CN113292746B - Method for preparing nano starch by emulsification of aminated starch and surfactant - Google Patents
Method for preparing nano starch by emulsification of aminated starch and surfactant Download PDFInfo
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- CN113292746B CN113292746B CN202110402569.0A CN202110402569A CN113292746B CN 113292746 B CN113292746 B CN 113292746B CN 202110402569 A CN202110402569 A CN 202110402569A CN 113292746 B CN113292746 B CN 113292746B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/12—Powdering or granulating
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B30/00—Preparation of starch, degraded or non-chemically modified starch, amylose, or amylopectin
- C08B30/12—Degraded, destructured or non-chemically modified starch, e.g. mechanically, enzymatically or by irradiation; Bleaching of starch
- C08B30/18—Dextrin, e.g. yellow canari, white dextrin, amylodextrin or maltodextrin; Methods of depolymerisation, e.g. by irradiation or mechanically
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2303/00—Characterised by the use of starch, amylose or amylopectin or of their derivatives or degradation products
- C08J2303/02—Starch; Degradation products thereof, e.g. dextrin
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Abstract
The invention discloses a method for preparing nano starch by emulsification of aminated starch and a surfactant, belonging to the technical field of modified starch development. Based on that amino is introduced into starch molecules and then dispersed in water to perform acid-base response, a surfactant is added into the dispersed phase, the generated hydration action forms a protective layer on the surface of the starch molecules to weaken the hydrogen bond acting force between the starch molecules, the electrostatic repulsion force and the hydrogen bond acting force between protonated amino groups inside the starch molecules reach an ideal state within a certain concentration range to granulate, and the granularity and the monodispersion state of nano starch particles can be regulated and controlled by controlling the factors such as the pH value of a system, the type of the surfactant and the like and assisting ultrasonic treatment. The method can control the particle size and the potential of the nano starch by the restrictive degradation and modification of the starch raw material, and prepare the nano particles with high monodispersity. The method for preparing the nano starch has the characteristics of short time consumption, high efficiency and environmental protection.
Description
Technical Field
A method for preparing nano starch based on emulsification of aminated starch and a surfactant relates to preparation of amino starch by starch controlled hydrolysis and silane coupling, preparation of nano starch by surfactant emulsification and electrostatic-hydrogen bond acting force balance, and belongs to the technical field of modified starch development.
Background
In recent years, nanoparticles have unique physical and chemical properties due to their high surface area and nano size, and are widely used in the fields of medicine, environment, food, and the like, and thus, it has become a research hotspot to widen their application range and improve their use effect. Nanoparticles can be classified into organic and inorganic types according to the source of raw materials. Inorganic nanoparticles of lead, mercury and tin are so hard and stable that they are not easily degraded and may cause many environmental toxicities. In contrast, biologically derived organic nanoparticles having good water solubility, biocompatibility, degradability and edibility are receiving increasing attention. Wherein the starch is an ideal nano-particle raw material based on the characteristics of wide sources, rich modifiable functional groups, low price and the like.
The nano starch as one derivative of starch mainly includes starch nanocrystal and starch nanoparticle. Starch nanocrystals can be obtained by hydrolyzing amorphous regions of starch granules by using sulfuric acid, but the long time consumption and low yield limit the industrial application of the starch nanocrystals; starch nanoparticles can be obtained by mechanical or chemical processes, belonging to amorphous structures, but suffer from the general disadvantages of high energy consumption, non-uniform particle size and the use of organic solvents.
Based on the problems in the process of preparing the nano starch and the final product, the amino is introduced into the starch molecule, the starch molecule is mixed with the surfactant, and the nano starch particles are prepared through the emulsification effect of the amino and the surfactant, so that the method is simple and rapid, the conditions are mild, the energy consumption is low, and the problems in the process of preparing the nano starch can be partially solved.
Disclosure of Invention
The invention aims to provide a novel method for quickly and efficiently preparing nano starch, and the method can be used for realizing the control of the granularity and the potential of the nano starch as required.
The technical scheme of the invention is as follows: a method for preparing nano starch based on emulsification of aminated starch and surfactant comprises using waxy corn starch as raw material, controlling starch molecular weight by pullulanase hydrolysis to obtain dextrin with a certain molecular weight range, coupling N-aminoethyl-gamma-aminopropyltrimethoxysilane, gamma-aminopropyltriethoxysilane or gamma-aminopropyltrimethoxysilane with silane to obtain amino starch, and reacting sodium dodecyl sulfate or sodium dodecyl sulfate with amino starch to obtain nano starch.
A method for preparing nano starch based on emulsification of aminated starch and surfactant comprises the following steps;
(1) starch controlled hydrolysis:
preparing 10-30% (w/v) waxy corn starch milk by using an acetic acid buffer solution with the pH value of 3-7, gelatinizing for 30min at 121 ℃, cooling, adding pullulanase for hydrolysis for 6-24 h, controlling the Dextrose Equivalent (DE) value of the hydrolysate to be 5-15, boiling to inactivate enzyme, and cooling to normal temperature for later use; the addition amount of pullulanase is 80-240 NPUN/g starch;
(2) preparation of amino starch:
adding a silane coupling agent into the starch hydrolysate, adjusting the pH of a system to be 1-5 (v/v) by using acetic acid, controlling the temperature to be 20-60 ℃, performing reflux reaction for 1-5 h, stirring the obtained amino starch solution overnight after the reaction is finished, and then performing freeze drying; carrying out Soxhlet extraction on a freeze-dried sample by taking absolute ethyl alcohol as a solvent, carrying out hot air drying treatment after 5-7 times of siphoning, and controlling the temperature to be 30-60 ℃; obtaining the amino starch.
(3) Preparing nano starch:
mixing the amino starch with 0.1-0.5% (v/v) acetic acid solution to prepare 0.1-1% (w/v) amino starch solution, and adjusting the pH of the system to 2-8 by NaOH. Mixing a surfactant with the solution, controlling the mass ratio of the amino starch to the surfactant to be 2: 1-8: 1, and stirring for 10-20 min (100 rpm); and then carrying out ultrasonic treatment on the solution, wherein the treatment power is 50-150W, the temperature is 0 ℃, the treatment time is 2s, the interval is 5s, the treatment time is 3-10 min, and finally the particle size of the nano starch is 80-500 nm and the surface potential is 20-40 mV.
Wherein the silane coupling agent in the step (2) is KH792 (NH)2(CH2)2NH(CH2)3Si(OCH3)3) Or gamma-aminopropyltriethoxysilane or gamma-aminopropyltrimethoxysilane.
Wherein the surfactant in the step (3) is sodium dodecyl sulfate or sodium dodecyl sulfate.
The invention has the beneficial effects that:
(1) the reaction amount of the amino groups in the amino starch is controlled, so that the control on the granularity of the nano starch can be easily realized;
(2) the preparation of the nano-starch by the surfactant and the amino starch has high efficiency, low energy consumption and easy realization of industrialization.
Detailed Description
Example 1
Preparing 10% (w/v) waxy corn starch milk by using pH-3 acetic acid buffer solution, gelatinizing for 30min at 121 ℃, cooling, adding 240NPUN/g pullulanase for hydrolysis, controlling the DE value of the hydrolysate to be 5, boiling to inactivate enzyme, and cooling to normal temperature for later use.
1% (v/v) of silane coupling agent KH792 (NH)2(CH2)2NH(CH2)3Si(OCH3)3) Mixing and adding into hydrolysate, adjusting pH of the system to 1 with acetic acid, controlling temperature to 60 deg.C, reflux reacting for 5h, stirring the obtained amino starch solution overnight after reaction, and freeze drying; soxhlet extraction is carried out on the amino starch by taking absolute ethyl alcohol as a solvent, hot air drying treatment is carried out after 5 times of siphonage, and the temperature is controlled to be 30 ℃.
An amino starch solution was prepared by dissolving amino starch (0.1%, w/v) in 0.1% (v/v) acetic acid aqueous solution, and the pH of the system was adjusted to 2 with NaOH. Mixing a surfactant (sodium dodecyl sulfate) with the solution, stirring (100rpm) for 10min, and controlling the mass ratio of the amino starch to the surfactant to be 8: 1; and then carrying out ultrasonic treatment on the solution, wherein the treatment power is 150W, the temperature is 0 ℃, the treatment time is 2s, the interval is 5s, the treatment time is 10min, and the particle size of the nano starch is 80nm and the surface potential is 20 mV.
Example 2
Preparing 30% (w/v) waxy corn starch milk by using acetic acid buffer solution with pH of 7, gelatinizing for 30min at 121 ℃, cooling, adding 80NPUN/g pullulanase for hydrolysis for 24h, controlling the DE value of the hydrolysate to be 15, boiling to inactivate enzyme, and cooling to normal temperature for later use.
5% (v/v) of a silane coupling agent KH792 (NH)2(CH2)2NH(CH2)3Si(OCH3)3) Mixing and adding into the hydrolysate, adjusting pH of the system to 5 with acetic acid, controlling temperature to 20 deg.C, refluxing for 1h, stirring the obtained amino starch solution overnight after reaction, and freeze drying; soxhlet extraction is carried out on the amino starch by taking absolute ethyl alcohol as a solvent, hot air drying treatment is carried out after 7 times of siphonage,the temperature was controlled at 60 ℃.
After dissolving amino starch (1%, w/v) in 0.5% (v/v) acetic acid aqueous solution to prepare an amino starch solution, the pH of the system was adjusted to 8 with NaOH. Mixing a surfactant (sodium dodecyl sulfate) with the solution, stirring for 20min (100rpm), and controlling the mass ratio of the amino starch to the surfactant to be 2: 1; and then carrying out ultrasonic treatment on the solution, wherein the treatment power is 50W, the temperature is 0 ℃, the treatment time is 2s, the interval is 5s, the treatment time is 3min, and the particle size of the nano starch is 500nm and the surface potential is 40 mV.
Claims (5)
1. A method for preparing nano starch based on emulsification of aminated starch and surfactant is characterized by comprising the following steps;
(1) starch controlled hydrolysis:
preparing 10-30% waxy corn starch milk by mass to volume ratio with an acetic acid buffer solution with pH = 3-7, gelatinizing for 30min at 121 ℃, cooling, adding pullulanase for hydrolysis for 6-24 h, controlling equivalent weight (DE value) of grapes in the hydrolysate to be 5-15, boiling to inactivate enzyme, and cooling to normal temperature for later use;
(2) preparation of amino starch:
adding a silane coupling agent into the starch hydrolysate, wherein the adding amount is 1-5% by volume, the pH of an acetic acid adjusting system is = 1-5, the temperature is controlled to be 20-60 ℃, reflux reaction is carried out for 1-5 h, the obtained amino starch solution is stirred overnight after the reaction is finished, and then freeze drying is carried out; carrying out Soxhlet extraction on a freeze-dried sample by taking absolute ethyl alcohol as a solvent, carrying out hot air drying treatment after 5-7 times of siphoning, and controlling the temperature to be 30-60 ℃; obtaining amino starch;
(3) preparing nano starch:
mixing amino starch with 0.1-0.5% by volume of acetic acid solution to prepare 0.1-1% by mass of amino starch solution, and adjusting the pH of the system to be 2-8 by NaOH; mixing a surfactant with the solution, controlling the mass ratio of the amino starch to the surfactant to be 2: 1-8: 1, and stirring at the rotating speed of 100rpm for 10-20 min; and then carrying out ultrasonic treatment on the solution to finally obtain the nano starch with the particle size of 80-500 nm and the surface potential of 20-40 mV.
2. The method for preparing nano starch based on the emulsification of aminated starch and surfactant according to claim 1, wherein the pullulanase in step (1) is added in an amount of 80-240 NPUN/g starch.
3. The method for preparing nano starch based on the emulsification of aminated starch and surfactant according to claim 1, wherein the silane coupling agent in step (2) is KH792 (NH)2(CH2)2NH(CH2)3Si(OCH3)3) Or gamma-aminopropyltriethoxysilane or gamma-aminopropyltrimethoxysilane.
4. The method for preparing nano starch based on the emulsification of aminated starch and surfactant according to claim 1, wherein the surfactant in step (3) is sodium lauryl sulfate or sodium lauryl sulfate.
5. The method for preparing nano starch based on the emulsification of aminated starch and surfactant according to claim 1, wherein the ultrasonic treatment power in step (3) is 50-150W, the temperature is 0 ℃, the treatment time is 2s, the interval is 5s, and the treatment time is 3-10 min.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104804200A (en) * | 2015-04-09 | 2015-07-29 | 青岛农业大学 | Process for moderate-temperature self-assembly preparation of nano starch from enzymolysis short amylose |
| CN112321853A (en) * | 2020-11-02 | 2021-02-05 | 广西民族大学 | Crystallinity-controllable starch nanoparticle, preparation method and application |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104804200A (en) * | 2015-04-09 | 2015-07-29 | 青岛农业大学 | Process for moderate-temperature self-assembly preparation of nano starch from enzymolysis short amylose |
| CN112321853A (en) * | 2020-11-02 | 2021-02-05 | 广西民族大学 | Crystallinity-controllable starch nanoparticle, preparation method and application |
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