CN108373563A - A kind of preparation method of biodegradable agricultural film - Google Patents
A kind of preparation method of biodegradable agricultural film Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01G—HORTICULTURE; CULTIVATION OF VEGETABLES, FLOWERS, RICE, FRUIT, VINES, HOPS OR SEAWEED; FORESTRY; WATERING
- A01G13/00—Protecting plants
- A01G13/02—Protective coverings for plants; Coverings for the ground; Devices for laying-out or removing coverings
- A01G13/0256—Ground coverings
- A01G13/0268—Mats or sheets, e.g. nets or fabrics
- A01G13/0275—Films
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2323/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2323/04—Homopolymers or copolymers of ethene
- C08J2323/06—Polyethene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
Abstract
The invention discloses a kind of preparation methods of biodegradable agricultural film, belong to agricultural film field.The present invention takes absolute ethyl alcohol, distilled water, nano-titanium dioxide, silane coupling agent, nano-titanium dioxide, silane coupling agent are put into container, absolute ethyl alcohol, distilled water is added, stirs evenly, adjusts pH value, magnetic agitation, filtering, obtains filter cake, filter cake is washed with absolute ethyl alcohol, re-dry obtains dried object；Extract, water are mixed, stirred evenly, dried object is added, is protected from light oscillation, is centrifuged, sediment is washed with deionized taking precipitate, vacuum freeze drying, and grinding obtains abrasive material；Wrappage, distilled water, hydrochloric acid solution are mixed, stirred evenly, pH ultrasonic disperses is adjusted, obtains dispersion；Dispersion, absolute ethyl alcohol are subjected to mixing and ball milling, obtain ball milling liquid, by azodiisobutyronitrile, polyvinyl resin, acetone, ball milling liquid ultrasonic disperse, recycles acetone, then suppressed to get biodegradable agricultural film on vulcanizing press.
Description
Technical field
The invention belongs to agricultural film fields, and in particular to the preparation method of a biodegradable agricultural film.
Background technology
Agricultural film and agricultural mulching, main component is polyethylene.It is mainly used for covering farm land, plays and improve ground temperature, soil of guaranteeing the quality
Earth humidity, the effect for promoting germination and seedling rapid growth, also inhibit the effect of weed growth.With plastics industry
It rapidly develops, agriculturally, due to the use of agricultural mulching, is effectively controlled the temperature and humidity of soil, reduces water
Divide the loss with nutriment, the high yield and stabilization of crops is promoted, to increase the benefit of agricultural production.
Agricultural plastic ground membrane starts to apply in 20 middle of century.Nineteen fifty-five Japan's first Application is carried out in strawberry production
It promotes.The beginning of the sixties, the country such as France, Italy, U.S. start in crop productions such as veterinary antibiotics, coffee, tobacco, cottons
It is upper to apply agricultural plastic ground membrane, obtain good result.Plastics agricultural mulching soverlay technique is introduced from 1978 from Japan in China
Since, film-mulching technique has obtained rapid popularization in agricultural production at home, greatly improves China's crop yield.
Agricultural film used at present is mostly used macromolecule PE, PVC polymer, and plastic film makees raw material with chemical fibre, main
Ingredient is polypropylene, polyvinyl chloride, can reach certain heat and moisture preserving effect, but mulch is disposable, when degradation
Between be up to 200 or three hundred years, with it is rear it is broken in farmland and be mingled with a large amount of sandy soil, it is difficult to recycle.It is annual all to have greatly
The residual film of amount is stayed in the soil.Plastic film is mostly tens thousand of to the hundreds thousand of polyethylene of molecular weight, they are difficult in nature
Degradation.These mulch fragments can form cloudy interlayer in the soil, make the constricted flows such as water, gas, the fertilizer in soil, cause soil knot
Structure is hardened, seriously endangers ecological environment, causes white pollution.Therefore, it solves the problems, such as residual mulching film contaminated soil, has become ground
The task of top priority of film mulching and planting technology.
Invention content
The technical problems to be solved by the invention：Be mostly used macromolecule PE, PVC polymer for current agricultural film, mainly at
It is divided into polypropylene, polyvinyl chloride, reaches certain heat and moisture preserving effect, but degradation time is long, with rear broken, causes white dirt
The problem of dye, provides a kind of preparation method of biodegradable agricultural film.
In order to solve the above technical problems, the present invention is using technical solution as described below：
A kind of preparation method of biodegradable agricultural film, which is characterized in that the preparation method includes the following steps：
（1）Count in parts by weight, take 20 ~ 30 parts of absolute ethyl alcohols, 4 ~ 6 parts of distilled water, 4 ~ 6 parts of nano-titanium dioxides, 0.1 ~ 0.2 part
Nano-titanium dioxide, silane coupling agent are put into container by silane coupling agent, and absolute ethyl alcohol, distilled water is added, stirs evenly,
PH value is adjusted to 3 ~ 4, magnetic agitation, filtering obtains filter cake, filter cake is washed 2 ~ 3 times with absolute ethyl alcohol, then dry in 58 ~ 60 DEG C of temperature
It is dry, obtain dried object；
（2）In mass ratio 1：10 ~ 15, extract, water are mixed, stirred evenly, the dry of extract quality 20 ~ 30% is added
Dry object is protected from light oscillation at 24 ~ 26 DEG C of temperature, centrifuges, and sediment is washed with deionized 3 ~ 4 times taking precipitate, and vacuum is cold
Be lyophilized it is dry, grinding, obtain abrasive material；
（3）In mass ratio 7 ~ 8：7~8：1, wrappage, distilled water, hydrochloric acid solution are mixed, stirred evenly, abrasive material is added
The abrasive material of quality 30 ~ 40%, adjusts pH value to 9 ~ 10, and the ultrasonic disperse at 40 ~ 45 DEG C of temperature obtains dispersion；
（4）In mass ratio 3：10, dispersion, absolute ethyl alcohol are subjected to mixing and ball milling, obtain ball milling liquid, in mass ratio 0.02：2：5,
Azodiisobutyronitrile, polyvinyl resin, acetone are mixed, stirred evenly, polyvinyl resin matter is added under peptizaiton
The ball milling liquid of amount 20 ~ 30%, ultrasonic disperse recycles acetone under vacuum, the prepolymerization at 80 ~ 85 DEG C of temperature, then temperature 150 ~
Compacting is to get biodegradable agricultural film on 160 DEG C of vulcanizing press.
The step（1）Middle silane coupling agent is gamma-methyl allyl acyloxypropyl trimethoxysilane.
The step（2）The preparation method of middle extract：
A. weathered coal is crushed, crosses 80 mesh sieve, it is dry, obtain dried object, in mass ratio 1：10, by dried object, dilute hydrochloric acid into
Row mixing, activates at 100 ~ 105 DEG C of temperature, is cooled to room temperature, filters, obtains filter residue, filter residue is washed with water to neutrality, is obtained
Neutrals；
B. in mass ratio 1：10, by neutrals, 0.2mol/L sodium hydroxide solutions, 98 ~ 100 DEG C of temperature stirred in water bath 1 ~
2h is cooled to room temperature, and centrifugation takes supernatant, adjusts pH value to 2 ~ 4, stands 20 ~ 24 h, and sediment is collected in filtering, dry,
Up to extract.
The step（3）The preparation method of middle wrappage：
A. lobster shell is cleaned, dries, pulverizes, obtain powder, in mass ratio 1：5 ~ 6, by powder, 0.2mol/L hydrochloric acid solutions
It is mixed, stirs 1 ~ 2h, filtering obtains filter residue, filter residue is washed with water to neutrality, obtains neutrals, in mass ratio 1：10, it will be neutral
Object, 0.05mol/L sodium hydroxide solutions are mixed, and 1 ~ 2h is stood in 90 ~ 100 DEG C of water-baths of temperature, and filtering obtains filter residue a；
B. filter residue a is washed with water to neutrality, be put into the 0.05mol/L liquor potassic permanganates of 5 ~ 6 times of filter residue a mass impregnate 1 ~
2h, filtering, obtains filter residue b, filter residue b is washed with water 2 ~ 3 times, the 0.01mol/L oxalic acid for placing into 10 ~ 12 times of filter residue b mass is molten
It in liquid, stirs and decolourizes at 60 ~ 70 DEG C of temperature, obtain decoloration object, decoloration object is washed with water to neutrality, in 60 ~ 70 DEG C of temperature
Lower drying is to get wrappage.
Compared with other methods, advantageous effects are the present invention：The present invention due to nano-titanium dioxide uvioresistant,
There is remarkable effect in terms of degerming, photocatalysis, especially has good screen to the ultraviolet light that wavelength is 280 ~ 330 regions nm
The effect of covering can promote the refinement of film crystal grain to play the role of nucleating agent, improve agricultural film to visible light transmission, and due to receiving
Rice corpuscles size is small can be well dispersed in film surface, to which agriculture film strength improves, while being carried out using silane coupling agent
It is modified, on the one hand due to, containing two groups that chemical property is different, it is anti-easily to play chemistry with mineral surfaces in coupling agent molecule
It answers, also polymerisation can occur with high molecular material, interface of the two groups between inorganic matter and organic matter plays bridge
Beam effect further increases agriculture film strength, adds one to improve the binding force of nano-titanium dioxide and polyvinyl resin
The mixture of natural macromolecular aromatic series, hydroxycarboxylic acid that kind is extracted by weathered coal, utilizes the adsorptivity of nano-titanium dioxide
Can, it is combined with polyvinyl resin, since mixture has various active group, is introduced into polyvinyl resin, to obtain
A kind of super absorbent resin is additionally added a kind of Biodegradable material extracted by lobster shell, compound with super absorbent resin,
So that super absorbent resin is degraded in use with Biodegradable material, can be made full use of by soil, to soil
Reparation improvement is carried out, while resin being degraded by the catalytic action of nano-titanium dioxide using the optical property of titanium dioxide
Biodegradable material for low molecular compound, addition is degraded by microorganisms naturally, and the microorganism due to assembling on product
The low molecular compound that can act on generation, it is that soil assimilates to make polymer finally, so as to effectively avoid causing white
The problem of pollution, reduces the pollution to environment.
Specific implementation mode
Nano-titanium dioxide is purchased from the prosperous safe micro-nano chemical plant in Shouguang City of Shandong Province, model C T-300.
Silane coupling agent is gamma-methyl allyl acyloxypropyl trimethoxysilane.
The preparation method of extract：
A. weathered coal is crushed, crosses 80 mesh sieve, it is dry, obtain dried object, in mass ratio 1：10, by dried object, dilute hydrochloric acid into
Row mixing, activates at 100 ~ 105 DEG C of temperature, is cooled to room temperature, filters, obtains filter residue, filter residue is washed with water to neutrality, is obtained
Neutrals；
B. in mass ratio 1：10, by neutrals, 0.2mol/L sodium hydroxide solutions, 98 ~ 100 DEG C of temperature stirred in water bath 1 ~
2h is cooled to room temperature, and centrifugation takes supernatant, adjusts pH value to 2 ~ 4, stands 20 ~ 24 h, and sediment is collected in filtering, dry,
Up to extract.
The preparation method of wrappage：
A. lobster shell is cleaned, dries, pulverizes, obtain powder, in mass ratio 1：5 ~ 6, by powder, 0.2mol/L hydrochloric acid solutions
It is mixed, stirs 1 ~ 2h, filtering obtains filter residue, filter residue is washed with water to neutrality, obtains neutrals, in mass ratio 1：10, it will be neutral
Object, 0.05mol/L sodium hydroxide solutions are mixed, and 1 ~ 2h is stood in 90 ~ 100 DEG C of water-baths of temperature, and filtering obtains filter residue a；
B. filter residue a is washed with water to neutrality, be put into the 0.05mol/L liquor potassic permanganates of 5 ~ 6 times of filter residue a mass impregnate 1 ~
2h, filtering, obtains filter residue b, filter residue b is washed with water 2 ~ 3 times, the 0.01mol/L oxalic acid for placing into 10 ~ 12 times of filter residue b mass is molten
It in liquid, stirs and decolourizes at 60 ~ 70 DEG C of temperature, obtain decoloration object, decoloration object is washed with water to neutrality, in 60 ~ 70 DEG C of temperature
Lower drying is to get wrappage.
A kind of preparation method of biodegradable agricultural film, the preparation method include the following steps：
（1）Count in parts by weight, take 20 ~ 30 parts of absolute ethyl alcohols, 4 ~ 6 parts of distilled water, 4 ~ 6 parts of nano-titanium dioxides, 0.1 ~ 0.2 part
Nano-titanium dioxide, silane coupling agent are put into container by silane coupling agent, and absolute ethyl alcohol, distilled water is added, stirs evenly,
PH value is adjusted to 3 ~ 4, with 800 ~ 900r/min, 1 ~ 2h of magnetic agitation, filtering obtains filter cake, filter cake is washed 2 ~ 3 times with absolute ethyl alcohol,
Again in 58 ~ 60 DEG C of dryings of temperature, dried object is obtained；
（2）In mass ratio 1：10 ~ 15, extract, water are mixed, stirred evenly, the dry of extract quality 20 ~ 30% is added
Dry object is protected from light 1 ~ 2d of oscillation in 24 ~ 26 DEG C of temperature under the conditions of 120 ~ 150r/min, with 3000 ~ 4000r/min centrifugation 8 ~
Sediment is washed with deionized 3 ~ 4 times, is freeze-dried at vacuum degree 13.3Pa by 10min, taking precipitate, and grinding must be ground
Grind object；
（3）In mass ratio 7 ~ 8：7~8：1, wrappage, distilled water, 0.1mol/L hydrochloric acid solutions are mixed, stirs evenly, adds
Enter the abrasive material of abrasive material quality 30 ~ 40%, adjust pH value to 9 ~ 10,50 ~ 55min of ultrasonic disperse at 40 ~ 45 DEG C of temperature is obtained
Dispersion；
（4）In mass ratio 3：10, dispersion, absolute ethyl alcohol are subjected to 4 ~ 5h of mixing and ball milling, obtain ball milling liquid, in mass ratio 0.02：
2：5, azodiisobutyronitrile, polyvinyl resin, acetone are mixed, stirred evenly, in 3000 ~ 4000r/min peptizaitons
The lower ball milling liquid that polyvinyl resin quality 20 ~ 30% is added, 1 ~ 2h of ultrasonic disperse recycle acetone, in temperature at vacuum 13.3Pa
10 min of prepolymerization at 80 ~ 85 DEG C, then on the vulcanizing press of 150 ~ 160 DEG C of temperature compacting to get biodegradable agricultural film.
Nano-titanium dioxide is purchased from the prosperous safe micro-nano chemical plant in Shouguang City of Shandong Province, model C T-300.
Silane coupling agent is gamma-methyl allyl acyloxypropyl trimethoxysilane.
The preparation method of extract：
A. weathered coal is crushed, crosses 80 mesh sieve, it is dry, obtain dried object, in mass ratio 1：10, by dried object, dilute hydrochloric acid into
Row mixing, activates at 100 DEG C of temperature, is cooled to room temperature, filters, obtains filter residue, filter residue is washed with water to neutrality, obtain neutral
Object；
B. in mass ratio 1：10, neutrals, 0.2mol/L sodium hydroxide solutions are waited in 98 DEG C of stirred in water bath 1h of temperature
It is cooled to room temperature, centrifuges, take supernatant, adjust pH value to 2, stand 20h, sediment is collected in filtering, dry to get extract.
The preparation method of wrappage：
A. lobster shell is cleaned, dries, pulverizes, obtain powder, in mass ratio 1：5, by powder, 0.2mol/L hydrochloric acid solutions into
Row mixing, stirs 1h, and filtering obtains filter residue, filter residue is washed with water to neutrality, obtains neutrals, in mass ratio 1：10, by neutrals,
0.05mol/L sodium hydroxide solutions are mixed, and 1h is stood in 90 DEG C of water-baths of temperature, and filtering obtains filter residue a；
B. filter residue a is washed with water to neutrality, is put into the 0.05mol/L liquor potassic permanganates of 5 times of filter residue a mass and impregnates 1h, mistake
Filter, obtains filter residue b, filter residue b is washed with water 2 times, place into the 0.01mol/L oxalic acid solutions of 10 times of filter residue b mass, in temperature
Stirring is decolourized at 60 DEG C, obtains decoloration object, and decoloration object is washed with water to neutrality, is dried to get wrappage under temperature 60 C.
A kind of preparation method of biodegradable agricultural film, the preparation method include the following steps：
（1）It counts in parts by weight, takes 20 parts of absolute ethyl alcohols, 4 parts of distilled water, 4 parts of nano-titanium dioxides, 0.1 part of silane coupling agent,
Nano-titanium dioxide, silane coupling agent are put into container, absolute ethyl alcohol, distilled water is added, stirs evenly, adjusting pH value to 3,
With 800r/min magnetic agitation 1h, filtering obtains filter cake, filter cake is washed 2 times with absolute ethyl alcohol, then in 58 DEG C of dryings of temperature, obtains dry
Dry object；
（2）In mass ratio 1：10, extract, water are mixed, stirred evenly, the dried object of extract quality 20% is added,
24 DEG C of temperature, be protected from light under the conditions of 120r/min oscillation 1d, with 3000r/min centrifuge 8min, taking precipitate, by sediment spend from
Sub- water washing 3 times, is freeze-dried at vacuum degree 13.3Pa, and grinding obtains abrasive material；
（3）In mass ratio 7：7：1, wrappage, distilled water, 0.1mol/L hydrochloric acid solutions are mixed, stirred evenly, addition is ground
The abrasive material of amount of substance 30% is ground, adjusts pH value to 9, the ultrasonic disperse 50min at 40 DEG C of temperature obtains dispersion；
（4）In mass ratio 3：10, dispersion, absolute ethyl alcohol are subjected to mixing and ball milling 4h, obtain ball milling liquid, in mass ratio 0.02：2：
5, azodiisobutyronitrile, polyvinyl resin, acetone are mixed, stirred evenly, is added under 3000r/min peptizaitons poly-
The ball milling liquid of vinyl quality 20%, ultrasonic disperse 1h recycle acetone at vacuum 13.3Pa, the prepolymerization at 80 DEG C of temperature
10 min, then on the vulcanizing press of 150 DEG C of temperature compacting to get biodegradable agricultural film.
Nano-titanium dioxide is purchased from the prosperous safe micro-nano chemical plant in Shouguang City of Shandong Province, model C T-300.
Silane coupling agent is γ-methacryloxy trimethoxy silane.
The preparation method of extract：
A. weathered coal is crushed, crosses 80 mesh sieve, it is dry, obtain dried object, in mass ratio 1：10, by dried object, dilute hydrochloric acid into
Row mixing, activates at 105 DEG C of temperature, is cooled to room temperature, filters, obtains filter residue, filter residue is washed with water to neutrality, obtain neutral
Object；
B. in mass ratio 1：10, neutrals, 0.2mol/L sodium hydroxide solutions are waited in 100 DEG C of stirred in water bath 2h of temperature
It is cooled to room temperature, centrifuges, take supernatant, adjust pH value to 4, stand for 24 hours, filtering, collect sediment, it is dry to get extract.
The preparation method of wrappage：
A. lobster shell is cleaned, dries, pulverizes, obtain powder, in mass ratio 1：6, by powder, 0.2mol/L hydrochloric acid solutions into
Row mixing, stirs 2h, and filtering obtains filter residue, filter residue is washed with water to neutrality, obtains neutrals, in mass ratio 1：10, by neutrals,
0.05mol/L sodium hydroxide solutions are mixed, and 2h is stood in 100 DEG C of water-baths of temperature, and filtering obtains filter residue a；
B. filter residue a is washed with water to neutrality, is put into the 0.05mol/L liquor potassic permanganates of 6 times of filter residue a mass and impregnates 2h, mistake
Filter, obtains filter residue b, filter residue b is washed with water 3 times, place into the 0.01mol/L oxalic acid solutions of 12 times of filter residue b mass, in temperature
Stirring is decolourized at 70 DEG C, obtains decoloration object, and decoloration object is washed with water to neutrality, is dried to get package under temperature 70 C
Object.
A kind of preparation method of biodegradable agricultural film, the preparation method include the following steps：
（1）It counts in parts by weight, takes 30 parts of absolute ethyl alcohols, 6 parts of distilled water, 6 parts of nano-titanium dioxides, 0.2 part of silane coupling agent,
Nano-titanium dioxide, silane coupling agent are put into container, absolute ethyl alcohol, distilled water is added, stirs evenly, adjusting pH value to 4,
With 900r/min magnetic agitation 2h, filtering obtains filter cake, filter cake is washed 3 times with absolute ethyl alcohol, then is dried in temperature 60 C, obtains dry
Dry object；
（2）In mass ratio 1：15, extract, water are mixed, stirred evenly, the dried object of extract quality 30% is added,
26 DEG C of temperature, is protected from light oscillation 2d under the conditions of 150r/min, centrifuge 10min with 4000r/min, taking precipitate spends sediment
Ion water washing 4 times, is freeze-dried at vacuum degree 13.3Pa, and grinding obtains abrasive material；
（3）In mass ratio 8：8：1, wrappage, distilled water, 0.1mol/L hydrochloric acid solutions are mixed, stirred evenly, addition is ground
The abrasive material of amount of substance 40% is ground, adjusts pH value to 10, ultrasonic disperse 55min, obtains dispersion under temperature 45 C；
（4）In mass ratio 3：10, dispersion, absolute ethyl alcohol are subjected to mixing and ball milling 5h, obtain ball milling liquid, in mass ratio 0.02：2：
5, azodiisobutyronitrile, polyvinyl resin, acetone are mixed, stirred evenly, is added under 4000r/min peptizaitons poly-
The ball milling liquid of vinyl quality 30%, ultrasonic disperse 2h recycle acetone at vacuum 13.3Pa, the prepolymerization at 85 DEG C of temperature
10 min, then on the vulcanizing press of 160 DEG C of temperature compacting to get biodegradable agricultural film.
Nano-titanium dioxide is purchased from the prosperous safe micro-nano chemical plant in Shouguang City of Shandong Province, model C T-300.
Silane coupling agent is gamma-methyl allyl acyloxypropyl trimethoxysilane.
The preparation method of extract：
A. weathered coal is crushed, crosses 80 mesh sieve, it is dry, obtain dried object, in mass ratio 1：10, by dried object, dilute hydrochloric acid into
Row mixing, activates at 103 DEG C of temperature, is cooled to room temperature, filters, obtains filter residue, filter residue is washed with water to neutrality, obtain neutral
Object；
B. in mass ratio 1：10, by neutrals, 0.2mol/L sodium hydroxide solutions, in 99 DEG C of stirred in water bath 1.5h of temperature,
It is cooled to room temperature, is centrifuged, supernatant is taken, pH value is adjusted to 3, stands 22h, sediment is collected in filtering, dry to get extraction
Object.
The preparation method of wrappage：
A. lobster shell is cleaned, dries, pulverizes, obtain powder, in mass ratio 1：5.5, by powder, 0.2mol/L hydrochloric acid solutions
It is mixed, stirs 1.5h, filtering obtains filter residue, filter residue is washed with water to neutrality, obtains neutrals, in mass ratio 1：10, it will be neutral
Object, 0.05mol/L sodium hydroxide solutions are mixed, and 1.5h is stood in 95 DEG C of water-baths of temperature, and filtering obtains filter residue a；
B. filter residue a is washed with water to neutrality, is put into the 0.05mol/L liquor potassic permanganates of 5.5 times of filter residue a mass and impregnates
1.5h, filtering, obtains filter residue b, filter residue b is washed with water 2 times, place into the 0.01mol/L oxalic acid solutions of 11 times of filter residue b mass
In, it stirs and decolourizes at 65 DEG C of temperature, obtain decoloration object, decoloration object is washed with water to neutrality, it is dry at 65 DEG C of temperature, i.e.,
Obtain wrappage.
A kind of preparation method of biodegradable agricultural film, the preparation method include the following steps：
（1）Count in parts by weight, take 25 parts of absolute ethyl alcohols, 5 parts of distilled water, 5 parts of nano-titanium dioxides, 0.15 part it is silane coupled
Nano-titanium dioxide, silane coupling agent are put into container by agent, and absolute ethyl alcohol, distilled water is added, stirs evenly, and adjust pH value
To 3.5, with 850r/min magnetic agitation 1.5h, filtering obtains filter cake, filter cake is washed 2 times with absolute ethyl alcohol, then dry in 59 DEG C of temperature
It is dry, obtain dried object；
（2）In mass ratio 1：12.5, extract, water are mixed, stirred evenly, the dried object of extract quality 25% is added,
In 25 DEG C of temperature, it is protected from light oscillation 1.5d under the conditions of 135r/min, 9min is centrifuged with 3500r/min, taking precipitate uses sediment
Deionized water is washed 3 times, is freeze-dried at vacuum degree 13.3Pa, is ground, is obtained abrasive material；
（3）In mass ratio 7.5：7.5：1, wrappage, distilled water, 0.1mol/L hydrochloric acid solutions are mixed, stirs evenly, adds
Enter the abrasive material of abrasive material quality 35%, adjust pH value to 9.5, the ultrasonic disperse 52.5min at 43 DEG C of temperature obtains dispersion；
（4）In mass ratio 3：10, dispersion, absolute ethyl alcohol are subjected to mixing and ball milling 4.5h, obtain ball milling liquid, in mass ratio 0.02：
2：5, azodiisobutyronitrile, polyvinyl resin, acetone are mixed, stirred evenly, is added under 3500r/min peptizaitons
The ball milling liquid of polyvinyl resin quality 25%, ultrasonic disperse 1.5h recycle acetone at vacuum 13.3Pa, pre- at 83 DEG C of temperature
Polymerize 10 min, then on the vulcanizing press of 155 DEG C of temperature compacting to get biodegradable agricultural film.
Comparative example：The agricultural film of company of Changyue County production.
Agricultural film obtained by examples detailed above and the agricultural film of comparative example are detected, broad been skin, broadbean leaf, broadbean stem mixture are taken
For 2kg as decomposition source, shell/leaf/stem mass ratio is 4/2/4, and mixture water content is 63%.It is placed in glass container, respectively will
200g agricultural films of the present invention（Thickness：0.025mm）And it in the agricultural film embedment decomposition source of comparative example, took out film every four days and sees
It examines, and weighs after drying, record result.Farmland covering is carried out using the agricultural film of the present invention and comparative example respectively, is observed after 120 days
Earth's surface surface has noresidue to deposit film, specific test result such as table 1.
Table 1：
| Test event | Example 1 | Example 2 | Example 3 | Reference examples |
| Incipient degradation agricultural film weight g | 200 | 200 | 200 | 200 |
| 4 days | 139 | 140 | 138 | 166~172 |
| 8 days | 47 | 46 | 45 | 88~92 |
| 12 days | 8.3 | 8.6 | 8.3 | 34~46 |
| 16 days | 3.3 | 3.1 | 3.4 | 30.1~32.6 |
Agricultural mulching of the invention has good degradability in summary, and after covering 120 days, visual observations earth's surface part is without residual
Leave-on film；Electron-microscope scanning result also shows mulch configuration of surface after decomposing 16 days and significant change also has occurred in structure, shows this
Agricultural mulching has degradability and use is rear non-breakable, is worthy to be popularized.
Claims (4)
1. a kind of preparation method of biodegradable agricultural film, which is characterized in that the preparation method includes the following steps：
（1）Count in parts by weight, take 20 ~ 30 parts of absolute ethyl alcohols, 4 ~ 6 parts of distilled water, 4 ~ 6 parts of nano-titanium dioxides, 0.1 ~ 0.2 part
Nano-titanium dioxide, silane coupling agent are put into container by silane coupling agent, and absolute ethyl alcohol, distilled water is added, stirs evenly,
PH value is adjusted to 3 ~ 4, magnetic agitation, filtering obtains filter cake, filter cake is washed 2 ~ 3 times with absolute ethyl alcohol, then dry in 58 ~ 60 DEG C of temperature
It is dry, obtain dried object；
（2）In mass ratio 1：10 ~ 15, extract, water are mixed, stirred evenly, the dry of extract quality 20 ~ 30% is added
Dry object is protected from light oscillation at 24 ~ 26 DEG C of temperature, centrifuges, and sediment is washed with deionized 3 ~ 4 times taking precipitate, and vacuum is cold
Be lyophilized it is dry, grinding, obtain abrasive material；
（3）In mass ratio 7 ~ 8：7~8：1, wrappage, distilled water, hydrochloric acid solution are mixed, stirred evenly, abrasive material is added
The abrasive material of quality 30 ~ 40%, adjusts pH value to 9 ~ 10, and the ultrasonic disperse at 40 ~ 45 DEG C of temperature obtains dispersion；
（4）In mass ratio 3：10, dispersion, absolute ethyl alcohol are subjected to mixing and ball milling, obtain ball milling liquid, in mass ratio 0.02：2：5,
Azodiisobutyronitrile, polyvinyl resin, acetone are mixed, stirred evenly, polyvinyl resin matter is added under peptizaiton
The ball milling liquid of amount 20 ~ 30%, ultrasonic disperse recycles acetone under vacuum, the prepolymerization at 80 ~ 85 DEG C of temperature, then temperature 150 ~
Compacting is to get biodegradable agricultural film on 160 DEG C of vulcanizing press.
2. the preparation method of biodegradable agricultural film according to claim 1, which is characterized in that the step（1）Middle silane
Coupling agent is gamma-methyl allyl acyloxypropyl trimethoxysilane.
3. the preparation method of biodegradable agricultural film according to claim 1, which is characterized in that the step（2）Middle extraction
The preparation method of object：
A. weathered coal is crushed, crosses 80 mesh sieve, it is dry, obtain dried object, in mass ratio 1：10, by dried object, dilute hydrochloric acid into
Row mixing, activates at 100 ~ 105 DEG C of temperature, is cooled to room temperature, filters, obtains filter residue, filter residue is washed with water to neutrality, is obtained
Neutrals；
B. in mass ratio 1：10, by neutrals, 0.2mol/L sodium hydroxide solutions, 98 ~ 100 DEG C of temperature stirred in water bath 1 ~
2h is cooled to room temperature, and centrifugation takes supernatant, adjusts pH value to 2 ~ 4, stands 20 ~ 24 h, and sediment is collected in filtering, dry,
Up to extract.
4. the preparation method of biodegradable agricultural film according to claim 1, which is characterized in that the step（3）Middle package
The preparation method of object：
A. lobster shell is cleaned, dries, pulverizes, obtain powder, in mass ratio 1：5 ~ 6, by powder, 0.2mol/L hydrochloric acid solutions
It is mixed, stirs 1 ~ 2h, filtering obtains filter residue, filter residue is washed with water to neutrality, obtains neutrals, in mass ratio 1：10, it will be neutral
Object, 0.05mol/L sodium hydroxide solutions are mixed, and 1 ~ 2h is stood in 90 ~ 100 DEG C of water-baths of temperature, and filtering obtains filter residue a；
B. filter residue a is washed with water to neutrality, be put into the 0.05mol/L liquor potassic permanganates of 5 ~ 6 times of filter residue a mass impregnate 1 ~
2h, filtering, obtains filter residue b, filter residue b is washed with water 2 ~ 3 times, the 0.01mol/L oxalic acid for placing into 10 ~ 12 times of filter residue b mass is molten
It in liquid, stirs and decolourizes at 60 ~ 70 DEG C of temperature, obtain decoloration object, decoloration object is washed with water to neutrality, in 60 ~ 70 DEG C of temperature
Lower drying is to get wrappage.
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Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2007073109A1 (en) * | 2005-12-23 | 2007-06-28 | Wan Pyo Hong | Biodegradable resin composition and plastic product made thereof |
| CN101831088A (en) * | 2010-04-23 | 2010-09-15 | 平顶山市蓝峰科技实业有限公司 | Marine microorganism completely degradable plastic |
| CN103834086A (en) * | 2014-03-19 | 2014-06-04 | 华南农业大学 | Efficient controllable photooxidation-biodegradable plastic film and preparation method thereof |
| CN104292600A (en) * | 2014-09-22 | 2015-01-21 | 井冈山大学 | Humic acid/EVA (ethylene-vinyl acetate) resin blending-modified degradable solid mulching film |
| CN105131383A (en) * | 2015-06-26 | 2015-12-09 | 青岛克立克信息技术有限公司 | High-efficiency and environmental-protection agricultural mulching film |
| CN106753829A (en) * | 2016-11-22 | 2017-05-31 | 闫博文 | A kind of preparation method of antibacterial corrosion-free type air conditioner cleaning agent |
| CN107022134A (en) * | 2017-05-06 | 2017-08-08 | 安徽瑞研新材料技术研究院有限公司 | A kind of environment-friendly degradable material producing process |
| CN107090053A (en) * | 2017-03-16 | 2017-08-25 | 天津工业大学 | The technology of chitosan magnetic is prepared from cray shell |
| CN107325502A (en) * | 2017-07-27 | 2017-11-07 | 陕西科技大学 | A kind of water conservation getting fat Biodegradable agricultural mulch film and preparation method thereof |
| CN107793621A (en) * | 2017-11-16 | 2018-03-13 | 李君� | A kind of biology and the Environment-friendlyplastic plastic bag and its manufacture method of the dual degraded of light |
-
2018
- 2018-03-28 CN CN201810263914.5A patent/CN108373563A/en active Pending
Patent Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2007073109A1 (en) * | 2005-12-23 | 2007-06-28 | Wan Pyo Hong | Biodegradable resin composition and plastic product made thereof |
| CN101831088A (en) * | 2010-04-23 | 2010-09-15 | 平顶山市蓝峰科技实业有限公司 | Marine microorganism completely degradable plastic |
| CN103834086A (en) * | 2014-03-19 | 2014-06-04 | 华南农业大学 | Efficient controllable photooxidation-biodegradable plastic film and preparation method thereof |
| CN104292600A (en) * | 2014-09-22 | 2015-01-21 | 井冈山大学 | Humic acid/EVA (ethylene-vinyl acetate) resin blending-modified degradable solid mulching film |
| CN105131383A (en) * | 2015-06-26 | 2015-12-09 | 青岛克立克信息技术有限公司 | High-efficiency and environmental-protection agricultural mulching film |
| CN106753829A (en) * | 2016-11-22 | 2017-05-31 | 闫博文 | A kind of preparation method of antibacterial corrosion-free type air conditioner cleaning agent |
| CN107090053A (en) * | 2017-03-16 | 2017-08-25 | 天津工业大学 | The technology of chitosan magnetic is prepared from cray shell |
| CN107022134A (en) * | 2017-05-06 | 2017-08-08 | 安徽瑞研新材料技术研究院有限公司 | A kind of environment-friendly degradable material producing process |
| CN107325502A (en) * | 2017-07-27 | 2017-11-07 | 陕西科技大学 | A kind of water conservation getting fat Biodegradable agricultural mulch film and preparation method thereof |
| CN107793621A (en) * | 2017-11-16 | 2018-03-13 | 李君� | A kind of biology and the Environment-friendlyplastic plastic bag and its manufacture method of the dual degraded of light |
Non-Patent Citations (5)
| Title |
|---|
| 新疆维吾尔族自治区科学技术情报研究所: "《腐植酸类物质的生产和应用》", 30 June 1978 * |
| 武军 等: "《绿色包装》", 31 March 2007, 中国轻工业出版社 * |
| 沈玉龙 等: "《绿色化学》", 30 April 2016, 中国环境科学出版社 * |
| 胡静: "《高新技术产业科普丛书 新教材》", 31 December 2011, 东南大学出版社 * |
| 陈礼跷，魏金芳，赵玲: "利用甲壳素制取生物降解塑料的探讨", 《中国塑料》 * |
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