CN112300428A - Preparation method of agricultural film material modified by morph-genetic aluminum oxide - Google Patents

Preparation method of agricultural film material modified by morph-genetic aluminum oxide Download PDF

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CN112300428A
CN112300428A CN202011118689.XA CN202011118689A CN112300428A CN 112300428 A CN112300428 A CN 112300428A CN 202011118689 A CN202011118689 A CN 202011118689A CN 112300428 A CN112300428 A CN 112300428A
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aluminum oxide
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贺辛亥
梁军浩
王亮
李建伟
孙元娜
刘菲
何丽忠
王博
马静妍
周光瑞
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Xian Polytechnic University
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    • C08J7/00Chemical treatment or coating of shaped articles made of macromolecular substances
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    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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    • C04B35/01Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/10Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminium oxide
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    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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    • C09D175/00Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
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    • C09D7/00Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
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    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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    • C08J2367/00Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
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    • C08J2475/00Characterised by the use of polyureas or polyurethanes; Derivatives of such polymers
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Abstract

The invention discloses a preparation method of an agricultural film material modified by morph-genetic aluminum oxide. The microcosmic Al of the scindapsus aureus leaf is prepared by the processes of alkali treatment, preparation of nano hydroxide, vacuum-pressure impregnation, aerobic sintering and annealing, functional adhesive and gluing and mould pressing of the scindapsus aureus leaf2O3Powder modified functional composite membrane material. The obtained microcosmic Al of the scindapsus aureus leaves2O3The powder modified functional composite film material has special ultravioletThe light absorption characteristic can shade the sun and adjust the illumination intensity, and can promote the growth of fruit trees by utilizing the special light absorption transfer characteristic, thereby having wider application prospect in the agricultural field.

Description

Preparation method of agricultural film material modified by morph-genetic aluminum oxide
Technical Field
The invention belongs to the technical field of preparation of functional composite membrane materials, and relates to a preparation method of an agricultural membrane material modified by morph-genetic aluminum oxide.
Background
At present, the known aluminum oxide with the genetic structure and the technology applied to agricultural film materials are as follows: 1. article "genetic transformation and microstructure research of plant Material" (doctor's paper of Shanghai university of transportation [ D)]2005, 4); 2. article "preparation of functional Material having Biohierarchical Structure and Performance study" (doctor's paper of Shanghai university of transportation [ D)]2008, 1); 3. article "biological template method for preparing Al2O3Morph-genetic ceramics (the seventh Chinese functional material and its academic conference discourse collection of application, 2010,10: 283-; 4. article "A novel Binder-513 multifunctional adhesive stick" (Black Longjiang university Proc. Nature science bulletin [ J)]1995,12(1): 110-); 5. article two kinds of organic and inorganic Al doped Al2O3/SiO2Comparison of composite Membrane Performance (journal of Western Ann engineering university [ J)],2020,34(6):1-6)。
The disclosed technology mainly relates to preparation of biological Al from natural plant morph-genetic structures such as ramie and wood2O3The ceramic material does not relate to the research of preparing functional adhesive by using alumina powder with a special morph-genetic structure of scindapsus aureus leaves and using the functional adhesive to prepare functional agricultural composite film materials.
Disclosure of Invention
The invention aims to provide a preparation method of an agricultural film material modified by morph-genetic aluminum oxide, and the prepared agricultural film material has the characteristic of unique ultraviolet light absorption characteristic.
The technical scheme adopted by the invention is that a preparation method of the agricultural film material modified by the morph-genetic aluminum oxide is implemented according to the following steps:
step 1, alkali treatment;
step 2, nano hydroxide and scindapsus aureus leaf/Al (OH)3Preparing;
step 3, morphism porous Al2O3Preparing ceramic powder;
step 4, blending the functional adhesive;
and 5, forming the composite film.
The invention is also characterized in that:
the step 1 is implemented according to the following steps: soaking the dried natural scindapsus aureus leaves in NaOH aqueous solution, washing the natural scindapsus aureus leaves with water to be neutral, and drying the leaves to obtain alkali-treated scindapsus aureus leaves.
In the step 1, the concentration of the NaOH aqueous solution is 15-25 wt%, the soaking time is 20-30 h, the drying temperature is 90-105 ℃, and the drying time is 2-3 h.
The step 2 is implemented according to the following steps: using Al2(SO4)3Preparation of Al (OH) by dropwise addition of aqueous solution to ammonia water by chemical coprecipitation3Nanometer hydroxide, immersing the alkali-treated scindapsus aureus leaf obtained in the step 1 into the hydroxide aqueous solution in a vacuum-pressure infiltration mode, taking out, drying and repeatedly operating to obtain scindapsus aureus leaf/Al (OH)3A precursor.
Al (OH) in the aqueous hydroxide solution of step 23The mass ratio of the green bonnie leaves to the alkali-treated green bonnie leaves is 94-95: 5 to 6.
Step 3 is specifically implemented according to the following steps: the dipped and dried scindapsus aureus leaf/Al (OH) obtained in the step 23Putting the precursor into an atmosphere furnace for heat preservation and sintering, taking out the precursor and then annealing to obtain morph-genetic porous Al2O3Ceramic powder.
In the step 3, the heat preservation sintering temperature is 900-1200 ℃, the heat preservation sintering time is 1-2 hours, the annealing temperature is 150-250 ℃, and the annealing time is 3-5 hours.
Step 4 is specifically implemented according to the following steps: taking the morph-genetic porous Al prepared in the step 32O3Ceramic powder, polyurethane adhesive, curing agent, 3-aminopropyl triethoxysilane with the concentration of 99 percent and benzotriazole are blended into the double-component polyurethane adhesive.
In the two-component polyurethane adhesive in the step 4, the mass ratio of the polyurethane adhesive, 3-aminopropyltriethoxysilane with the concentration of 99 percent, benzotriazole is 7: 1: 0.1: 0.2 morphism porous Al2O3The ceramic powder accounts for 5-8% of the double-component polyurethane adhesive by weight.
Step 5 is specifically implemented according to the following steps: uniformly coating the two-component polyurethane adhesive prepared in the step 4 on an aluminizer and a PET film by adopting a coating machine, carrying out compression molding, controlling the temperature and curing, and thus obtaining the microcosmic Al of the scindapsus aureus leaves2O3Powder modified functional composite membrane material.
The invention has the beneficial effects that:
1. the invention provides Al with microcosmic morphology of scindapsus aureus leaves based on the function modification effect of the morphotropism structure of the scindapsus aureus leaves2O3A method for preparing a powder modified functional composite membrane material.
2. The microcosmic Al of the scindapsus aureus leaves prepared by the method2O3The powder modified functional composite film material has unique ultraviolet light absorption characteristic and wide application prospect in the field of functional agricultural films.
Drawings
FIG. 1 shows a genetic state porous Al of the preparation method of the genetic state alumina modified agricultural film material2O3A low-power micro-morphology graph of the ceramic powder;
FIG. 2 shows a genetic state porous Al of the preparation method of the genetic state alumina modified agricultural film material2O3High-power micro-morphology graph of ceramic powder;
FIG. 3 is a comprehensive curve of sample pore volume-pore size distribution of the preparation method of the agricultural membrane material modified by morph-genetic aluminum oxide.
Detailed Description
The present invention will be described in detail with reference to the following embodiments.
Example 1
A preparation method of an agricultural film material modified by morph-genetic aluminum oxide is implemented according to the following steps:
step 1, alkali treatment;
step 2, nano hydroxide and scindapsus aureus leaf/Al (OH)3Preparing;
step 3, morphism porous Al2O3Preparing ceramic powder;
step 4, blending the functional adhesive;
and 5, forming the composite film.
The step 1 is implemented according to the following steps: soaking the dried natural scindapsus aureus leaves in NaOH aqueous solution, washing the natural scindapsus aureus leaves with water to be neutral, and drying the leaves to obtain alkali-treated scindapsus aureus leaves.
In the step 1, the concentration of the NaOH aqueous solution is 22 wt%, the soaking time is 27h, the drying temperature is 101 ℃, and the drying time is 2.5 h.
The step 2 is implemented according to the following steps: using Al2(SO4)3Preparation of Al (OH) by dropwise addition of aqueous solution to ammonia water by chemical coprecipitation3Nanometer hydroxide, immersing the alkali-treated scindapsus aureus leaf obtained in the step 1 into the hydroxide aqueous solution in a vacuum-pressure infiltration mode, taking out, drying and repeatedly operating to obtain scindapsus aureus leaf/Al (OH)3A precursor.
Al (OH) in the aqueous hydroxide solution of step 23The mass ratio of the green bonnie leaves treated by alkali to the green bonnie leaves treated by alkali is 94.5: 5.5.
step 3 is specifically implemented according to the following steps: the dipped and dried scindapsus aureus leaf/Al (OH) obtained in the step 23Putting the precursor into an atmosphere furnace for heat preservation and sintering, taking out the precursor and then annealing to obtain morph-genetic porous Al2O3The ceramic powder is shown in fig. 1 and 2.
In the step 3, the heat preservation sintering temperature is 900-1200 ℃, the heat preservation sintering time is 1.6h, the annealing temperature is 210 ℃, and the annealing time is 4 h.
Step 4 is specifically implemented according to the following steps: taking the morph-genetic porous Al prepared in the step 32O3Ceramic powder, polyurethane adhesive, curing agent, 3-aminopropyl triethoxysilane with the concentration of 99 percent and benzotriazole are blended into the double-component polyurethane adhesive.
In the two-component polyurethane adhesive in the step 4, the mass ratio of the polyurethane adhesive, 3-aminopropyltriethoxysilane with the concentration of 99 percent, benzotriazole is 7: 1: 0.1: 0.2 morphism porous Al2O3The ceramic powder accounts for 6.3 percent of the weight of the double-component polyurethane adhesive.
Step 5 is specifically implemented according to the following steps: uniformly coating the two-component polyurethane adhesive prepared in the step 4 on an aluminizer and a PET film by adopting a coating machine, carrying out compression molding, controlling the temperature and curing, and thus obtaining the microcosmic Al of the scindapsus aureus leaves2O3Powder modified functional composite membrane material.
As can be seen from fig. 1: al (OH) adsorbed on the surface of the microcosmic pore wall of scindapsus aureus leaf3Powder is subjected to aerobic sintering (template replacement process), and Al with similar leaf-shaped micro-morphology is obtained after in-situ chemical reaction2O3The powder can be seen to basically keep the characteristic of macroscopic leaf-shaped structure under a low-power scanning electron microscope, but in the aerobic sintering process, the template supporting effect is general, and the morph-genetic structure is not complete enough.
As can be seen in fig. 2: the genetic Al of the scindapsus aureus can be seen under a high-power scanning electron microscope2O3The powder is in a porous particle structure and is uniformly dispersed.
As can be seen in fig. 3: it can be seen that the average pore diameter is 8.66653nm, the most probable pore diameter is 2.202nm, and the BJH desorption cumulative total pore volume is 0.07408cm3(ii) in terms of/g. Both the differential pore volume-pore diameter distribution curve and the integral pore volume-pore diameter distribution curve show that the pore diameter distribution curves have relatively concentrated number of pore diameter distribution rules in the ranges of 2 nm-8 nm and 10 nm-20 nm, and the pore diameters are continuously distributed from 2 nm-90 nm, thereby indicating the morphism Al2O3The powder has a connection from micropores to mesopores and then to macroporesThe characteristics are continuously distributed, but the macro pores with the size of more than 50nm are fewer and the size is larger. The ultraviolet light has obvious absorption effect in the wave band ranges of 2 nm-8 nm and 10 nm-20 nm, but the absorption effect on the wave band above 50nm is weakened.
Example 2
A preparation method of an agricultural film material modified by morph-genetic aluminum oxide is implemented according to the following steps:
step 1, alkali treatment;
step 2, nano hydroxide and scindapsus aureus leaf/Al (OH)3Preparing;
step 3, morphism porous Al2O3Preparing ceramic powder;
step 4, blending the functional adhesive;
and 5, forming the composite film.
The step 1 is implemented according to the following steps: soaking the dried natural scindapsus aureus leaves in NaOH aqueous solution, washing the natural scindapsus aureus leaves with water to be neutral, and drying the leaves to obtain alkali-treated scindapsus aureus leaves.
In the step 1, the concentration of the NaOH aqueous solution is 15 wt%, the soaking time is 20h, the drying temperature is 90 ℃, and the drying time is 2 h.
The step 2 is implemented according to the following steps: using Al2(SO4)3Preparation of Al (OH) by dropwise addition of aqueous solution to ammonia water by chemical coprecipitation3Nanometer hydroxide, immersing the alkali-treated scindapsus aureus leaf obtained in the step 1 into the hydroxide aqueous solution in a vacuum-pressure infiltration mode, taking out, drying and repeatedly operating to obtain scindapsus aureus leaf/Al (OH)3A precursor.
Al (OH) in the aqueous hydroxide solution of step 23The mass ratio of the green bonnie leaves treated by alkali is 94: 6.
step 3 is specifically implemented according to the following steps: the dipped and dried scindapsus aureus leaf/Al (OH) obtained in the step 23Putting the precursor into an atmosphere furnace for heat preservation and sintering, taking out the precursor and then annealing to obtain morph-genetic porous Al2O3Ceramic powder.
In the step 3, the heat preservation sintering temperature is 900 ℃, the heat preservation sintering time is 1h, the annealing temperature is 150 ℃, and the annealing time is 3 h.
Step 4 is specifically implemented according to the following steps: taking the morph-genetic porous Al prepared in the step 32O3Ceramic powder, polyurethane adhesive, curing agent, 3-aminopropyl triethoxysilane with the concentration of 99 percent and benzotriazole are blended into the double-component polyurethane adhesive.
In the two-component polyurethane adhesive in the step 4, the mass ratio of the polyurethane adhesive, 3-aminopropyltriethoxysilane with the concentration of 99 percent, benzotriazole is 7: 1: 0.1: 0.2 morphism porous Al2O3The ceramic powder accounts for 5 percent of the weight of the double-component polyurethane adhesive.
Step 5 is specifically implemented according to the following steps: uniformly coating the two-component polyurethane adhesive prepared in the step 4 on an aluminizer and a PET film by adopting a coating machine, carrying out compression molding, controlling the temperature and curing, and thus obtaining the microcosmic Al of the scindapsus aureus leaves2O3Powder modified functional composite membrane material.
Example 3
A preparation method of an agricultural film material modified by morph-genetic aluminum oxide is implemented according to the following steps:
step 1, alkali treatment;
step 2, nano hydroxide and scindapsus aureus leaf/Al (OH)3Preparing;
step 3, morphism porous Al2O3Preparing ceramic powder;
step 4, blending the functional adhesive;
and 5, forming the composite film.
The step 1 is implemented according to the following steps: soaking the dried natural scindapsus aureus leaves in NaOH aqueous solution, washing the natural scindapsus aureus leaves with water to be neutral, and drying the leaves to obtain alkali-treated scindapsus aureus leaves.
In the step 1, the concentration of the NaOH aqueous solution is 25 wt%, the soaking time is 30h, the drying temperature is 105 ℃, and the drying time is 3 h.
The step 2 is implemented according to the following steps: using Al2(SO4)3Preparation of Al (OH) by dropwise addition of aqueous solution to ammonia water by chemical coprecipitation3Nano hydroxide, treating the alkali obtained in the step 1Soaking the green bonnie leaves in the hydroxide aqueous solution in a vacuum-pressure infiltration manner, taking out and drying the green bonnie leaves, and repeatedly operating to obtain the green bonnie leaves/Al (OH)3A precursor.
Al (OH) in the aqueous hydroxide solution of step 23The mass ratio of the green bonnie leaves treated by alkali is 95: 5.
step 3 is specifically implemented according to the following steps: the dipped and dried scindapsus aureus leaf/Al (OH) obtained in the step 23Putting the precursor into an atmosphere furnace for heat preservation and sintering, taking out the precursor and then annealing to obtain morph-genetic porous Al2O3Ceramic powder.
In the step 3, the heat preservation sintering temperature is 1200 ℃, the heat preservation sintering time is 2 hours, the annealing temperature is 250 ℃, and the annealing time is 5 hours.
Step 4 is specifically implemented according to the following steps: taking the morph-genetic porous Al prepared in the step 32O3Ceramic powder, polyurethane adhesive, curing agent, 3-aminopropyl triethoxysilane with the concentration of 99 percent and benzotriazole are blended into the double-component polyurethane adhesive.
In the two-component polyurethane adhesive in the step 4, the mass ratio of the polyurethane adhesive, 3-aminopropyltriethoxysilane with the concentration of 99 percent, benzotriazole is 7: 1: 0.1: 0.2 morphism porous Al2O3The ceramic powder accounts for 8 percent of the weight of the double-component polyurethane adhesive.
Step 5 is specifically implemented according to the following steps: uniformly coating the two-component polyurethane adhesive prepared in the step 4 on an aluminizer and a PET film by adopting a coating machine, carrying out compression molding, controlling the temperature and curing, and thus obtaining the microcosmic Al of the scindapsus aureus leaves2O3Powder modified functional composite membrane material.

Claims (10)

1. A preparation method of an agricultural film material modified by morph-genetic aluminum oxide is characterized by comprising the following steps:
step 1, alkali treatment;
step 2, nano hydroxide and scindapsus aureus leaf/Al (OH)3Preparing;
step 3, morphism porous Al2O3Of ceramic powdersPreparing;
step 4, blending the functional adhesive;
and 5, forming the composite film.
2. The preparation method of the agricultural film material modified by the morph-genetic aluminum oxide according to claim 1, wherein the step 1 is implemented by the following steps: soaking the dried natural scindapsus aureus leaves in NaOH aqueous solution, washing the natural scindapsus aureus leaves with water to be neutral, and drying the leaves to obtain alkali-treated scindapsus aureus leaves.
3. The preparation method of the agricultural film material modified by the morph-genetic aluminum oxide according to claim 2, wherein the concentration of the NaOH aqueous solution in the step 1 is 15 wt% -25 wt%, the soaking time is 20 h-30 h, the drying temperature is 90-105 ℃, and the drying time is 2-3 h.
4. The preparation method of the agricultural film material modified by the morph-genetic aluminum oxide as claimed in claim 2, wherein the step 2 is implemented by the following steps: using Al2(SO4)3Preparation of Al (OH) by dropwise addition of aqueous solution to ammonia water by chemical coprecipitation3Nanometer hydroxide, immersing the alkali-treated scindapsus aureus leaf obtained in the step 1 into the hydroxide aqueous solution in a vacuum-pressure infiltration mode, taking out, drying and repeatedly operating to obtain scindapsus aureus leaf/Al (OH)3A precursor.
5. The preparation method of the agricultural film material modified by the morph-genetic aluminum oxide as claimed in claim 4, wherein Al (OH) in the hydroxide aqueous solution of the step 23The mass ratio of the green bonnie leaves to the alkali-treated green bonnie leaves is 94-95: 5 to 6.
6. The preparation method of the agricultural film material modified by the morph-genetic aluminum oxide as claimed in claim 4, wherein the step 3 is implemented according to the following steps: the dipped and dried scindapsus aureus leaf/Al (OH) obtained in the step 23Putting the precursor into an atmosphere furnace for heat preservation and sintering, taking out and annealing,obtaining the morph-genetic porous Al2O3Ceramic powder.
7. The preparation method of the agricultural film material modified by the morph-genetic aluminum oxide according to claim 6, wherein in the step 3, the temperature-keeping sintering temperature is 900-1200 ℃, the temperature-keeping sintering time is 1-2 hours, the annealing temperature is 150-250 ℃, and the annealing time is 3-5 hours.
8. The preparation method of the agricultural film material modified by the morph-genetic aluminum oxide as claimed in claim 6, wherein the step 4 is implemented according to the following steps: taking the morph-genetic porous Al prepared in the step 32O3Ceramic powder, polyurethane adhesive, curing agent, 3-aminopropyl triethoxysilane with the concentration of 99 percent and benzotriazole are blended into the double-component polyurethane adhesive.
9. The preparation method of the agricultural film material modified by the morph-genetic aluminum oxide according to claim 6, wherein the mass ratio of the polyurethane adhesive, 3-aminopropyltriethoxysilane with a concentration of 99%, benzotriazole in the two-component polyurethane adhesive of step 4 is 7: 1: 0.1: 0.2 morphism porous Al2O3The ceramic powder accounts for 5-8% of the double-component polyurethane adhesive by weight.
10. The preparation method of the agricultural film material modified by the morph-genetic aluminum oxide as claimed in claim 8, wherein the step 5 is implemented according to the following steps: uniformly coating the two-component polyurethane adhesive prepared in the step 4 on an aluminizer and a PET film by adopting a coating machine, carrying out compression molding, controlling the temperature and curing, and thus obtaining the microcosmic Al of the scindapsus aureus leaves2O3Powder modified functional composite membrane material.
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CN113955781A (en) * 2021-10-20 2022-01-21 西安工程大学 Morph-genetic porous alumina with scindapsus aureus leaves as template and preparation method thereof

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