CN107298948A - A kind of SGP films of high stability and preparation method thereof - Google Patents

A kind of SGP films of high stability and preparation method thereof Download PDF

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Publication number
CN107298948A
CN107298948A CN201710675231.6A CN201710675231A CN107298948A CN 107298948 A CN107298948 A CN 107298948A CN 201710675231 A CN201710675231 A CN 201710675231A CN 107298948 A CN107298948 A CN 107298948A
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parts
high stability
sgp films
dispersant
hydrogen peroxide
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王超
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Shandong Fangding Safety Glass Tech Co Ltd
Shandong Fangding Safety Glass Technology Co Ltd
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Shandong Fangding Safety Glass Tech Co Ltd
Shandong Fangding Safety Glass Technology Co Ltd
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Priority to CN201710675231.6A priority Critical patent/CN107298948A/en
Publication of CN107298948A publication Critical patent/CN107298948A/en
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J7/00Adhesives in the form of films or foils
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02Non-macromolecular additives
    • C09J11/06Non-macromolecular additives organic
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J123/00Adhesives based on homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Adhesives based on derivatives of such polymers
    • C09J123/02Adhesives based on homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Adhesives based on derivatives of such polymers not modified by chemical after-treatment
    • C09J123/04Homopolymers or copolymers of ethene
    • C09J123/08Copolymers of ethene
    • C09J123/0846Copolymers of ethene with unsaturated hydrocarbons containing other atoms than carbon or hydrogen atoms
    • C09J123/0869Acids or derivatives thereof
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00Properties
    • C08L2201/08Stabilised against heat, light or radiation or oxydation
    • 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
    • C08L2205/03Polymer mixtures characterised by other features containing three or more polymers in a blend
    • C08L2205/035Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Manufacture Of Macromolecular Shaped Articles (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

The invention discloses SGP films of a kind of high stability and preparation method thereof, the SGP films include according to the raw material of parts by weight:60 120 parts of ethylene methyl acrylate copolymer, 3 30 parts of cellulose, 5 30 parts of rosin, 10 45 parts of plasticizer, 3 25 parts of paraffin, 0.1 5 parts of silane coupler, 15 40 parts of ethylene glycol, 0.01 5 parts of ultra-violet absorber, 0.1 5 parts of hydrogen peroxide decomposition agent, 0.01 5 parts of dispersant, 0.05 5 parts of antioxidant.Each raw material is mixed evenly, then produced through casting machine extrusion casting film-forming piece.The present invention is using SGP films made from above-mentioned raw materials and preparation technology, and properties of product are stable and material is uniformly dispersed, and anti-uv-ray, infrared resistant ability are good, and intensity is high, and can keep good transparency and definition.The raw material that the present invention is used is easy to get, preparation technology disposal molding, and technique is simple, is easily controlled, suitable for industrialized production.

Description

A kind of SGP films of high stability and preparation method thereof
Technical field
The present invention relates to laminated glass field of material technology, the SGP films of specifically a kind of high stability and its preparation side Method.
Background technology
Laminated glass be by two panels or divided glass, between pressed from both sides one or more layers organic polymer intermediate coat, by spy Different high temperature precompressed(Or vacuumize)And after high-temperature high-pressure craft processing, make that glass and intermediate coat permanent adhesive be integrated is compound Glass product.Even if glass fragmentation, fragment can be also bonded on film, broken glass surface still keeps clean and tidy smooth.This is just It effectively prevent the generation that fall event was stabbed and penetrated to fragment, it is ensured that personal safety.Most of building glass is all using folder Layer glass, this is not only to avoided injury accident, also as laminated glass has fabulous antidetonation invasive ability.Intermediate coat can be resisted The continuous attack of the lethal weapons such as hammer, firewood knife, moreover it is possible to resist bullet within the long duration and penetrate, its safety precaution degree is It is high.Wherein conventional laminated glass intermediate coat has:PVB, SGP, EVA, PU etc..But existing intermediate coat cause transparency and Poor definition, it is impossible to meet demand.
The content of the invention
It is an object of the invention to provide SGP films of a kind of high stability and preparation method thereof, to solve above-mentioned background The problem of being proposed in technology.
To achieve the above object, the present invention provides following technical scheme:
A kind of SGP films of high stability, include according to the raw material of parts by weight:Ethylene-methyl acrylate copolymer 60-120 Part, 3-30 parts of cellulose, 5-30 parts of rosin, 10-45 parts of plasticizer, 3-25 parts of paraffin, 0.1-5 parts of silane coupler, ethylene glycol 15-40 parts, 0.01-5 parts of ultra-violet absorber, 0.1-5 parts of hydrogen peroxide decomposition agent, 0.01-5 parts of dispersant, antioxidant 0.05-5 parts.
It is used as further scheme of the invention:Ultra-violet absorber is septichen phenyl ester, 2,4- dihydroxy hexichol One kind in ketone, ESCALOL 567.
It is used as further scheme of the invention:Hydrogen peroxide decomposition agent is one in phosphinate and phosphorodithioate Kind.
It is used as further scheme of the invention:Dispersant is stearmide, glyceryl tristearate, vinyl stearic bicine diester One kind in amine.
It is used as further scheme of the invention:The SGP films of the high stability, include according to the raw material of parts by weight:Second Alkene -65-115 parts of methacrylate copolymer, 4-28 parts of cellulose, 8-28 parts of rosin, 12-42 parts of plasticizer, paraffin 5-22 Part, 0.1-4 parts of silane coupler, 18-35 parts of ethylene glycol, 0.01-4 parts of ultra-violet absorber, hydrogen peroxide decomposition agent 0.1-4 Part, 0.01-4 parts of dispersant, 0.1-4 parts of antioxidant.
It is used as further scheme of the invention:The SGP films of the high stability, include according to the raw material of parts by weight:Second Alkene -70-110 parts of methacrylate copolymer, 5-25 parts of cellulose, 10-25 parts of rosin, 15-40 parts of plasticizer, paraffin 8-20 Part, 0.2-3 parts of silane coupler, 20-35 parts of ethylene glycol, 0.02-3 parts of ultra-violet absorber, hydrogen peroxide decomposition agent 0.2-3 Part, 0.01-3 parts of dispersant, 0.1-3 parts of antioxidant.
A kind of preparation method of the SGP films of high stability, comprises the following steps:
According to parts by weight, ethylene-methyl acrylate copolymer, cellulose, rosin, plasticizer, paraffin, silane are weighed respectively even Join agent, ethylene glycol, ultra-violet absorber, hydrogen peroxide decomposition agent, dispersant, antioxidant, by cellulose, rosin, plasticising Agent, paraffin, silane coupler, ethylene glycol, ultra-violet absorber, hydrogen peroxide decomposition agent, dispersant, antioxidant are added to In ethylene-methyl acrylate copolymer, it is mixed evenly, then casting film-forming piece is extruded through casting machine, produces SGP films.
It is used as further scheme of the invention:Casting machine feeding section temperature is 190-210 DEG C, and melt zone temperature is 180- 220 DEG C, 150-170 DEG C of discharge end temperature.
It is used as further scheme of the invention:The mixing time is 0.5-10h.
It is used as further scheme of the invention:Mixing speed is 100-400r/min.
Compared with prior art, the beneficial effects of the invention are as follows:
The present invention is uniformly dispersed using SGP films made from above-mentioned raw materials and preparation technology, material, properties of product extremely stablize and Intensity is high, and anti-uv-ray, infrared resistant ability are good, and can keep good transparency and definition.What the present invention was used Raw material is easy to get, preparation technology disposal molding, and technique is simple, is easily controlled, suitable for industrialized production.
Embodiment
Below in conjunction with the embodiment of the present invention, the technical scheme in the embodiment of the present invention is clearly and completely described, Obviously, described embodiment is only a part of embodiment of the invention, rather than whole embodiments.Based in the present invention Embodiment, the every other embodiment that those of ordinary skill in the art are obtained under the premise of creative work is not made, all Belong to the scope of protection of the invention.
Embodiment 1
In the embodiment of the present invention, a kind of SGP films of high stability, including following raw material:Ethylene-methyl acrylate copolymer 60kg, cellulose 3kg, rosin 5kg, plasticizer 10kg, paraffin 3kg, silane coupler 0.1kg, ethylene glycol 15kg, ultraviolet are inhaled Receive agent 0.01kg, hydrogen peroxide decomposition agent 0.1kg, dispersant 0.01kg, antioxidant 0.05kg.
Ultra-violet absorber is septichen phenyl ester.Hydrogen peroxide decomposition agent is phosphinate.Dispersant is hard Acyl amine.
The preparation method of the SGP films of the high stability, comprises the following steps:
Ethylene-methyl acrylate copolymer, cellulose, rosin, plasticizer, paraffin, silane are weighed respectively according to above-mentioned weight Coupling agent, ethylene glycol, ultra-violet absorber, hydrogen peroxide decomposition agent, dispersant, antioxidant, by cellulose, rosin, increasing Mould agent, paraffin, silane coupler, ethylene glycol, ultra-violet absorber, hydrogen peroxide decomposition agent, dispersant, antioxidant addition Into ethylene-methyl acrylate copolymer, 0.5h is mixed with 100r/min mixing speed.Again through casting machine extrudate flow Prolong into diaphragm, produce SGP films.Wherein casting machine feeding section temperature is 190 DEG C, and melt zone temperature is 180 DEG C, discharge end temperature 150℃。
Embodiment 2
In the embodiment of the present invention, a kind of SGP films of high stability, including following raw material:Ethylene-methyl acrylate copolymer 120kg, cellulose 30kg, rosin 30kg, plasticizer 45kg, paraffin 25kg, silane coupler 5kg, ethylene glycol 40kg, ultraviolet Absorbent 5kg, hydrogen peroxide decomposition agent 5kg, dispersant 5kg, antioxidant 5kg.
Ultra-violet absorber is 2,4-DihydroxyBenzophenone.Hydrogen peroxide decomposition agent is phosphorodithioate.It is scattered Agent is glyceryl tristearate.
The preparation method of the SGP films of the high stability, comprises the following steps:
Ethylene-methyl acrylate copolymer, cellulose, rosin, plasticizer, paraffin, silane are weighed respectively according to above-mentioned weight Coupling agent, ethylene glycol, ultra-violet absorber, hydrogen peroxide decomposition agent, dispersant, antioxidant, by cellulose, rosin, increasing Mould agent, paraffin, silane coupler, ethylene glycol, ultra-violet absorber, hydrogen peroxide decomposition agent, dispersant, antioxidant addition Into ethylene-methyl acrylate copolymer, 10h is mixed with 400r/min mixing speed.Again through casting machine extrudate flow Prolong into diaphragm, produce SGP films.Wherein casting machine feeding section temperature is 210 DEG C, and melt zone temperature is 220 DEG C, discharge end temperature 170℃。
Embodiment 3
In the embodiment of the present invention, a kind of SGP films of high stability, including following raw material:Ethylene-methyl acrylate copolymer 65kg, cellulose 4kg, rosin 8kg, plasticizer 12kg, paraffin 5kg, silane coupler 0.1kg, ethylene glycol 18kg, ultraviolet are inhaled Receive agent 0.01kg, hydrogen peroxide decomposition agent 0.1kg, dispersant 0.01kg, antioxidant 0.1kg.
Ultra-violet absorber is ESCALOL 567.Hydrogen peroxide decomposition agent is phosphinate.It is scattered Agent is vinyl bis-stearamides.
The preparation method of the SGP films of the high stability, comprises the following steps:
Ethylene-methyl acrylate copolymer, cellulose, rosin, plasticizer, paraffin, silane are weighed respectively according to above-mentioned weight Coupling agent, ethylene glycol, ultra-violet absorber, hydrogen peroxide decomposition agent, dispersant, antioxidant, by cellulose, rosin, increasing Mould agent, paraffin, silane coupler, ethylene glycol, ultra-violet absorber, hydrogen peroxide decomposition agent, dispersant, antioxidant addition Into ethylene-methyl acrylate copolymer, 2h is mixed with 150r/min mixing speed.Extrude and be cast through casting machine again Into diaphragm, SGP films are produced.Wherein casting machine feeding section temperature is 195 DEG C, and melt zone temperature is 190 DEG C, discharge end temperature 155℃。
Embodiment 4
In the embodiment of the present invention, a kind of SGP films of high stability, including following raw material:Ethylene-methyl acrylate copolymer 115kg, cellulose 28kg, rosin 28kg, plasticizer 42kg, paraffin 22kg, silane coupler 4kg, ethylene glycol 35kg, ultraviolet Absorbent 4kg, hydrogen peroxide decomposition agent 4kg, dispersant 4kg, antioxidant 4kg.
Ultra-violet absorber is septichen phenyl ester.Hydrogen peroxide decomposition agent is phosphinate.Dispersant is hard Acyl amine.
The preparation method of the SGP films of the high stability, comprises the following steps:
Ethylene-methyl acrylate copolymer, cellulose, rosin, plasticizer, paraffin, silane are weighed respectively according to above-mentioned weight Coupling agent, ethylene glycol, ultra-violet absorber, hydrogen peroxide decomposition agent, dispersant, antioxidant, by cellulose, rosin, increasing Mould agent, paraffin, silane coupler, ethylene glycol, ultra-violet absorber, hydrogen peroxide decomposition agent, dispersant, antioxidant addition Into ethylene-methyl acrylate copolymer, 8h is mixed with 200r/min mixing speed.Extrude and be cast through casting machine again Into diaphragm, SGP films are produced.Wherein casting machine feeding section temperature is 205 DEG C, and melt zone temperature is 210 DEG C, discharge end temperature 165℃。
Embodiment 5
In the embodiment of the present invention, a kind of SGP films of high stability, including following raw material:Ethylene-methyl acrylate copolymer 70kg, cellulose 5kg, rosin 10kg, plasticizer 15kg, paraffin 8kg, silane coupler 0.2kg, ethylene glycol 20kg, ultraviolet Absorbent 0.02kg, hydrogen peroxide decomposition agent 0.2kg, dispersant 0.01kg, antioxidant 0.1kg.
Ultra-violet absorber is septichen phenyl ester.Hydrogen peroxide decomposition agent is phosphinate.Dispersant is hard Acyl amine.
The preparation method of the SGP films of the high stability, comprises the following steps:
Ethylene-methyl acrylate copolymer, cellulose, rosin, plasticizer, paraffin, silane are weighed respectively according to above-mentioned weight Coupling agent, ethylene glycol, ultra-violet absorber, hydrogen peroxide decomposition agent, dispersant, antioxidant, by cellulose, rosin, increasing Mould agent, paraffin, silane coupler, ethylene glycol, ultra-violet absorber, hydrogen peroxide decomposition agent, dispersant, antioxidant addition Into ethylene-methyl acrylate copolymer, 4h is mixed with 300r/min mixing speed.Extrude and be cast through casting machine again Into diaphragm, SGP films are produced.Wherein casting machine feeding section temperature is 200 DEG C, and melt zone temperature is 200 DEG C, discharge end temperature 160℃。
Embodiment 6
In the embodiment of the present invention, a kind of SGP films of high stability, including following raw material:Ethylene-methyl acrylate copolymer It is 110kg, cellulose 5-25kg, rosin 25kg, plasticizer 40kg, paraffin 20kg, silane coupler 3kg, ethylene glycol 35kg, ultraviolet Light absorbers 3kg, hydrogen peroxide decomposition agent 3kg, dispersant 3kg, antioxidant 3kg.
Ultra-violet absorber is ESCALOL 567.Hydrogen peroxide decomposition agent is phosphorodithioate. Dispersant is glyceryl tristearate.
The preparation method of the SGP films of the high stability, comprises the following steps:
Ethylene-methyl acrylate copolymer, cellulose, rosin, plasticizer, paraffin, silane are weighed respectively according to above-mentioned weight Coupling agent, ethylene glycol, ultra-violet absorber, hydrogen peroxide decomposition agent, dispersant, antioxidant, by cellulose, rosin, increasing Mould agent, paraffin, silane coupler, ethylene glycol, ultra-violet absorber, hydrogen peroxide decomposition agent, dispersant, antioxidant addition Into ethylene-methyl acrylate copolymer, 5h is mixed with 250r/min mixing speed.Extrude and be cast through casting machine again Into diaphragm, SGP films are produced.Wherein casting machine feeding section temperature is 200 DEG C, and melt zone temperature is 205 DEG C, discharge end temperature 160℃。
The performance test of 1-6 products of the embodiment of the present invention is as described below, as a result as shown in table 1-2:
(1)Physical property is evaluated and tested according to ISO system certifications.
(2)Test condition is:Room temperature is 10-25 degrees Celsius, humidity 10-30%.
Table 1
Performance indications Tensile strength/MPa Acid number/(mgKOH/g)
Standard items 60.5 4.0
Embodiment 1 82.3 4.4
Embodiment 2 82.6 4.5
Embodiment 3 83.3 4.6
Embodiment 4 83.6 4.6
Embodiment 5 84.8 4.7
Embodiment 6 85.1 4.7
Table 2
Performance indications Ultraviolet isolating rate/% Infrared ray rejection rate/% Visible light transmissivity/% Shading coefficient
Standard items 56.5 80 80 0.72
Embodiment 1 95.6 81 81 0.71
Embodiment 2 96.4 82 82 0.70
Embodiment 3 99.7 85 84 0.69
Embodiment 4 100 82 84 0.68
Embodiment 5 100 87 86 0.67
Embodiment 6 100 88 85 0.68
From experimental data, embodiment 1-6 properties are superior to standard items.
It is obvious to a person skilled in the art that the invention is not restricted to the details of above-mentioned one exemplary embodiment, Er Qie In the case of without departing substantially from spirit or essential attributes of the invention, the present invention can be realized in other specific forms.Therefore, no matter From the point of view of which point, embodiment all should be regarded as exemplary, and be nonrestrictive, the scope of the present invention is by appended power Profit is required rather than described above is limited, it is intended that all in the implication and scope of the equivalency of claim by falling Change is included in the present invention.
Moreover, it will be appreciated that although the present specification is described in terms of embodiments, not each embodiment is only wrapped Containing an independent technical scheme, this narrating mode of specification is only that for clarity, those skilled in the art should Using specification as an entirety, the technical solutions in the various embodiments may also be suitably combined, forms those skilled in the art It may be appreciated other embodiment.

Claims (10)

1. the SGP films of a kind of high stability, it is characterised in that include according to the raw material of parts by weight:Ethylene-methyl acrylate 60-120 parts of copolymer, 3-30 parts of cellulose, 5-30 parts of rosin, 10-45 parts of plasticizer, 3-25 parts of paraffin, silane coupler 0.1-5 parts, 15-40 parts of ethylene glycol, 0.01-5 parts of ultra-violet absorber, 0.1-5 parts of hydrogen peroxide decomposition agent, dispersant 0.01-5 parts, 0.05-5 parts of antioxidant.
2. the SGP films of high stability according to claim 1, it is characterised in that ultra-violet absorber is o-hydroxy One kind in phenyl formate, 2,4-DihydroxyBenzophenone, ESCALOL 567.
3. the SGP films of high stability according to claim 1, it is characterised in that hydrogen peroxide decomposition agent is sub- phosphine One kind in acid esters and phosphorodithioate.
4. the SGP films of high stability according to claim 1, it is characterised in that dispersant is stearmide, three tristearin One kind in acid glyceride, vinyl bis-stearamides.
5. the SGP films of high stability according to claim 1, it is characterised in that include according to the raw material of parts by weight:Second Alkene -65-115 parts of methacrylate copolymer, 4-28 parts of cellulose, 8-28 parts of rosin, 12-42 parts of plasticizer, paraffin 5-22 Part, 0.1-4 parts of silane coupler, 18-35 parts of ethylene glycol, 0.01-4 parts of ultra-violet absorber, hydrogen peroxide decomposition agent 0.1-4 Part, 0.01-4 parts of dispersant, 0.1-4 parts of antioxidant.
6. the SGP films of high stability according to claim 5, it is characterised in that include according to the raw material of parts by weight:Second Alkene -70-110 parts of methacrylate copolymer, 5-25 parts of cellulose, 10-25 parts of rosin, 15-40 parts of plasticizer, paraffin 8-20 Part, 0.2-3 parts of silane coupler, 20-35 parts of ethylene glycol, 0.02-3 parts of ultra-violet absorber, hydrogen peroxide decomposition agent 0.2-3 Part, 0.01-3 parts of dispersant, 0.1-3 parts of antioxidant.
7. a kind of preparation method of the SGP films of high stability as described in claim 1-6 is any, it is characterised in that including Following steps:
According to parts by weight, ethylene-methyl acrylate copolymer, cellulose, rosin, plasticizer, paraffin, silane are weighed respectively even Join agent, ethylene glycol, ultra-violet absorber, hydrogen peroxide decomposition agent, dispersant, antioxidant, by cellulose, rosin, plasticising Agent, paraffin, silane coupler, ethylene glycol, ultra-violet absorber, hydrogen peroxide decomposition agent, dispersant, antioxidant are added to In ethylene-methyl acrylate copolymer, it is mixed evenly, then casting film-forming piece is extruded through casting machine, produces SGP films.
8. the preparation method of the SGP films of high stability according to claim 7, it is characterised in that casting machine feeding section Temperature is 190-210 DEG C, and melt zone temperature is 180-220 DEG C, 150-170 DEG C of discharge end temperature.
9. the preparation method of the SGP films of high stability according to claim 7, it is characterised in that mix the time For 0.5-10h.
10. the preparation method of the SGP films of high stability according to claim 7, it is characterised in that mixing speed is 100-400r/min。
CN201710675231.6A 2017-08-09 2017-08-09 A kind of SGP films of high stability and preparation method thereof Withdrawn CN107298948A (en)

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Application publication date: 20171027