CN103013333B - Preparation method of liquid covering material for agricultural purposes - Google Patents
Preparation method of liquid covering material for agricultural purposes Download PDFInfo
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- CN103013333B CN103013333B CN201210521749.1A CN201210521749A CN103013333B CN 103013333 B CN103013333 B CN 103013333B CN 201210521749 A CN201210521749 A CN 201210521749A CN 103013333 B CN103013333 B CN 103013333B
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Abstract
The invention relates to a preparation method of a liquid covering material for agricultural purposes. The method comprises: mixing 0.01-20 parts of polyethylene glycol, 0.01-10 parts of diacid, 0.01-10 parts of diol, and 0.01-1 part of a catalyst by mole ratio, and subjecting the mixture to a stirring reaction in an oil bath of 50DEG C-250DEG C so as to obtain a compound; by mass, taking 0.1-10 parts of the compound, adding 0.1-20 parts of water soluble cellulose, 0.1-10 parts of a membrane-forming agent, 0.1-10 parts of a surfactant, 0.2-10 parts of a plasticizer, 0.1-10 parts of a wet strength agent, 0.05-5 parts of a stabilizer, 0.1-10 parts of a crosslinking agent and 100-1000 parts of water, and subjecting the mixture to a stirring reaction at 30DEG C-100DEG ; then reducing the pressure to remove foams, and conducting cooling to room temperature; and adding water to perform dilution, and carrying out filtration, thus obtaining the liquid covering material. The liquid covering material for agricultural purposes prepared in the invention can disperse or dissolve in water, can coagulate into a membrane after being sprayed in soil and can achieve a good effect. The prepared material has the characteristics of low economic cost, no residue, no toxicity and harmlessness.
Description
Technical field
The invention belongs to macromolecular liquid material produce technical field, particularly a kind of preparation method of agricultural liquids covering material.
Background technology
Agricultural liquids coverture is also referred to as liquid ground film, that there is certain viscosity, the novel complexes material of gel-like film can be formed after spraying, there is good water retention capacity and Meteorological effect effect, and it is biodegradable, product can be used as fertilizer and uses, soil constituent can be improved, improve soil nutrient, increase the resistance of crop, to soil, groundwater quality and environment do not produce harmful effect, and can the anti-grass of insect protected, certain promoter action is had to plant growth, due to its asepsis environment-protecting, Soil structure can be improved again, promote plant growth, improve the quality and yield of crop, therefore can the type material of plastics agricultural mulching as an alternative.Materials of New Type Liquid Mulching Film is mainly oil and by-product category, natural polymer degradable material and chemosynthesis polymer degradable material etc., because raw material sources are extensive, degraded is complete both rear, becomes the focus of current environment-friendly material area research.
Natural polymer such as the raw materials such as Mierocrystalline cellulose, starch, xylogen are easy to get, cheap, mostly containing the hydrophilic radical such as hydroxyl, carboxyl, are easily dispersed in water, and use conveniently, effect is better; But film-formation result is poor when being used alone, mechanical property and mechanical strength properties have to be strengthened.
Summary of the invention
In order to solve above-mentioned the deficiencies in the prior art, the object of the invention is to propose a kind of agricultural liquids covering material prepared by hydrophilic biodegradable macromolecular material method as raw material, have that source is wide, economy is easy to get, the feature of residual less, toxicological harmless.
To achieve these goals, the technical solution used in the present invention is as follows:
A preparation method for agricultural liquids covering material, comprises following preparation process,
The first step, in molar ratio by 0.01 ~ 20 part of polyoxyethylene glycol, 0.01 ~ 10 part of diacid, 0.01 ~ 10 part of glycol, the catalyzer of 0.01 ~ 1 part, in the oil bath of 50 DEG C ~ 250 DEG C, stirring reaction 0.5 ~ 10 hour, obtains mixture; Second step, after mixture prepared by the first step is cooled to room temperature, by mass parts, get 0.1-10 part mixture, the water soluble cellulose of 0.1 ~ 20 part is added again, the membrane-forming agent of 0.1 ~ 10 part, 0.1 ~ 10 part of tensio-active agent in got mixture, the softening agent of 0.2 ~ 10 part, the Wet Strength Resin of 0.1 ~ 10 part, the stablizer of 0.05 ~ 5 part, the linking agent of 0.1 ~ 10 part, the water of 100 ~ 1000 parts, stirring reaction 0.3 ~ 12 hour at 30 DEG C ~ 100 DEG C; 3rd step, after reaction terminates, reduce pressure the foam sloughed in product, is cooled to room temperature; 4th step, by cooled sample filtering, obtaining filtrate is agricultural liquids covering material.
Preferably, the molecular weight of described polyoxyethylene glycol is 200 ~ 20000g/mol.
Preferably, described diacid is one or more mixture in propanedioic acid, succinic acid, hexanodioic acid, suberic acid, sebacic acid, terephthalic acid, maleic acid, FUMARIC ACID TECH GRADE, cyclohexane cyclohexanedimethanodibasic, diethyl alkyd, dodecanedioic acid, tetradecane diacid; Described glycol is one or more mixture in glycol ether, ethylene glycol, propylene glycol, butyleneglycol, hexylene glycol, nonanediol, cyclohexanedimethanol; Described catalyzer is one or more mixture in stannous octoate, tin protochloride, antimony glycol, butyl (tetra) titanate, two (methyl aceto acetate) metatitanic acid diisopropyl ester, zinc acetate, phosphoric acid one hydrogen magnesium.
Preferably, described water soluble cellulose is one or more mixture in methylcellulose gum, carboxymethyl cellulose, Natvosol, hydroxypropylcellulose, Vltra tears, hypromellose, half fiber; Described membrane-forming agent is one or more mixture in gelatin, gum arabic, agar, starch, dextrin, polyvinyl alcohol, ethylene-vinyl acetate copolymer, polyvinyl acetal, methyl acrylate-methyl acrylic copolymer; Described tensio-active agent is one or more mixture in metal carboxylate, phosphoric acid salt, Sulfonates, sulfuric acid ester, polyoxyethylene glycol, polyacrylamide, alginic acid, gelatin, derivatived cellulose; Described softening agent is one or more mixture in adipic acid ester, phthalic acid ester, phosphoric acid ester, Vanay, citrate, epoxy soybean oil, octyl epoxy stearate; Described Wet Strength Resin bag is one or more mixture in urea-formaldehyde resin, melamine resin, Polyamide-Polyamsne-Epichlorohydrin resin, resol, butadiene-styrene latex, dialdehyde starch, polyacrylamide; Described stablizer is one or more mixture in tetramethylolmethane, Xylitol, N.F,USP MANNITOL, epoxy soybean oil, salicylate, glyceryl ester; Described linking agent is one or more mixture in polyoxyethylene glycol, polypropylene glycol, TriMethylolPropane(TMP), glycidyl ether, zinc oxide, aluminum chloride, boric acid, borax, vinylformic acid, aziridine, tosic acid.
Preferably, by the mass parts identical with second step, refilter after cooled sample first being added in the 4th step the water dilution of 10 ~ 100 parts.
Preferably, in the 3rd step, the time of the foam that decompression is sloughed in product is 0.5 ~ 5 hour.
Relative to prior art, the present invention has the following advantages: the present invention adopts the macromolecular material of hydrophilic biodegradable to prepare liquid complex as raw material, can under optimum conditions, be that solvent carries out being obtained by reacting liquid covering material with water.Reaction is carried out under the lesser temps of 30 DEG C-100 DEG C, the material molecule amount prepared is controlled, there is certain viscosity, easily macromolecular network colloid is formed in water, strong with the adhesive attraction of soil, have certain strength and stability, water is that polymer substance disperses or dissolves by solvent as far as possible, has the advantages that Financial cost is low, residual less, nontoxic.
Embodiment
Below in conjunction with embodiment, preparation method of the present invention is described in further detail.
Embodiment 1 ~ 5
The preparation method of a kind of agricultural liquids covering material of the present invention, comprises the following steps:
The first step, be the polyoxyethylene glycol of 200 ~ 20000g/mol, 0.01 ~ 10 part of diacid, 0.01 ~ 10 part of glycol, the catalyzer of 0.01 ~ 1 part in molar ratio by the molecular weight of 0.01 ~ 20 part, in the oil bath of 50 DEG C ~ 250 DEG C, stirring reaction 0.5 ~ 10 hour, obtains mixture;
Second step, after mixture prepared by the first step is cooled to room temperature, by mass parts, get 0.1-10 part mixture, the water soluble cellulose of 0.1 ~ 20 part is added again, the membrane-forming agent of 0.1 ~ 10 part, 0.1 ~ 10 part of tensio-active agent in mixture, the softening agent of 0.2 ~ 10 part, the Wet Strength Resin of 0.1 ~ 10 part, the stablizer of 0.05 ~ 5 part, the linking agent of 0.1 ~ 10 part, the water of 100 ~ 1000 parts, stirring reaction 0.3 ~ 12 hour at 30 DEG C ~ 100 DEG C;
3rd step, after reaction terminates, decompression sloughs foam in product 0.5 ~ 5 hour, is cooled to room temperature;
4th step, cooled sample is added the water dilution of 10 ~ 100 parts, filter, obtaining filtrate is agricultural liquids covering material.
Diacid comprises: propanedioic acid, succinic acid, hexanodioic acid, suberic acid, sebacic acid, terephthalic acid, maleic acid, FUMARIC ACID TECH GRADE, cyclohexane cyclohexanedimethanodibasic, diethyl alkyd, dodecanedioic acid, tetradecane diacid etc.
Glycol comprises: glycol ether, ethylene glycol, propylene glycol, butyleneglycol, hexylene glycol, nonanediol, cyclohexanedimethanol etc.
Catalyzer comprises: stannous octoate, tin protochloride, antimony glycol, butyl (tetra) titanate, two (methyl aceto acetate) metatitanic acid diisopropyl ester, zinc acetate, phosphoric acid one hydrogen magnesium etc.;
Water soluble cellulose comprises: methylcellulose gum, carboxymethyl cellulose, Natvosol, hydroxypropylcellulose, Vltra tears, hypromellose, hemicellulose etc.
Membrane-forming agent comprises: natural high moleculer eompound (gelatin, gum arabic, agar, starch, dextrin), polyvinyl alcohol, ethylene-vinyl acetate copolymer (EVA), polyvinyl acetal, methyl acrylate-methyl acrylic copolymer etc.
Tensio-active agent comprises: metal carboxylate, phosphoric acid salt, Sulfonates, sulfuric acid ester, polyoxyethylene glycol, polyacrylamide, alginic acid, gelatin, derivatived cellulose etc.
Softening agent comprises: adipic acid ester, phthalic acid ester, phosphoric acid ester, Vanay, citrate, epoxy soybean oil, octyl epoxy stearate etc.
Wet Strength Resin comprises: urea-formaldehyde resin, melamine resin, Polyamide-Polyamsne-Epichlorohydrin resin, resol, butadiene-styrene latex, dialdehyde starch, polyacrylamide etc.
Stablizer comprises: tetramethylolmethane, Xylitol, N.F,USP MANNITOL, epoxy soybean oil, salicylate, glyceryl ester etc.
Linking agent comprises: polyoxyethylene glycol, polypropylene glycol, TriMethylolPropane(TMP), glycidyl ether, zinc oxide, aluminum chloride, boric acid, borax, vinylformic acid, aziridine, tosic acid etc.
The concrete operations condition of the embodiment of the present invention 1 ~ 5 and formula rate refer to table 1.
Table 1 operational condition and formula rate
Adopt the liquid covering material prepared by NDJ-79 type rotary viscosity measuring embodiment 1-5, its viscosity is 10 ~ 500mpas; Take the liquid covering material casting film-forming on polyfluortetraethylene plate prepared by 5 ~ 50g embodiment 1-5, the thickness of film is 0.05 ~ 1mm, and adopt 2600 type ultraviolet spectrophotometers to measure dried composite membrane, the transparence of composite membrane is: 70 ~ 98%; Adopt the mechanical property of universal testing machine test compound film: tensile strength is: 0.5 ~ 35MPa, and elongation at break is: 10 ~ 100%.Adopt the liquid covering material mulching soil prepared by embodiment 1-5, in one week, the accumulation soil moisture is: 10 ~ 40 DEG C.
Above data show: the liquid covering material prepared by the inventive method has certain viscosity, effectively can be adsorbed in soil surface, dried film thickness is thinner, there is good transmittance, and can the soil moisture be increased, form interaction to a certain degree between the matrix material that Mechanical Data table is formed, composite membrane has good toughness.Liquid covering material prepared by the present invention, has certain viscosity, is that polymer substance disperses or dissolves by solvent as far as possible with water, and Financial cost is low, residual less, nontoxic.
Claims (4)
1. a preparation method for agricultural liquids covering material, is characterized in that, comprises following preparation process:
The first step, in molar ratio by 0.01 ~ 20 part of polyoxyethylene glycol, 0.01 ~ 10 part of diacid, 0.01 ~ 10 part of glycol, the catalyzer of 0.01 ~ 1 part, in the oil bath of 50 DEG C ~ 250 DEG C, stirring reaction 0.5 ~ 10 hour, obtains mixture;
Second step, after mixture prepared by the first step is cooled to room temperature, by mass parts, get 0.1-10 part mixture, the water soluble cellulose of 0.1 ~ 20 part is added again, the membrane-forming agent of 0.1 ~ 10 part, 0.1 ~ 10 part of tensio-active agent in got mixture, the softening agent of 0.2 ~ 10 part, the Wet Strength Resin of 0.1 ~ 10 part, the stablizer of 0.05 ~ 5 part, the linking agent of 0.1 ~ 10 part, the water of 100 ~ 1000 parts, stirring reaction 0.3 ~ 12 hour at 30 DEG C ~ 100 DEG C;
3rd step, after reaction terminates, reduce pressure the foam sloughed in product, is cooled to room temperature;
4th step, by cooled sample filtering, obtaining filtrate is agricultural liquids covering material;
Described diacid is one or more mixture in propanedioic acid, succinic acid, hexanodioic acid, suberic acid, sebacic acid, terephthalic acid, maleic acid, FUMARIC ACID TECH GRADE, cyclohexane cyclohexanedimethanodibasic, diethyl alkyd, dodecanedioic acid, tetradecane diacid;
Described glycol is one or more mixture in glycol ether, ethylene glycol, propylene glycol, butyleneglycol, hexylene glycol, nonanediol, cyclohexanedimethanol;
Described catalyzer is one or more mixture in stannous octoate, tin protochloride, antimony glycol, butyl (tetra) titanate, two (methyl aceto acetate) metatitanic acid diisopropyl ester, zinc acetate, phosphoric acid one hydrogen magnesium;
Described water soluble cellulose is one or more mixture in methylcellulose gum, carboxymethyl cellulose, Natvosol, hydroxypropylcellulose, Vltra tears, hypromellose, half fiber;
Described membrane-forming agent is one or more mixture in gelatin, gum arabic, agar, starch, dextrin, polyvinyl alcohol, ethylene-vinyl acetate copolymer, polyvinyl acetal, methyl acrylate-methyl acrylic copolymer;
Described tensio-active agent is one or more mixture in metal carboxylate, phosphoric acid salt, Sulfonates, sulfuric acid ester, polyacrylamide, alginic acid, gelatin, derivatived cellulose;
Described softening agent is one or more mixture in adipic acid ester, phthalic acid ester, phosphoric acid ester, Vanay, citrate, epoxy soybean oil, octyl epoxy stearate;
Described Wet Strength Resin is one or more mixture in urea-formaldehyde resin, melamine resin, Polyamide-Polyamsne-Epichlorohydrin resin, resol, butadiene-styrene latex, dialdehyde starch, polyacrylamide;
Described stablizer is one or more mixture in tetramethylolmethane, Xylitol, N.F,USP MANNITOL, epoxy soybean oil, salicylate, glyceryl ester;
Described linking agent is one or more mixture in polypropylene glycol, TriMethylolPropane(TMP), glycidyl ether, zinc oxide, aluminum chloride, boric acid, borax, vinylformic acid, aziridine, tosic acid.
2. the preparation method of a kind of agricultural liquids covering material according to claim 1, is characterized in that: the molecular weight of described polyoxyethylene glycol is 200 ~ 20000.
3. the preparation method of a kind of agricultural liquids covering material according to claim 1, is characterized in that: refilter after cooled sample first being added in the 4th step the water dilution of 10 ~ 100 parts.
4. the preparation method of a kind of agricultural liquids covering material according to claim 1, is characterized in that: in the 3rd step, the time of the foam that decompression is sloughed in product is 0.5 ~ 5 hour.
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| CN201210521749.1A CN103013333B (en) | 2012-12-07 | 2012-12-07 | Preparation method of liquid covering material for agricultural purposes |
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| CN201210521749.1A CN103013333B (en) | 2012-12-07 | 2012-12-07 | Preparation method of liquid covering material for agricultural purposes |
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| CN103013333B true CN103013333B (en) | 2015-02-25 |
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| CN109566369A (en) * | 2017-09-26 | 2019-04-05 | 天祝藏族自治县绿龙农业科技发展有限公司 | Artificial sponge's soil, preparation method and its application in terms of press strip in the sky |
| CN108707250A (en) * | 2018-05-18 | 2018-10-26 | 俞小峰 | A kind of preparation method of degradable agricultural film |
| CN109180971B (en) * | 2018-07-17 | 2020-12-15 | 江西威骏科技股份有限公司 | Water-retaining environment-friendly lignin-starch-kenaf composite mulching film and preparation method thereof |
| CN115678112B (en) * | 2022-10-28 | 2023-09-19 | 武汉轻工大学 | Preparation method of complex cellulose carboxymethylation and composite membrane thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101161718A (en) * | 2007-11-27 | 2008-04-16 | 中国科学院长春应用化学研究所 | Biological degradation liquid film and preparation method |
| CN101602849A (en) * | 2009-07-09 | 2009-12-16 | 湖南大学 | Dimer acid modified unsaturated polyester resin and synthetic method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101161718A (en) * | 2007-11-27 | 2008-04-16 | 中国科学院长春应用化学研究所 | Biological degradation liquid film and preparation method |
| CN101602849A (en) * | 2009-07-09 | 2009-12-16 | 湖南大学 | Dimer acid modified unsaturated polyester resin and synthetic method thereof |
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