CN113563636B - Preparation method of enhanced light stabilizer for straw netting - Google Patents
Preparation method of enhanced light stabilizer for straw netting Download PDFInfo
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Abstract
The invention belongs to the technical field of plastic additive preparation, in particular to a preparation method of a reinforced light stabilizer for a baling net, which solves the problems that in the prior art, polyethylene plastic has poor light stability, the existing light stabilizer has poor compatibility with plastic or lacks an antioxidant additive, is easy to oxidize and decompose, reduces the service life and the like, and comprises the following steps: after zinc oxide acid treatment, mixing with cerium carbonate and zirconium dioxide; dispersing the mixed powder with polyvinyl alcohol aqueous solution, adding diethylenetriaminepentaacetic acid and vinyl tri (2-methoxy ethoxy) silane, and mixing to obtain a modifier; dissolving tert-octylphenol in absolute ethanol, and adding carbon disulfide and 4-n-butylamino-1-butanol to react to obtain a reactant; and dissolving the reactant in a mixed solvent, and adding the modifier for mixing to obtain the light stabilizer. The light stabilizer of the invention can obviously improve the performances of light aging resistance, oxidation resistance, heat resistance and the like of the grass baling net.
Description
Technical Field
The invention relates to the technical field of polycarbonate materials, in particular to a preparation method of a reinforced light stabilizer for a straw net.
Background
The fabric for binding straw or pasture is called as a straw binding net, and the material for producing the straw binding net mainly selects plastic materials with wear resistance, corrosion resistance and strong toughness, and is mostly polyethylene plastic. Polyethylene (PE) is a thermoplastic resin obtained by polymerizing ethylene. In industry, copolymers of ethylene with small amounts of alpha-olefins are also included. Polyethylene is odorless, nontoxic and wax-like in hand feeling, has excellent low-temperature resistance (the lowest use temperature can reach-100 to-70 ℃, the chemical stability is good, most of acid-base corrosion can be resisted (acid with oxidation property cannot be resisted). The polyethylene plastic is insoluble in a common solvent at normal temperature, has small water absorption and excellent electrical insulation property, and is widely applied in daily life.
The Chinese invention patent CN105237971A discloses a novel compound light stabilizer, which is prepared by compounding the following components in parts by weight: 65-50 parts of 2,2' -methylenebis (4-tert-octyl-6-benzotriazole phenol); 30-40 parts of poly (4-hydroxy-2, 6-tetramethyl-1-piperidineethanol) succinate; 5-10 parts of 2, 6-tetramethyl-4-piperidinol stearate. The light stabilizer is prepared by mixing and compounding three light stabilizers with specific compound structures, and has excellent light stability, thermal stability, durability and ageing resistance. Although the light stabilizer formed by the ternary compounding system can be better compatible in a plastic product, and the blind spots of the light stabilizer generated by local unevenness are avoided, the three light stabilizers are all long-chain piperidyl stearate structures, so that the cost is higher, the antioxidant auxiliary agent is lacked, the oxidation decomposition is easy, and the service life is shortened. Based on the statement, the invention provides a preparation method of the enhanced light stabilizer for the baling net.
Disclosure of Invention
The invention aims to solve the problems that the prior polyethylene plastic has poor light stability, the prior light stabilizer has poor compatibility with the plastic or lacks an antioxidant auxiliary agent, is easy to oxidize and decompose, reduces the service life and the like in the prior art, and provides a preparation method of the enhanced light stabilizer for a baling net.
A preparation method of a reinforced light stabilizer for a baling net comprises the following steps:
s1, carrying out acid leaching treatment on nano zinc oxide, washing and drying to obtain acid-treated zinc oxide, adding the acid-treated zinc oxide, cerium carbonate and zirconium dioxide into a ball mill together, and fully ball-milling and mixing to obtain mixed powder;
s2, adding the mixed powder obtained in the step S1 into a polyvinyl alcohol aqueous solution with the concentration of 17-25%, adding diethylenetriamine pentaacetic acid and vinyl tri (2-methoxyethoxy) silane while stirring and dispersing, stirring and mixing for 20-40min, and drying at the temperature of 95-102 ℃ to constant weight to obtain a modified substance;
s3, adding p-tert-octylphenol into absolute ethyl alcohol at the temperature of 3-15 ℃, stirring and dissolving under heat preservation, adding carbon disulfide and 4-n-butylamino-1-butanol under stirring, and continuously stirring and reacting under heat preservation for 2-3 hours to obtain a reactant;
and S4, dissolving the reactant in the step S3 by adding a mixed solvent, adding the modifier in the step S2, stirring and dispersing, dispersing and uniformly mixing, carrying out ultrasonic microwave treatment for 50-60min, controlling the ultrasonic frequency to be 28-34kHz, the ultrasonic power to be 250-350W, the microwave frequency to be 500-700MHz and the microwave power to be 400-500W, and then centrifuging, washing by absolute ethyl alcohol and drying to obtain the required enhanced light stabilizer.
Preferably, the acid leaching treatment in step S1 specifically refers to: adding the nano zinc oxide into hydrochloric acid solution with the temperature of 57-64 ℃ and the concentration of 0.8-2mol/L, stirring and mixing uniformly, performing ultrasonic dispersion for 10-20min, and then standing and preserving heat for 5-8h.
Preferably, the mass ratio of the nano zinc oxide to the hydrochloric acid solution is 1.
Preferably, the mass ratio of the acid-treated zinc oxide to the cerium carbonate to the zirconium dioxide in the step S1 is 18-20.
Preferably, the mass ratio of the mixed powder, the polyvinyl alcohol aqueous solution, the diethylenetriaminepentaacetic acid and the vinyl tris (2-methoxyethoxy) silane in the step S2 is 22-26.
Preferably, the mass ratio of p-tert-octylphenol, absolute ethanol, carbon disulfide and 4-n-butylamino-1-butanol in the step S3 is 5-8.
Preferably, the mixed solvent in the step S4 is a mixed solution of chloroform, petroleum ether and ethanol in a mass ratio of 3-4.
Preferably, the amount of the mixed solvent added in step S4 is 11 to 14 times of the total amount of the reactants.
The preparation method of the enhanced light stabilizer for the baling net provided by the invention has the following beneficial effects:
1. the method comprises the steps of treating nano zinc oxide acid, ball-milling and mixing the treated nano zinc oxide acid with cerium carbonate and zirconium dioxide, and then adding diethylenetriamine pentaacetic acid and vinyl tri (2-methoxyethoxy) silane to modify mixed powder in the presence of a polyvinyl alcohol aqueous solution to obtain a modified substance; the modified product obtained by the invention has good functions of high temperature resistance, corrosion resistance, shading, ultraviolet shielding and the like.
2. In the presence of absolute ethyl alcohol, p-tert-octylphenol reacts with carbon disulfide and 4-n-butylamino-1-butanol to prepare a reactant, the reactant and a modifier are mixed and subjected to ultrasonic microwave treatment to prepare the compound enhanced light stabilizer, and the light stabilizer prepared by the method not only has the function of resisting ultraviolet radiation, but also has the function of an antioxidant, and has good heat resistance, thermal oxidation and thermodynamic stability; the modified polyolefin plastic has good compatibility with plastics, especially has chelation effect on polyolefin plastics, and not only can effectively improve the weather resistance of the polyolefin plastics, but also can improve the environmental stress cracking resistance of the polyolefin plastics.
3. The preparation method is simple, the preparation conditions are mild, and the obtained enhanced light stabilizer has a remarkable effect of improving the weather resistance of the grass baling net, can remarkably improve the light aging resistance, the oxidation resistance, the heat resistance and the like of the grass baling net, and has the characteristics of uniform dispersion and stable performance.
Detailed Description
The present invention will be further illustrated with reference to the following specific examples.
Example one
S1, adding nano zinc oxide into a hydrochloric acid solution with the temperature of 57 ℃ and the concentration of 0.8mol/L, uniformly stirring and mixing, performing ultrasonic dispersion for 10min, standing, performing heat preservation for 5h, washing and drying to obtain acid-treated zinc oxide, adding the acid-treated zinc oxide, cerium carbonate and zirconium dioxide into a ball mill together according to a mass ratio of 18;
s2, adding the mixed powder in the step S1 into a 17% polyvinyl alcohol aqueous solution, stirring and dispersing, adding diethylenetriamine pentaacetic acid and vinyl tris (2-methoxyethoxy) silane, stirring and mixing for 20min, and drying at the temperature of 95 ℃ to constant weight to obtain a modified substance, wherein the mass ratio of the mixed powder, the polyvinyl alcohol aqueous solution, the diethylenetriamine pentaacetic acid and the vinyl tris (2-methoxyethoxy) silane is 22;
s3, adding p-tert-octylphenol into anhydrous ethanol with the temperature of 3 ℃, keeping the temperature, stirring and dissolving, adding carbon disulfide and 4-n-butylamino-1-butanol while stirring, and continuing to keep the temperature, stirring and reacting for 2 hours to obtain a reactant, wherein the mass ratio of the p-tert-octylphenol to the anhydrous ethanol to the carbon disulfide to the 4-n-butylamino-1-butanol is 5;
s4, adding a mixed solvent into the reactant in the step S3 for dissolving, adding the modifier in the step S2 for stirring and dispersing, after dispersing and mixing uniformly, carrying out ultrasonic microwave treatment for 50min, controlling the ultrasonic frequency to be 28kHz, the ultrasonic power to be 250W, the microwave frequency to be 500MHz and the microwave power to be 400W, then carrying out centrifugation, absolute ethyl alcohol washing and drying to obtain the required enhanced light stabilizer, wherein the mixed solvent is a mixed solution of trichloromethane, petroleum ether and ethyl alcohol in a mass ratio of 3.
Example two
The invention provides a preparation method of a reinforced light stabilizer for a baling net, which comprises the following steps:
s1, adding nano zinc oxide into a hydrochloric acid solution with the temperature of 60 ℃ and the concentration of 1.4mol/L, uniformly stirring and mixing, performing ultrasonic dispersion for 15min, standing, performing heat preservation for 6.5h, washing and drying to obtain acid-treated zinc oxide, adding the acid-treated zinc oxide, cerium carbonate and zirconium dioxide into a ball mill together according to a mass ratio of 19;
s2, adding the mixed powder in the step S1 into a polyvinyl alcohol aqueous solution with the concentration of 21%, stirring and dispersing, adding diethylenetriamine pentaacetic acid and vinyl tris (2-methoxyethoxy) silane, stirring and mixing for 30min, and drying at the temperature of 98 ℃ to constant weight to obtain a modified substance, wherein the mass ratio of the mixed powder, the polyvinyl alcohol aqueous solution, the diethylenetriamine pentaacetic acid and the vinyl tris (2-methoxyethoxy) silane is 24;
s3, adding p-tert-octylphenol into anhydrous ethanol at the temperature of 9 ℃, keeping the temperature, stirring and dissolving, adding carbon disulfide and 4-n-butylamino-1-butanol while stirring, and continuously keeping the temperature, stirring and reacting for 2.5 hours to obtain a reactant, wherein the mass ratio of the p-tert-octylphenol to the anhydrous ethanol to the carbon disulfide to the 4-n-butylamino-1-butanol is 6.5;
and S4, adding a mixed solvent into the reactant in the step S3 for dissolving, adding the modifier in the step S2 for stirring and dispersing, uniformly dispersing and mixing, performing ultrasonic microwave treatment for 55min, controlling the ultrasonic frequency to be 31kHz, the ultrasonic power to be 300W, the microwave frequency to be 600MHz and the microwave power to be 450W, and then performing centrifugation, absolute ethanol washing and drying to obtain the required enhanced light stabilizer, wherein the mixed solvent is a mixed solution of trichloromethane, petroleum ether and ethanol in a mass ratio of 3.5.
EXAMPLE III
The invention provides a preparation method of a reinforced light stabilizer for a baling net, which comprises the following steps:
s1, adding nano zinc oxide into a hydrochloric acid solution with the temperature of 64 ℃ and the concentration of 2mol/L, stirring and mixing uniformly, performing ultrasonic dispersion for 20min, standing and heat preservation for 8h, washing and drying to obtain acid-treated zinc oxide, adding the acid-treated zinc oxide, cerium carbonate and zirconium dioxide into a ball mill together according to a mass ratio of 20;
s2, adding the mixed powder obtained in the step S1 into a polyvinyl alcohol aqueous solution with the concentration of 25%, stirring and dispersing, adding diethylenetriamine pentaacetic acid and vinyl tris (2-methoxyethoxy) silane, stirring and mixing for 40min, and drying at the temperature of 102 ℃ to constant weight to obtain a modified substance, wherein the mass ratio of the mixed powder to the polyvinyl alcohol aqueous solution to the diethylenetriamine pentaacetic acid to the vinyl tris (2-methoxyethoxy) silane is (26);
s3, adding p-tert-octylphenol into absolute ethanol at the temperature of 15 ℃, keeping the temperature, stirring and dissolving, adding carbon disulfide and 4-n-butylamino-1-butanol while stirring, and continuously keeping the temperature, stirring and reacting for 3 hours to obtain a reactant, wherein the mass ratio of p-tert-octylphenol to absolute ethanol to carbon disulfide to 4-n-butylamino-1-butanol is (8);
and S4, adding a mixed solvent into the reactant in the step S3 for dissolving, adding the modifier in the step S2 for stirring and dispersing, performing ultrasonic microwave treatment for 60min after uniform dispersion and mixing, controlling the ultrasonic frequency to be 34kHz, the ultrasonic power to be 350W, the microwave frequency to be 700MHz and the microwave power to be 500W, and then performing centrifugation, absolute ethanol washing and drying to obtain the required enhanced light stabilizer, wherein the mixed solvent is a mixed solution of chloroform, petroleum ether and ethanol in a mass ratio of 4.
Comparative example 1
The invention provides a preparation method of a reinforced light stabilizer for a baling net, which comprises the following steps:
s1, adding nano zinc oxide into a hydrochloric acid solution with the temperature of 57 ℃ and the concentration of 0.8mol/L, uniformly stirring and mixing, performing ultrasonic dispersion for 10min, standing, performing heat preservation for 5h, washing and drying to obtain acid-treated zinc oxide, adding the acid-treated zinc oxide, cerium carbonate and zirconium dioxide into a ball mill together according to a mass ratio of 18;
s2, adding p-tert-octylphenol into anhydrous ethanol at the temperature of 3 ℃, keeping the temperature, stirring and dissolving, adding carbon disulfide and 4-n-butylamino-1-butanol while stirring, and continuously keeping the temperature, stirring and reacting for 2 hours to obtain a reactant, wherein the mass ratio of the p-tert-octylphenol to the anhydrous ethanol to the carbon disulfide to the 4-n-butylamino-1-butanol is (5);
and S3, adding a mixed solvent into the reactant in the step S2 for dissolving, adding the mixed powder in the step S1, stirring and dispersing, uniformly dispersing and mixing, performing ultrasonic microwave treatment for 50min, controlling the ultrasonic frequency to be 28kHz, the ultrasonic power to be 250W, the microwave frequency to be 500MHz and the microwave power to be 400W, and then performing centrifugation, absolute ethanol washing and drying to obtain the required enhanced light stabilizer, wherein the mixed solvent is a mixed solution of chloroform, petroleum ether and ethanol with a mass ratio of 3.
Comparative example No. two
The invention provides a preparation method of a reinforced light stabilizer for a baling net, which comprises the following steps:
s1, adding nano zinc oxide into a hydrochloric acid solution with the temperature of 57 ℃ and the concentration of 0.8mol/L, uniformly stirring and mixing, performing ultrasonic dispersion for 10min, standing, performing heat preservation for 5h, washing and drying to obtain acid-treated zinc oxide;
s2, adding the acid-treated zinc oxide in the step S1 into a 17% polyvinyl alcohol aqueous solution, adding diethylenetriamine pentaacetic acid and vinyl tris (2-methoxyethoxy) silane while stirring and dispersing, stirring and mixing for 20min, and drying at a temperature of 95 ℃ to constant weight to obtain a modified product, wherein the mass ratio of the acid-treated zinc oxide to the polyvinyl alcohol aqueous solution to the diethylenetriamine pentaacetic acid to the vinyl tris (2-methoxyethoxy) silane is 22;
s3, adding p-tert-octylphenol into anhydrous ethanol at the temperature of 3 ℃, keeping the temperature, stirring and dissolving, adding carbon disulfide and 4-n-butylamino-1-butanol while stirring, and continuously keeping the temperature, stirring and reacting for 2 hours to obtain a reactant, wherein the mass ratio of the p-tert-octylphenol to the anhydrous ethanol to the carbon disulfide to the 4-n-butylamino-1-butanol is (5);
s4, adding a mixed solvent into the reactant in the step S3 for dissolving, adding the modifier in the step S2 for stirring and dispersing, uniformly dispersing and mixing, performing ultrasonic microwave treatment for 50min, controlling the ultrasonic frequency to be 28kHz, the ultrasonic power to be 250W, the microwave frequency to be 500MHz and the microwave power to be 400W, and then performing centrifugation, absolute ethanol washing and drying to obtain the required enhanced light stabilizer, wherein the mixed solvent is a mixed solution of trichloromethane, petroleum ether and ethanol with the mass ratio of 3.
Comparative example No. three
The invention provides a preparation method of a reinforced light stabilizer for a grass-baling net, which comprises the following steps:
s1, adding nano zinc oxide into a hydrochloric acid solution with the temperature of 57 ℃ and the concentration of 0.8mol/L, uniformly stirring and mixing, performing ultrasonic dispersion for 10min, standing, performing heat preservation for 5h, washing and drying to obtain acid-treated zinc oxide, adding the acid-treated zinc oxide, cerium carbonate and zirconium dioxide into a ball mill together according to a mass ratio of 18;
s2, adding the mixed powder in the step S1 into a 17% polyvinyl alcohol aqueous solution, stirring and dispersing, adding diethylenetriamine pentaacetic acid and vinyl tris (2-methoxyethoxy) silane, stirring and mixing for 20min, and drying at the temperature of 95 ℃ to constant weight to obtain a modified substance, wherein the mass ratio of the mixed powder, the polyvinyl alcohol aqueous solution, the diethylenetriamine pentaacetic acid and the vinyl tris (2-methoxyethoxy) silane is 22;
and S3, adding the modifier in the step S2 into a mixed solvent, stirring and dispersing, performing ultrasonic microwave treatment for 50min, controlling the ultrasonic frequency to be 28kHz, the ultrasonic power to be 250W, the microwave frequency to be 500MHz and the microwave power to be 400W, and then performing centrifugation, absolute ethyl alcohol washing and drying to obtain the required enhanced light stabilizer, wherein the mixed solvent is a mixed solution of chloroform, petroleum ether and ethanol with the mass ratio of 3.
The light stabilizer prepared in the first to third examples and the first to third comparative examples is added into the polyethylene plastic, the adding amount of the light stabilizer is 0.3 percent of the total amount of the polyethylene plastic, the mixture is extruded at 180 ℃ to be processed into a grass binding net of 0.5m multiplied by 1m, and the tensile strength before and after aging is tested according to GB/T13022-1991 (the aging condition is lamp tube type: UVB-340; irradiance (340 nm): 0.76W/square meter/nm; black standard temperature: 60 +/-3 ℃/50 +/-3 ℃, and illumination/condensation cycle: 480min/240 min), the following results are obtained:
the above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (8)
1. A preparation method of a reinforced light stabilizer for a baling net is characterized by comprising the following steps:
s1, carrying out acid leaching treatment on nano zinc oxide, washing and drying to obtain acid-treated zinc oxide, adding the acid-treated zinc oxide, cerium carbonate and zirconium dioxide into a ball mill together, and fully ball-milling and mixing to obtain mixed powder;
s2, adding the mixed powder obtained in the step S1 into a polyvinyl alcohol aqueous solution with the concentration of 17-25%, adding diethylenetriamine pentaacetic acid and vinyl tri (2-methoxyethoxy) silane while stirring and dispersing, stirring and mixing for 20-40min, and drying at the temperature of 95-102 ℃ to constant weight to obtain a modified substance;
s3, adding p-tert-octylphenol into absolute ethyl alcohol at the temperature of 3-15 ℃, keeping the temperature, stirring and dissolving, adding carbon disulfide and 4-n-butylamino-1-butanol while stirring, and continuously keeping the temperature, stirring and reacting for 2-3 hours to obtain a reactant;
and S4, dissolving the reactant in the step S3 by adding a mixed solvent, adding the modifier in the step S2, stirring and dispersing, dispersing and uniformly mixing, carrying out ultrasonic microwave treatment for 50-60min, controlling the ultrasonic frequency to be 28-34kHz, the ultrasonic power to be 250-350W, the microwave frequency to be 500-700MHz and the microwave power to be 400-500W, and then centrifuging, washing by absolute ethyl alcohol and drying to obtain the required enhanced light stabilizer.
2. The method for preparing the enhanced light stabilizer for the baling net according to claim 1, wherein the acid leaching treatment in step S1 specifically refers to: adding the nano zinc oxide into hydrochloric acid solution with the temperature of 57-64 ℃ and the concentration of 0.8-2mol/L, stirring and mixing uniformly, performing ultrasonic dispersion for 10-20min, and then standing and preserving heat for 5-8h.
3. The method for preparing the enhanced light stabilizer for the baling net according to claim 2, wherein the mass ratio of the nano zinc oxide to the hydrochloric acid solution is 1.
4. The method for preparing the enhanced light stabilizer for the baling net according to claim 1, wherein the mass ratio of acid-treated zinc oxide, cerium carbonate and zirconium dioxide in step S1 is 18-20.
5. The method for preparing the enhanced light stabilizer for the baling net according to claim 1, wherein the mass ratio of the mixed powder, the aqueous solution of polyvinyl alcohol, the diethylenetriaminepentaacetic acid and the vinyltris (2-methoxyethoxy) silane in the step S2 is 22-26.
6. The method for preparing the enhanced light stabilizer for the baling net according to claim 1, wherein the mass ratio of p-tert-octylphenol, absolute ethanol, carbon disulfide and 4-n-butylamino-1-butanol in step S3 is 5-8.
7. The method for preparing the enhanced light stabilizer for the grass netting according to claim 1, wherein the mixed solvent in the step S4 is a mixed solution of chloroform, petroleum ether and ethanol in a mass ratio of 3-4.
8. The method for preparing the enhanced light stabilizer for baling net according to claim 1, wherein the amount of the mixed solvent added in step S4 is 11-14 times of the total amount of the reactants.
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| CN103031056A (en) * | 2012-12-18 | 2013-04-10 | 安徽六方重联机械股份有限公司 | Metal surface silane treating agent containing aqueous nano-zinc oxide and preparation method thereof |
| CN103045086A (en) * | 2012-12-18 | 2013-04-17 | 安徽六方重联机械股份有限公司 | Metal surface silane treating agent and preparation method thereof |
| CN112048125A (en) * | 2020-08-11 | 2020-12-08 | 卞培培 | Anti-aging polypropylene material based on fiber reinforcement and preparation method thereof |
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| US9976036B2 (en) * | 2014-09-05 | 2018-05-22 | Sakai Chemical Industry Co., Ltd. | Organic solvent dispersion of zirconium oxide particles and method for producing same |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103031056A (en) * | 2012-12-18 | 2013-04-10 | 安徽六方重联机械股份有限公司 | Metal surface silane treating agent containing aqueous nano-zinc oxide and preparation method thereof |
| CN103045086A (en) * | 2012-12-18 | 2013-04-17 | 安徽六方重联机械股份有限公司 | Metal surface silane treating agent and preparation method thereof |
| CN112048125A (en) * | 2020-08-11 | 2020-12-08 | 卞培培 | Anti-aging polypropylene material based on fiber reinforcement and preparation method thereof |
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