CN100488986C - Preparation method of dense molecular weight distribution starch product - Google Patents
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Abstract
本发明公开了一种密集分子量分布淀粉产品的制备方法。该方法先将淀粉原料与蒸馏水置于分散装置中处理、真空过滤、干燥；然后添加无水乙醇，均质分散处过滤，加入无水乙醇介质，氧化锆球磨介质，适量十二烷基苯磺酸钠表面活性剂为助磨剂，球磨处理；再将溶液室温静置20～24小时后过滤或离心处理；最后将产物喷雾干燥或在40～45℃烘箱中真空干燥，研磨成粉，即制得密集分子量分布淀粉产品。该方法生产的淀粉产品分子结构发生改变，分子量分布区间明显窄化，导致水溶性、流变性、生物降解性等一系列理化性质变化，扩展了淀粉产品的应用范围；该方法生产成本低、安全、效率高、得率高。The invention discloses a preparation method of a starch product with dense molecular weight distribution. In this method, the starch raw material and distilled water are placed in a dispersing device for processing, vacuum filtered, and dried; then absolute ethanol is added, filtered at the homogeneously dispersed place, anhydrous ethanol medium, zirconia ball milling medium, and an appropriate amount of dodecylbenzenesulfonate are added. Sodium acid surfactant is used as a grinding aid, which is treated by ball milling; then the solution is allowed to stand at room temperature for 20-24 hours and then filtered or centrifuged; finally, the product is spray-dried or vacuum-dried in an oven at 40-45°C, and ground into powder, namely A dense molecular weight distribution starch product is obtained. The molecular structure of the starch product produced by this method changes, and the molecular weight distribution range is obviously narrowed, resulting in a series of changes in physical and chemical properties such as water solubility, rheology, and biodegradability, and expanding the application range of the starch product; the production cost of this method is low and safe. , High efficiency and high yield.
Description
Technical field
The present invention relates to the preparation of starch product in the technical field of producing of agricultural-food, be specifically related to a kind of preparation method of dense molecular weight distribution starch product.
Background technology
Starch is one of the abundantest natural matter of nature, people can change into the starch in different sorts and source by chemistry, physics or biological method have different properties, the modification product innovation of special purpose, thereby expanded the application performance and the scope of starch product greatly.But, people are when research and preparing various starch matrix novel materials, often ignored the further investigation of starch molecule molecular weight basic characteristic, and the basic theory of the formation mechanism of compact district segment molecule amount distribution serial starch and molecular configuration composition respective change.So-called compact district segment molecule amount distribution starch, promptly the starch product relative molecular mass from the macromolecular material theory, belongs to the speciality polymer category within a distributed area that is rather narrow.The starch polymer of this type, often molecular structure has different significantly with traditional starch product, and then have influence on every important physicochemical property, make starch product may have certain unusual performance, or even the variation of matter, these unusual performances may have great importance to the application of starch matrix novel material.
Some traditional starch conversion method can tentatively change the molecular weight distribution of starch, for example use the effect of sour sex change, heat and relevant enzyme, all can make starch molecule generation degraded to a certain degree, and, then make starch molecule have a more complicated fork structure by graft copolymerization or crosslinking technological.Analyze from the molecular composition aspect, these processing cause the relative variation of a starch and chain starch ingredients content, and the relative molecular mass that has influenced starch molecule to a certain extent distributes.But these technological method main purposes are modifications of starch, and emphasis does not lie in weight distributing characteristic research, and are not the starch series product of product classification with the molecular weight distribution also on the market.
Summary of the invention
The objective of the invention is to overcome the shortcoming of traditional treated starch, a kind of dense molecular weight distribution starch product preparation method is provided.This method can obtain having good physico-chemical property, starch product with low cost, and this base-material can be widely used in normal food, chemical industry articles for use, the type material, particularly at some specific area, can substitute expensive traditional material.
Purpose of the present invention is achieved through the following technical solutions.
A kind of preparation method of dense molecular weight distribution starch product comprises the steps and processing condition:
The first step is 1 kilogram with solid-to-liquid ratio: 4～5 liters starch material and distilled water place diverting device to handle 10～15min, vacuum filtration, dry 36～45h in 40～45 ℃ of baking ovens;
Second step was 1 kilogram with solid-to-liquid ratio: 4～5 liters starch and dehydrated alcohol homogeneous dispersion treatment 10～15min through the first step drying treatment, filter, it is 1 kilogram by solid-to-liquid ratio again: add dehydrated alcohol for 8～10 liters, and the zirconia ball grinding media and an amount of Sodium dodecylbenzene sulfonate tensio-active agent of adding starch butt quality 1% as grinding aid, ball-milling processing 150～200h under normal temperature;
The solution chamber of the 3rd step second step gained is gentle and quiet puts 20～24 hours after-filtration or centrifugal;
The 4th step was pulverized the product spray drying or the vacuum-drying in 40～45 ℃ of baking ovens of the 3rd step gained, promptly made dense molecular weight distribution starch product.
The centrifugal treating in described the 3rd step is that the supernatant liquor after centrifugal is discarded, and the distilled water wash of adding capacity 3 times is to remove the trace soluble impurity that amount of localized heat may be produced under the mechanical force.
In the mass percent concentration of system, described Sodium dodecylbenzene sulfonate tensio-active agent add-on is 0.1～0.3%.
Principle of the present invention:
1, be applicable to that raw material of the present invention mainly is a native starch, the quality of raw material itself and granular size have certain influence to the quality transitivity of finished product, also cause the difference of manufacturing cost.Key of the present invention is that the mechanical force of raw material is handled, and the design of effect system has material impact to the quality of whole prod, because it influences the performance fully of the limit degree and the Mechanochemical Effect of mechanical force.In addition, the protection of effect system, effective discharge of heat is the yield even the success or failure of remarkably influenced product also.In general, utilize this production method, the yam starch that grain diameter is bigger (15～120 μ m), the crystal form structure that it is initial, can change amorphous structure completely into, its meso-position radius drops to about 4.5 μ m from 38.48 μ m, 50.0% grain graininess is below 5 μ m, the chain starch content rises to about 27% from 17%, the variation of these molecular structures and component directly causes the macromole in the product significantly to reduce even disappears, the molecular weight distribution section sharply narrows, and the obtained unimodal molecular weight interval of using different raw materials is 40000～60000, other starch product of 90000～100000 grades.
2, starch has crystalline texture, is made up of a chain starch and a starch, and the molecular chain of a chain starch and a starch is arranged the duplex conformation that has constituted starch molecule.Chain starch molecule amount is less, and a starch molecule amount is bigger, and straight chain is different with branched-chain component content in the different starch, makes molecular weight distribution have difference, and then influences its applicability.In the industrial or agricultural field, the multiple physico-chemical property of starch, essence all has suitable cognation with the molecular weight distribution of starch.On perfect molecular weight distribution corresponding theory basis, the Biofunctional materials of exploitation different application purpose, polymer materials, composite high-performance energy material, filamentary material have stronger specific aim.For example, the investigator finds that ventilation property, transparency, the processing characteristics of agricultural film are related with the material molecular weight distribution both at home and abroad, China region is wide, it is totally different that north-south climate differs, therefore, binding molecule amount distribution corresponding theory and guides and develops the agricultural film that different areas are suitable for and can save resource, promote agricultural foison, is of value to national long-term stability and national sustained economic development.In addition, on direct products used, the required starch standard specimen of instrument micrometric measurements such as chromatogram had strict demand to the molecular weight size, and these standard specimens require high to sources of initial raw materials, refining through multiple operation, are worth very high.If the series product that can obtain various molecular weight requirements smoothly can effectively reduce the cost of scientific research and analytical test.Fat mimetic also is to adopt enzymatic degradation of starch, and degraded starch particulate mean diameter is at 2～5 μ m, and the starch product that is generated has the fine and smooth mouthfeel of fat, can partly replace fat in some food, and its structure has the molecular weight distribution of higher density.Comprehensively it seems, this technology at first is based on the starch science theory, compact district segment molecule amount distribution of products at the synthetic different series of different application, not only opened up deeply this area research degree of depth, and, have good scientific research value and social development meaning for high-performance biology and matrix material provide good prospects for application.
3, the collision of mechanical force, impact cause the granularity of material particles to diminish, specific surface area increases, but in granularity gradually in the process of refinement, if material can not get abundant dispersion, can under same mechanical force (also having other effect simultaneously), impel the reunion of material particles so again as model ylid bloom action, electrostatic double layer electrostatic interaction etc., from and increase apparent particle size, reduce specific surface area.Therefore, can think that the mechanical force process after to a certain degree, is accompanied by the qualitative change of physicochemical property on a series of particle microcosmic, the reversing process that a refinement is reunited will occur.When the speed of these positive and negative two processes equates, just reached running balance, the grain graininess value of reaching capacity, at this moment, further the prolonged mechanical power effect time is futile, and the higher breaking tenacity of material because mechanical force at this moment has been not enough to contend with can only be used to keep this running balance.In order to realize the present invention better, according to the degree that requires of material particles character and highly dense section, the required mechanical force time is different.
The starch product that the compact district segment molecule amount that the present invention produces distributes, the starch granules size is near nano level under limiting case, and great changes will take place for physico-chemical property, as cold water solubles etc., should corresponding adjustment in manipulation technology.Ultimate aim is according to the requirement of different molecular weight distribution section, the superior prod of controlled production different application performance.
The present invention compares with existing traditional starch conversion production technology, has following advantage and beneficial effect:
(1) the present invention is with a kind of special technology, and producing with the molecular weight distribution section is the starchbased product of classification, thereby has solved the deficiency that existing starch product is divided, and is with a wide range of applications in the starch industry field;
(2) adopt mechanical force as main means, avoided employing industrial chemicals building-up reactions, thereby simplified production technique and cost, safety and environmental protection efficient height more helps the application prospect on related industries;
(3) the present invention both can produce traditional starch application products, also can produce high performance special material, biomaterial, polymer composite, and production cost is low, added value is high.
(4) the present invention produces the raw materials used agricultural-food of natural reproducible that are, has both improved the added value of agricultural byproducts, is fit to the strategic planning of national sustainable development again, has very high social benefit and economic benefit, has also enriched the research field of starch science simultaneously.
Embodiment
In order to understand the present invention better, the invention will be further described below in conjunction with embodiment, but the scope of protection of present invention is not limited to the scope that embodiment represents.
Embodiment 1:
The first step is added distilled water with yam starch 500g in the solid-to-liquid ratio of kg/liter and is placed APV1000 type clarifixator (also can be other diverting device) to handle 15min, vacuum filtration, dry 45h in 40 ℃ of baking ovens at 1: 4; To guarantee the abundant dispersion of starch granules, in order to the performance fully of back Mechanochemical Effect.
Second step is in the above-mentioned process starch of drying treatment, solid-to-liquid ratio in kg/liter is added dehydrated alcohol at 1: 4, homogeneous dispersion treatment 15min, in the solid-to-liquid ratio of kg/liter be 1: 8 add anhydrous ethanol medium and 5g zirconia ball grinding media thereafter, and in 0.3% mass percent concentration, adding the SDS tensio-active agent is grinding aid, ball-milling processing 150h under normal temperature.
Go up that the solution chamber of step gained is gentle and quiet puts 20 hours after-filtration the 3rd step;
The 4th supernatant liquor of step after centrifugal discards, and adds the distilled water wash 3 times of capacity again, to remove the trace soluble impurity that amount of localized heat may be produced under the mechanical force.
The 5th step is dry in 40 ℃ of baking ovens with the product of gained, pulverizes, and promptly gets the 484g dense molecular weight distribution starch product.Through this product molecular weight distribution section of molecular gel chromatogram test analysis 90000～100000.
After tested, compare with ative starch, this starch sample changes non-crystalline state into by polycrystalline state, and spirane structure becomes loose (X-ray diffraction test), and the chain starch content increases to 27.2% by 17.3%, and specific surface area is by 0.33m
2/ g increases to 9.13m
2/ g, solubleness increases to 88.22% by 0.54% under 40 ℃, and microbial process is 30d altogether, and remaining starch content reduces to 15.6% by 81.5%.The net carbon dioxide formation speed is far longer than ative starch, especially at degraded initial stage 0～6d, reaches peak value when about 3d.
Embodiment 2:
The first step with yam starch 500g in kilogram: the solid-to-liquid ratio 1:5 that rises meter adds distilled water and places MZS type clarifixator to handle 12min, vacuum filtration, dry about 36h in 45 ℃ of baking ovens;
Second step is in the above-mentioned process starch of drying treatment, in kilogram: the solid-to-liquid ratio 1:5 that rises meter adds dehydrated alcohol, homogeneous dispersion treatment 12min, thereafter in kilogram: the solid-to-liquid ratio that rises is that 1:10 adds anhydrous ethanol medium, 5g zirconia ball grinding media, 0.1% mass percent concentration SDS tensio-active agent is a grinding aid, ball-milling processing 200h under normal temperature.
The 3rd step go up the solution chamber of step gained gentle and quiet put after 22 hours centrifugal;
The product cold water solubles is found in the test of the 4th step.
The 5th step promptly got the 489g dense molecular weight distribution starch product with the product spray drying of gained.Through this product molecular weight distribution section of molecular gel chromatogram test analysis 40000～60000.
After tested, compare with ative starch, this starch sample changes non-crystalline state into fully by polycrystalline state, and spirane structure becomes loose (X-ray diffraction test), and the chain starch content increases to 27.5% by 17.3%, and specific surface area is by 0.33m
2/ g increases to 9.04m
2/ g, solubleness increases to 92.56% by 0.54% under 40 ℃, and microbial process is 30d altogether, and remaining starch content reduces to 13.8% by 81.5%.The net carbon dioxide formation speed is far longer than ative starch, especially at degraded initial stage 0～6d, reaches peak value when about 3d.
Embodiment 3:
The first step with 500g W-Gum raw material in kilogram: the solid-to-liquid ratio that rises meter is added distilled water and is placed MZS type clarifixator to handle 10min, vacuum filtration, dry 40h in 43 ℃ of baking ovens at 1: 4.5;
Second step is in the above-mentioned process starch of drying treatment, in kilogram: the solid-to-liquid ratio 1:5 that rises meter adds dehydrated alcohol, homogeneous dispersion treatment 10min, thereafter in kilogram: the solid-to-liquid ratio that rises is that 1:8 adds anhydrous ethanol medium, 5g zirconia ball grinding media, 0.3% mass percent concentration SDS tensio-active agent is a grinding aid, ball-milling processing 150h under normal temperature.
Go up that the solution chamber of step gained is gentle and quiet puts 24 hours after-filtration the 3rd step;
The 4th supernatant liquor of step after centrifugal discards, and adds the distilled water wash 2 times of capacity again, to remove the trace soluble impurity that amount of localized heat may be produced under the mechanical force.
The 5th step is dry in 40 ℃ of baking ovens with the product of gained, pulverizes, and promptly gets the 485g dense molecular weight distribution starch product.Through this product molecular weight distribution section of molecular gel chromatogram test analysis 120000～160000.
After tested, compare with ative starch, this starch sample changes non-crystalline state into by polycrystalline state, and spirane structure becomes loose (X-ray diffraction test), and the chain starch content increases to 31.3% by 26.5%, and specific surface area is by 0.54m
2/ g increases to 5.67m
2/ g, solubleness increases to 85.33% by 0.76% under 40 ℃, and microbial process is 30d altogether, and remaining starch content reduces to 26.4% by 85.6%.The net carbon dioxide formation speed is far longer than ative starch, especially at degraded initial stage 0～10d, reaches peak value when about 8d.
Embodiment 4:
The first step with 500g W-Gum raw material in kilogram: the solid-to-liquid ratio 1:5 that rises meter adds distilled water and places APV1000 type clarifixator to handle 13min, vacuum filtration, dry 38h in 42 ℃ of baking ovens;
Second step is in the above-mentioned process starch of drying treatment, in kilogram: the solid-to-liquid ratio 1:5 that rises meter adds dehydrated alcohol, homogeneous dispersion treatment 15min, thereafter in kilogram: the solid-to-liquid ratio that rises is that 1:9 adds anhydrous ethanol medium, 5g zirconia ball grinding media, 0.2% mass percent concentration SDS tensio-active agent is a grinding aid, ball-milling processing 180h under normal temperature.
The 3rd step go up the solution chamber of step gained gentle and quiet put after 24 hours centrifugal;
The 4th supernatant liquor of step after centrifugal discards, and adds the distilled water wash 4 times of capacity again, to remove the trace soluble impurity that amount of localized heat may be produced under the mechanical force.
The 5th step is dry in 40 ℃ of baking ovens with the product of gained, pulverizes, and promptly gets the 491g dense molecular weight distribution starch product.Through this product molecular weight distribution section of molecular gel chromatogram test analysis 110000～140000.
After tested, compare with ative starch, this starch sample changes non-crystalline state into by polycrystalline state, and spirane structure becomes loose (X-ray diffraction test), and the chain starch content increases to 31.5% by 26.5%, and specific surface area is by 0.54m
2/ g increases to 5.45m
2/ g, solubleness increases to 87.27% by 0.76% under 40 ℃, and microbial process is 30d altogether, and remaining starch content reduces to 24.6% by 85.6%.The net carbon dioxide formation speed is far longer than ative starch, especially at degraded initial stage 0～10d, reaches peak value when about 8d.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1161045A (en) * | 1994-09-29 | 1997-10-01 | 弗雷泽纽斯股份公司 | Method for producing starch degradation products |
| US20020065411A1 (en) * | 2000-10-06 | 2002-05-30 | Gustavsson Nils Ove | Starch |
| CN1392159A (en) * | 2001-06-14 | 2003-01-22 | 梅世昌 | Process for preparing medical starch with narrowly distributing molecular weight |
| US20040096560A1 (en) * | 1995-06-06 | 2004-05-20 | Iowa State University Research Foundation, Inc. | Nutritional products containning modified starches |
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2006
- 2006-11-27 CN CNB2006101237927A patent/CN100488986C/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1161045A (en) * | 1994-09-29 | 1997-10-01 | 弗雷泽纽斯股份公司 | Method for producing starch degradation products |
| US20040096560A1 (en) * | 1995-06-06 | 2004-05-20 | Iowa State University Research Foundation, Inc. | Nutritional products containning modified starches |
| US20020065411A1 (en) * | 2000-10-06 | 2002-05-30 | Gustavsson Nils Ove | Starch |
| CN1392159A (en) * | 2001-06-14 | 2003-01-22 | 梅世昌 | Process for preparing medical starch with narrowly distributing molecular weight |
Non-Patent Citations (2)
| Title |
|---|
| 淀粉与淀粉制品工艺学. 高嘉安，5,12,19，中国农业出版社. 2001 |
| 淀粉与淀粉制品工艺学. 高嘉安，5,12,19，中国农业出版社. 2001 * |
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