic starch calcium produced by the method has good fluidity, good hydrophobicity and high safety.
In order to solve the technical problems, the invention provides a preparation method of hydrophobic starch calcium, which comprises the following steps: 1) stirring raw starch, modified starch or starch derivatives and water at a constant temperature of 25-40 ℃ to form 30-40 wt.% starch emulsion; 2) adjusting the pH value of the emulsion to 7.5-9.5 by using 1-10 wt.% of alkaline solution at a reaction system of 25-40 ℃; 3) adding anhydride into the reaction system at 25-40 ℃, wherein the amount of the added anhydride is 0.1-100 wt% of the absolute dry weight of the starch or the starch derivative; continuously adding 1-10 wt.% of alkaline solution or calcium salt to keep the pH value of the emulsion at 7.5-9.5, and continuously reacting for 2-15 hours after the pH value of the reaction system is stable; 4) after the reaction is finished, adding acid to adjust the pH value to 6.0, then adding water to wash and filter, drying at 50 ℃, crushing and sieving to obtain white hydrophobic starch calcium.
in a preferred technical scheme of the present invention, preferably, the native starch includes corn starch, waxy corn starch, tapioca starch, sweet potato starch, pea starch, kudzu root starch, wheat starch, barley starch, sorghum starch, millet starch, rice starch, and glutinous rice starch; the modified starch is pregelatinized starch, acid-treated starch, alkali-treated starch, bleached starch, oxidized starch, enzyme-treated starch, acetic starch, sodium carboxymethyl starch, sodium starch phosphate, and hydroxypropyl starch; the starch derivative is selected from the group consisting of mono-starch phosphate, di-starch phosphate, acetylated di-starch adipate, acetylated di-starch glyceride, acetylated di-starch phosphate, di-starch glyceride, di-starch phosphate, hydroxypropyl di-starch glyceride, phosphorylated di-starch phosphate and octenyl succinic acid starch sodium.
In a preferred embodiment of the present invention, the acid anhydride is acetic anhydride, maleic anhydride, succinic anhydride, methylsuccinic anhydride, allylsuccinic anhydride, pentenylsuccinic anhydride, heptylsuccinic anhydride, octenylsuccinic anhydride, nonenylsuccinic anhydride, decenylsuccinic anhydride, dodecenylsuccinic anhydride, octadecylsuccinic anhydride.
In a preferred embodiment of the present invention, preferably, the alkaline solution is an alkali metal hydroxide, an alkaline earth metal hydroxide, an alkali metal salt, or an alkaline earth metal salt; the alkali metal hydroxide is sodium hydroxide and potassium hydroxide; the alkaline earth metal hydroxide is calcium hydroxide; the alkali metal salt is potassium carbonate, sodium acetate and potassium succinate; the calcium salt is selected from calcium chloride, calcium hydrogen phosphate, calcium carbonate, calcium hydroxy phosphate, calcium sulfate, calcium nitrate, calcium phosphate, calcium citrate, calcium malate, calcium gluconate, calcium fumarate, calcium lactate, and calcium alginate.
In a preferred embodiment of the present invention, the amount of the acid anhydride added is preferably 1 to 100 wt.% of the absolute dry weight of the starch or starch derivative. More preferably, the amount of acid anhydride added is 1 to 50 wt.% of the oven dry amount of starch or starch derivative. Most preferably, the amount of acid anhydride added is between 3% and 10% by weight of the oven dry amount of starch or starch derivative.
In the preferred embodiment of the present invention, the reaction system is preferably maintained at a temperature of 28 to 35 ℃.
In the preferred technical scheme of the invention, the concentration of the added dilute sodium hydroxide solution is preferably 2-6 wt.%. More preferably, the concentration of the added dilute sodium hydroxide solution is 3-5 wt.%.
The hydrophobic starch calcium product belongs to modified starch of adsorbent, has good fluidity, good hydrophobicity and good safety, is an excellent adsorbent, and can be widely applied to skin care products such as adsorbent of cold spray products, talcum powder, prickly heat powder and the like.
Detailed Description
The present invention will be further described with reference to the following examples, which are only for illustrating the technical solutions of the present invention and are not to be construed as limiting the present invention.
Example 1
Putting 100 parts of corn starch and 233 parts of purified water into a four-neck flask, uniformly stirring at the stirring speed of 100rpm, putting the flask into a constant-temperature water bath kettle at 25 ℃, dropwise adding 1 wt.% of sodium hydroxide solution to adjust the pH value of the emulsion to 8.0, adding 1 part of acetic anhydride, continuously dropwise adding 1 wt.% of sodium hydroxide solution to keep the pH value of the emulsion at 7.0-9.5, adding 1 part of calcium chloride after the pH value of the system is stable, continuing to react for 3 hours, adding 1 wt.% of hydrochloric acid to adjust the pH value of the emulsion to 6.0, adding 300 parts of purified water, uniformly stirring, sieving with 500-mesh filter cloth to obtain a filter cake, putting the filter cake into an oven at 50 ℃ for drying, and crushing and sieving with a 120-mesh sieve to obtain white hydrophobic. The activation index H was 20.32% and the angle of repose was 29.407 °.
Example 2
100 parts of cassava starch and 233 parts of purified water are put into a four-neck flask and uniformly stirred, the stirring speed is 150rpm, the four-neck flask is placed in a constant-temperature water bath kettle at 27 ℃, 2 wt.% of sodium hydroxide solution is dropwise added to enable the pH value of the emulsion to be 8.5, 3 parts of allyl succinic anhydride is added, 2 wt.% of sodium hydroxide solution is continuously dropwise added to enable the pH value of the emulsion to be 7.0-8.5, after the pH value of the system is stable, 3 parts of calcium phosphate is added, the reaction is continued for 4 hours, 5 wt.% of hydrochloric acid is added to adjust the pH value of the emulsion to be 6.0, 400 parts of purified water is added, the mixture is uniformly stirred, the mixture is filtered through 500 meshes of filter cloth to obtain a filter cake, the filter cake is placed. The activation index H was 21.85% and the angle of repose was 27.523 ℃.
Example 3
100 parts of potato starch and 200 parts of purified water are put into a four-neck flask and uniformly stirred at the stirring speed of 200rpm, the four-neck flask is placed in a constant-temperature water bath kettle at 29 ℃, 3 wt.% of calcium lactate solution is dropwise added to enable the pH value of the emulsion to be 7.5, 5 parts of octenyl succinic anhydride is added, 3 wt.% of calcium lactate solution is continuously dropwise added to enable the pH value of the emulsion to be kept at 7.0-8.5, after the pH value of the system is stable, 5 parts of calcium chloride is added, the reaction is continued for 5 hours, 8 wt.% of hydrochloric acid is added to adjust the pH value of the emulsion to be 6.0, 500 parts of purified water is added, the mixture is uniformly stirred and is filtered by 500 meshes of filter cloth to obtain a filter cake, the filter cake is. The activation index H was 52.36% and the angle of repose 24.336 deg.
Example 4
Putting 100 parts of oxidized starch and 200 parts of purified water into a four-neck flask, uniformly stirring at the stirring speed of 250rpm, putting the flask into a constant-temperature water bath kettle at 31 ℃, dropwise adding 4 wt.% of potassium carbonate solution to adjust the pH value of the emulsion to 8.5, adding 7 parts of maleic anhydride, continuously dropwise adding 4 wt.% of potassium carbonate solution to keep the pH value of the emulsion at 7.0-8.5, adding 7 parts of calcium carbonate after the pH value of the system is stable, continuously reacting for 6 hours, adding 10 wt.% of hydrochloric acid to adjust the pH value of the emulsion to 6.0, adding 600 parts of purified water, uniformly stirring, sieving with 500-mesh filter cloth to obtain a filter cake, putting the filter cake into a 50 ℃ oven for drying, and crushing and sieving with a 120-mesh sieve to obtain white hydrophobic. The activation index H was 69.18% and the angle of repose was 22.124 °.
Example 5
100 parts of sodium carboxymethyl starch and 150 parts of purified water are put into a four-neck flask and uniformly stirred at the stirring speed of 300rpm, the four-neck flask is placed in a constant-temperature water bath kettle at 33 ℃, 5 wt.% of calcium gluconate solution is dropwise added to enable the pH value of the emulsion to reach 9.0, 9 parts of pentenyl succinic anhydride is added, 5 wt.% of calcium gluconate solution is continuously dropwise added to enable the pH value of the emulsion to be kept at 7.0-8.5, after the pH value of the system is stable, the reaction is continued for 6 hours, 12% hydrochloric acid is added to adjust the pH value of the emulsion to be 6.0, 700 parts of purified water is added, the mixture is uniformly stirred, the mixture is filtered through 500-mesh filter cloth to obtain a filter cake, the filter cake is placed in a 50 ℃ oven. The activation index H was found to be 87.05% and the angle of repose was found to be 21.325 °.
Example 6
100 parts of double-starch phosphate and 150 parts of purified water are put into a four-neck flask and uniformly stirred, the four-neck flask is placed in a constant-temperature water bath kettle at 35 ℃, 6 wt.% of sodium acetate solution is dripped to enable the pH value of emulsion to be 8.0, 15 parts of decenyl succinic anhydride is added, 6 wt.% of sodium acetate solution is continuously dripped to enable the pH value of emulsion to be kept at 7.0-8.5, after the pH value of a system is stable, 15 parts of calcium sulfate is added, reaction is continued for 8 hours, 14 wt.% of hydrochloric acid is added to adjust the pH value of the emulsion to be 6.0, 800 parts of purified water is added and uniformly stirred, filter cakes are obtained by passing through 500-mesh filter cloth, the filter cakes are placed in a 50 ℃ oven to be dried. The activation index H was 98.23% and the angle of repose was 18.324 °.
Example 7
100 parts of acetylated distarch phosphate and 233 parts of purified water are put into a four-neck flask and uniformly stirred, the four-neck flask is placed in a constant-temperature water bath kettle at 37 ℃, 7 wt.% of calcium alginate solution is dripped to enable the pH value of the emulsion to be 8.0, 30 parts of nonenyl succinic anhydride is added, 7 wt.% of calcium alginate solution is continuously dripped to enable the pH value of the emulsion to be kept at 7.0-8.5, after the pH value of the system is stable, the reaction is continued for 10 hours, 16 wt.% of hydrochloric acid is added to adjust the pH value of the emulsion to be 6.0, 1000 parts of purified water is added and uniformly stirred, a filter cake is obtained after the mixture is filtered by a 500-mesh filter cloth, the filter cake is placed in an oven. The activation index H was 98.83% and the angle of repose was 18.011 °.
Example 8
100 parts of hydroxypropyl distarch phosphate and 200 parts of purified water are put into a four-neck flask and uniformly stirred, the flask is placed in a constant-temperature water bath kettle at 38 ℃, 8 wt.% of potassium succinate solution is dripped to ensure that the pH value of the emulsion is 7.5, 45 parts of dodecenyl succinic anhydride is added, 8 wt.% of potassium succinate solution is continuously dripped to ensure that the pH value of the emulsion is kept between 7.0 and 8.5, 45 parts of calcium nitrate is added after the pH value of the system is stable, the reaction is continued for 12 hours, 20 wt.% of hydrochloric acid is added to regulate the pH value of the emulsion to be 6.0, 1500 parts of purified water is added and uniformly stirred, the mixture is filtered by 500-mesh filter cloth to obtain a filter cake, the filter cake is placed in a 50 ℃ oven to. The activation index H was 99.27% and the angle of repose was 17.832 ℃.
Example 9
100 parts of phosphorylated distarch phosphate and 150 parts of purified water are put into a four-neck flask and uniformly stirred, the flask is placed in a constant-temperature water bath kettle at 39 ℃, 9 wt.% of sodium hydroxide solution is dripped to enable the pH value of the emulsion to reach 9.5, 60 parts of methyl succinic anhydride is added, 9 wt.% of sodium hydroxide solution is continuously dripped to enable the pH value of the emulsion to be kept at 7.0-8.5, 60 parts of calcium hydrophosphate is added after the pH value of the system is stable, the reaction is continued for 15 hours, 25 wt.% of hydrochloric acid is added to adjust the pH value of the emulsion to be 6.0, 2000 parts of purified water is added and uniformly stirred, the mixture is filtered by 500 meshes of filter cloth to obtain a filter cake, the filter cake is placed in a 50 ℃ oven. The activation index H was 99.33% and the angle of repose was 17.817 °.
Example 10
100 parts of sodium starch octenyl succinate (10%) and 150 parts of purified water are put into a four-neck flask and uniformly stirred, the flask is placed in a constant-temperature water bath kettle at 40 ℃, 10 wt.% of calcium malate solution is dripped to keep the pH value of the emulsion to be 7.5-8.0, the reaction is continued for 7 hours, 1200 parts of purified water is added and uniformly stirred, filter cloth with 500 meshes is sieved to obtain a filter cake, the filter cake is placed in an oven at 50 ℃ for drying, and the filter cake is crushed and sieved by a 120-mesh sieve to obtain white hydrophobic calcium starch. The activation index H was found to be 95.27% and the angle of repose 19.216 deg..
Example 11
100 parts of pregelatinized starch and 200 parts of purified water are put into a four-neck flask and uniformly stirred, the four-neck flask is placed in a constant-temperature water bath kettle at 35 ℃, 3 wt.% of calcium hydroxide solution is dripped to enable the pH value of the emulsion to be 8.5, 6 parts of succinic anhydride is added, 3 wt.% of calcium hydroxide solution is continuously dripped to enable the pH value of the emulsion to be kept at 7.0-8.5, after the pH value of the system is stable, the reaction is continued for 4 hours, 4 wt.% of hydrochloric acid is added to adjust the pH value of the emulsion to be 6.0, 500 parts of purified water is added and uniformly stirred, a filter cake is obtained after the mixture is filtered through 500 meshes of filter cloth, the filter cake is placed in an oven at 50. The activation index H was 61.45% and the angle of repose was 23.057 °.
Example 12
100 parts of hydroxypropyl starch and 233 parts of purified water are put into a four-neck flask and uniformly stirred, the four-neck flask is placed in a constant-temperature water bath kettle at 38 ℃, 3 wt.% of sodium hydroxide solution is dropwise added to enable the pH value of the emulsion to be 8.0, 3 parts of octadecenyl succinic anhydride is added, 3 wt.% of sodium hydroxide solution is continuously dropwise added to enable the pH value of the emulsion to be 7.0-8.5, after the pH value of the system is stable, 3 parts of calcium hydroxy phosphate is added, the reaction is continued for 3 hours, 4 wt.% of hydrochloric acid is added to adjust the pH value of the emulsion to be 6.0, 300 parts of purified water is added and uniformly stirred, a filter cake is obtained by passing through 500-mesh filter cloth, the filter cake is placed in an oven at 50 ℃. The activation index H was found to be 39.27% and the angle of repose was found to be 27.836 °.
Example 13
100 parts of starch acetate and 180 parts of purified water are put into a four-neck flask and uniformly stirred, the four-neck flask is placed in a constant-temperature water bath kettle at 38 ℃, 4 wt.% of calcium citrate solution is dropwise added to enable the pH value of the emulsion to reach 7.5, 5 parts of heptenyl succinic anhydride is added, 4 wt.% of calcium citrate solution is continuously dropwise added to enable the pH value of the emulsion to be kept at 7.0-8.5, after the pH value of the system is stable, the reaction is continued for 3 hours, 1 wt.% of hydrochloric acid is added to adjust the pH value of the emulsion to be 6.0, 200 parts of purified water is added and uniformly stirred, a filter cake is obtained after the mixture is filtered through 500-mesh filter cloth, the filter cake is placed in an oven at. The activation index H was 52.24% and the angle of repose was 24.133 °.
Although the embodiments of the present invention have been described, it will be understood by those skilled in the art that various changes and substitutions may be made thereto without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (6)
1. A preparation method of hydrophobic starch calcium comprises the following steps:
1) Stirring the starch derivative and water at a constant temperature of 25-40 ℃ to form 30-40 wt.% starch emulsion;
2) Adjusting the pH value of the emulsion to 7.5-9.5 by using 1-10 wt.% of alkaline solution at a reaction system of 25-40 ℃;
3) Adding anhydride into the reaction system at 25-40 ℃, wherein the amount of the added anhydride is 0.1-100 wt% of the absolute dry weight of the starch derivative; continuously adding 1-10 wt.% of alkaline solution to keep the pH value of the emulsion at 7.5-9.5, adding calcium salt after the pH value of the reaction system is stable, and continuously reacting for 2-15 hours; wherein the anhydride is maleic anhydride, succinic anhydride, methylsuccinic anhydride, allylsuccinic anhydride, pentenylsuccinic anhydride, heptylsuccinic anhydride, octenylsuccinic anhydride, nonenylsuccinic anhydride, decenylsuccinic anhydride, octadecenylsuccinic anhydride; the calcium salt is calcium hydrogen phosphate, calcium carbonate, calcium hydroxy phosphate, calcium sulfate, calcium nitrate, calcium phosphate, calcium citrate, calcium malate, calcium gluconate, calcium fumarate, calcium lactate, or calcium alginate;
4) After the reaction is finished, adding acid to adjust the pH value to 6.0, then adding water to wash and filter, drying at 50 ℃, crushing and sieving to obtain white hydrophobic starch calcium; the starch derivative is selected from the group consisting of distarch phosphate, acetylated distarch phosphate, hydroxypropyl distarch phosphate, phosphorylated distarch phosphate, and octenyl succinic acid starch sodium.
2. the preparation method according to claim 1, wherein the alkaline solution is potassium carbonate, sodium acetate, potassium succinate.
3. The method according to claim 1, wherein the acid anhydride is added in an amount of 1 to 100 wt.% based on the absolute dry weight of the starch derivative.
4. the method according to claim 3, wherein the amount of the acid anhydride added is 1 to 50 wt.% of the absolute dry amount of the starch derivative.
5. The method according to claim 4, wherein the acid anhydride is added in an amount of 3 to 10 wt.% based on the absolute dry weight of the starch derivative.
6. The production method according to claim 1, wherein the reaction system is maintained at a temperature of 28 to 35 ℃.
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| AU2021220119A1 (en) * | 2020-02-12 | 2022-08-18 | Corn Products Development, Inc. | Compositions of free flowing hydrophobic carbohydrate derivatives and methods for use |
| TWI766606B (en) * | 2021-03-10 | 2022-06-01 | 健茂生物科技股份有限公司 | Calcium dietary supplement tablet corresponding to blood type |
| CN112915066B (en) * | 2021-04-08 | 2022-09-09 | 贵州威门药业股份有限公司 | Glabrous sarcandra herb formula granules and preparation method thereof |
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| CN102070722A (en) * | 2010-02-03 | 2011-05-25 | 内蒙古奈伦农业科技股份有限公司 | Octenyl succinate distarch phosphate and preparation method and applications thereof |
| KR20120002404A (en) * | 2011-01-26 | 2012-01-05 | 대상 주식회사 | Process for preparing hydrophobic starch |
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| US5797984A (en) * | 1997-04-15 | 1998-08-25 | National Starch And Chemical Investment Holding Corporation | Water resistant starch based foams |
| WO2001077244A2 (en) * | 2000-04-05 | 2001-10-18 | National Starch And Chemical Investment Holding Corporation | Water based adhesive composition with release properties |
| CN1962696A (en) * | 2006-11-10 | 2007-05-16 | 浙江大学 | Process for producing starch octenylsucciniate |
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