CN114133651A - Lasting anti-fog and non-drip polyethylene film master batch and preparation method thereof - Google Patents

Lasting anti-fog and non-drip polyethylene film master batch and preparation method thereof Download PDF

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CN114133651A
CN114133651A CN202111362878.6A CN202111362878A CN114133651A CN 114133651 A CN114133651 A CN 114133651A CN 202111362878 A CN202111362878 A CN 202111362878A CN 114133651 A CN114133651 A CN 114133651A
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master batch
drip
antifogging
polyethylene film
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CN114133651B (en
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王豹
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Anhui Guofeng Plastic Industry Co Ltd
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Anhui Guofeng Plastic Industry Co Ltd
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    • 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
    • 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
    • C08J2323/08—Copolymers of ethene
    • 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
    • C08J2423/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
    • C08J2423/02—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
    • C08J2423/04—Homopolymers or copolymers of ethene
    • C08J2423/06—Polyethene
    • 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
    • C08J2423/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
    • C08J2423/02—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
    • C08J2423/04—Homopolymers or copolymers of ethene
    • C08J2423/08—Copolymers of ethene
    • 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
    • C08J2433/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
    • C08J2433/04—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters
    • C08J2433/06—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters of esters containing only carbon, hydrogen, and oxygen, the oxygen atom being present only as part of the carboxyl radical
    • C08J2433/10—Homopolymers or copolymers of methacrylic acid esters
    • C08J2433/12—Homopolymers or copolymers of methyl methacrylate
    • 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
    • C08K2003/2227—Oxides; Hydroxides of metals of aluminium
    • 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
    • C08K2003/2296—Oxides; Hydroxides of metals of zinc
    • 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
    • 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
    • C08K5/00—Use of organic ingredients
    • C08K5/04—Oxygen-containing compounds
    • C08K5/10—Esters; Ether-esters
    • C08K5/101—Esters; Ether-esters of monocarboxylic acids
    • C08K5/103—Esters; Ether-esters of monocarboxylic acids with polyalcohols

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  • Manufacturing & Machinery (AREA)
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Abstract

The invention discloses a durable antifogging dripless polyethylene film master batch, which comprises the following components in parts by mass: 65-78 parts of linear low-density polyethylene, 22-35 parts of low-density polyethylene, 3-7 parts of ethylene-vinyl acetate copolymer, 0.1-1 part of antifogging agent, 2-5 parts of dripless agent and 0.1-1 part of metal oxide. The invention also discloses a preparation method of the film master batch. The master batch has excellent processability and can be mixed with the special resin for the greenhouse film in any proportion to blow a wide film, the master batch can enhance the toughness, cold resistance, non-dripping effect and durability of the anti-fogging effect of the film, and the anti-fogging non-dripping duration can be kept above 3 years.

Description

Lasting anti-fog and non-drip polyethylene film master batch and preparation method thereof
Technical Field
The invention relates to the technical field of plastic film high polymer materials, in particular to a durable antifogging dripless polyethylene film master batch and a preparation method thereof.
Background
At present, the most important agricultural application of the polyethylene non-drip film is to use the polyethylene non-drip film as a greenhouse film. The plastic greenhouse plays an important role in the early sowing and the maturation of vegetables and melons and fruits, provides fresh vegetables all the year round and makes great contribution to meeting the living needs of people. The main function of the plastic greenhouse is to increase the temperature in the greenhouse. However, the drip-proof agent such as 540B, 622A or W94 in the polyethylene drip-free film master batch used by most agricultural mulch film manufacturers (or produced by the manufacturers) only has the drip-proof effect, so that the fog in the greenhouse is large, flowering vegetables such as cucumbers, watermelons, eggplants and the like are easy to be infected with diseases, and the yield and harvest are influenced.
In addition, the existing polyethylene antifogging non-drip film is prepared by adding a certain proportion of fluorine antifogging agent (such as an antifogging agent perfluoroalkane) into the original non-drip master batch, so that the produced non-drip film has a certain antifogging property. The polyethylene anti-fog drop film has poor non-drop persistence and the anti-fog drop persistence period is only about 3-10 months. Therefore, prolonging the non-drip duration of the polyethylene greenhouse film becomes a key problem which must be solved by common efforts in the field of polyethylene greenhouse film processing.
Disclosure of Invention
Based on the technical problems in the background art, the invention provides a durable antifogging non-dropping polyethylene film master batch and a preparation method thereof.
The invention provides a durable antifogging dripless polyethylene film master batch, which comprises the following components in parts by mass: 65-78 parts of linear low-density polyethylene, 22-35 parts of low-density polyethylene, 3-7 parts of ethylene-vinyl acetate copolymer, 0.1-1 part of antifogging agent, 2-5 parts of dripless agent and 0.1-1 part of metal oxide;
the non-dropping agent is maleic anhydride-methyl methacrylate graft copolymer which is prepared by grafting maleic anhydride onto methyl methacrylate under the action of an initiator.
Preferably, the maleic anhydride grafting rate of the non-dropping agent is 18% or more.
Preferably, the raw materials for preparing the non-dropping agent comprise methyl methacrylate, maleic anhydride and an initiator, wherein the mass ratio of the methyl methacrylate to the maleic anhydride to the initiator is 100: (21.6-31.5): (0.09-0.15).
Preferably, the method for preparing the non-dropping agent comprises the following steps:
(1) in an inert atmosphere, carrying out heat preservation stirring reaction on methyl methacrylate and part of initiator at 65-75 ℃ for 20-40 min;
(2) cooling to 45-55 ℃, adding the rest of initiator, hot water at the temperature of 45-55 ℃ and maleic anhydride, carrying out heat preservation stirring reaction for 20-40 min, then heating to 85-95 ℃, carrying out heat preservation stirring reaction for 2-4 h, cooling to 45-55 ℃ after the reaction is finished, removing a water phase, washing an organic phase with water, and drying the obtained solid product to obtain the catalyst.
Preferably, the initiator is at least one of azobisisobutyronitrile, azobisisoheptonitrile and dimethyl azobisisobutyrate.
Preferably, the initiator added in step (1) accounts for 60-70% of the total mass of the initiator.
Preferably, the ratio of methyl methacrylate to hot water is 1 g: (1.5-3) mL.
Preferably, the antifogging agent is at least one of polyglycerol fatty acid ester, polyethylene oxide glycerol fatty acid ester, sorbitan fatty acid ester, polyoxyethylene sorbitol fatty acid ester, polyoxyethylene sorbitan monolaurate and polyoxyethylene sorbitan monopalmitate.
Preferably, the metal oxide is nano aluminum oxide, nano zinc oxide or a combination thereof.
The preparation method of the lasting anti-fog and non-drip polyethylene film master batch is characterized by comprising the following steps:
s1, uniformly mixing linear low-density polyethylene, low-density polyethylene and ethylene-vinyl acetate copolymer at a high speed to obtain a mixture A;
s2, uniformly mixing the mixture A with an antifogging agent, a non-dropping agent and a metal oxide at a high speed to obtain a mixture B;
and S3, adding the mixture B into a double-screw extruder for reaction, and then extruding, cooling and granulating to obtain the lasting anti-fog non-drip film master batch.
Preferably, in S1 and S2, the time for high-speed mixing is 3-5 min.
Preferably, in S3, the reaction temperature is 170-220 ℃ and the reaction time is 3-5 min.
The invention has the following beneficial effects:
1. the invention adopts the combination of the long-chain fatty acid and ester antifogging agent and the novel dripless agent to prepare the antifogging dripless master batch, has better antifogging dripless effect and has durable antifogging dripless performance.
2. EVA is a thermoplastic resin having rubber elasticity, and has good toughness, flexibility, stress cracking resistance, adhesion, and the like. EVA and polyolefin resin are blended to be used as a modifier, and elastic particles are added to PE molecular chains. Because of its low glass transition temperature and low viscosity, when blended with PE, a suitable second phase forms with the increase in EVA. Because both groups have ethylene groups and have better compatibility, the polyethylene film has strong toughening effect on PE, and enhances the capability of the PE for bearing external force and solvent to crack, thereby enhancing the toughness, cold resistance, no-drip effect and durability of antifogging effect.
3. The nanometer alumina is in a spherical structure, has better adsorbability on the surface, better dispersibility in PE, good interfusion with PE resin interface, small particle size and large specific surface area, is used for PE films, and has the advantages of difficult film cracking, no white point, and nanometer adsorption function, thereby prolonging the initial time of film fog drops.
The invention solves the difficulty of large fog in the greenhouse, solves the problem of short effective period of the fog-proof drop of the existing fog-proof drop film, and makes contributions to reducing the plant diseases and insect pests of vegetables, particularly flowering vegetables and improving the yield of the vegetables.
Detailed Description
The technical solution of the present invention will be described in detail below with reference to specific examples.
Example 1
A durable antifogging non-drip polyethylene film master batch comprises the following components in parts by mass: 65 parts of linear low-density polyethylene, 35 parts of low-density polyethylene, 3 parts of ethylene-vinyl acetate copolymer, 0.1 part of polyglycerol fatty acid ester, 2 parts of dripless and 0.1 part of nano-alumina.
The preparation method of the dripless agent comprises the following steps:
(1) adding 100g of methyl methacrylate and 0.06g of azobisisobutyronitrile into a 500ml four-mouth bottle provided with a stirrer, a reflux condenser tube, a dropping funnel and nitrogen, placing in a water bath, starting cooling water, introducing nitrogen, starting the stirrer, heating to 70 ℃, preserving heat and stirring for 30 min;
(2) cooling to 50 ℃, adding 0.03g of azobisisobutyronitrile, adding 200mL of distilled water at 50 ℃, quickly adding 21.6g of maleic anhydride, carrying out heat preservation and stirring reaction for 30min, then heating to 90 ℃, carrying out heat preservation and stirring reaction for 3h, removing the water bath after the reaction is finished, naturally cooling to 50 ℃, then pouring into a separating funnel, separating the water phase, washing the organic phase with 200mL of deionized water for 3 times, and drying the obtained solid product in a vacuum oven at 50 ℃ to obtain the product.
1.0g of the obtained dripless agent is dissolved in 25ml of trichloromethane, 20 mul of internal standard isobutanol is added, the content of the maleic anhydride is detected to be 14.4 percent by a SQ-204 gas chromatograph, and the grafting rate of the maleic anhydride is calculated to be 18.1 percent.
The preparation method of the lasting anti-fog and non-drip polyethylene film master batch comprises the following steps:
s1, mixing linear low-density polyethylene, low-density polyethylene and ethylene-vinyl acetate copolymer at a high speed for 4min to obtain a mixture A;
s2, mixing the mixture A with polyglycerol fatty acid ester, no-drop agent and metal oxide at a high speed for 4min to obtain a mixture B;
and S3, adding the mixture B into a double-screw extruder for reaction at the reaction temperature of 200 ℃ for 4min, and then extruding, cooling and granulating to obtain the lasting anti-fog non-drip film master batch.
Example 2
A durable antifogging non-drip polyethylene film master batch comprises the following components in parts by mass: 70 parts of linear low-density polyethylene, 30 parts of low-density polyethylene, 5 parts of ethylene-vinyl acetate copolymer, 0.3 part of polyglycerol fatty acid ester, 3 parts of dripless and 0.5 part of nano-alumina.
Among them, the preparation method of the non-dropping agent was the same as that of example 1.
The preparation method of the film master batch is the same as that of example 1.
Example 3
A durable antifogging non-drip polyethylene film master batch comprises the following components in parts by mass: 75 parts of linear low-density polyethylene, 25 parts of low-density polyethylene, 7 parts of ethylene-vinyl acetate copolymer, 0.7 part of polyglycerol fatty acid ester, 5 parts of dripless and 0.8 part of nano-alumina.
Among them, the preparation method of the non-dropping agent was the same as that of example 1.
The preparation method of the film master batch is the same as that of example 1.
Comparative example 1
Comparative example 1 differs from example 1 only in that: the components of the film master batch do not contain a non-dropping agent.
Comparative example 2
Comparative example 2 differs from example 1 only in that: the components of the film master batch do not contain nano alumina.
Test examples
The antifogging and dripless polyethylene master batches prepared in examples 1-3 and comparative examples 1-2 are applied to a polyethylene film, and the specific method comprises the following steps: uniformly mixing low-density polyethylene (LDPE), linear low-density polyethylene (LLDPE) and antifogging non-drip polyethylene film master batch according to the mass ratio of 15:70:15, adding the mixture into a double-screw extruder, extruding and blow-molding to obtain the antifogging non-drip polyethylene film, wherein the temperature of each section of the double-screw extruder is as follows: a first stage: 170 ℃ and a second stage: 180 ℃ and three stages: 190 ℃ and four stages: 185 ℃ and five stages: 180 ℃ is carried out. And (3) carrying out performance test on the prepared film, wherein the test method comprises the following steps:
1. initial antifogging property: and (3) placing the beaker in a constant-temperature water tank at 60 ℃, and observing the water stain condition on the surface of the film within 15min, wherein the ambient temperature is room temperature. A, no change in membrane surface; b, generating water stains on the membrane surface, but disappearing within 3 min; c, generating water stains on the membrane surface, but disappearing within 15 min; d, after 15min, the film surface still has water stains, but is transparent.
2. High temperature anti-fogging property: a square greenhouse film with the length of 15cm, the width of 15cm and the thickness of about 0.08mm is covered on a 500mL beaker, the cup opening is tightened, and 300mL of water is filled in the beaker. Then the beaker is placed in a constant temperature water tank at 60 ℃ with an inclination angle of 15 degrees and the ambient temperature is room temperature. 1/3 where the area of the droplets on the film exceeded the film face at 60 ℃ was considered to be ineffective. The time that the shelf film spends from initial use to failure is defined as the non-drip duration of the shelf film.
3. Low temperature anti-fogging: a square greenhouse film with the length of 15cm, the width of 15cm and the thickness of about 0.08mm is covered on a 500mL beaker, the cup opening is tightened, and 300mL of water is filled in the beaker. Then the beaker is placed in a constant temperature water tank at 18 ℃ and the ambient temperature is-5 ℃. A droplet area on the film exceeding 1/4 was considered to be a failure.
4. And (3) evaluating the drip-proof durability of the greenhouse film: and (4) carrying out actual observation on the coverage of the farmland greenhouse, wherein the distribution area of the scaly water drops on the inner surface of the greenhouse film reaches 50% days. ●: the distribution area of scaly water drops on the inner surface of the greenhouse film reaches below 50 percent, and the film has good transparency. O: the distribution area of scaly water drops on the inner surface of the greenhouse film reaches more than 50 percent, and the transparency of the film is poor.
The results of the performance test of the above films are shown in table 1:
TABLE 1 film Performance test results
Figure BDA0003359520940000071
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 (10)

1. The lasting antifogging non-drip polyethylene film master batch is characterized by comprising the following components in parts by mass: 65-78 parts of linear low-density polyethylene, 22-35 parts of low-density polyethylene, 3-7 parts of ethylene-vinyl acetate copolymer, 0.1-1 part of antifogging agent, 2-5 parts of dripless and 0.1-1 part of metal oxide;
the non-dropping agent is maleic anhydride-methyl methacrylate graft copolymer which is prepared by grafting maleic anhydride onto methyl methacrylate under the action of an initiator.
2. The durable antifog non-drip polyethylene film master batch according to claim 1, wherein the non-drip agent has a maleic anhydride grafting ratio of 18% or more.
3. The permanent antifogging non-dropping polyethylene film master batch according to claim 1, wherein the preparation raw material of the non-dropping agent comprises methyl methacrylate, maleic anhydride and an initiator, wherein the mass ratio of the methyl methacrylate to the maleic anhydride to the initiator is 100: (21.6-31.5): (0.09-0.15).
4. The permanent antifog non-drip polyethylene film master batch according to claim 1, characterized in that said non-drip agent is prepared by:
(1) in an inert atmosphere, carrying out heat preservation stirring reaction on methyl methacrylate and part of initiator at 65-75 ℃ for 20-40 min;
(2) cooling to 45-55 ℃, adding the rest of initiator, hot water at the temperature of 45-55 ℃ and maleic anhydride, carrying out heat preservation stirring reaction for 20-40 min, then heating to 85-95 ℃, carrying out heat preservation stirring reaction for 2-4 h, cooling to 45-55 ℃ after the reaction is finished, removing a water phase, washing an organic phase with water, and drying the obtained solid product to obtain the catalyst.
5. The durable antifog non-drip polyethylene film masterbatch according to claim 1, wherein the initiator is at least one of azobisisobutyronitrile, azobisisoheptonitrile, and dimethyl azobisisobutyrate.
6. The sustained antifogging non-drip polyethylene film masterbatch according to claim 1, wherein the antifogging agent is at least one of polyglycerol fatty acid ester, polyethylene oxide glycerol fatty acid ester, sorbitan fatty acid ester, polyoxyethylene sorbitol fatty acid ester, polyoxyethylene sorbitan monolaurate, and polyoxyethylene sorbitan monopalmitate.
7. The durable anti-fog non-drip polyethylene film masterbatch according to claim 1, wherein the metal oxide is nano aluminum oxide, nano zinc oxide or a combination thereof.
8. A preparation method of the durable antifogging non-dripping polyethylene film master batch as claimed in any one of claims 1 to 7, characterized by comprising the following steps:
s1, uniformly mixing linear low-density polyethylene, low-density polyethylene and ethylene-vinyl acetate copolymer at a high speed to obtain a mixture A;
s2, uniformly mixing the mixture A with an antifogging agent, a non-dropping agent and a metal oxide at a high speed to obtain a mixture B;
and S3, adding the mixture B into a double-screw extruder for reaction, and then extruding, cooling and granulating to obtain the lasting anti-fog non-drip film master batch.
9. The preparation method of the durable antifogging non-dripping polyethylene film master batch according to claim 8, wherein in S1 and S2, the time of high-speed mixing is 3-5 min.
10. The preparation method of the durable antifogging non-dripping polyethylene film master batch according to claim 8, wherein in S3, the reaction temperature is 170-220 ℃ and the reaction time is 3-5 min.
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CN103571024A (en) * 2012-07-19 2014-02-12 中国石油天然气股份有限公司 Long-acting polyolefin anti-fogging film master batch
CN103571022A (en) * 2012-07-19 2014-02-12 中国石油天然气股份有限公司 Polyethylene anti-fogging film master batch
CN104774360A (en) * 2014-12-28 2015-07-15 北京华腾新材料股份有限公司 New long-effect dripping agricultural polyolefin shed film and preparation method thereof
CN111320804A (en) * 2020-03-24 2020-06-23 张露 Aluminum oxide multifunctional greenhouse film master batch and preparation method and application thereof

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