CN104530546A - Special anti-reflection reinforced master batch for agricultural greenhouse film and preparation method of anti-reflection reinforced master batch - Google Patents

Special anti-reflection reinforced master batch for agricultural greenhouse film and preparation method of anti-reflection reinforced master batch Download PDF

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Publication number
CN104530546A
CN104530546A CN201410810792.9A CN201410810792A CN104530546A CN 104530546 A CN104530546 A CN 104530546A CN 201410810792 A CN201410810792 A CN 201410810792A CN 104530546 A CN104530546 A CN 104530546A
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master batch
film
special
silicon
canopy film
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CN104530546B (en
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徐静
米庆华
谭业明
韩宾
张坤
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Shandong Agricultural University
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Shandong Agricultural University
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L23/00Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
    • C08L23/02Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
    • C08L23/04Homopolymers or copolymers of ethene
    • C08L23/08Copolymers of ethene
    • C08L23/0807Copolymers of ethene with unsaturated hydrocarbons only containing more than three carbon atoms
    • C08L23/0815Copolymers of ethene with aliphatic 1-olefins
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00Processes of treating or compounding macromolecular substances
    • C08J3/20Compounding polymers with additives, e.g. colouring
    • C08J3/22Compounding polymers with additives, e.g. colouring using masterbatch techniques
    • C08J3/226Compounding polymers with additives, e.g. colouring using masterbatch techniques using a polymer as a carrier
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/002Physical properties
    • C08K2201/003Additives being defined by their diameter
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/011Nanostructured additives
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/014Additives containing two or more different additives of the same subgroup in C08K
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00Properties
    • C08L2201/10Transparent films; Clear coatings; Transparent materials
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/02Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
    • C08L2205/025Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/03Polymer mixtures characterised by other features containing three or more polymers in a blend
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2207/00Properties characterising the ingredient of the composition
    • C08L2207/06Properties of polyethylene
    • C08L2207/066LDPE (radical process)

Abstract

The invention belongs to the field of materials and particularly relates to a special anti-reflection reinforced master batch for an agricultural greenhouse film and a preparation method of the anti-reflection reinforced master batch. The master batch is prepared from carrier resin as a matrix in combination with selected sub-nanometer and nano-silicon oxide and a dispersant. By the master batch, the haze of the polyethylene film can be significantly reduced, the light transmittance and tensile strength of the film are significantly increased, wherein the haze of the greenhouse film can be ensured to be less than or equal to 11% and the light transmittance is equal to or greater than 90% and the thermal-insulation performance of the greenhouse film can be increased and is higher than that of the existing polyethylene film.

Description

Special anti-reflection enhancing master batch of a kind of agricultural canopy film and preparation method thereof
Technical field
The invention belongs to Material Field, be specifically related to special anti-reflection enhancing master batch of the special master batch of a kind of plastic greenhouse film, particularly a kind of agricultural canopy film and preparation method thereof.
Background technology
First of the output of China's agripast canopy film and the area coverage Jun Ju world, wherein polyethylene green house film is the main plastic sheeting for farm use kind of China, main raw is linear low density polyethylene (LLDPE) and Low Density Polyethylene (LDPE), is generally both blended complex.Canopy film thickness generally between 0.04 ~ 0.12mm, transmittance < 90%, mist degree > 20%.There are some researches show, reduce the mist degree of film, improve transmittance, overwintering cultivation photosynthesis of plant in booth can be promoted, improve crop yield, crop ripen in advance is gone on the market.Therefore, develop in plastic greenhouse film low haze, high transparency agricultural canopy film for the most of crop yield of raising, increase crop economy benefit extremely important.
Mist degree is mainly subject to the characteristic of resin, the content of additive, and the size impact of crystallization in film manufacturing process.Reduce the mist degree of polyethylene film improve transparent in usually adopt the method adding nucleator and transparent agent.Normally used is the mineral-type small molecules such as the organics such as glucitols, organic phosphate, phosphoric acid ester and talcum powder, silicon-dioxide, mica, polynite, and high transparency polymkeric substance.As CN102746563A discloses the preparation method of the transparent canopy film special material of a kind of LLDPE, adopt organic or inorganic nucleator, static inhibitor, Zinic stearas, LLDPE vector resin, the transparent canopy film special material of preparation LLDPE; Effectively can improve properties of transparency, the mechanical property of film; CN102120843A discloses a kind of sub-nano barium sulfate activeness and quietness transparent masterbatches and preparation method thereof, adopt sub-nano-powder and dispersion agent, lubricant, coupling agent, vector resin jointly to prepare while the mechanical property improving film article, the film masterbatch of its transparency can also be improved; ZL200510026428.4 discloses a kind of transparent film masterbatch and preparation method thereof, adopt that inorganic powder is 2000 to 2500 order talcum powder and rare-earth coupling agent, transparent film masterbatch that stearic acid monoglycerides and the complex carrier that is made up of Low Density Polyethylene or linear low density polyethylene and metallocene PE prepare excellent optical performance jointly; CN103627072 A discloses kind polyolefine high transparency film masterbatch prepared by a kind of modified titanium, nucleator, mLLDPE-g-MAA grafts and mLLDPE vector resin.
Mainly add transparent nucleater in the film according to above-mentioned patent discovery low haze film in the market and reduce Film Haze, but organic nucleating agent price is very expensive, and add organic nucleating agent easily produce carbonization phenomenon after forcing machine is heated for a long time, affect the stability of product; And add the compatibility problem that inorganic powder nucleator also exists the nonpolar macromole of polyethylene and small molecules inorganic powder.Visible above-mentioned patented technology and other low haze films of the prior art all also exist certain defect.
Summary of the invention
The present invention is directed to many weak points that above-mentioned prior art exists, provide special anti-reflection enhancing master batch of a kind of agricultural canopy film and preparation method thereof, this master batch take vector resin as matrix, sub-nano silicon, nano silicon and the dispersion agent selected is coordinated to obtain, this master batch can significantly reduce polyethylene green house film mist degree, significantly improve its transmittance and tensile strength, wherein can guarantee mist degree≤11%, transmittance >=90% of canopy film, tensile strength improves nearly 30%, and the heat-insulating property of canopy film can be improved, higher than the level of existing polyethylene green house film.
Contriver finds through research, only have nucleator quantity abundant and with polyethylene, there is good consistency and just can be uniformly dispersed, reach that nucleus is uniformly distributed, spherulite size diminishes, make the properties of transparency of PE film be improved and improve mechanical property simultaneously, under the guidance of above-mentioned thought, contriver obtains following concrete technical scheme and is:
The special anti-reflection enhancing master batch of a kind of agricultural canopy film, is characterized in that: its main ingredient is counted by weight:
Vector resin 70 ~ 90 parts, sub-nano silicon 1 ~ 15 part, nano silicon 1 ~ 5 part, dispersion agent 4-10 part;
Wherein said vector resin is the mixture of LLDPE, mLLDPE, LDPE, and wherein each component proportion is counted by weight: LLDPE55 ~ 70 part, mLLDPE 10 ~ 15 parts, LDPE15 ~ 30 part; Described sub-nano silicon is the in-situ modified silicon-dioxide of organosilazanes coupling agent or the in-situ modified silicon-dioxide of organo silane coupling agent or its mixture, its grain size 25 ~ 100nm;
Described nano silicon is the in-situ modified silicon-dioxide of organosilazanes coupling agent or the in-situ modified silicon-dioxide of organo silane coupling agent or its mixture, its grain size≤25nm;
The amount ratio of described sub-nano silicon/nano silicon is 1 ~ 15/1 ~ 5;
Described dispersion agent be trolamine, hexamethyldisilazane, BD series organic silicon surfactant in one or more;
Described BD series organic silicon surfactant comprises BD-3055 or BD-3071 or BD-3031.
Why adopt above-mentioned compositional selecting, major cause is:
LLDPE, LDPE and mLLDPE that matrix resin is selected are the common used material of canopy film, be applicable to the many single layer of material of polyolefins to extrude and multi-layer co-extruded film, the consistency between above-mentioned resin can be improved, and ensure the good dispersion of silicon-dioxide in canopy film and functional, select above-mentioned matrix resin raw material to be easy to get and cost is lower.
The present invention selects organosilazanes coupling agent is in-situ modified or organo silane coupling agent is in-situ modified Subnano-class, nanometer grade silica as nucleator simultaneously, its major cause has: 1. organic azane silicone couplet or the in-situ modified silicon-dioxide of organo silane coupling agent, properties-correcting agent with the form of chemical bond and silicon-dioxide key and, in conjunction with firm, can not come off along with intensification and shearing in following process process, lasting to the dispersion effect of silicon-dioxide; 2. the improved silica of two kinds of yardsticks is selected, and carry out composite under aforementioned proportion, can make it in film resin, play synergy, cross-linked structure is presented in film resin, dispersion effect and nucleating effect reach best, improve the melt strength of resin to the full extent, especially improve the melt strength of LLDPE, film subtract thick, anti-reflection while increase its mechanical property; 3. the Si-O key in silicon-dioxide is at 700 ~ 1100cm -1scope has strong absorption, effectively can improve the heat-insulating property of canopy film.
Nanometer and sub-nano silicon are owing to there being larger specific surface area, and therefore hydroxyl is easily rich in surface, even if adopt the silicon-dioxide of organic modification, still have part of hydroxyl and remain.And preferably above-mentioned dispersion agent, the polar group hydroxyl reaction that nanometer and sub-nano-silica surface remain can be fallen in the course of processing, silicon-dioxide is made more easily to be adsorbed in nonpolar macromolecular chain surface, improve its consistency with polymer organic phase further, reduce molecular surface energy, to reduce between particle agglomeration mutually, thus enable silicon dioxide granule evenly, be stably dispersed in polymeric matrix, finally realize toughen and intensify to polymkeric substance and anti-reflection effect.
In addition, present invention also offers the preparation method of above-mentioned master batch, concrete steps are as follows:
First each component is prepared burden in proportion, mix with after adopt twin screw extruder to carry out melt blending granulation again, screw rod each district temperature is 170 ~ 200 DEG C, and screw speed is 80 ~ 300r/min, is drying to obtain the special anti-reflection enhancing master batch of canopy film;
Wherein said being mixed into mixes 15 ~ 30min in high-speed mixer, and rotating speed is 600 ~ 650r/min, or in Banbury mixer mixing 20 ~ 40min, banburying temperature is 130 ~ 200 DEG C.
Adopt above-mentioned preparation method, first mixed by the materials such as vector resin, make the interaction of various storeroom more tight, the final master batch performance obtained is better.
In sum, after adopting this technical scheme provided by the present invention, particle diameter is little, mutually work in coordination with in film resin the little organically-modified sub-nanometer of light scatter, nano silicon, increase nucleus quantity and reduce grain-size, increase the consistency with vector resin, enhanced film resin melt strength, reduces Film Haze, can improve mechanical property while enhancing the transparency.The present invention simultaneously does not add transparent organic nucleating agent, and product stability is good.
Embodiment
Further illustrate the present invention below in conjunction with embodiment, those skilled in the art can be made more fully to understand the present invention, but do not limit the present invention in any way.
Embodiment 1
The special anti-reflection enhancing master batch of a kind of agricultural canopy film, its component is composed as follows by weight:
LLDPE 55 parts;
MLLDPE 9 parts;
LDPE 16 parts;
Sub-nano silicon 14 parts;
Nano silicon 2 parts;
Trolamine 1.5 parts;
BD-3055 2.5 parts;
Preparation technology: each component is prepared burden in proportion, then be mix 15 minutes in the high-speed mixer of 600r/min at rotating speed, twin screw extruder is adopted to carry out melt blending, temperature controls at 170 ~ 200 DEG C, screw speed is 80 ~ 300r/min, by the shearing of screw rod or rotor, mixing, silicon-dioxide is uniformly dispersed in vector resin, then carries out granulation, dry obtained master batch.
Embodiment 2
The special anti-reflection enhancing master batch of a kind of agricultural canopy film, its component is composed as follows by weight:
LLDPE 57 parts;
MLLDPE 12 parts;
LDPE 23 parts;
Sub-nano silicon 13 parts;
Nano silicon 1.5 parts;
Trolamine 1 part;
Hexamethyldisilazane 1.5 parts;
BD-3031 2 parts;
Preparation technology: above component in Banbury mixer mixing 30 minutes, temperature 130-200 DEG C, adopts twin screw extruder extruding pelletization after discharging again, and screw rod each district temperature controls at 170-200 DEG C, screw speed is 80-300r/min, finally carries out being drying to obtain the special master batch of canopy film.
Embodiment 3
The special anti-reflection enhancing master batch of a kind of agricultural canopy film, its component is composed as follows by weight:
LLDPE 60 parts;
LDPE 20 parts;
MLLDPE 10 parts;
Sub-nano silicon 6 parts;
Nano silicon 1 part;
Hexamethyldisilazane 3 parts;
BD-3071 2 parts
Preparation technology: each component is prepared burden in proportion, then be mix 20 minutes in the high-speed mixer of 610r/min at rotating speed, twin screw extruder is adopted to carry out melt blending, temperature controls at 170-200 DEG C, screw speed is 80-300r/min, by the shearing of screw rod or rotor, mixing, silicon-dioxide is uniformly dispersed in vector resin, then carries out granulation, the dry obtained special master batch of canopy film.
Experimental example
The special anti-reflection enhancing master batch of agricultural canopy film prepared by embodiment 1,2 and 3 is applied in the production process of polyethylene green house film, weight in wherein said polyethylene green house film hundred parts of ratios are LLDPE60%, LDPE21%, mLLDPE10%, commercially available nothing drips master batch 6%, and 3% of surplus is master batch involved in the present invention;
The special master batch of canopy film of the present invention and other above-mentioned constituent materialss are placed in high-speed mixer to stir 15 minutes, after Homogeneous phase mixing, pass through double-screw extruding pelletizing, compound is placed in the hopper extruding inflation film manufacturing machine, extrusion-blown modling is tubular film (film thickness is 0.08mm) uniformly, through cutting, point rolling into film, being labeled as respectively: implement canopy film 1, implement canopy film 2, implement canopy film 3.Do not add the special master batch of canopy film of the present invention, the film adopting other commercially available master batches to make, is labeled as: comparative example.Test result is in table 1:
Example Mist degree, % Transmittance, % Tensile strength, Mpa Elongation at break, %
Comparative example 21.5 88.1 21.3 500
Implement canopy film 1 10.1 93.4 27.4 568
Implement canopy film 2 9.88 93.9 28.2 579
Implement canopy film 3 9.73 93.8 27.9 571
Visible this master batch can significantly reduce polyethylene green house film mist degree, significantly improve its transmittance and tensile strength, wherein can guarantee mist degree≤11%, transmittance >=90% of canopy film, tensile strength improves nearly 30%, and can improve the heat-insulating property of canopy film, higher than the level of existing polyethylene green house film.

Claims (4)

1. the special anti-reflection enhancing master batch of agricultural canopy film, is characterized in that: its main ingredient is counted by weight:
Vector resin 70 ~ 90 parts, sub-nano silicon 1 ~ 15 part, nano silicon 1 ~ 5 part, dispersion agent 4 ~ 10 parts;
Wherein said vector resin is the mixture of LLDPE, mLLDPE, LDPE, and wherein each component proportion is counted by weight: LLDPE55 ~ 70 part, mLLDPE 10 ~ 15 parts, LDPE15 ~ 30 part;
Described sub-nano silicon is the in-situ modified silicon-dioxide of organosilazanes coupling agent or the in-situ modified silicon-dioxide of organo silane coupling agent or its mixture, its grain size 25 ~ 100nm;
Described nano silicon is the in-situ modified silicon-dioxide of organosilazanes coupling agent or the in-situ modified silicon-dioxide of organo silane coupling agent or its mixture, its grain size≤25nm;
The amount ratio of described sub-nano silicon/nano silicon is 1 ~ 15/1 ~ 5.
2. the special anti-reflection enhancing master batch of agricultural canopy film according to claim 1, is characterized in that:
Described dispersion agent be trolamine, hexamethyldisilazane, BD series organic silicon surfactant in one or more.
3. the special anti-reflection enhancing master batch of agricultural canopy film according to claim 2, is characterized in that:
Described BD series organic silicon surfactant comprises BD-3055 or BD-3071 or BD-3031.
4. the preparation method of the special anti-reflection enhancing master batch of agricultural canopy film described in claim 1, its concrete steps are as follows:
First each component is prepared burden in proportion, mix with after adopt twin screw extruder to carry out melt blending granulation again, screw rod each district temperature is 170 ~ 200 DEG C, and screw speed is 80 ~ 300r/min, is drying to obtain the special anti-reflection enhancing master batch of canopy film;
Wherein said being mixed into mixes 15 ~ 30min in high-speed mixer, and rotating speed is 600 ~ 650r/min, or in Banbury mixer mixing 20 ~ 40min, banburying temperature is 130 ~ 200 DEG C.
CN201410810792.9A 2014-12-22 2014-12-22 Special anti-reflection reinforced master batch for agricultural greenhouse film and preparation method of anti-reflection reinforced master batch Active CN104530546B (en)

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Cited By (6)

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CN107383575A (en) * 2017-07-13 2017-11-24 山东农业大学 A kind of special chilli oil master batch of agricultural mulching
CN109679121A (en) * 2018-11-29 2019-04-26 柳州市海达新型材料科技有限公司 High-content inorganic particle modified filler masterbatch
CN110256755A (en) * 2019-07-16 2019-09-20 北京水木九天科技有限公司 A kind of greenhouse coloured film based on plant growth characteristics
CN111218053A (en) * 2020-02-25 2020-06-02 南京勇聚新材料科技有限公司 High-transparency antifogging master batch and preparation method thereof
CN111378221A (en) * 2020-01-07 2020-07-07 江苏精良高分子材料有限公司 Stiffness-increasing master batch for improving barrier property of LLDPE (Linear Low Density polyethylene) film and preparation method thereof
CN112048208A (en) * 2020-09-16 2020-12-08 张兴富 Fireproof insulating coating and preparation method thereof

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107383575A (en) * 2017-07-13 2017-11-24 山东农业大学 A kind of special chilli oil master batch of agricultural mulching
CN109679121A (en) * 2018-11-29 2019-04-26 柳州市海达新型材料科技有限公司 High-content inorganic particle modified filler masterbatch
CN110256755A (en) * 2019-07-16 2019-09-20 北京水木九天科技有限公司 A kind of greenhouse coloured film based on plant growth characteristics
CN111378221A (en) * 2020-01-07 2020-07-07 江苏精良高分子材料有限公司 Stiffness-increasing master batch for improving barrier property of LLDPE (Linear Low Density polyethylene) film and preparation method thereof
CN111218053A (en) * 2020-02-25 2020-06-02 南京勇聚新材料科技有限公司 High-transparency antifogging master batch and preparation method thereof
CN112048208A (en) * 2020-09-16 2020-12-08 张兴富 Fireproof insulating coating and preparation method thereof

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