CN103224566A - New technology for raising crystallization degree of starch nanoparticles by heat-moisture treatment - Google Patents
New technology for raising crystallization degree of starch nanoparticles by heat-moisture treatment Download PDFInfo
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- CN103224566A CN103224566A CN2013101623062A CN201310162306A CN103224566A CN 103224566 A CN103224566 A CN 103224566A CN 2013101623062 A CN2013101623062 A CN 2013101623062A CN 201310162306 A CN201310162306 A CN 201310162306A CN 103224566 A CN103224566 A CN 103224566A
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Abstract
The invention discloses a new method for raising crystallization degree of starch nanoparticles by a heat-moisture treatment. The new method comprises the following steps: fully mixing starch nanoparticles prepared by various methods with certain distilled water, sealing under the high-temperature condition for a certain period of time after moisture is balanced, and carrying out vacuum freeze drying to obtain starch nanocrystals with high crystallization degree. The technology provided by the invention is simple to operate, has high production efficiency, and is suitable for starch nanoparticles prepared by various methods. The prepared starch nanocrystals with high crystallization degree have high physical strength and stable chemical properties. After the starch nanocrystals are added into a membrane material, mechanical strength of the material is obviously raised, and moisture resistance and water resistance are improved.
Description
Technical field
The invention provides the novel method that improves starch nanometer granule degree of crystallinity in the mode of wet heat treatment, belong to the nano structural material technical field.
Background technology
[0002] nano material is the following material that has development prospect most, and its potential importance is unquestionable.Along with the continuous maturation and the development of technology, there has been increasing people to pay attention to exploitation and used natural nano-material.
Starch is natural biomacromolecule, have the low characteristics of wide material sources, biodegradable, good biocompatibility and cost, with it is that the synthetic materials of raw material can be by biodegradable advantage, is that the nanotechnology of raw material will become the most important thing in the research coming years with starch.Degree of crystallinity is to weigh an important indicator of starch nanometer granule, the nano particle of high-crystallinity, and physical strength is big, and chemical property is stable, does not also have a kind of effective ways that improve degree of crystallinity at present.
In recent years, adopt the mineral acid hydrolysis starch granules to prepare starch nanometer granule, Jean-Luc Putaux etc., have made output and have been approximately the 0.5%(massfraction about 40 days with the high salt concentration acid hydrolysis) starch nano crystal grain, its degree of crystallinity is about 65%; H é lene Angellier etc. prepare starch nano crystal grain by optimizing acidolysis condition, adopt the sulfuric acid of 3.16mol/L in 40 ℃ of silicon are bathed, to stir 5 days, output has been brought up to the 15%(massfraction), and prepare nano composite material among applying it to enhancing natural rubber, thermoplastic starch and poly(lactic acid), degree of crystallinity brings up to 70% simultaneously; Delong Song etc. adopt the mode of extruding that starch is mixed with water and glycerine, are placed in the twin-screw formula squeezer, prepare degree of crystallinity at 2～4% starch nanometer granule; Sun Qingjie etc. utilize the pars amorpha of biological enzyme hydrolysis starch granules, prepare starch nano crystal grain by physical means such as ultrasonic wave then, and degree of crystallinity is increased to 40%; With the starch debranching of biological enzyme after to gelatinization, recrystallization obtains nano particle to Sun Qingjie etc. first, though its output reaches more than 95%, its degree of crystallinity also has only 35%.
The present invention will provide a kind of method of raising starch nanometer granule degree of crystallinity of high-efficiency environment friendly, i.e. damp and hot the or dry heat treatment of nano-scale particle to obtaining.Under hot conditions, relative displacement takes place between the starch molecular chain, the molecule interchain forms more hydrogen bond, and degree of fitting increases, and finally obtains degree of crystallinity and be the starch nano crystal more than 85%, and is higher more than 50% than ative starch degree of crystallinity.The technical solution adopted in the present invention is: to the starch nanometer granule equilibrium water content that experiment obtains, and the sealing pyroprocessing, after reaction for some time, lyophilize obtains nanometer starch crystal.
Nanometer starch crystal is a kind of good nano-composite material, it joined in the thermoplastic composite film, and mechanical property that not only can strongthener, and can reduce the water vapour and the oxygen perviousness of material.By wet heat treatment, effectively improve the ordered arrangement of starch molecular chain, make the easier formation of hydrogen bond between the starch molecular chain, improve the degree of crystallinity of nano particle.The nanometer starch crystal of preparing in addition and the nano composite material of thermoplastic starch, research each component content is to the laminated film Effect on Performance, the result shows the starch nanometer granule that adds high-crystallinity, has improved the mechanical property and the barrier property of thermoplastic starch greatly.
The present invention has the following advantages: 1. simple to operate, be fit to scale operation; 2. production unit there is not corrosion; 3. production efficiency height; 4. do not add any inorganic reagent, edible in producing.
Embodiment
The present invention is achieved like this, and the preparation process method is:
(1) determination of moisture: get a certain amount of starch nanometer granule, place the determination of moisture instrument, measure its moisture content;
(2) regulate moisture content: the moisture content fixed according to last pacing, in starch nanometer granule, add a certain amount of distilled water, moisture content to 15～25% of control starch nanometer granule mixes;
(3) equilibrium water content: the starch nanometer granule constant temperature that mixes is stored 12h;
(4) wet heat treatment: will go up starch nanometer granule sealing that the step prepares be kept at 100～150 ℃ 10～15 hours down, take out, freeze-drying obtains the nanometer starch crystal of high-crystallinity.
Can prepare environmental protection according to this step, the degree of crystallinity height, the nanometer starch crystal of stable in properties, used laboratory apparatus is simple, is easy to achievements conversion, and this preparation method all can obviously improve the degree of crystallinity of the starch nanometer granule that the whole bag of tricks makes.
Be described further below in conjunction with the invention of example, but the present invention is not limited only to these examples a kind of novel environment friendly nanometer starch crystal biological preparation method.
Embodiment 1
Take by weighing the starch nanometer granule that 20g makes through sulphuric acid hydrolysis with waxy corn starch, in powder, spray a certain amount of distilled water, mix, 4 ℃ left standstill 10 hours, the control moisture content is 20%, airtightly place in the high-pressure sterilizing pot 121 ℃ to keep 5 hours it again, take out after vacuum lyophilization can obtain the nanometer starch crystal that degree of crystallinity obviously improves.
Embodiment 2
Taking by weighing 15g is raw material with the Starch rice, the starch nanometer granule that adopts the enzymolysis pars amorpha to make through ultrasonic disruption, measure its moisture content, calculate the quality of answering adding distil water then, in powder of nanometric particles, spray distilled water, the control moisture content is 15%, handles 10 hours at 100 ℃ of lower seals, takes out vacuum lyophilization and obtains nanometer starch crystal.
Embodiment 3
Taking by weighing 25g is raw material with glutinous property yam starch, enzyme takes off and props up the starch nanometer granule that recrystallization makes again after the employing starch pasting, at first measure moisture content, adding distilled water then makes the moisture content of starch nanometer granule remain on 20%, mix, the room temperature sealing is preserved and is spent the night, and the starch nanometer granule with sealing places high-pressure sterilizing pot to handle 4 hours down for 121 ℃ again, takes out the degree of crystallinity of final vacuum lyophilize can obviously raising starch nanometer granule.
Adopt the starch nanometer granule of the certain moisture content of pyroprocessing, obtain degree of crystallinity and be 60～85% nanometer starch crystal, increase substantially the degree of crystallinity of starch nanometer granule, particulate hardness and chemical stability are obviously improved, its range of application that enlarges, be fit to large-scale industrialized production, for the production application of nano material provides efficient strong approach.
Claims (2)
1. new technology that adopts wet heat treatment to improve starch nanometer granule degree of crystallinity, it is characterized in that having following characteristics: the starch nanometer granule that can adopt the whole bag of tricks to make is a raw material, its degree of crystallinity improves more than 50% after the wet heat treatment.
2. method for preparing the nanometer starch crystal of high-crystallinity as claimed in claim 1, this method is carried out as follows:
(1) determination of moisture: get a certain amount of starch nanometer granule, place the determination of moisture instrument, measure its moisture content;
(2)Regulate moisture content: the moisture content fixed according to last pacing, in starch nanometer granule, add a certain amount of distilled water, moisture content to 15～25% of control starch nanometer granule mixes;
(3)Equilibrium water content: the starch nanometer granule constant temperature that mixes is stored 12h;
(4)Wet heat treatment: will go up starch nanometer granule sealing that the step prepares be kept at 100～150 ℃ 10～15 hours down, take out, freeze-drying obtains the nanometer starch crystal of high-crystallinity;
In the present invention, raw material is the starch nanometer granule of prepared in various methods, can adopt high-pressure sterilizing pot to handle 4～6 hours down during wet heat treatment at 121 ℃, also can be in 90～100 ℃ of baking ovens encapsulation process 10～12 hours, its purpose is that high temperature can make starch molecular chain be subjected to displacement, form more hydrogen bond, degree of crystallinity increases, and particulate hardness just can increase.
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| CN201310162306.2A CN103224566B (en) | 2013-05-06 | 2013-05-06 | A kind of method adopting wet heat treatment to improve starch nanometer granule degree of crystallinity |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN108341886A (en) * | 2018-03-01 | 2018-07-31 | 浙江大学 | A kind of humid heat treatment technique obtaining nanometer starch crystal from ative starch |
| CN112321853A (en) * | 2020-11-02 | 2021-02-05 | 广西民族大学 | Crystallinity-controllable starch nanoparticle, preparation method and application |
| CN114621359A (en) * | 2022-03-23 | 2022-06-14 | 青岛农业大学 | Steam blanching modified starch and preparation method and application thereof |
| CN115044106A (en) * | 2022-06-30 | 2022-09-13 | 青岛农业大学 | Preparation method of anti-ultraviolet high-strength starch nano composite film |
Citations (2)
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| WO2000073352A1 (en) * | 1999-05-28 | 2000-12-07 | The Penn State Research Foundation | Manufacture of boiling-stable granular resistant starch by acid hydrolysis and hydrothermal treatment |
| JP2004267119A (en) * | 2003-03-10 | 2004-09-30 | Makoto Fujii | Method and apparatus for treating starch-based farm product, and product treated thereby |
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2013
- 2013-05-06 CN CN201310162306.2A patent/CN103224566B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2000073352A1 (en) * | 1999-05-28 | 2000-12-07 | The Penn State Research Foundation | Manufacture of boiling-stable granular resistant starch by acid hydrolysis and hydrothermal treatment |
| JP2004267119A (en) * | 2003-03-10 | 2004-09-30 | Makoto Fujii | Method and apparatus for treating starch-based farm product, and product treated thereby |
Non-Patent Citations (3)
| Title |
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| 任丽丽: "淀粉纳米晶的改性及其在热塑性淀粉复合材料中的应用", 《中国优秀博士学位论文全文数据库 工程科技Ⅰ辑》, no. 9, 15 September 2012 (2012-09-15), pages 024 - 8 * |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN104804200B (en) * | 2015-04-09 | 2017-08-29 | 青岛农业大学 | The short middle temperature self assembly of amylose of one kind enzymolysis prepares nano-starch technique |
| CN108341886A (en) * | 2018-03-01 | 2018-07-31 | 浙江大学 | A kind of humid heat treatment technique obtaining nanometer starch crystal from ative starch |
| CN112321853A (en) * | 2020-11-02 | 2021-02-05 | 广西民族大学 | Crystallinity-controllable starch nanoparticle, preparation method and application |
| CN114621359A (en) * | 2022-03-23 | 2022-06-14 | 青岛农业大学 | Steam blanching modified starch and preparation method and application thereof |
| CN115044106A (en) * | 2022-06-30 | 2022-09-13 | 青岛农业大学 | Preparation method of anti-ultraviolet high-strength starch nano composite film |
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| CN103224566B (en) | 2016-04-06 |
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