CN106866829A - A kind of preparation method of hydrophobicity starch calcium - Google Patents
A kind of preparation method of hydrophobicity starch calcium Download PDFInfo
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- CN106866829A CN106866829A CN201510919523.0A CN201510919523A CN106866829A CN 106866829 A CN106866829 A CN 106866829A CN 201510919523 A CN201510919523 A CN 201510919523A CN 106866829 A CN106866829 A CN 106866829A
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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 kind of preparation method of hydrophobicity starch calcium, the preparation method comprises the following steps：1) by ative starch, denaturation or starch derivatives and water, constant temperature stirs to form 30%~40wt.% starch emulsions under 25 DEG C~40 DEG C reaction systems；2) under 25 DEG C~40 DEG C reaction systems, the pH value of the emulsion to 7.5~8.5 is adjusted with alkaline solution；3) under 25 DEG C~40 DEG C reaction systems, acid anhydrides is added；It is continuously added alkaline solution or calcium salt to keep the pH value 7.5~8.5 of emulsion, after continuing to react certain hour；4) under 25 DEG C~40 DEG C reaction systems, acid for adjusting pH value to 6.0 is added；5) water washing filtering, 50 DEG C of drying is added to dry, pulverize and sieve and obtain white hydrophobic starch calcium.Hydrophobicity starch calcium product of the invention belongs to adsorbent class converted starch, and good fluidity, hydrophobicity is good, and security is good, is a kind of excellent adsorbent, can be widely applied to the skin-protection products such as adsorbent, talcum powder, the prickly-heat powder of cold spray product.
Description
Technical field
The invention belongs to starch deep process technology field, more particularly to a kind of hydrophobicity starch calcium
Preparation method.
Background technology
It is well known that former hydrophobicity starch refers to octenyl succinic acid starch aluminium, according to
GB2760-2014《National food safety standard food additives use standard》Regulation is from food
Product additive allows to use deletion in kind.Due to hydrophobicity starch have good mobility and
Hydrophobicity, the skin-protection product such as the adsorbent being widely used in cold spray product and talcum powder prickly-heat powder
In, and existing other converted starches are unable to reach the mobility and hydrophobicity of former hydrophobicity starch
It is required that, be that this inventor produces hydrophobicity starch calcium by many experiments, its mobility and dredge
It is aqueous can be comparable with former hydrophobicity starch, due to being starch calcium, its security is similar to starch
Sodium, in can be used as food additives and making an addition to skin-protection product.
The content of the invention
The present invention is to solve substituting former hydrophobicity starch, there is provided a kind of hydrophobicity starch calcium
Preparation method, using the inventive method produce hydrophobicity starch calcium good fluidity, hydrophobicity it is good,
It is safe.
In order to solve the above-mentioned technical problem, the present invention provides a kind of preparation side of hydrophobicity starch calcium
Method, the preparation method comprises the following steps：1) ative starch, converted starch or starch are derived
The constant temperature under 25 DEG C~40 DEG C reaction systems stirs to form 30%~40wt.% starch milks thing with water
Liquid；2) under 25 DEG C~40 DEG C reaction systems, the breast is adjusted with the alkaline solution of 1~10wt.%
The pH value of liquid is to 7.5~9.5；3) under 25 DEG C~40 DEG C reaction systems, acid anhydrides is added, institute
The acid anhydrides amount of addition is 0.1%~100wt.% of starch or starch derivatives oven-dry weight；It is continuously added
The alkaline solution or calcium salt of 1~10wt.% are keeping the pH value 7.5~9.5 of emulsion, question response system
After pH stable, continue to react 2-15 hours；4) after reaction terminates, acid for adjusting pH is added
Value adds water washing filtering, 50 DEG C of drying and dries, pulverizes and sieves and obtain white hydrophobic to 6.0
Property starch calcium.
In the preferred technical solution of the present invention, it is preferable that the ative starch include cornstarch,
Waxy corn starch, tapioca, starch from sweet potato, potato starch, pea starch, the root of kudzu vine form sediment
Powder, wheaten starch, barley starch, sorghum starch, small rice starch, rice starch, glutinous rice form sediment
Powder；The converted starch is pregelatinized starch, acid treated starches, alkali process starch, bleaching shallow lake
Powder, oxidized starch, enzyme treated starch, acetic starch, sodium carboxymethyl starch, sodium starch phosphate,
Hydroxypropul starch；The starch derivatives is mono-starch phosphate, double starch phosphates, acetyl
Change distarch adipate, the glycerinum amyli ester of acetylation two, Ultra Tex 2, two
Glycerinum amyli ester, PASELLI EASYGEL, hydroxypropyl PASELLI EASYGEL, the starch of hydroxypropyl two are sweet
Grease, phosphorylation PASELLI EASYGEL, starch Sodium Octenyl Succinate.
In the preferred technical solution of the present invention, it is preferable that the acid anhydrides be aceticanhydride, maleic anhydride,
Succinyl oxide, methyl succinic acid anhydrides, allyl succinic anhydride, pentenyl succinyl oxide, heptene
Base succinyl oxide, octenyl succinic acid anhydride, nonenyl succinic acid acid anhydride, decenyl succinic acid anhydride,
Dodecenylsuccinic anhydride, octadecenyl succinic anhydride.
In the preferred technical solution of the present invention, it is preferable that the alkaline solution is alkali metal hydrogen-oxygen
Compound, alkaline earth metal hydroxide, alkali metal salt, alkali salt；The alkali metal hydrogen-oxygen
Compound is NaOH, potassium hydroxide；The alkaline earth metal hydroxide is calcium hydroxide；Institute
Alkali metal salt is stated for potassium carbonate, sodium acetate, Potassium Suceinate；The calcium salt is calcium chloride, phosphoric acid
Hydrogen calcium, calcium carbonate, calcium hydroxy phosphate, calcium sulfate, calcium nitrate, calcium phosphate, calcium citrate,
Calcium citrate, calcium malate, calcium gluconae, calcium fumarate, calcium lactate, calcium alginate.
In the preferred technical solution of the present invention, it is preferable that the amount of the acid anhydrides for being added be starch or
1~100wt.% of starch derivatives oven-dry weight.It is highly preferred that the amount of the acid anhydrides for being added is shallow lake
1%~50wt.% of powder or starch derivatives oven-dry weight.Most preferably, the amount of the acid anhydrides for being added
It is starch or 3%~10wt.% of starch derivatives oven-dry weight.
In the preferred technical solution of the present invention, it is preferable that the reaction system is maintained at 28-35 DEG C
At a temperature of.
In the preferred technical solution of the present invention, it is preferable that add the concentration of diluted sodium hydroxide solution
It is 2~6wt.%.It is highly preferred that the concentration for adding diluted sodium hydroxide solution is 3~5wt.%.
Hydrophobicity starch calcium product of the invention belongs to adsorbent class converted starch, good fluidity,
Hydrophobicity is good, and security is good, is a kind of excellent adsorbent, can be widely applied to cold spray product
The skin-protection product such as adsorbent, talcum powder, prickly-heat powder.
Specific embodiment
Below with reference to embodiment, the present invention will be further described, and embodiments of the invention are only used for
Illustrate technical scheme, and the non-limiting present invention.
Embodiment 1
Stirred in 100 parts of cornstarch and 233 parts of purified water input four-hole boiling flasks, stirring speed
It is 100rpm to spend, and is placed in 25 DEG C of thermostat water baths, and 1wt.% sodium hydroxide solutions are added dropwise makes breast
Liquid pH value adds 1 part of aceticanhydride to 8.0, and 1wt.% sodium hydroxide solutions are constantly added dropwise makes emulsion
PH value keeps 7.0~9.5, after after system pH stabilization, adds 1 part of calcium chloride, continues to react
3 hours, it was 6.0 300 parts of purified waters of addition to add 1wt.% hydrochloric acid regulation ph value of emulsion, is stirred
Mix uniform, cross 500 mesh filter clothes, obtain filter cake, filter cake is placed in 50 DEG C of drying in oven, pass through
Crush 120 mesh sieves and obtain white hydrophobic starch calcium.Activation index H=20.32% is measured, not
Angle till=29.407 °.
Embodiment 2
Stirred in 100 portions of tapiocas and 233 parts of purified water input four-hole boiling flasks, stirring speed
It is 150rpm to spend, and is placed in 27 DEG C of thermostat water baths, and 2wt.% sodium hydroxide solutions are added dropwise makes breast
Liquid pH value adds 3 parts of allyl succinic anhydrides to 8.5, and 2wt.% NaOH is constantly added dropwise
Solution makes ph value of emulsion keep 7.0~8.5, after after system pH stabilization, adds 3 parts of calcium phosphate,
Continue to react 4 hours, it is 6.0 to add 5wt.% hydrochloric acid regulation ph value of emulsion, adds 400 parts
Purified water, is stirred, and crosses 500 mesh filter clothes, obtains filter cake, and filter cake is placed in into 50 DEG C of baking ovens
Interior drying, the mesh sieve of size-reduced mistake 120 obtains white hydrophobic starch calcium.Measure activation index
H=21.85%, angle of repose=27.523 °.
Embodiment 3
Stirred in 100 parts of potato starches and 200 parts of purified water input four-hole boiling flasks, stirring speed
It is 200rpm to spend, and is placed in 29 DEG C of thermostat water baths, and 3wt.% calcium lactate solutions are added dropwise makes breast
Liquid pH value adds 5 parts of octenyl succinic acid anhydrides to 7.5,3wt.% calcium lactates is constantly added dropwise molten
Liquid makes ph value of emulsion keep 7.0~8.5, after after system pH stabilization, adds 5 parts of calcium chloride,
Continue to react 5 hours, it is 6.0 to add 8wt.% hydrochloric acid regulation ph value of emulsion, adds 500 parts
Purified water, is stirred, and crosses 500 mesh filter clothes, obtains filter cake, and filter cake is placed in into 50 DEG C of baking ovens
Interior drying, the mesh sieve of size-reduced mistake 120 obtains white hydrophobic starch calcium.Measure activation index
H=52.36%, angle of repose=24.336 °.
Embodiment 4
Stirred in 100 parts of oxidized starch and 200 parts of purified water input four-hole boiling flasks, stirring speed
It is 250rpm to spend, and is placed in 31 DEG C of thermostat water baths, and 4wt.% solution of potassium carbonate is added dropwise makes emulsion
PH value adds 7 parts of maleic anhydrides to 8.5, and 4wt.% solution of potassium carbonate is constantly added dropwise makes emulsion
PH value keeps 7.0~8.5, after after system pH stabilization, adds 7 parts of calcium carbonate, continues to react
6 hours, it was 6.0 to add 10wt.% hydrochloric acid regulation ph value of emulsion, adds 600 parts of purified waters,
Stir, cross 500 mesh filter clothes, obtain filter cake, filter cake is placed in 50 DEG C of drying in oven,
The mesh sieve of size-reduced mistake 120 obtains white hydrophobic starch calcium.Activation index H=69.18% is measured,
Angle of repose=22.124 °.
Embodiment 5
Stirred in 100 parts of sodium carboxymethyl starches and 150 parts of purified water input four-hole boiling flasks, stirred
Speed is mixed for 300rpm, is placed in 33 DEG C of thermostat water baths, 5wt.% calcium gluconaes are added dropwise molten
Liquid makes ph value of emulsion to 9.0, adds 9 parts of pentenyl succinyl oxides, and 5wt.% Portugals are constantly added dropwise
Grape saccharic acid calcium solution makes ph value of emulsion keep 7.0~8.5, after after system pH stabilization, continues anti-
Answer 6 hours, it is 6.0 to add 12% hydrochloric acid regulation ph value of emulsion, adds 700 parts of purified waters,
Stir, cross 500 mesh filter clothes, obtain filter cake, filter cake is placed in 50 DEG C of drying in oven,
The mesh sieve of size-reduced mistake 120 obtains white hydrophobic starch calcium.Activation index H=87.05% is measured,
Angle of repose=21.325 °.
Embodiment 6
Stirred in 100 parts of double starch phosphates and 150 parts of purified water input four-hole boiling flasks, put
Make ph value of emulsion to 8.0 in 6wt.% SASs in 35 DEG C of thermostat water baths, are added dropwise, plus
Enter 15 parts of decenyl succinic acid anhydrides, 6wt.% SASs are constantly added dropwise protects ph value of emulsion
7.0~8.5 are held, after after system pH stabilization, 15 parts of calcium sulfate is added, continue to react 8 hours,
It is 6.0 to add 14wt.% hydrochloric acid regulation ph value of emulsion, adds 800 parts of purified waters, is stirred,
500 mesh filter clothes are crossed, filter cake is obtained, filter cake is placed in 50 DEG C of drying in oven, size-reduced mistake 120
Mesh sieve obtains white hydrophobic starch calcium.Measure activation index H=98.23%, angle of repose
=18.324 °.
Embodiment 7
Stirring is equal in 100 parts of Ultra Tex 2s and 233 parts of purified water input four-hole boiling flasks
It is even, it is placed in 37 DEG C of thermostat water baths, 7wt.% calcium alginate solution is added dropwise makes ph value of emulsion
To 8.0,30 parts of nonenyl succinic acid acid anhydrides are added, 7wt.% calcium alginate solution is constantly added dropwise to be made
Ph value of emulsion keeps 7.0~8.5, after after system pH stabilization, continues to react 10 hours, plus
It is 6.0 to enter 16wt.% hydrochloric acid regulation ph value of emulsion, adds 1000 parts of purified waters, is stirred,
500 mesh filter clothes are crossed, filter cake is obtained, filter cake is placed in 50 DEG C of drying in oven, size-reduced mistake 120
Mesh sieve obtains white hydrophobic starch calcium.Measure activation index H=98.83%, angle of repose
=18.011 °.
Embodiment 8
Stirring is equal in 100 parts of hydroxypropyl PASELLI EASYGELs and 200 parts of purified water input four-hole boiling flasks
It is even, it is placed in 38 DEG C of thermostat water baths, 8wt.% Potassium Suceinate solution is added dropwise makes ph value of emulsion
To 7.5,45 parts of dodecenylsuccinic anhydrides are added, 8wt.% Potassium Suceinate solution is constantly added dropwise
Ph value of emulsion is kept 7.0~8.5, after after system pH stabilization, add 45 parts of calcium nitrate,
Continue to react 12 hours, it is 6.0 to add 20wt.% hydrochloric acid regulation ph value of emulsion, adds 1500
Part purified water, is stirred, and crosses 500 mesh filter clothes, obtains filter cake, and filter cake is placed in into 50 DEG C of bakings
Drying in case, the mesh sieve of size-reduced mistake 120 obtains white hydrophobic starch calcium.Measure activation index
H=99.27%, angle of repose=17.832 °.
Embodiment 9
Stirring is equal in 100 parts of phosphorylation PASELLI EASYGELs and 150 parts of purified water input four-hole boiling flasks
It is even, it is placed in 39 DEG C of thermostat water baths, 9wt.% sodium hydroxide solutions are added dropwise makes ph value of emulsion
To 9.5,60 parts of methyl succinic acid anhydrides are added, 9wt.% sodium hydroxide solutions are constantly added dropwise makes breast
Liquid pH value keeps 7.0~8.5, after after system pH stabilization, adds 60 parts of calcium monohydrogen phosphates, after
Continuous reaction 15 hours, it is 6.0 to add 25wt.% hydrochloric acid regulation ph value of emulsion, adds 2000
Part purified water, is stirred, and crosses 500 mesh filter clothes, obtains filter cake, and filter cake is placed in into 50 DEG C of bakings
Drying in case, the mesh sieve of size-reduced mistake 120 obtains white hydrophobic starch calcium.Measure activation index
H=99.33%, angle of repose=17.817 °.
Embodiment 10
100 parts of starch Sodium Octenyl Succinates (10%) and 150 parts of purified water input four-hole boiling flasks
In stir, be placed in 40 DEG C of thermostat water baths, be added dropwise 10wt.% calcium malate solution make breast
Liquid pH value is kept to 7.5-8.0, continues to react 7 hours, adds 1200 parts of purified waters, stirring
Uniformly, 500 mesh filter clothes are crossed, filter cake is obtained, filter cake 50 DEG C of drying in oven is placed in, through powder
The mesh sieve of broken mistake 120 obtains white hydrophobic starch calcium.Activation index H=95.27% is measured, is stopped
Angle=19.216 °.
Embodiment 11
Stirred in 100 parts of pregelatinized starch and 200 parts of purified water input four-hole boiling flasks, be placed in
In 35 DEG C of thermostat water baths, 3wt.% aqua calcises are added dropwise makes ph value of emulsion to 8.5, plus
Enter 6 parts of succinyl oxides, 3wt.% aqua calcises are constantly added dropwise keeps ph value of emulsion
7.0~8.5, after after system pH stabilization, continue to react 4 hours, add the regulation of 4wt.% hydrochloric acid
Ph value of emulsion is 6.0, adds 500 parts of purified waters, is stirred, and crosses 500 mesh filter clothes, is obtained
To filter cake, filter cake is placed in 50 DEG C of drying in oven, the mesh sieve of size-reduced mistake 120 obtains white and dredges
Aqueous starch calcium.Measure activation index H=61.45%, angle of repose=23.057 °.
Embodiment 12
Stirred in 100 parts of hydroxypropul starch and 233 parts of purified water input four-hole boiling flasks, be placed in
In 38 DEG C of thermostat water baths, 3wt.% sodium hydroxide solutions are added dropwise makes ph value of emulsion to 8.0, plus
Enter 3 parts of octadecenyl succinic anhydrides, 3wt.% sodium hydroxide solutions are constantly added dropwise makes ph value of emulsion
7.0~8.5 are kept, after after system pH stabilization, 3 parts of calcium hydroxy phosphates is added, continues to react 3
Hour, it is 6.0 to add 4wt.% hydrochloric acid regulation ph value of emulsion, adds 300 parts of purified waters, is stirred
Mix uniform, cross 500 mesh filter clothes, obtain filter cake, filter cake is placed in 50 DEG C of drying in oven, pass through
Crush 120 mesh sieves and obtain white hydrophobic starch calcium.Activation index H=39.27% is measured, not
Angle till=27.836 °.
Embodiment 13
Stirred in 100 portions of acetic starches and 180 parts of purified water input four-hole boiling flasks, be placed in
In 38 DEG C of thermostat water baths, 4wt.% calcium citrate solution is added dropwise makes ph value of emulsion to 7.5, plus
Enter 5 parts of heptenyl succinic acid acid anhydrides, 4wt.% calcium citrate solution is constantly added dropwise makes ph value of emulsion
7.0~8.5 are kept, after after system pH stabilization, continues to react 3 hours, add 1wt.% salt
Acid regulation ph value of emulsion is 6.0, adds 200 parts of purified waters, is stirred, and crosses the filter of 500 mesh
Cloth, obtains filter cake, and filter cake is placed in into 50 DEG C of drying in oven, and the mesh sieve of size-reduced mistake 120 is obtained
White hydrophobic starch calcium.Measure activation index H=52.24%, angle of repose=24.133 °.
It is described above specific embodiment of the invention, but ordinary skill in the art
Personnel, can also be to this hair it is understood that in the case of without departing from the spirit and scope of the present invention
Bright specific embodiment makees various changes and replacement, and these changes and replacement all fall in the present invention
In the range of claims are limited.
Claims (10)
1. a kind of preparation method of hydrophobicity starch calcium, the preparation method comprises the following steps：
1) by ative starch, converted starch or starch derivatives and water in 25 DEG C~40 DEG C reaction systems
Lower constant temperature stirs to form 30%~40wt.% starch emulsions；
2) under 25 DEG C~40 DEG C reaction systems, the breast is adjusted with the alkaline solution of 1~10wt.%
The pH value of liquid is to 7.5~9.5；
3) under 25 DEG C~40 DEG C reaction systems, acid anhydrides is added, the acid anhydrides amount for being added is shallow lake
0.1%~100wt.% of powder or starch derivatives oven-dry weight；It is continuously added the alkaline molten of 1~10wt.%
Liquid or calcium salt after question response system pH stabilization, are continued with keeping the pH value 7.5~9.5 of emulsion
Reaction 2-15 hours；
4) reaction terminate after, add acid for adjusting pH value to 6.0, add water washing filtering, 50 DEG C
Drying dries, pulverizes and sieves and obtain white hydrophobic starch calcium.
2. preparation method according to claim 1, wherein, the ative starch includes corn
Starch, waxy corn starch, tapioca, starch from sweet potato, potato starch, pea starch,
Pueraria starch, wheaten starch, barley starch, sorghum starch, small rice starch, rice starch,
Glutinous rice starch；The converted starch be pregelatinized starch, acid treated starches, alkali process starch,
Bleaching starch, oxidized starch, enzyme treated starch, acetic starch, sodium carboxymethyl starch, phosphoric acid
Sodium starch, hydroxypropul starch；The starch derivatives is mono-starch phosphate, double starch phosphates
Ester, acetylated distarch adipate, the glycerinum amyli ester of acetylation two, the starch phosphorus of acetylation two
Acid esters, two glycerinum amyli esters, PASELLI EASYGEL, hydroxypropyl PASELLI EASYGEL, hydroxypropyl
Two glycerinum amyli esters, phosphorylation PASELLI EASYGEL, starch Sodium Octenyl Succinate.
3. preparation method according to claim 1, wherein, the acid anhydrides is aceticanhydride, horse
Come acid anhydrides, succinyl oxide, methyl succinic acid anhydrides, allyl succinic anhydride, pentenyl butanedioic acid
Acid anhydride, heptenyl succinic acid acid anhydride, octenyl succinic acid anhydride, nonenyl succinic acid acid anhydride, decene base amber
Amber acid anhydrides, dodecenylsuccinic anhydride, octadecenyl succinic anhydride.
4. preparation method according to claim 1, wherein, the alkaline solution is alkali gold
Category hydroxide, alkaline earth metal hydroxide, alkali metal salt, alkali salt；The alkali gold
Category hydroxide is NaOH, potassium hydroxide；The alkaline earth metal hydroxide is hydroxide
Calcium；The alkali metal salt is potassium carbonate, sodium acetate, Potassium Suceinate；The calcium salt be calcium chloride,
Calcium monohydrogen phosphate, calcium carbonate, calcium hydroxy phosphate, calcium sulfate, calcium nitrate, calcium phosphate, citric acid
Calcium, calcium citrate, calcium malate, calcium gluconae, calcium fumarate, calcium lactate, alginic acid
Calcium.
5. the preparation method according to claim 1 or 3, wherein, the acid anhydrides for being added
It is 1~100wt.% of starch or starch derivatives oven-dry weight to measure.
6. preparation method according to claim 5, wherein, the amount of the acid anhydrides for being added is
1%~50wt.% of starch or starch derivatives oven-dry weight.
7. preparation method according to claim 6, wherein, the amount of the acid anhydrides for being added is
3%~10wt.% of starch or starch derivatives oven-dry weight.
8. preparation method according to claim 1, wherein, the reaction system is maintained at
At a temperature of 28-35 DEG C.
9. preparation method according to claim 1, wherein, add diluted sodium hydroxide solution
Concentration be 2~6wt.%.
10. preparation method according to claim 9, wherein, add dilute sodium hydroxide molten
The concentration of liquid is 3~5wt.%.
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| CN112915066A (en) * | 2021-04-08 | 2021-06-08 | 贵州威门药业股份有限公司 | Glabrous sarcandra herb formula granules and preparation method thereof |
| 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 |
| CN115087425A (en) * | 2020-02-12 | 2022-09-20 | 玉米产品开发公司 | Compositions of free-flowing hydrophobic carbohydrate derivatives and methods of use thereof |
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| 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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