CN113563661B - Long-acting weather-resistant master batch for agricultural film, and preparation method and application thereof - Google Patents

Long-acting weather-resistant master batch for agricultural film, and preparation method and application thereof Download PDF

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CN113563661B
CN113563661B CN202010776681.6A CN202010776681A CN113563661B CN 113563661 B CN113563661 B CN 113563661B CN 202010776681 A CN202010776681 A CN 202010776681A CN 113563661 B CN113563661 B CN 113563661B
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master batch
parts
agricultural
light stabilizer
agricultural film
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CN113563661A (en
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陆涛
刘旭
谢胜利
张周裔乐
张跃
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Suqian Unitechem Co ltd
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    • C08J3/00—Processes of treating or compounding macromolecular substances
    • C08J3/20—Compounding polymers with additives, e.g. colouring
    • C08J3/22—Compounding polymers with additives, e.g. colouring using masterbatch techniques
    • C08J3/226—Compounding polymers with additives, e.g. colouring using masterbatch techniques using a polymer as a carrier
    • 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
    • C08J2423/08—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
    • C08J2483/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
    • C08J2483/04—Polysiloxanes
    • 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
    • C08K5/0008—Organic ingredients according to more than one of the "one dot" groups of C08K5/01 - C08K5/59
    • C08K5/005—Stabilisers against oxidation, heat, light, ozone
    • 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
    • C08K5/13—Phenols; Phenolates
    • C08K5/132—Phenols containing keto groups, e.g. benzophenones
    • 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
    • C08K5/13—Phenols; Phenolates
    • C08K5/134—Phenols containing ester groups
    • 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
    • C08K5/16—Nitrogen-containing compounds
    • C08K5/34—Heterocyclic compounds having nitrogen in the ring
    • C08K5/3467—Heterocyclic compounds having nitrogen in the ring having more than two nitrogen atoms in the ring
    • C08K5/3477—Six-membered rings
    • C08K5/3492—Triazines
    • 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
    • C08K5/49—Phosphorus-containing compounds
    • C08K5/51—Phosphorus bound to oxygen
    • C08K5/52—Phosphorus bound to oxygen only
    • C08K5/524—Esters of phosphorous acids, e.g. of H3PO3
    • C08K5/526—Esters of phosphorous acids, e.g. of H3PO3 with hydroxyaryl compounds
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
    • Y02A40/00—Adaptation technologies in agriculture, forestry, livestock or agroalimentary production
    • Y02A40/10—Adaptation technologies in agriculture, forestry, livestock or agroalimentary production in agriculture
    • Y02A40/25—Greenhouse technology, e.g. cooling systems therefor

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  • Chemical Kinetics & Catalysis (AREA)
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  • Processes Of Treating Macromolecular Substances (AREA)
  • Manufacture Of Macromolecular Shaped Articles (AREA)

Abstract

The invention discloses a long-acting weather-proof master batch for agricultural films, which comprises the following raw materials in parts by weight: 40-70 parts of polyethylene resin; 5-20 parts of light stabilizer; 5-30 parts of polyorganosiloxane. After the master batch provided by the invention is added to an agricultural film product, the opposite impact effect of acid pesticides and hindered amine light stabilizer can be greatly reduced, and the protection of the hindered amine light stabilizer on the photo-oxidative aging of the agricultural film resin is ensured, so that the service life of the agricultural film product can be greatly prolonged. The invention also discloses a preparation method and application of the master batch.

Description

Long-acting weather-resistant master batch for agricultural film, and preparation method and application thereof
Technical Field
The invention relates to the technical field of polymer processing modification. More particularly relates to a long-acting weather-proof master batch for agricultural films, a preparation method and application thereof.
Background
At the beginning of the 50 s of the 20 th century, agricultural film covering technology has emerged and is rapidly spreading in japan, europe, america, etc. The technology has the functions of preserving soil moisture, increasing temperature, saving water, inhibiting weeds and the like, and the application of the technology brings about the multiple increase of agricultural yield and benefit, and realizes the leap of agricultural productivity and the change of production modes, so that under the current social population form, agricultural films become an essential agricultural material for advanced agriculture.
With the expansion of the covering area of the agricultural film, the abandoned agricultural film fragments enter the farmland soil to influence the permeability of the soil, prevent crops from absorbing moisture and root growth, gradually deteriorate the farmland quality and seriously destroy the agricultural ecological environment. Various countries gradually recognize that economic benefits brought by agricultural film use cannot be pursued only, and the environmental impact brought by the economic benefits cannot be ignored. Only developing long-life agricultural film, greatly reducing the production of agricultural film, solving the recovery problem of good agricultural film, and eliminating the pollution of waste film to soil is the correct way for sustainable development of agriculture. China has become the country of the first dosage of agricultural film at present, face the severe "white pollution" pressure, agricultural film decrement and recycle have been unprecedented.
At present, agricultural films in China mainly comprise LDPE, LLDPE and EVA resins, and the LLDPE resins have fewer branching points in the molecular structure and better weather resistance, but when the LLDPE resins are exposed to sunlight, impurities or chromophores such as carbonyl groups in the system absorb high-energy ultraviolet light, so that a large number of free radicals are generated in the resin structure. Under the action of oxygen, a large number of carbonyl, hydroxyl and olefin structures can be formed, so that the agricultural film is discolored, the light transmittance is reduced, and even the phenomenon of shed breaking is caused. This phenomenon of aging of the optical and mechanical properties of the resin caused by ultraviolet light is called photo-oxidative aging. The most direct mode of delaying the photo-oxidative aging of the high polymer material is to add light stabilization, wherein the hindered amine light stabilizer is 2-4 times of the traditional light stabilizer in protection effect, and is the most studied and most developed variety in various light stabilizers. In recent years, the use of the HALS 622 and the B225 or the B215 and the use of the HALS 944 and the B900 together are used for producing ageing-resistant PE and EVA greenhouse films, and the development of long-life agricultural films is better promoted.
Although the hindered amine light stabilizer HALS can endow the resin with high-efficiency photo-oxidative aging resistance, the resin is strong in alkalinity and easy to react with acidic substances to generate inorganic salts, so that the problem of failure occurs. The use of large amounts of pesticides and sulphur is an essential part of the agricultural field, for example: iron ions, sulfur and activated halogens (derivatives of chlorine, bromine, etc.) and sulfur powder in the pesticide. In the background of the annual increase of pesticide amount, the development of the longevity greenhouse film is greatly limited.
Disclosure of Invention
The invention aims to provide a long-acting weather-proof master batch for agricultural films, which can greatly reduce the opposite impact of acid pesticides and hindered amine light stabilizers after being added into agricultural film products, and ensure the protection of the hindered amine light stabilizers on the photo-oxidative aging of the agricultural film resins, so that the service life of the agricultural film products can be greatly prolonged.
The second aim of the invention is to provide a preparation method of a long-acting weather-proof master batch for agricultural films.
The third purpose of the invention is to provide the application of the long-acting weather-proof master batch for the agricultural film.
In order to achieve the first object, the present invention adopts the following technical scheme:
the long-acting weather-proof master batch for the agricultural film comprises the following raw materials in parts by weight:
40-70 parts of polyethylene resin;
5-20 parts of light stabilizer;
5-30 parts of polyorganosiloxane.
Further, the light stabilizer comprises a mixture of a hindered amine light stabilizer and an ultraviolet absorber, wherein the mass ratio of the hindered amine light stabilizer to the ultraviolet absorber is 3:1-5:1.
Further, the hindered amine light stabilizer is one or more selected from the group consisting of HALS 119, HALS 622 and HALS 371. Exemplary amounts of hindered amine light stabilizer added include, but are not limited to, 5-10 parts, 8-10 parts, etc.
Further, the ultraviolet absorber is one or more selected from UV 531, UV 326 and UV 328.
The compounding of the proper hindered amine light stabilizer and the ultraviolet absorber can greatly increase the protection of the agricultural film resin against photo-oxidative aging.
Further, the polyorganosiloxane has a structural formula (R 2 SiO) n Wherein R is an alkyl group having 1 to 20 carbon atoms, and the polyorganosiloxane has a number average molecular weight of 3000 to 80000.
Further, the polyethylene resin is a linear low density polyethylene resin, and the melt flow rate is 0.5-3 g/10min. Illustratively, the polyethylene resin is added in an amount including, but not limited to, 50-70 parts, 60-70 parts, etc.
Further, the raw materials also comprise 2-8 parts of antioxidant; preferably, the antioxidant is selected from one or more of AO 1010, AO1076, AO 168 and AO 626.
Further, the master batch comprises the following raw materials in parts by weight, wherein the total mass is 100 parts:
Figure BDA0002618688220000021
in order to achieve the second object, the present invention adopts the following technical scheme:
a preparation method of master batch for long-acting weather-resistant agricultural films comprises the following steps:
uniformly mixing the polyorganosiloxane, the polyethylene resin, the light stabilizer and the antioxidant to obtain a mixture;
extruding and granulating the mixture by a double-screw extruder to obtain the master batch.
Further, the twin screw extruder has an aspect ratio of 30: 1-40: 1.
further, in the extrusion granulation process, the temperatures of each section of the twin-screw extruder are set as follows: the conveying section is 100-150 ℃, the melting section is 160-190 ℃, the metering section is 190-220 ℃, and the tail end of the double-screw extruder is vacuumized and exhausted.
The double screw extruder is selected to extrude and granulate, and the parameters of extrusion and granulation are controlled, so that the dispersibility of the auxiliary agent in the agricultural film product is more facilitated, and the long-term photooxidation stability of the agricultural film is improved.
In order to achieve the third purpose, the invention provides application of the master batch for the long-acting weather-resistant agricultural film in the production of the agricultural film.
Further, the base resin material of the agricultural film is LLDPE, EVA, or a mixture of LLDPE and EVA.
Further, the addition amount of the master batch is 5 to 7 weight percent of the matrix resin.
The beneficial effects of the invention are as follows:
the master batch for the long-acting weather-proof agricultural film provided by the invention selects the specific hindered amine light stabilizer with large molecular weight, can stably exist in an agricultural film (for example, LLDPE) film for a long time, is migration-resistant and precipitation-resistant, and ensures that the hindered amine light stabilizer can provide a foundation for long-term protection of the agricultural film; the polyorganosiloxane can gradually permeate to the resin surface in the processing process to form a hydrophobic and oleophobic isolation layer, so that the permeation of acidic pesticide to the pesticide film resin (such as LLDPE resin) can be greatly reduced. The specific hindered amine in the invention reduces the direct reaction of the hindered amine with the acid pesticide, and the specific hindered amine and the acid pesticide greatly reduce the opposite impact of the pesticide on the HALS. The antioxidant can provide thermal processing protection for agricultural film resins (such as LLDPE resins), so that the whole formula system can provide omnibearing and durable photo-oxidative aging protection for agricultural film products.
Detailed Description
In order to more clearly illustrate the present invention, the present invention will be further described with reference to preferred embodiments. It is to be understood by persons skilled in the art that the following detailed description is illustrative and not restrictive, and that this invention is not limited to the details given herein.
Example 1
A preparation method of a long-acting weather-resistant special material for agricultural films and application of the long-acting weather-resistant special material in LLDPE casting films comprises the following steps:
the resin carrier and adjuvant were weighed according to the formulation shown in Table 1, wherein the LLDPE resin had a melt flow rate of 0.8g/10min and the test conditions were 190℃and 2.16kg; wherein one end of the alkyl side chain of the used polyorganosiloxane is methyl, the other alkyl side chain is n-dodecane, and the number average molecular weight is 1 ten thousand.
The raw materials of each component are placed into a mixer for 7min, and are put into a double-screw extrusion granulator for granulation, wherein the process temperature of each section is one zone of 100 ℃, two zones of 130 ℃, three zones of 170 ℃, four zones of 180 ℃, five zones of 200 ℃, six zones of 200 ℃ and the temperature of a machine head of 190 ℃.
The master batch prepared by the method is added into LLDPE matrix according to the mass fraction of 6%, the master batch is uniformly mixed by a mixer, and is cast into a film with the thickness of 80um by a casting machine, wherein the temperature of each section of the casting machine is 130 ℃ in a first region, 155 ℃ in a second region and 165 ℃ in a third region.
Example 2
Example 1 was repeated, except that the raw material formulation was different from example 1, specifically as shown in table 1.
Example 3
Example 1 was repeated, except that the raw material formulation was different from example 1, specifically as shown in table 1.
Example 4
Example 1 was repeated, except that the raw material formulation was different from example 1, specifically as shown in table 1.
Example 5
Example 1 was repeated, except that the prepared master batch was added to the LLDPE matrix in a proportion of 5% by mass, the remaining conditions being unchanged.
Example 6
Example 2 was repeated, except that the masterbatch prepared was added to the LLDPE matrix in a proportion of 7% by mass, the remaining conditions being unchanged.
Comparative examples 1 to 5
Example 1 was repeated, except that the raw material formulation was different from example 1, specifically as shown in table 1.
Table 1 formulation for each example and comparative example
Figure BDA0002618688220000031
Figure BDA0002618688220000041
Test process:
cutting film samples of each example and comparative example (with length and width of 8cm and 5cm respectively), putting the film samples into a beaker, adding a prepared sulfurous acid aqueous solution (the sulfurous acid analytical pure reagent and pure water are prepared according to the volume ratio of 1:6), immersing the solution into the film, sealing a beaker mouth by using a winding film, immersing for 10 days, taking out the samples, repeatedly flushing the samples with pure water for 5 times, and performing aging test for later use; the film samples were subjected to contact angle testing of the aqueous phase prior to immersion.
In UV 340 (irradiation intensity: 0.76W/m) 2 ) The aging test standard is ASTM G154-12, the tensile strength before and after aging is tested, the elongation at break is tested, and the tensile property test standard is GB/T1040.3-2006. The results are shown in Table 2 below.
Table 2 performance test data for each of the examples and comparative examples
Figure BDA0002618688220000042
It should be understood that the foregoing examples of the present invention are provided merely for clearly illustrating the present invention and are not intended to limit the embodiments of the present invention, and that various other changes and modifications may be made therein by one skilled in the art without departing from the spirit and scope of the present invention as defined by the appended claims.

Claims (13)

1. The long-acting weather-proof master batch for the agricultural film is characterized by comprising the following raw materials in parts by weight:
40-70 parts of polyethylene resin;
5-20 parts of light stabilizer;
5-30 parts of polyorganosiloxane;
the light stabilizer comprises a mixture of a hindered amine light stabilizer and an ultraviolet absorber, wherein the mass ratio of the hindered amine light stabilizer to the ultraviolet absorber is 3:1-5:1;
the hindered amine light stabilizer is one or more selected from HALS 119, HALS 622 and HALS 371.
2. The master batch for agricultural films according to claim 1, wherein the ultraviolet absorber is one or more selected from UV 531, UV 326 and UV 328.
3. The master batch for agricultural films according to claim 1, wherein the raw materials further comprise 2-8 parts of an antioxidant.
4. The master batch for agricultural films according to claim 3, wherein the antioxidant is one or more selected from AO 1010, AO1076, AO 168 and AO 626.
5. The master batch for agricultural films according to claim 1, wherein the polyorganosiloxane has a structural formula (R 2 SiO) n, wherein R is an alkyl group having 1 to 20 carbon atoms, and the polyorganosiloxane has a number average molecular weight of 3000 to 80000.
6. The master batch for agricultural films according to claim 5, wherein the polyethylene resin is a linear low density polyethylene resin having a melt flow rate of 0.5 to 3g/10min.
7. The master batch for agricultural films according to claim 1, wherein the master batch comprises the following raw materials in parts by mass, based on 100 parts by mass:
Figure FDA0004073423370000011
8. the method for preparing the master batch for the long-acting weather-resistant agricultural film according to any one of claims 1 to 7, which is characterized by comprising the following steps:
uniformly mixing the polyorganosiloxane, the polyethylene resin, the light stabilizer and the antioxidant to obtain a mixture;
extruding and granulating the mixture by a double-screw extruder to obtain the master batch.
9. The method of claim 8, wherein the twin screw extruder has an aspect ratio of 30: 1-40: 1.
10. the method according to claim 8, wherein during extrusion granulation, the temperatures of the sections of the twin-screw extruder are set as follows: the conveying section is 100-150 ℃, the melting section is 160-190 ℃, the metering section is 190-220 ℃, and the tail end of the double-screw extruder is vacuumized and exhausted.
11. Use of the master batch for long-acting weather-resistant agricultural films according to any one of claims 1 to 7 in the production of agricultural films.
12. The use according to claim 11, wherein the base resin material of the agricultural film is LLDPE, EVA or a mixture of LLDPE and EVA.
13. The use according to claim 12, wherein the masterbatch is added in an amount of 5-7 wt% of the matrix resin.
CN202010776681.6A 2020-04-28 2020-08-05 Long-acting weather-resistant master batch for agricultural film, and preparation method and application thereof Active CN113563661B (en)

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Citations (5)

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Publication number Priority date Publication date Assignee Title
CN102924797A (en) * 2011-08-10 2013-02-13 中国石油天然气股份有限公司 Weather-resistant polyethylene agricultural film resin composition and preparation method thereof
CN104910500A (en) * 2015-07-06 2015-09-16 蓝星（成都）新材料有限公司 Polyethylene pearlescent coloring master batch and preparation method thereof
WO2018129115A1 (en) * 2017-01-04 2018-07-12 Great Lakes Polymers Holdings Corporation Dba Great Lakes Polymer Technologies Polyorganosiloxane and polyolefin blend composition in drawn polymer products
CN109422944A (en) * 2017-08-31 2019-03-05 比亚迪股份有限公司 Polyolefin composition and polyolefin master batch and polyolefin film and incrustation composite material and preparation method
CN109679186A (en) * 2018-12-21 2019-04-26 上海高分子功能材料研究所 A kind of polyethylene master batch containing compounding light stabilizer and compound antioxidant

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102924797A (en) * 2011-08-10 2013-02-13 中国石油天然气股份有限公司 Weather-resistant polyethylene agricultural film resin composition and preparation method thereof
CN104910500A (en) * 2015-07-06 2015-09-16 蓝星（成都）新材料有限公司 Polyethylene pearlescent coloring master batch and preparation method thereof
WO2018129115A1 (en) * 2017-01-04 2018-07-12 Great Lakes Polymers Holdings Corporation Dba Great Lakes Polymer Technologies Polyorganosiloxane and polyolefin blend composition in drawn polymer products
CN109422944A (en) * 2017-08-31 2019-03-05 比亚迪股份有限公司 Polyolefin composition and polyolefin master batch and polyolefin film and incrustation composite material and preparation method
CN109679186A (en) * 2018-12-21 2019-04-26 上海高分子功能材料研究所 A kind of polyethylene master batch containing compounding light stabilizer and compound antioxidant

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