CN113087812B - Preparation method of high-fluidity starch - Google Patents
Preparation method of high-fluidity starch Download PDFInfo
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- CN113087812B CN113087812B CN202110440903.1A CN202110440903A CN113087812B CN 113087812 B CN113087812 B CN 113087812B CN 202110440903 A CN202110440903 A CN 202110440903A CN 113087812 B CN113087812 B CN 113087812B
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- 229920002472 Starch Polymers 0.000 title claims abstract description 71
- 239000008107 starch Substances 0.000 title claims abstract description 68
- 235000019698 starch Nutrition 0.000 title claims abstract description 66
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 38
- 239000000243 solution Substances 0.000 claims abstract description 30
- 238000010438 heat treatment Methods 0.000 claims abstract description 26
- 238000006243 chemical reaction Methods 0.000 claims abstract description 25
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000000284 extract Substances 0.000 claims abstract description 16
- 238000005406 washing Methods 0.000 claims abstract description 16
- 239000002253 acid Substances 0.000 claims abstract description 15
- FLISWPFVWWWNNP-BQYQJAHWSA-N dihydro-3-(1-octenyl)-2,5-furandione Chemical compound CCCCCC\C=C\C1CC(=O)OC1=O FLISWPFVWWWNNP-BQYQJAHWSA-N 0.000 claims abstract description 15
- 235000018553 tannin Nutrition 0.000 claims abstract description 15
- 229920001864 tannin Polymers 0.000 claims abstract description 15
- 239000001648 tannin Substances 0.000 claims abstract description 15
- 239000008367 deionised water Substances 0.000 claims abstract description 14
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 14
- 229910052751 metal Inorganic materials 0.000 claims abstract description 12
- 239000002184 metal Substances 0.000 claims abstract description 12
- 238000001035 drying Methods 0.000 claims abstract description 10
- 239000003513 alkali Substances 0.000 claims abstract description 9
- 239000011259 mixed solution Substances 0.000 claims abstract description 8
- 238000001816 cooling Methods 0.000 claims abstract description 7
- 238000001914 filtration Methods 0.000 claims abstract description 5
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- 238000003756 stirring Methods 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 13
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 12
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 12
- 241000196324 Embryophyta Species 0.000 claims description 9
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical group Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 8
- 235000013336 milk Nutrition 0.000 claims description 7
- 239000008267 milk Substances 0.000 claims description 7
- 210000004080 milk Anatomy 0.000 claims description 7
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 6
- 229920002261 Corn starch Polymers 0.000 claims description 6
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
- 239000008120 corn starch Substances 0.000 claims description 6
- 235000019253 formic acid Nutrition 0.000 claims description 6
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 4
- 240000006394 Sorghum bicolor Species 0.000 claims description 3
- 235000011684 Sorghum saccharatum Nutrition 0.000 claims description 3
- 229910052782 aluminium Inorganic materials 0.000 claims description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 3
- 229940100486 rice starch Drugs 0.000 claims description 3
- 229910001220 stainless steel Inorganic materials 0.000 claims description 3
- 239000010935 stainless steel Substances 0.000 claims description 3
- 210000000051 wattle Anatomy 0.000 claims description 3
- 229940100445 wheat starch Drugs 0.000 claims description 3
- PFTAWBLQPZVEMU-DZGCQCFKSA-N (+)-catechin Chemical compound C1([C@H]2OC3=CC(O)=CC(O)=C3C[C@@H]2O)=CC=C(O)C(O)=C1 PFTAWBLQPZVEMU-DZGCQCFKSA-N 0.000 claims description 2
- 241001070941 Castanea Species 0.000 claims description 2
- 235000014036 Castanea Nutrition 0.000 claims description 2
- ADRVNXBAWSRFAJ-UHFFFAOYSA-N catechin Natural products OC1Cc2cc(O)cc(O)c2OC1c3ccc(O)c(O)c3 ADRVNXBAWSRFAJ-UHFFFAOYSA-N 0.000 claims description 2
- 235000005487 catechin Nutrition 0.000 claims description 2
- 229950001002 cianidanol Drugs 0.000 claims description 2
- 238000010907 mechanical stirring Methods 0.000 claims description 2
- 230000007935 neutral effect Effects 0.000 claims description 2
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims description 2
- 235000017557 sodium bicarbonate Nutrition 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 4
- 229910021645 metal ion Inorganic materials 0.000 abstract description 10
- 239000002245 particle Substances 0.000 abstract description 5
- 238000011065 in-situ storage Methods 0.000 abstract description 4
- 239000000706 filtrate Substances 0.000 description 4
- KCYQMQGPYWZZNJ-BQYQJAHWSA-N hydron;2-[(e)-oct-1-enyl]butanedioate Chemical compound CCCCCC\C=C\C(C(O)=O)CC(O)=O KCYQMQGPYWZZNJ-BQYQJAHWSA-N 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 238000007873 sieving Methods 0.000 description 4
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 238000013016 damping Methods 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 230000002378 acidificating effect Effects 0.000 description 2
- 239000003431 cross linking reagent Substances 0.000 description 2
- 150000002148 esters Chemical class 0.000 description 2
- 125000001165 hydrophobic group Chemical group 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 229910017053 inorganic salt Inorganic materials 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 240000004957 Castanea mollissima Species 0.000 description 1
- 235000018244 Castanea mollissima Nutrition 0.000 description 1
- 235000017788 Cydonia oblonga Nutrition 0.000 description 1
- 229920000881 Modified starch Polymers 0.000 description 1
- 239000004368 Modified starch Substances 0.000 description 1
- 235000016976 Quercus macrolepis Nutrition 0.000 description 1
- 240000003152 Rhus chinensis Species 0.000 description 1
- 235000014220 Rhus chinensis Nutrition 0.000 description 1
- 239000006087 Silane Coupling Agent Substances 0.000 description 1
- 150000004645 aluminates Chemical class 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 150000001450 anions Chemical group 0.000 description 1
- 239000008346 aqueous phase Substances 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 239000007822 coupling agent Substances 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 230000009969 flowable effect Effects 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 150000004676 glycans Chemical class 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 235000019426 modified starch Nutrition 0.000 description 1
- -1 papermaking Substances 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 230000029553 photosynthesis Effects 0.000 description 1
- 238000010672 photosynthesis Methods 0.000 description 1
- 229920001282 polysaccharide Polymers 0.000 description 1
- 239000005017 polysaccharide Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 229910001415 sodium ion Inorganic materials 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
Classifications
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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
- C08B31/003—Crosslinking of starch
- C08B31/006—Crosslinking of derivatives of starch
-
- 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
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Biochemistry (AREA)
- Materials Engineering (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
The invention discloses a preparation method of high-fluidity starch, which is characterized by comprising the following steps: (1) Adding deionized water into starch, then dropwise adding a mixed solution of octenyl succinic anhydride and alcohol, and finally filtering, washing and drying; (2) Adding deionized water into a dry sample, adding 5-10 parts by mass of plant tannin extract for reaction, and finally cooling to room temperature; (3) Dropwise adding acid liquor into the solution, passing through a metal screen, heating the solution after passing through the screen to 30-40 ℃, reacting for 30-120 min, adding alkali liquor, adjusting the pH to 3.5-4.5, heating to 45-50 ℃, continuing to react for 30-60 min, centrifuging after the reaction is finished, washing and drying to obtain the required high-fluidity starch. Compared with the prior art, the preparation method has simple operation, can obtain metal ions in situ, has uniform reaction, and can prepare the high-fluidity starch with uniform particle size.
Description
Technical Field
The invention relates to the technical field of starch modification, in particular to a preparation method of high-fluidity starch.
Background
The natural starch is widely existed in roots, stems and seeds of plants, is a polysaccharide substance which is generated by the plants after photosynthesis and is mainly used for energy storage, and because of the characteristics of wide sources, renewability, biodegradability and the like, the natural starch and modified products thereof are widely applied to the fields of food, medicine, papermaking, chemical industry, cosmetics and the like.
Since native starch contains a large number of hydroxyl groups in its molecule and is liable to form intramolecular hydrogen bonds, native starch granules tend to aggregate and cohere with each other and have poor flowability even in a dry state, thereby limiting the applicability thereof. Hydrophilic groups in the starch molecule are responsible for its poor flowability, and thus the increase in flowability can be achieved by introducing hydrophobic groups in its molecule or shielding the hydrophilicity of the surface.
For example, patent application No. CN200710304696.7 (publication No. CN 101230151A) discloses a high fluidity and strong hydrophobicity starch and its preparation method, which comprises coating an aluminate coupling agent and a silane coupling agent on the surface of starch particles by a dry method, and coating the outermost layer with a fluidity improver of silica or alumina layer to obtain better fluidity. However, the method mainly depends on physical mixing and coating, and if the method is not uniform, the flowing effect is influenced; the invention patent with the patent application number of CN201210141066.3 (with the publication number of CN 102702368A) discloses a method for preparing flowable starch by a dry method, the method needs a dry reactor, the experimental condition requirement is higher, unreacted octenyl succinic acid is not removed after octenyl succinic acid is esterified in the first stage, the amount of high-valence metal ion salt solution sprayed into the reactor in the later stage is less, the reaction uniformity with starch is poorer, and the anion group of the metal ion can react with sodium ions in starch ester after the metal ion reacts with starch, so that other inorganic salt components are introduced.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a preparation method of high-fluidity starch, which is simple to operate, can obtain metal ions in situ and has uniform reaction, aiming at the current situation of the prior art, and the method can be used for preparing the high-fluidity starch with uniform particle size.
The technical scheme adopted by the invention for solving the technical problem is as follows: a preparation method of high-fluidity starch is characterized by comprising the following steps:
(1) Adding deionized water into 100 parts by mass of starch to prepare 20-40 wt% starch milk, dropwise adding alkali liquor to control the pH to 7.5-9.0, dropwise adding 1-3 parts by mass of mixed solution of octenyl succinic anhydride and alcohol, reacting for 30-240 min, adjusting the pH to be neutral by using acid liquor, and finally filtering, washing and drying;
wherein the volume ratio of octenyl succinic anhydride to alcohol in the mixed solution of octenyl succinic anhydride and alcohol is 1;
(2) Adding deionized water into 100 parts by mass of the dried sample obtained in the step (1) to prepare starch paste with the concentration of 10-40 wt%, placing the starch paste into an ultrasonic reactor, then dropwise adding acid liquor, controlling the pH value to 4.5-6.5, externally mechanically stirring for 20-40 min, then adding 5-10 parts by mass of plant tannin extract, heating to 30-40 ℃ for reaction for 30-240 min, then using the acid liquor to adjust the pH value to 3.8-4.0, heating to 45-50 ℃ for continuous reaction for 30-60 min, and finally cooling to room temperature;
(3) And (3) dropwise adding acid liquor into the solution obtained in the step (2) to adjust the pH value to 2.5-3.0, passing through a metal screen, heating the solution passing through the screen to 30-40 ℃, reacting for 30-120 min, adding alkali liquor to adjust the pH value to 3.5-4.5, heating to 45-50 ℃, continuing to react for 30-60 min, centrifuging after the reaction is finished, and washing and drying to obtain the required high-fluidity starch.
Preferably, the starch in step (1) is at least one of waxy corn starch, waxy sorghum starch, waxy rice starch and wheat starch.
Preferably, the alcohol in the mixed solution of octenyl succinic anhydride and alcohol in step (1) is one of methanol, ethanol and isopropanol.
Preferably, the alkali solution in step (1) is a NaOH solution, and the acid solution is dilute hydrochloric acid.
Preferably, the power of the ultrasonic reactor in the step (2) is 300-1000W, and the frequency is 28-40 kHz.
Preferably, the rotation speed of the mechanical stirring in the step (2) is 200-400 rpm.
Preferably, the acid solution in step (2) is dilute hydrochloric acid and formic acid in sequence.
Preferably, the plant tannin extract in step (2) is at least one of catechin, quince, oak cup, chestnut, and wattle bark plant tannin extract.
Preferably, the metal screen in step (3) is at least one of a wire mesh, an aluminum wire mesh and a stainless steel mesh.
Preferably, the metal screen mesh in step (3) is a 24-mesh, 40-mesh, 80-mesh and 120-mesh metal screen mesh step by step.
Preferably, the acid solution in step (3) is dilute sulfuric acid, and the alkali solution is sodium bicarbonate solution.
The working principle of the invention is as follows: hydrophobic groups (octenyl succinic acid) are connected to starch molecules through an aqueous phase method, then cross-linking agents (tannin extracts and metal ion cross-linking agents) are combined to shield hydroxyl groups on the surface of OS-starch, so that the hydrophobicity of the OS-starch is increased, wherein metal ions are obtained in situ by filtering acidic starch milk combined with the tannin extracts through a metal screen, and the uniformity of the particle size of the prepared high-fluidity starch can be ensured.
Compared with the prior art, the invention has the advantages that:
(1) Octenyl succinic acid is grafted to starch molecules in a water phase, so that the requirement on reaction equipment is not high, and unreacted octenyl succinic anhydride is removed through alcohol washing and water washing;
(2) The ultrasonic generator is introduced into the reaction process of the plant tannin extract, the metal ions and the starch, so that the reaction efficiency is increased, and the reaction is more uniform;
(3) The starch ester crosslinked with the tannin extract is adjusted to be acidic, and is filtered by metal screens with different meshes, the metal screens can prepare metal ions in situ while playing a filtering role, the operation is simple, other inorganic salt components can not be introduced, and the metal ions can be further complexed with the starch and the tannin extract by changing the environment, so that the modified starch with uniform particle size and high fluidity can be obtained.
Detailed Description
The present invention will be described in further detail with reference to examples.
Example 1:
(1) Adding a proper amount of deionized water into 100 parts of waxy corn starch in parts by mass to prepare starch milk with the concentration of 30wt%, dropwise adding a NaOH solution to control the pH to 8.5, dropwise adding 3 parts of OSA/ethanol solution (namely a mixed solution of octenyl succinic anhydride and ethanol, wherein the volume ratio of the octenyl succinic anhydride to the ethanol is 1;
(2) Taking 100 parts of freeze-dried sample, adding a proper amount of deionized water to prepare starch paste with the concentration of 20wt%, placing the starch paste into an ultrasonic reactor, dropwise adding dilute hydrochloric acid to control the pH value to be 5.0, mechanically stirring for 30min, setting the parameters of an ultrasonic reaction field to be 35kHz and 600W, setting the stirring parameters to be 300rmp, adding 8 parts of Chinese gall tannin extract, heating to 35 ℃, reacting for 120min, adjusting the pH value to 3.9 by using formic acid, heating to 45 ℃, continuously mechanically stirring for 40min, and cooling to room temperature;
(3) Adjusting reaction pH to 2.8 with dilute sulfuric acid, gradually sieving with 24 mesh, 40 mesh, 80 mesh and 120 mesh wire sieves, heating the obtained filtrate to 35 deg.C, reacting for 60min, and adding NaHCO 3 Adjusting the pH value of the solution to 4.0, heating to 48 ℃, continuing to react for 40min, centrifuging after the reaction is finished, washing with water for 3 times, washing with alcohol for 3 times, and drying to obtain a sample.
Example 2:
(1) Adding a proper amount of deionized water into 100 parts of glutinous rice starch in parts by mass to prepare 20wt% starch milk, dropwise adding a NaOH solution to control the pH to 7.5, dropwise adding 1 part of OSA/isopropanol solution (the volume ratio of octenyl succinic anhydride to ethanol is 1;
(2) Taking 100 parts of freeze-dried sample, adding a proper amount of deionized water to prepare starch paste with the concentration of 10wt%, placing the starch paste into an ultrasonic reactor, dropwise adding dilute hydrochloric acid to control the pH value to be 4.5, mechanically stirring for 20min, setting parameters of an ultrasonic reaction field to be 28kHz and 300W, setting stirring parameters to be 200rmp, adding 5 parts of castanea mollissima extract, heating to 30 ℃, reacting for 30min, adjusting the pH value to be 3.8 by using formic acid, heating to 45 ℃, continuously mechanically stirring for 40min, and cooling to room temperature;
(3) Adjusting reaction pH to 2.5 with dilute sulfuric acid, gradually sieving with 24 mesh, 40 mesh, 80 mesh and 120 mesh aluminum wire mesh sieves, heating the obtained filtrate to 30 deg.C, reacting for 30min, and adding NaHCO 3 Adjusting the pH value of the solution to 3.5, heating to 45 ℃, continuing to react for 30min, centrifuging after the reaction is finished,washing with water for 3 times, washing with alcohol for 3 times, and drying to obtain the sample.
Example 3:
(1) Adding a proper amount of deionized water into 100 parts of wheat starch in parts by mass to prepare starch milk with the concentration of 40wt%, dropwise adding a NaOH solution to control the pH to 9.0, dropwise adding 2 parts of OSA/ethanol solution (the volume ratio of octenyl succinic anhydride to ethanol is 1;
(2) Taking 100 parts of freeze-dried sample, adding a proper amount of deionized water to prepare starch paste with the concentration of 40wt%, placing the starch paste into an ultrasonic reactor, dropwise adding dilute hydrochloric acid to control the pH value to be 6.5, mechanically stirring for 40min, setting parameters of an ultrasonic reaction field to be 40kHz and 1000W, setting parameters of stirring to be 400rmp, adding 10 parts of acorn tannin extract, heating to 40 ℃, reacting for 240min, adjusting the pH value to be 4.0 by using formic acid, heating to 50 ℃, continuously mechanically stirring for 60min, and cooling to room temperature;
(3) Adjusting reaction pH to 3.0 with dilute sulfuric acid, gradually sieving with 24 mesh, 40 mesh, 80 mesh and 120 mesh stainless steel sieve, heating the obtained filtrate to 40 deg.C, reacting for 120min, and adding NaHCO 3 Adjusting the pH value of the solution to 4.5, heating to 45 ℃, continuing to react for 60min, centrifuging after the reaction is finished, washing with water for 3 times, washing with alcohol for 3 times, and drying to obtain a sample.
Example 4:
(1) Adding a proper amount of deionized water into 100 parts of waxy sorghum starch in parts by mass to prepare starch milk with the concentration of 40wt%, dropwise adding a NaOH solution to control the pH to 7.5, dropwise adding 3 parts of OSA/ethanol solution (the volume ratio of octenyl succinic anhydride to ethanol is 1;
(2) Taking 100 parts of freeze-dried sample, adding a proper amount of deionized water to prepare starch paste with the concentration of 25wt%, placing the starch paste into an ultrasonic reactor, dropwise adding dilute hydrochloric acid to control the pH value to be 4.5, mechanically stirring for 40min, setting parameters of an ultrasonic reaction field to be 40kHz,300W, setting stirring parameters to be 400rmp, adding 8 parts of wattle bark tannin extract, heating to 40 ℃, reacting for 240min, adjusting the pH value to be 4.0 by using formic acid, heating to 50 ℃, continuously mechanically stirring for 45min, and then cooling to room temperature;
(3) Adjusting reaction pH to 3.0 with dilute sulfuric acid, gradually sieving with 24 mesh, 40 mesh, 80 mesh and 120 mesh sieve, heating the obtained filtrate to 40 deg.C, reacting for 90min, and adding NaHCO 3 Adjusting the pH value of the solution to 4.5, heating to 45 ℃, continuing to react for 60min, centrifuging after the reaction is finished, washing with water for 3 times, washing with alcohol for 3 times, and drying to obtain a sample.
The flowability of the powder sample can be characterized by the angle of repose, and the smaller the angle of repose, the better the flowability.
The angle of repose of waxy corn starch and the high fluidity starch obtained in example 1 was determined using a powder comprehensive property tester, and the specific test method was: the damping table is arranged in a positioning hole in the center of the instrument, a material receiving disc and an angle of repose sample table are arranged on the damping table, and the upper plane of the angle of repose sample table can be ensured to be in a horizontal state by adjusting screws below the damping table. Closing the front door of the instrument, preparing a sample, adjusting a timer to 3min, opening a vibrating screen cover and a vibrating screen switch, slowly feeding materials at a feeding port by using a small spoon, sprinkling the materials on a sample table through a screen and a discharging port to form a cone, stopping feeding after a symmetrical cone is formed, closing the vibrating screen, placing a goniometer at the left side of a sample tray and close to a material pile, measuring from three different positions when measuring the angle of repose, and calculating the average value as one measurement, wherein each sample is measured for 3 times.
Table 1 lists the angles of repose for the different samples, and it can be seen that the fluidity of waxy corn starch obtained by the present method is significantly increased.
Table 1:
| sample (I) | Angle of repose |
| Waxy corn starch | 56.07±0.73 |
| Example 1 | 14.48±0.53 |
Claims (9)
1. A preparation method of high-fluidity starch is characterized by comprising the following steps:
(1) Adding deionized water into 100 parts by mass of starch to prepare starch milk with the concentration of 20-40wt%, dropwise adding alkali liquor to control the pH to 7.5-9.0, dropwise adding 1-3 parts by mass of a mixed solution of octenyl succinic anhydride and alcohol, reacting for 30-240min, adjusting the pH to be neutral by using acid liquor, and finally filtering, washing and drying;
wherein the volume ratio of octenyl succinic anhydride to alcohol in the mixed solution of octenyl succinic anhydride and alcohol is 1 to 4-6;
(2) Adding deionized water into 100 parts by mass of the dried sample obtained in the step (1), preparing starch paste with the concentration of 10-40wt%, placing the starch paste into an ultrasonic reactor, then dropwise adding acid liquor, controlling the pH to 4.5-6.5, externally adding a machine, stirring for 20-40min, then adding 5-10 parts by mass of plant tannin extract, heating to 30-40 ℃, reacting for 30-240min, then adjusting the pH to 3.8-4.0 by using the acid liquor, heating to 45-50 ℃, continuing to react for 30-60min, and finally cooling to room temperature;
(3) Dropwise adding an acid solution into the solution obtained in the step (2) to adjust the pH value to 2.5-3.0, passing through a metal screen, heating the solution after passing through the screen to 30-40 ℃, reacting for 30-120min, adding an alkali liquor to adjust the pH value to 3.5-4.5, heating to 45-50 ℃, continuing to react for 30-60min, centrifuging after the reaction is finished, washing and drying to obtain the required high-fluidity starch;
the metal screen in the step (3) is at least one of a wire mesh, an aluminum wire mesh and a stainless steel mesh.
2. The method for preparing high fluidity starch according to claim 1, wherein: the starch in the step (1) is at least one of waxy corn starch, waxy sorghum starch, waxy glutinous rice starch and wheat starch.
3. The method for producing high fluidity starch according to claim 1, wherein: the alcohol in the mixed solution of the octenyl succinic anhydride and the alcohol in the step (1) is one of methanol, ethanol and isopropanol.
4. The method for producing high fluidity starch according to claim 1, wherein: the alkali liquor in the step (1) is NaOH solution, and the acid liquor is dilute hydrochloric acid.
5. The method for producing high fluidity starch according to claim 1, wherein: the power of the ultrasonic reactor in the step (2) is 300 to 1000W, and the frequency is 28 to 40 kHz;
the rotation speed of the mechanical stirring in the step (2) is 200 to 400rpm.
6. The method for preparing high fluidity starch according to claim 1, wherein: and (3) sequentially using dilute hydrochloric acid and formic acid as the acid solution in the step (2).
7. The method for producing high fluidity starch according to claim 1, wherein: the plant tannin extract in the step (2) is at least one of catechin, gallnut, oak cup, chestnut tree and wattle bark plant tannin extract.
8. The method for preparing high fluidity starch according to claim 1, wherein: the metal screen passing in the step (3) is specifically a metal screen passing through 24 meshes, 40 meshes, 80 meshes and 120 meshes step by step.
9. A method for preparing a high fluidity starch according to any one of claims 1 to 8, wherein: the acid solution in the step (3) is dilute sulfuric acid, and the alkali solution is sodium bicarbonate.
Priority Applications (1)
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| CN1696183A (en) * | 2003-11-19 | 2005-11-16 | 陈建操 | Crosslinking agent |
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