CN103013333A - 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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- CN103013333A CN103013333A CN2012105217491A CN201210521749A CN103013333A CN 103013333 A CN103013333 A CN 103013333A CN 2012105217491 A CN2012105217491 A CN 2012105217491A CN 201210521749 A CN201210521749 A CN 201210521749A CN 103013333 A CN103013333 A CN 103013333A
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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 agricultural preparation method of liquid covering material.
Background technology
Agricultural is also referred to as liquid ground film with coverstock, to have certain viscosity, can form the novel complexes material of gel-like film after spraying, have good water retention capacity and heat the soil moisture conservation effect, and biodegradable, product can be used as fertilizer and uses, and can improve soil constituent, improve soil nutrient, increase the resistance of crop, to soil, groundwater quality and environment do not produce harmful effect, and can insect protected prevent grass, plant growth there is certain promoter action, because its asepsis environment-protecting can improve Soil structure again, promote plant growth, improve the quality and yield of crop, therefore can be used as the type material of substituted for plastic agricultural mulching.Materials of New Type Liquid Mulching Film is mainly oil and by-product category, natural polymer degradable material and chemosynthesis polymer degradable material etc., and both become the focus of present environment-friendly material area research because raw material sources are extensive, degraded is complete afterwards.
The raw materials such as natural polymer such as Mierocrystalline cellulose, starch, xylogen are easy to get, and are cheap, mostly contain the hydrophilic radicals such as hydroxyl, carboxyl, easily are dispersed in water, and use conveniently, and effect is better; But film-formation result is relatively poor when using separately, and 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 ofly prepare agricultural with the method for liquid covering material with the hydrophilic biodegradable macromolecular material as raw material, have the source extensively, economy is easy to get, the characteristics of residual less, toxicological harmless.
To achieve these goals, the technical solution used in the present invention is as follows:
A kind of agricultural comprises following preparation process with the preparation method of liquid covering material,
The first step, with 0.01～20 part of polyoxyethylene glycol, 0.01～10 part of diacid, 0.01～10 part of glycol, 0.01～1 part catalyzer, stirring reaction is 0.5～10 hour in 50 ℃～250 ℃ oil bath, gets mixture in molar ratio; Second step is after the mixture of the first step preparation is cooled to room temperature, by mass parts, get 0.1-10 part mixture, the water soluble cellulose that adds again 0.1～20 part in the mixture of getting, 0.1～10 part membrane-forming agent, 0.1～10 part of tensio-active agent, 0.2～10 parts softening agent, 0.1～10 parts Wet Strength Resin, 0.05～5 part stablizer, 0.1～10 part linking agent, 100～1000 parts water was 30 ℃～100 ℃ lower stirring reactions 0.3～12 hour; In the 3rd step, after reaction finished, the foam in the product was sloughed in decompression, is cooled to room temperature; In the 4th step, with cooled sample filtering, obtain filtrate and be agricultural liquid 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, the tetradecane diacid; Described glycol is one or more mixture in glycol ether, ethylene glycol, propylene glycol, butyleneglycol, hexylene glycol, nonanediol, the 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, the 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, the methacrylic ester-Sipacril 2739OF; 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, the 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, the 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, the polyacrylamide; Described stablizer is one or more mixture in tetramethylolmethane, Xylitol, N.F,USP MANNITOL, epoxy soybean oil, salicylate, the 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, the tosic acid.
Preferably, by the mass parts identical with second step, in the 4th step cooled sample added first and refilter after 10～100 parts water dilutes.
Preferably, the time that the foam in the product is sloughed in decompression in the 3rd step is 0.5～5 hour.
With respect 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 be under optimum conditions, and react take water as solvent and to obtain the liquid covering material.Reaction is carried out under 30 ℃-100 ℃ lesser temps, the material molecule amount of preparing is controlled, has certain viscosity, in water, easily form the macromolecular network colloid, strong with the adhesive attraction of soil, have certain strength and stability, water is that solvent disperses or dissolves polymer substance as far as possible, has low, residual less, the nontoxic characteristics of Financial cost.
Embodiment
Below in conjunction with embodiment preparation method of the present invention is described in further detail.
Embodiment 1 ~ 5
A kind of agricultural of the present invention preparation method of liquid covering material may further comprise the steps:
The first step, be the polyoxyethylene glycol of 200～20000g/mol, 0.01～10 part of diacid, 0.01～10 part of glycol, 0.01～1 part catalyzer in molar ratio with 0.01～20 part molecular weight, stirring reaction is 0.5～10 hour in 50 ℃～250 ℃ oil bath, gets mixture;
Second step is after the mixture of the first step preparation is cooled to room temperature, by mass parts, get 0.1-10 part mixture, the water soluble cellulose that adds again 0.1～20 part in the mixture, 0.1～10 part membrane-forming agent, 0.1～10 part of tensio-active agent, 0.2～10 parts softening agent, 0.1～10 parts Wet Strength Resin, 0.05～5 part stablizer, 0.1～10 part linking agent, 100～1000 parts water was 30 ℃～100 ℃ lower stirring reactions 0.3～12 hour;
In the 3rd step, after reaction finished, the foam 0.5～5 hour in the product was sloughed in decompression, is cooled to room temperature;
The 4th step, with the water dilution of 10～100 parts of cooled sample addings, filter, obtain filtrate and be agricultural liquid 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, methacrylic ester-Sipacril 2739OF 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.
Concrete operations condition and the formula rate of the embodiment of the invention 1 ~ 5 see table 1 for details.
Table 1 operational condition and formula rate
Adopt the prepared liquid covering material of NDJ-79 type rotary viscosity measuring embodiment 1-5, its viscosity is 10 ~ 500mpas; Take by weighing the prepared liquid covering material casting film-forming on polyfluortetraethylene plate of 5 ~ 50g embodiment 1-5, the thickness of film is 0.05 ~ 1mm, adopts 2600 type ultraviolet spectrophotometers to measure dried composite membrane, and 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, elongation at break is: 10 ~ 100%.Adopt the prepared liquid covering material mulching soil of embodiment 1-5, the accumulation soil moisture is in the week: 10 ~ 40 ℃.
Above data show: the prepared liquid covering material of the inventive method has certain viscosity, can effectively be adsorbed in soil surface, dried film thickness is thinner, has preferably transmittance, and can increase the soil moisture, form interaction to a certain degree between the formed matrix material of Mechanical Data table, composite membrane has preferably toughness.The liquid covering material of the present invention's preparation has certain viscosity, as far as possible polymer substance is dispersed or dissolved take water as solvent, and Financial cost is low, residual less, nontoxic.
Claims (6)
1. an agriculture preparation method with the liquid covering material is characterized in that, comprises following preparation process:
The first step, with 0.01～20 part of polyoxyethylene glycol, 0.01～10 part of diacid, 0.01～10 part of glycol, 0.01～1 part catalyzer, stirring reaction is 0.5～10 hour in 50 ℃～250 ℃ oil bath, gets mixture in molar ratio;
Second step is after the mixture of the first step preparation is cooled to room temperature, by mass parts, get 0.1-10 part mixture, the water soluble cellulose that adds again 0.1～20 part in the mixture of getting, 0.1～10 part membrane-forming agent, 0.1～10 part of tensio-active agent, 0.2～10 parts softening agent, 0.1～10 parts Wet Strength Resin, 0.05～5 part stablizer, 0.1～10 part linking agent, 100～1000 parts water was 30 ℃～100 ℃ lower stirring reactions 0.3～12 hour;
In the 3rd step, after reaction finished, the foam in the product was sloughed in decompression, is cooled to room temperature;
In the 4th step, with cooled sample filtering, obtain filtrate and be agricultural liquid covering material.
2. a kind of agricultural according to claim 1 is with the preparation method of liquid covering material, and it is characterized in that: the molecular weight of described polyoxyethylene glycol is 200～20000g/mol.
3. a kind of agricultural according to claim 1 is characterized in that with the preparation method of liquid 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, the tetradecane diacid;
Described glycol is one or more mixture in glycol ether, ethylene glycol, propylene glycol, butyleneglycol, hexylene glycol, nonanediol, the 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, the phosphoric acid one hydrogen magnesium.
4. a kind of agricultural according to claim 1 is characterized in that with the preparation method of liquid covering material: 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, the methacrylic ester-Sipacril 2739OF;
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, the 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, the 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, the polyacrylamide;
Described stablizer is one or more mixture in tetramethylolmethane, Xylitol, N.F,USP MANNITOL, epoxy soybean oil, salicylate, the 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, the tosic acid.
5. a kind of agricultural according to claim 1 is characterized in that with the preparation method of liquid covering material: refilter after in the 4th step cooled sample being added first 10～100 parts water dilution.
6. a kind of agricultural according to claim 1 is characterized in that with the preparation method of liquid covering material: to slough the time of the foam in the product be 0.5～5 hour in decompression in the 3rd step.
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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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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108707250A (en) * | 2018-05-18 | 2018-10-26 | 俞小峰 | A kind of preparation method of degradable agricultural film |
| CN109180971A (en) * | 2018-07-17 | 2019-01-11 | 张玉英 | A kind of environmentally friendly lignin-starch-bluish dogbane composite mulching film of water conservation and preparation method |
| 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 |
| CN115678112A (en) * | 2022-10-28 | 2023-02-03 | 武汉轻工大学 | Preparation method of holocellulose carboxymethylation and composite membrane thereof |
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| 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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2012
- 2012-12-07 CN CN201210521749.1A patent/CN103013333B/en active Active
Patent 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 |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN109180971A (en) * | 2018-07-17 | 2019-01-11 | 张玉英 | A kind of environmentally friendly lignin-starch-bluish dogbane composite mulching film of water conservation and preparation method |
| 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 |
| CN115678112A (en) * | 2022-10-28 | 2023-02-03 | 武汉轻工大学 | Preparation method of holocellulose carboxymethylation and composite membrane 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 |
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