CN101857665A - Fully-degradable starch hydrogel and preparation method thereof - Google Patents
Fully-degradable starch hydrogel and preparation method thereof Download PDFInfo
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Abstract
The invention relates to fully-degradable starch hydrogel and a preparation method thereof. The fully-degradable starch hydrogel comprises the following components: starch, free radical polymeric monomer, a crosslinking agent and a water soluble free-radical cycle combination initiator. The preparation method comprises the following steps: preparing the starch into a suspending liquid with a high concentration, and pre-pasting the suspending liquid; adding the free radical polymeric monomer, the crosslinking agent, and the water soluble free-radical cycle combination initiator; polymerizing; cutting up; drying; and at last, crushing to obtain the fully-degradable starch hydrogel. The invention has the beneficial effects that the mass fraction of the fully-degradable starch hydrogel is larger than 30% by weight; since the concentration of the starch suspending liquid is high and the pre-pasting temperature is low, the fully-degradable starch hydrogel is suitable for a plurality of starches; since the cycle combination initiator is used, the using amount of cerium is greatly lower than the conventional using amount of graft reaction, and the product has excellent repeatedly water-absorbing and water conserving properties and high gel strength; the main production raw materials of the invention are abundantly reserved. The invention has the advantages that short processing flow is short, environment pollution does not occur in the preparation process, the investment is saved, the large-scale production is beneficial and the like.
Description
Technical field
The present invention relates to a kind of fully-degradable starch hydrogel and preparation method thereof.
Background technology
Under the deficient day by day overall background of petroleum resources, effectively utilize reproducible natural polymer, prepare super absorbent resin or water-holding agent as biological materials such as starch, Mierocrystalline cellulose, chitosan, sodium alginates, become the focus of research.
Starch is class natural polymer commonly used.Publication number is CN1554684A, denomination of invention discloses a kind of preparation method of powerful starch system water absorbing and preserving for " preparation method of the simple and easy gelatinization super water-absorbing water-retaining agent of starch ", this preparation method is made of gelatinization step and polymerization procedure, and initiator is single graft copolymerization evocating agent; Publication number is CN1408741A, denomination of invention discloses a kind of preparation method of starch base water-holding agent for " preparation method of anti-drought water-retaining agent ", this method adds 10～30% starch and 15～25% water at 80～100 ℃ of following gelatinization 0.5～1h in having the container of stirring, add 40～70% unsaturated vinyl monomers and an amount of initiator during gelatinization postcooling to 30～80 ℃, dispersion agent and linking agent, under nitrogen protection, under 30～80 ℃ of conditions, react 0.5～3.5h, the reaction back is neutralized to pH6.0～8.0 with alkali, through vacuum-drying, make anti-drought water-retaining agent after the pulverizing; Its gelatinization point is 80 degree, and initiator is single graft copolymerization evocating agent.Publication number is that CN1317494A discloses a kind of sweet potato high water absorption graft starch and production method thereof, this method is selected sweet potato starch, industrial spirit, vinylformic acid, N, N-methylene diacrylamine, ferrous ammonium sulphate, ceric ammonium nitrate, potassium permanganate, manganese sulfate, sodium polyphosphate and sodium hydroxide are raw material, initiator is the combination of ceric ammonium nitrate and potassium permanganate, and carries out the high temperature gelatinization.Publication number position CN101045776A etc. discloses a kind of method of synthesizing high water absorption resin by glutinous wheat starch, and this method is a raw material with Waxy wheat starch, Acrylic Acid Monomer, adopts the ammonium persulfate initiator that is of little use.
The usage quantity of natural polymer starch is lower in the above traditional biomass high-absorbent material, is 10wt%～15wt%, among the preparation technology, or adopts 80～100 ℃ high temperature gelatinization technology, or adopts single graft copolymerization evocating agent.
Summary of the invention
Problem to be solved by this invention is that proposing a kind of at above-mentioned prior art is main basic substance with starch, energy complete biodegradable, the fully-degradable starch hydrogel that cost is low, liquid absorbency rate is high.
Another object of the present invention provides the preparation method of above-mentioned fully-degradable starch hydrogel, and this preparation technology is simple.
The present invention for the solution that problem adopted of the above-mentioned proposition of solution is: fully-degradable starch hydrogel, it is characterized in that including following component: starch, free yl polymerizating monomer, linking agent and water-soluble free radical circulation composite initiator, described components contents is: the interpolation weight of starch is 0.5～4.5 times of free yl polymerizating monomer, the interpolation weight of linking agent is 0.05%～0.70% of free yl polymerizating monomer, described water-soluble free radical circulation composite initiator is cerous ammonium nitrate and persulphate circulation composite initiator, wherein Ce
4+Addition be 0.005%～0.10% of free yl polymerizating monomer amount of substance, S
2O
8 2-Addition be Ce
4+0.5～10 times of amount of substance.
Press such scheme, described component also includes alkali, and the addition of alkali is 40%～90% (degree of neutralization) of free yl polymerizating monomer amount of substance.
Press such scheme, described components contents is preferably: the interpolation weight of starch is 0.8～2.0 times of free yl polymerizating monomer; The interpolation weight of linking agent is 0.08%～0.30% of free yl polymerizating monomer; The addition of alkali is 60%～85% of a free yl polymerizating monomer amount of substance; Ce
4+Addition be 0.01%～0.05% of free yl polymerizating monomer amount of substance; S
2O
8 2-Addition be Ce
4+1～5 times of amount of substance.
Press such scheme, described free yl polymerizating monomer is any one or more than one the mixture in vinylformic acid, acrylate, acrylamide, 2-acrylamido-2-methyl propane sulfonic acid and 2-acrylamido-2-methyl propane sulfonic acid salt, described linking agent is N, N '-methylene-bisacrylamide.
Preparation method's of the present invention technical scheme is characterized in that including following steps:
1) get material: the interpolation weight of starch is 0.5～4.5 times of free yl polymerizating monomer, the interpolation weight of linking agent is 0.05%～0.70% of free yl polymerizating monomer, described water-soluble free radical circulation composite initiator is cerous ammonium nitrate and persulphate circulation composite initiator, wherein Ce
4+Addition be 0.005%～0.10% of free yl polymerizating monomer amount of substance, S
2O
8 2-Addition be Ce
4+0.5～10 times of amount of substance is chosen above-mentioned raw materials;
2) preparation technology and condition: starch is mixed with high-concentration suspension liquid carries out pre-gelatinization: carry out pre-gelatinization 5～100 minutes at 20～80 ℃, add free yl polymerizating monomer, linking agent and water-soluble free radical circulation composite initiator, 30～70 ℃ of polymerizations 4～8 hours, chopping, drying obtains fully-degradable starch hydrogel through pulverizing at last.
Press such scheme, also be added with alkali, the addition of alkali is 40%～90% of a free yl polymerizating monomer amount of substance.
Press such scheme, the compound method of described high-concentration suspension liquid is: it is the suspension of 20wt%～50wt% that starch and water are mixed the concentration that is made into.
Press such scheme, preferred suspension concentration is 25wt%～35wt%.
Press such scheme, preferably 40～70 ℃ of pre-gelatinizations 10～30 minutes.
Press such scheme, described drying is meant at 50～100 ℃ carries out drying.
Introduce the present invention below in detail:
1. starch
All organs of most of higher plants all contain starch, and these organs that contain starch have the endosperm of pollen, leaf, stem, bulb, rhizome, fruit, flower and pericarp, cotyledon, embryo and seed.Except that higher plant, in liver moss, pteridophyte, some protozoon, algae and bacterium, also can find starch.Regardless of originating, the starch of all natural formation is tiny particle, and every kind of starch has its inherent characteristic, as shape and size, can distinguish the source of starch by microscope.Commodity starch can be divided three classes: the first kind comprises stem (potato), piece root (cassava, the root of kudzu vine and sweet potato) and marrow (sago) starch; Second class comprises common cereal starch (corn, wheat, Chinese sorghum and rice), and this two kind of starch all has obvious different on chemical ingredients and physical properties; The 3rd class comprises wax (being glutinous property) starch (waxy corn, wax Chinese sorghum and wax rice), though these waxy starches extract from cereal, its physical properties is more similar to root starch.
(1) W-Gum (Maize Starch) corn starch granules size is medium, is shaped as circle and polygon.The 1Kg W-Gum contains 1 * 10
12Individual particle, the specific surface area of W-Gum are 300m
2/ Kg.The U.S. produces the maximum country of W-Gum in the world, accounts for more than 75% of the total starch yield in the world, and about 70% W-Gum is converted into maize treacle and glucose.
(2) yam starch (Potato Starch) potato starch particle is oval, and tangible wheel line is arranged around eccentric omphalion, and the particle diameter of yam starch is big (15～100 μ m), and yam starch producing country mainly concentrates on European countries in the world.Potato starch product is used for food, paper, textiles, tackiness agent and drilling mud more.
(3) tapioca (flour) (Tapioca Starch) tapioca (flour) particle is a circle circular or that an end blocks, and tapioca (flour) is from the root manufacturing of cassava plant, and main product is in Thailand, Brazil, Philippines, Nigeria, Malaysia and Angola.Tapioca (flour) is a kind of typical starchy roots, is usually used in the production of food and tackiness agent.
(4) waxy corn starch (Waxy Maize Starch) waxy corn starch particle shape is similar to corn starch granules, is circle or polygon.Waxy corn originates in China, is introduced a large amount of plantations in back by the U.S., is a kind of rex of conventional corn plant, and this starch granule does not contain amylose molecule, only contains amylopectin.When using iodinate, be red-purple, be blue look unlike conventional corn starch.Cut with the hilt corn particle, cut surface is as the gloss of the content of wax, and waxy corn hence obtains one's name.Waxy corn starch is used for making the thickening material of tackiness agent and foodstuffs industry more.
(5) wheat starch (Wheat Starch) wheat starch granule particle size range is wider, and in the majority with less spheroidal particle (2～10 μ m) and bigger spheroidal particle (20～35 μ m), and wheat starch is byproducts of making wheat gluten in many countries.Wheat starch is usually used in the production of bakery product industry and tackiness agent.
(6) sorghum starch (Milo Starch) sorghum starch particle is polygon and circle, and its character is similar to conventional corn starch.In the U.S., a small amount of sorghum starch is converted into glucose syrup.The wax sorghum starch extracts from the wax Chinese sorghum, and its character is very similar to waxy corn starch.
(7) Starch rice (Rice Starch) Starch rice is all commodity starch particle minimums, and its particle is tending towards concentrating in groups, and it is raw materials used for producing impaired broken rice in the rice food milling that great majority are made Starch rice.Starch rice can be used as the face powder in pudding and ice-cream thickening material, the makeup.
(8) sago starch (Sago Starch) sago starch is bigger oval particle, is to be made by the sago palm tree, mainly originates in Indonesia.Contain adularescent, softish amylasceous substance in the sago marrow, sago starch extracts from these marrows exactly.Sago starch can be used in pudding, candy and the textiles.
(9) pueraria starch (Arrowroot Starch) pueraria starch is that root by special horse traction tower (Maranta) makes through wet milling process, mainly originates in the special island of Vincent in the West Indies, particularly Caribbean.The amount of finish of pueraria starch is very little, is mainly used in the processing of a few food (biscuit, pudding etc.).
(10) grain diameter bigger (15～55 μ m) of sweet potato starch (Sweet Potato Starch) sweet potato starch, gelatinization point is lower, and gellifying property is good.
The present invention can be a raw material with above any kind of starch, is good with W-Gum and tapioca (flour), and the interpolation weight of starch is 0.5-4.5 times of free yl polymerizating monomer, preferred 0.8～2.0 times.
2. free yl polymerizating monomer
The present invention selects water-soluble free yl polymerizating monomer for use, it is characterized by to contain the carbon-carbon double bond that Raolical polymerizable can take place.The weight concentration of free yl polymerizating monomer in aqueous solution is 10～40wt%, preferred 20～30wt%.
When described free yl polymerizating monomer is organic acid, the available bases neutralization, the addition of alkali is 40%～90% (degree of neutralization) of the amount of organic acidic material.
3. cerous ammonium nitrate and persulphate free radical circulation composite initiator (Ce
4+-S
2O
8 2-)
Ammonium persulphate ((NH
4)
2S
2O
8) can initiation reaction, and finally form gel, but require temperature of reaction higher (more than 70 ℃), and long reaction time.Ce
4+Cause comparatively fast under neutrality or solutions of weak acidity, grafting speed is fast, and effect is better, and the products obtained therefrom water absorbent rate is also the highest.
Ce
4+-S
2O
8 2-The trigger rate of free radical circulation composite initiator is greater than Ce
4+And S
2O
8 2-The independent trigger rate that causes.Water-soluble free radical circulation composite initiator (Ce
4+-S
2O
8 2-) middle Ce
4+Addition be 0.005%～0.10% of free yl polymerizating monomer amount of substance, preferred 0.01%～0.05%, S
2O
8 2-Addition be Ce
4+0.5～4 times of amount of substance, preferred 1～3 times.
4. linking agent
The linking agent per molecule that uses among the present invention contains two polymerisable unsaturated groups at least.Typical linking agent has: bisacrylamide such as N, N '-methylene-bisacrylamide.
The consumption of linking agent is 0.05～0.50% of a free yl polymerizating monomer weight, preferred 0.08～0.30% (weight).
5. liquid absorbency rate measuring method
In the present invention, adopt following method to measure and calculate the liquid absorbency rate of inhaling distilled water, tap water and physiological saline:
The granulated product that takes by weighing after 1.0g drying and the pulverization process places the 500-1000ml beaker, granulated product after adding 1000ml distilled water or 500ml tap water or taking by weighing 1.0g drying and pulverization process places the 150ml beaker to add 100ml0.9%NaCl solution, after leaving standstill 24 hours, with 30 order mesh screens with unnecessary water elimination, weigh up gel quality affects, be calculated as follows water absorbent rate:
Liquid absorbency rate=(gel quality affects-dry glue quality)/dry glue quality.
Beneficial effect of the present invention is: by the fully-degradable starch hydrogel (technical, super absorbent resin and water-holding agent all belong to the hydrogel concept field) that prescription of the present invention and method are produced, massfraction is greater than 30wt%.Because starch suspension concentration height, pre-gelatinization point low (being generally more than 80 degree) is so be applicable to multiple starch; Owing to use circulation composite initiator (Ce
4+-S
2O
8 2-), the cerium consumption is significantly less than common graft reaction consumption, and product has the good performance of water-absorbing-retaining repeatedly, higher gel-strength, biodegradable can be in the effect of fields such as industry, agricultural gardening, daily necessities performance environmental protection water-absorbing material; Main production raw material reserves of the present invention are very abundant, and have technical process weak point, preparation process non-environmental-pollution, reduced investment, are convenient to advantages such as large-scale production.
Description of drawings
Fig. 1 is a tapioca (flour) and by the diffuse reflectance infrared spectroscopy of products therefrom of the present invention, below each embodiment product feature of all having this figure to show.A. tapioca (flour) wherein; B. product;
Fig. 2 is a tapioca (flour) and by products therefrom XRD figure of the present invention, below each embodiment product feature of all having this figure to show.A. tapioca (flour) wherein; B. product.
Embodiment
In order to understand the present invention better, further illustrate content of the present invention below in conjunction with embodiment, but content of the present invention not only is confined to the following examples.
Embodiment 1:
30g tapioca (flour) and 87g water are made into starch suspension (25.6wt%), in 79 ℃ of pre-gelatinizations 10 minutes, be cooled to 40 ℃, add 0.1mmol/ml ceric ammonium nitrate solution 1ml, behind the 10min, add solution (making its degree of neutralization with sodium hydroxide is 70%), 0.02gN that 23g vinylformic acid is made in three batches, N '-methylene-bisacrylamide and lml (50mg/ml) ammonium persulphate, every batch of interval 20 minutes; Be warming up to 60 ℃ of polymerization 4h afterwards.With the chopping of gained jel product, in 50 ℃ of dryings,, get the particulate state finished product again through mechanical disintegration to 0.1～5.0mm, through test, inhale the pure water multiplying power greater than 150 times.
Embodiment 2:
40g tapioca (flour) and 95g water are made into starch suspension (30wt%), in 50 ℃ of pre-gelatinizations 20 minutes, be warming up to 60 ℃, add 0.1mmol/ml ceric ammonium nitrate solution 1ml, behind the 10min, add solution (making its degree of neutralization with sodium hydroxide is 85%), 0.15gN that 23g vinylformic acid is made in three batches, N '-methylene-bisacrylamide and 2ml (50mg/ml) ammonium persulphate, every batch of interval 20 minutes; Be incubated 70 ℃ of polymerization 4h afterwards.With the chopping of gained jel product, in 100 ℃ of dryings,, get the particulate state finished product again through mechanical disintegration to 0.1～5.0mm, through test, inhale the pure water multiplying power greater than 150 times.
Embodiment 3:
60g tapioca (flour) and 120g water are made into starch suspension (33.3wt%), in 35 ℃ of pre-gelatinizations 35 minutes, be warming up to 60 ℃, add 0.1mmol/ml ceric ammonium nitrate solution 1ml, behind the 10min, add solution (making its degree of neutralization with potassium hydroxide is 60%), 0.10gN that 23g vinylformic acid is made in three batches, N '-methylene-bisacrylamide and 4ml (50mg/ml) ammonium persulphate, every batch of interval 20 minutes; Be incubated 60 ℃ of polymerization 8h afterwards.With the chopping of gained jel product, in 70 ℃ of dryings,, get the particulate state finished product again through mechanical disintegration to 0.1～5.0mm, inhale the pure water multiplying power greater than 150 times.
Embodiment 4:
30g W-Gum and 87g water are made into starch suspension (25.6wt%), in 20 ℃ of pre-gelatinizations 40 minutes, be warming up to 45 ℃, add 0.1mmol/ml ceric ammonium nitrate solution 1ml, behind the 10min, add solution (making its degree of neutralization with sodium hydroxide is 75%), 0.08gN that 23g vinylformic acid is made in three batches, N '-methylene-bisacrylamide and 2ml (50mg/ml) ammonium persulphate, every batch of interval 20 minutes; Be incubated 40 ℃ of polymerization 8h afterwards.With the chopping of gained jel product, in 70 ℃ of dryings,, get the particulate state finished product again through mechanical disintegration to 0.1～5.0mm, inhale the pure water multiplying power greater than 150 times.
Embodiment 5:
60g tapioca (flour) and 120g water are made into starch suspension (33.3%), in 35 ℃ of pre-gelatinizations 35 minutes, be warming up to 60 ℃, add 0.1mmol/ml ceric ammonium nitrate solution 1ml, behind the 10min, add solution, 0.08gN that 20g vinylformic acid (making its degree of neutralization with sodium hydroxide is 60%) and 3g acrylamide monomer are made in three batches, N '-methylene-bisacrylamide and 4ml (50mg/ml) ammonium persulphate, every batch of interval 20 minutes; Be incubated 60 ℃ of polymerization 8h afterwards.With the chopping of gained jel product, in 70 ℃ of dryings,, get the particulate state finished product again through mechanical disintegration to 0.1～5.0mm, inhale the pure water multiplying power greater than 150 times.
Embodiment 6
40g tapioca (flour) and 95g water are made into starch suspension (30wt%), in 50 ℃ of pre-gelatinizations 20 minutes, be warming up to 60 ℃, add 0.1mmol/ml ceric ammonium nitrate solution 1ml, behind the 10min, add solution, 0.15gN that the 23g acrylamide is made in three batches, N '-methylene-bisacrylamide and 2ml (50mg/ml) ammonium persulphate, every batch of interval 20 minutes; Be incubated 70 ℃ of polymerization 4h afterwards.With the chopping of gained jel product, in 100 ℃ of dryings,, get the particulate state finished product again through mechanical disintegration to 0.1～5.0mm, through test, inhale the pure water multiplying power greater than 150 times.
Claims (10)
1. fully-degradable starch hydrogel, it is characterized in that including following component: starch, free yl polymerizating monomer, linking agent and water-soluble free radical circulation composite initiator, described components contents is: the interpolation weight of starch is 0.5～4.5 times of free yl polymerizating monomer, the interpolation weight of linking agent is 0.05%～0.70% of free yl polymerizating monomer, described water-soluble free radical circulation composite initiator is cerous ammonium nitrate and persulphate circulation composite initiator, wherein Ce
4+Addition be 0.005%～0.10% of free yl polymerizating monomer amount of substance, S
2O
8 2-Addition be Ce
4+0.5～10 times of amount of substance.
2. by the described fully-degradable starch hydrogel of claim 1, it is characterized in that described component also includes alkali, the addition of alkali is 40%～90% of a free yl polymerizating monomer amount of substance.
3. by the described fully-degradable starch hydrogel of claim 2, it is characterized in that described components contents is preferably: the interpolation weight of starch is 0.8～2.0 times of free yl polymerizating monomer; The interpolation weight of linking agent is 0.08%～0.30% of free yl polymerizating monomer; The addition of alkali is 60%～85% of a free yl polymerizating monomer amount of substance; Ce
4+Addition be 0.01%～0.05% of free yl polymerizating monomer amount of substance; S
2O
8 2-Addition be Ce
4+1～5 times of amount of substance.
4. by claim 1 or 2 or 3 described fully-degradable starch hydrogels, it is characterized in that described free yl polymerizating monomer is any one or more than one the mixture in vinylformic acid, acrylate, acrylamide, 2-acrylamido-2-methyl propane sulfonic acid and 2-acrylamido-2-methyl propane sulfonic acid salt, described linking agent is N, N '-methylene-bisacrylamide.
5. the preparation method of the described fully-degradable starch hydrogel of claim 1 is characterized in that including following steps:
1) get material: the interpolation weight of starch is 0.5～4.5 times of free yl polymerizating monomer, the interpolation weight of linking agent is 0.05%～0.70% of free yl polymerizating monomer, described water-soluble free radical circulation composite initiator is cerous ammonium nitrate and persulphate circulation composite initiator, wherein Ce
4+Addition be 0.005%～0.10% of free yl polymerizating monomer amount of substance, S
2O
8 2-Addition be Ce
4+0.5～10 times of amount of substance is chosen above-mentioned raw materials;
2) preparation technology and condition: starch is mixed with high-concentration suspension liquid carries out pre-gelatinization: carry out pre-gelatinization 5～100 minutes at 20～80 ℃, add free yl polymerizating monomer, linking agent and water-soluble free radical circulation composite initiator, 30～70 ℃ of polymerizations 4～8 hours, chopping, drying obtains fully-degradable starch hydrogel through pulverizing at last.
6. by the preparation method of the described fully-degradable starch hydrogel of claim 5, it is characterized in that also being added with alkali, the addition of alkali is 40%～90% of a free yl polymerizating monomer amount of substance.
7. by the preparation method of claim 5 or 6 described fully-degradable starch hydrogels, it is characterized in that the compound method of described high-concentration suspension liquid is: it is the suspension of 20wt%～50wt% that starch and water are mixed the concentration that is made into.
8. by the preparation method of the described fully-degradable starch hydrogel of claim 7, it is characterized in that suspension concentration is 25wt%～35wt%.
9. by the preparation method of claim 5 or 6 described fully-degradable starch hydrogels, it is characterized in that 40～70 ℃ of pre-gelatinizations 10～30 minutes.
10. by the preparation method of claim 5 or 6 described fully-degradable starch hydrogels, it is characterized in that described drying is meant at 50～100 ℃ carries out drying.
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| CN105294941A (en) * | 2015-09-28 | 2016-02-03 | 威海汉邦生物环保科技有限公司 | Method for synthesizing super absorbent resin by utilizing polysaccharide biological flocculant |
| CN105769748A (en) * | 2016-04-19 | 2016-07-20 | 桂林理工大学 | Cassava starch hydrogel nostoc commune extract mask matrix and preparation method thereof |
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