CN100352845C - Plant polyphenol water-loss reducer and its preparation method - Google Patents
Plant polyphenol water-loss reducer and its preparation method Download PDFInfo
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- CN100352845C CN100352845C CNB2004100094166A CN200410009416A CN100352845C CN 100352845 C CN100352845 C CN 100352845C CN B2004100094166 A CNB2004100094166 A CN B2004100094166A CN 200410009416 A CN200410009416 A CN 200410009416A CN 100352845 C CN100352845 C CN 100352845C
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- water
- plant polyphenol
- starch
- polyphenol
- holding agent
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Abstract
The present invention discloses a plant polyphenol water-holding agent and a preparation method thereof, which is characterized in that after starch dextrinization, under the action of an initiating agent, unsaturated monomers have a free radical type graft copolymerization reaction and carry out grafting crosslink under the action of a crosslinking agent; the reactivity of graft copolymerization is used, and plant polyphenol is accessed to grafted and crosslinked products. The plant polyphenol water-holding agent has the effect of resisting microorganism erosion, and water absorption multiplying power is from 500 to 700 times. At the same time, the plant polyphenol water-holding agent has better effects of holding water, storing water, resisting wind, keeping seedlings, resisting drought and strengthening the seedlings.
Description
[technical field]
The present invention relates to a kind of water-loss reducer of soil, specifically, the present invention relates to a kind of water-holding agent that contains plant polyphenol.The invention still further relates to the preparation method of described plant polyphenol water-holding agent.
[background technology]
Being widely used in the absorbent resin of arid and semi-arid lands forestry afforestation at present, generally is starch grafting type, requires to have higher water-absorbent and water-retentivity preferably, and water-absorbent repeatedly.
This class water-retaining agent be with after the starch pasting with the graft copolymerization of alkene class hydrophilic monomer, have and promote tree seed seedling rate height, come up early, growth is fast, the advantage that storage rate is high.The suction soil that forms behind it and the soil uniform mixing, the saturated aqueous rate of soil are obviously compared according to high, and soil available water is increased, and increased value increases with the increase of high water absorbent consumption.
But general water-retaining agent because the relation of chemical ingredients, in soil storage period long, all can be subjected to the erosion of soil microorganisms, water-retaining agent is degraded, directly influence the effect of water-retaining agent, this is an open question in the present soil water-retaining agent.
Plant polyphenol is that a class extensively is present in the intravital polyphenols of plant, and the content in plant is only second to Mierocrystalline cellulose, hemicellulose and xylogen, mainly is present in skin, root, wood, leaf, the fruit of plant.Its complex structure, chemical property is active, and often exists with the form of mixtures of the homologue of a large amount of similar performances.They still have some general character on molecular structure: (1) phenolic hydroxyl group number is numerous, and is the most typical with ortho position phenolic hydroxyl group (pyrogallol, pyrocatechol); (2) molecular weight is bigger, and wider distribution.
The inventor has carried out big quantity research and test according to the characteristics of plant polyphenol, utilizes phenolic hydroxyl group and carboxyl in the tannin molecule to form hydrogen bond with other molecules, carries out modification, thereby develops the water-holding agent of the present invention that can overcome above-mentioned technological deficiency.
[summary of the invention]
[technical problem to be solved]
The purpose of this invention is to provide a kind of plant polyphenol water-holding agent that overcomes above-mentioned technological deficiency.
Another object of the present invention is a kind of preparation method of plant polyphenol water-holding agent of the present invention.
[technical scheme]
Plant polyphenol water-holding agent of the present invention is characterized in that it is to be made by following component graft copolymerization:
Plant polyphenol: 0.5-40 weight part
Starch derivative: 10-60 weight part
Unsaturated monomer: 30-300 weight part
Described component is preferably as follows (by weight):
Plant polyphenol: 10-30 weight part
Starch derivative: 20-50 weight part
Unsaturated monomer: 50-200 weight part
Plant polyphenol water-holding agent of the present invention is characterized in that it is to be prepared from by following method:
(1) solution preparation: above-mentioned weight part plant polyphenol and unsaturated monomer wiring solution-forming is standby, and the mass concentration of the preferred contained plant polyphenol of described plant polyphenol solution is 0.25-4%, and unsaturated monomer solution quality concentration is 10-30%.
(2) gelatinization of starch: above-mentioned weight part starch is joined in the reactor of packing into, adds water. under the condition of logical nitrogen, be heated to 50-95 ℃ and stir gelatinization 0.5-2.0 hour;
(3) graft copolymerization: after gelatinization is finished, the temperature of system is cooled to 40-60 ℃, under the condition of logical nitrogen, order adds initiator, monomer solution, linking agent, 40-60 ℃ the reaction 1.5-2.0 hour after, add the plant polyphenol solution reaction after 0.5-1.0 hour, stopping logical nitrogen, be warming up to 60 ℃.
(4) hydrolysis reaction: add sodium hydroxide solution, constant temperature hydrolysis 1.5-3.0 hour;
(5) aftertreatment of hydrolysate: with distilled water hydrolysate is soaked, washs, make the pH value of product be 6.5-7.5, dewater, dry,, obtain pulverous product of the present invention through grinding to constant weight.
Wherein said plant polyphenol is Hydrolysable Tannins or condensed tannin.Hydrolysable Tannins is a gallic acid ester class polyphenol, is preferably a kind of in gallotannin, the Ellagitannins; Condensed tannin is flavanol compound polyphenol or proanthocyanidin, and the flavanol compound polyphenol is preferably one or more in Flavonol monomer, the Flavonol polymer, and proanthocyanidin is preferably one or more in monomer proanthocyanidin, the polymer proanthocyanidin.
Described starch derivative is cross-linking starch, phosphate ester starch, carboxymethyl starch, graft starch, starch ester.Be preferably a kind of in cross-linking starch, phosphate ester starch, graft starch, the starch ester.Described unsaturated monomer is acrylamide, vinylformic acid, acrylate, vinyl cyanide etc., is preferably acrylamide.
Raw material large-scale industrialization productions such as the used plant polyphenol of the present invention, starch derivative, unsaturated monomer, and can buy from market.For example plant polyphenol can be selected the larch extract that the Inner Mongol inferior gram stone tannin extract factory produces for use, the acrylamide that the cross-linking starch that starch derivative can select for use Zaozhuang City, Shandong Province east modified starch company limited to produce, unsaturated monomer can select for use Zichuan, Shandong gold Hue worker company limited to produce.
The preparation method of plant polyphenol water-holding agent of the present invention is characterized in that this method comprises the steps:
(1) gelatinization of starch: starch is joined in the reactor of packing into, adds water. under the condition of logical nitrogen, be heated to 50-95 ℃ and stir gelatinization 0.5-2.0 hour;
(2) graft copolymerization: after gelatinization is finished, the temperature of system is cooled to 40-60 ℃, under the condition of logical nitrogen, order adds initiator, monomer solution, linking agent, 40-60 ℃ the reaction 1.5-2.0 hour after, add the plant polyphenol solution reaction after 0.5-1.0 hour, stopping logical nitrogen, be warming up to 60 ℃.
(3) hydrolysis reaction: add sodium hydroxide solution, constant temperature hydrolysis 1.5-3.0 hour;
(4) aftertreatment of hydrolysate: with distilled water hydrolysate is soaked, washs, make the pH value of product be 6.5-7.5, dewater, dry,, obtain pulverous product of the present invention through grinding to constant weight.
Wherein said initiator is one or more of Potassium Persulphate, ammonium persulphate or cerous nitrate, is preferably Potassium Persulphate; Linking agent is one or more in N-N '-methylene-bisacrylamide, bisacrylamide, two Methacrylamide or the urine fat, is preferably two Methacrylamides.
Wherein said initiator amount is the 0.7-3.0% of monomer mass, and dosage of crosslinking agent is the 0.6-2.0% of monomer mass.
Wherein, the mass concentration of the preferred contained plant polyphenol of described plant polyphenol solution is 0.25-4%, and unsaturated monomer solution quality concentration is 10-30%.
[beneficial effect]
According to the characteristics of plant polyphenol, utilize phenolic hydroxyl group in the tannin molecule and carboxyl to form hydrogen bond especially with other molecules, carry out modification, the water-holding agent of developing of the present invention not only has the effect of water conservation and suction, also has sterilization and soil improvement action.
Because the adstringency of plant polyphenol has the evil of causing for some soil pests and acts on, make the water-retaining agent that is placed on for a long time in the soil can not be subjected to the influence of microorganism like this, and biological degradation takes place, this is the unique aspect of this water-retaining agent.
Secondly, by plant polyphenol and Fe
3+Mating reaction and redoxomorphism, change the redox potential of ferro element, improve Fe in the soil
2+Ionic concentration increase the property of giving of ferro element in the soil, and tannin itself is exactly the composition of many plants, and is nuisanceless, meets the principle of Green Chemistry.
After adopting water-retaining agent of the present invention to handle nursery stock, can build a partial moist environment artificially at the seedling root place, make nursery stock can keep growth vigor for a long time, promote root growth, prolong the wilting phase, ride out period of drought, and then improve the surrival rate of afforestation.
Plant polyphenol water-holding agent water absorbent rate 500-700 of the present invention times, 3 years effective acting time.Use product afforestation of the present invention in the arid and semi-arid area, can improve plant percent about 20%, improve turnout about 30%.And through evidence, this water-retaining agent has the effect of opposing microbial attack.Therefore, its applied range, can concede the land to forestry, defend and control sand and engineering such as sandstorm improvement in widespread use.
[embodiment]
List non-restrictive example below, further specify the present invention:
Embodiment 1.
In 20 parts of cross-linking starchs (weight part, down with), the reactor of packing into, add 1000 parts in water, logical nitrogen, stir, be heated to 80 ℃ of gelatinization half an hour; Be cooled to 40 ℃ then, adding mass concentration is 500 parts of 0.2% potassium persulfate solutions, add mass concentration then and be 500 parts of 16% acrylamide solns, and add N-N '-methylene-bisacrylamide (be monomer mass 1.25%), stirring reaction 2 hours at a slow speed under 40 ℃; Add 500 parts of tanning solutions (mass concentration is 2%) then, react half an hour; Stop logical nitrogen, be warming up to 60 ℃, 1000 parts of the aqueous sodium hydroxide solutions of adding 1mol/l, constant temperature hydrolysis 2 hours; Then the hydrolysate that obtains is washed with water to the pH value be 7, dewater, dry to constant weight, through grinding, obtain pulverous product of the present invention.
Embodiment 2.
In 40 parts of starch esters (weight part, down with), the reactor of packing into, add 1000 parts in water, logical nitrogen, stir, be heated to 80 ℃ of gelatinization half an hour; Be cooled to 40 ℃ then, adding mass concentration is 500 parts of 0.2% ammonium persulfate solutions, adds mass concentration then and be 1000 parts of 30% acrylate solution, and add urine fat (for monomer mass 1.25%), stirring reaction 2 hours at a slow speed under 40 ℃; Add 800 parts of tanning solutions (mass concentration is 2%) then, react half an hour; Stop logical nitrogen, be warming up to 60 ℃, 1000 parts of the aqueous sodium hydroxide solutions of adding 1mol/l, constant temperature hydrolysis 2 hours; Then the hydrolysate that obtains is washed with water to the pH value be 7, dewater, dry to constant weight, through grinding, obtain pulverous product of the present invention.
Embodiment 3.
In 60 parts of graft starchs (weight part, down with), the reactor of packing into, add 1000 parts in water, logical nitrogen, stir, be heated to 80 ℃ of gelatinization half an hour; Be cooled to 40 ℃ then, adding mass concentration is 500 parts of 0.2% cerous nitrate solutions, adds mass concentration then and be 500 parts of 20% acrylonitrile solutions, and adds two Methacrylamides (be monomer mass 1.25%), stirring reaction 2 hours at a slow speed under 40 ℃; Add 500 parts of tanning solutions (mass concentration is 2%) then, react half an hour; Stop logical nitrogen, be warming up to 60 ℃, 1000 parts of the aqueous sodium hydroxide solutions of adding 1mol/l, constant temperature hydrolysis 2 hours; Then the hydrolysate that obtains is washed with water to the pH value be 7, dewater, dry to constant weight, through grinding, obtain pulverous product of the present invention.
The comparative example 1
| Absorption speed | Water-intake rate (g/g) | Biological degradation | |
| General water-retaining agent | 1min reaches maximum absorption speed | 500-1000 | Mottling was arranged in 3 months |
| This water-retaining agent | 1min reaches maximum absorption speed | 700-800 | Do not see mottling in 3 months |
Though above the present invention is described in detail with a general description of the specific embodiments, on basis of the present invention, can make some modifications or improvements it, this will be apparent to those skilled in the art.Therefore, not departing from the these modifications or improvements basically of spirit of the present invention, all belong to the scope of protection of present invention.
Claims (6)
1, a kind of plant polyphenol water-holding agent, it is to obtain by the following method:
(1) gelatinization of starch derivative: starch derivative is joined in the reactor, adds water, under the condition of logical nitrogen, be heated to 50-95 ℃ and stir gelatinization 0.5-2 hour;
(2) graft copolymerization: after gelatinization is finished, the temperature of system is cooled to 40-60 ℃, under the condition of logical nitrogen, order adds initiator, unsaturated monomer solution, linking agent, 40-60 ℃ the reaction 1.5-2.0 hour after, add the plant polyphenol solution reaction after 0.5-1 hour, stopping logical nitrogen, be warming up to 60 ℃;
(3) hydrolysis reaction: add sodium hydroxide solution, constant temperature hydrolysis 1.5-3.0 hour;
(4) aftertreatment of hydrolysate: with distilled water hydrolysate is soaked, washs, make the pH value of product be 6.5-7.5, dewater, dry,, obtain pulverous plant polyphenol water-holding agent through grinding to constant weight,
Described plant polyphenol, starch derivative, unsaturated monomer content are respectively:
Plant polyphenol: 0.5-40 weight part
Starch derivative: 10-60 weight part
Unsaturated monomer: 30-300 weight part
Wherein said starch derivative is selected from: cross-linking starch, phosphate ester starch, carboxymethyl starch, graft starch, starch ester;
Wherein said plant polyphenol is Hydrolysable Tannins and/or condensed tannin, and the mass concentration of described plant polyphenol solution is 0.25-4%;
Wherein said unsaturated monomer is any one in acrylamide, vinylformic acid, acrylate, the vinyl cyanide, and the mass concentration of described unsaturated monomer solution is 10-30%.
2, plant polyphenol water-holding agent according to claim 1 is characterized in that described Hydrolysable Tannins is the esters of gallic acid polyphenol.
3, plant polyphenol water-holding agent according to claim 2 is characterized in that described esters of gallic acid polyphenol is one or more in tannin, the Ellagitannins.
4, plant polyphenol water-holding agent according to claim 1 is characterized in that described condensed tannin is flavanol compound polyphenol or proanthocyanidin.
5, plant polyphenol water-holding agent according to claim 4 is characterized in that described flavanol compound polyphenol is one or more in Flavonol monomer, the Flavonol polymer; Proanthocyanidin is one or more in monomer proanthocyanidin, the polymer proanthocyanidin.
6,, it is characterized in that described starch derivative is cross-linking starch, phosphate ester starch, graft starch, starch ester according to the arbitrary described plant polyphenol water-holding agent of claim 1-5.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100094166A CN100352845C (en) | 2004-08-10 | 2004-08-10 | Plant polyphenol water-loss reducer and its preparation method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100094166A CN100352845C (en) | 2004-08-10 | 2004-08-10 | Plant polyphenol water-loss reducer and its preparation method |
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| Publication Number | Publication Date |
|---|---|
| CN1733814A CN1733814A (en) | 2006-02-15 |
| CN100352845C true CN100352845C (en) | 2007-12-05 |
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| CNB2004100094166A Expired - Fee Related CN100352845C (en) | 2004-08-10 | 2004-08-10 | Plant polyphenol water-loss reducer and its preparation method |
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102041799B (en) * | 2010-11-17 | 2012-04-04 | 南京工业大学 | Method for manufacturing water retaining/absorption dam for intercepting fire fighting wastewater |
| CN106010558A (en) * | 2016-05-31 | 2016-10-12 | 山东胜伟园林科技有限公司 | Phosphate fertilizer slow-release water retaining agent used for cotton in saline and alkaline land, and preparation method thereof |
| CN109705874A (en) * | 2018-12-28 | 2019-05-03 | 北京城市之光生态环境有限公司 | A kind of water-loss reducer of soil and preparation method thereof |
| CN110642357B (en) * | 2019-10-31 | 2021-01-26 | 内江师范学院 | Flocculating agent for microalgae capture and preparation method and application thereof |
| CN110885380A (en) * | 2019-12-27 | 2020-03-17 | 蚌埠天成包装科技股份有限公司 | Chlorogenic acid grafted modified starch, degradable preservative film and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1290053A (en) * | 1969-05-28 | 1972-09-20 | ||
| CN1134950A (en) * | 1995-01-10 | 1996-11-06 | 诺瓦蒙特股份公司 | Thermoplastic compositions comprising starch and other components from natural origin |
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2004
- 2004-08-10 CN CNB2004100094166A patent/CN100352845C/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1290053A (en) * | 1969-05-28 | 1972-09-20 | ||
| CN1134950A (en) * | 1995-01-10 | 1996-11-06 | 诺瓦蒙特股份公司 | Thermoplastic compositions comprising starch and other components from natural origin |
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| CN1733814A (en) | 2006-02-15 |
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Assignee: Beijing Linda Forestry Technology Co., Ltd. Assignor: Beijing Forestry University Contract fulfillment period: 2008.1.1 to 2013.1.1 contract change Contract record no.: 2010990000046 Denomination of invention: Plant polyphenol water-loss reducer and its preparation method Granted publication date: 20071205 License type: Exclusive license Record date: 2010.1.27 |
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Free format text: EXCLUSIVE LICENSE; TIME LIMIT OF IMPLEMENTING CONTACT: 2008.1.1 TO 2013.1.1; CHANGE OF CONTRACT Name of requester: BEIJING FORESTRY UNIVERSITY FORESTRY SCIENCE CO., Effective date: 20100127 |
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Granted publication date: 20071205 Termination date: 20130810 |