CN108456374A - A kind of phosphomolybdic acid iron smoke-inhibiting PVC plank and preparation method thereof - Google Patents

A kind of phosphomolybdic acid iron smoke-inhibiting PVC plank and preparation method thereof Download PDF

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Publication number
CN108456374A
CN108456374A CN201810135998.4A CN201810135998A CN108456374A CN 108456374 A CN108456374 A CN 108456374A CN 201810135998 A CN201810135998 A CN 201810135998A CN 108456374 A CN108456374 A CN 108456374A
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smoke
mass parts
phosphomolybdic acid
pvc
inhibiting
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陈绪煌
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Hubei University of Technology
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Hubei University of Technology
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L27/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers
    • C08L27/02—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment
    • C08L27/04—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment containing chlorine atoms
    • C08L27/06—Homopolymers or copolymers of vinyl chloride
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B25/00—Phosphorus; Compounds thereof
    • C01B25/16—Oxyacids of phosphorus; Salts thereof
    • 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
    • C08K3/24—Acids; Salts thereof
    • C08K3/26—Carbonates; Bicarbonates
    • C08K2003/265—Calcium, strontium or barium carbonate
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00—Properties
    • C08L2201/02—Flame or fire retardant/resistant
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00—Polymer mixtures characterised by other features
    • C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
    • C08L2205/035—Polymer 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)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Inorganic Chemistry (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

The invention belongs to high molecular material application field, it is related to a kind of phosphomolybdic acid iron smoke-inhibiting PVC plank and preparation method thereof, component and its parts by weight are：100 mass parts of PVC resin powder, 2~3 mass parts of stabilizer, 2~3 mass parts of processing aid, 0.5~1 mass parts of lubricant, 3~5 mass parts of toughener, 8~15 mass parts of filler, 4~6 mass parts of anti-flaming smoke-inhibiting agent.The phosphomolybdic acid iron that the present invention is prepared using phosphomolybdic acid and iron hydroxide as raw material, using hydro-thermal method is added in conjunction with other auxiliary agents in PVC board production, simple for process, yield is high, and flame-retardant smoke inhibition is with obvious effects as anti-flaming smoke-inhibiting agent.

Description

A kind of phosphomolybdic acid iron smoke-inhibiting PVC plank and preparation method thereof
Technical field
The invention belongs to high molecular material application field, it is related to a kind of phosphomolybdic acid iron smoke-inhibiting PVC plank and preparation method thereof.
Background technology
PVC is one of five big synthetic thermoplastic plastics, and yield is only second to polyethylene, and PVC is based on hard tough products. PVC sheet is widely used in advertisement, packaging, decoration industry, is developed with fast speed.But PVC sheet combustion process generates a large amount of Smog limits its application in advertisement and ornament materials.Therefore the flame-proof smoke-suppressing for improving PVC sheet is that PVC sheet is opened The key for sending out application, to promoting its application in relevant industries to be of great significance.
Traditional smoke suppressant is expensive, also not environmentally.The smoke suppressant of primary commercial application at present is molybdenum trioxide and ammonium octamolybdate Combination, but the cationic cracking reaction of polyvinyl chloride polyenoid chain is catalyzed under molybdenum trioxide high temperature, cause aliphatic hydrocarbon to increase, and then fire It burns and discharges more heats, therefore also need to fire retardant and be used in conjunction with each other.A kind of phosphorus molybdenum is disclosed in patent 201610195945.2 Sour zinc fire-resistant smoke-inhibiting PVC sheet material, zinc have the ability of stronger inhibition PVC discolorations, and the later stage is because of the ZnCl generated2With extremely strong Catalysis take off HCl effects so that its long-term resistance to burnings property is very poor, zinc occurs and burns phenomenon, therefore the dosage of reduction zinc, utilizes it Its suppression cigarette element can be such that the process that PVC is synthesized more stablizes.In addition the case using Calcium Phosphomolybdate, suppression cigarette are also Lewis acid mechanism, but calcium itself is acted on without flame-retardant smoke inhibition, and compound flame-retardant smoke inhibition is ineffective.
Invention content
To solve the above problems, a kind of phosphomolybdic acid iron smoke-inhibiting PVC plank of present invention offer and preparation method thereof.
The present invention provides a kind of phosphomolybdic acid iron smoke-inhibiting PVC plank, and component and its parts by weight are：100 mass of PVC resin powder Part, 2~5 mass parts of stabilizer, 1.5~3 mass parts of processing aid, 0.5~2 mass parts of lubricant, 3~5 mass parts of toughener, 8~15 mass parts of filler, 4~6 mass parts of anti-flaming smoke-inhibiting agent.
Specifically, the PVC resin powder is SG-5 resins.
Specifically, the stabilizer is Ca-Zn composite heat stabilizer.
Specifically, the processing aid is acrylate copolymer.
Specifically, the lubricant is paraffin and stearic acid.
Specifically, the toughener is methyl methacrylate-butadiene-styrene terpolymer.
Specifically, the filler is 1250 mesh calcium carbonate.
Specifically, the anti-flaming smoke-inhibiting agent is phosphomolybdic acid iron, using phosphomolybdic acid and iron hydroxide as raw material, using hydro-thermal method It is prepared.
The present invention provides the preparation method of any of the above-described kind of phosphomolybdic acid iron smoke-inhibiting PVC plank, includes the following steps：
1) PVC resin powder and processing aid are added to homogenizer and are mixed, after temperature reaches 100~130 DEG C, stirred It mixes 2~5 minutes, discharges it and be added in extruder when being cooled to 40~60 DEG C；
2) it is squeezed out through parallel double-screw extruder, screw zones temperature is：140~170 DEG C of transportation section, compression section 150~ 180 DEG C, 160~190 DEG C of melt zone, 160~180 DEG C of head；
3) pass through the plank that calender comes out, can be prepared by the PVC board of flame-retardant smoke inhibition by removing, being cooled to room temperature.
The smoke-suppression mechanism of the present invention is：Phosphomolybdic acid iron (Fe [PMo12O40]) transition metal salt, it is a kind of very only The heteropolyacid salt of special structure with Keggin and containing there are four types of the compounds (iron, phosphorus, molybdenum, oxygen) of element.Wherein iron, molybdenum compound be all It is verified that having smoke suppressing；Phosphorus compound belongs to the air source and acid source of expansion type flame retardant, before ensureing for smoke suppressing Put forward condition.Specifically, molybdenum, iron react to form strong Lewis acid-XO with HCl with Lewis acid smoke suppression mechanism2Cl2, pass through chloride Repetition catalysis, and then Friedel-Crafts reaction occurs, forms the charcoal that is cross-linked into of polyenoid chain, reduce the production of benzene and aromatic hydrocarbons Amount, to play the role of pressing down cigarette, the collaboration of two elements promotes the smoke suppressing of PVC.In addition, molybdenum has the flame retardant effect of nitrogen, phosphorus Facilitation.
PVC resin powder SG-5 resins, are matrixes；Stabilizer is Ca-Zn composite heat stabilizer, and it is steady to improve PVC process It is qualitative, and be stabilizer；Processing aid is acrylate copolymer, and abbreviation ACR promotes polyvinyl chloride resin plasticizing；Lubricant For paraffin and stearic acid, paraffin is external lubricant, and stearic acid is in-lubricant；Filler is 1250 mesh precipitated calcium carbonates, promotes PVC Plasticizing, improves its toughness and tensile strength；Toughener methyl methacrylate-butadiene-styrene terpolymer, referred to as MBS improves system toughness.
The beneficial effects of the present invention are：It is raw material by phosphomolybdic acid and iron hydroxide, PVC board is prepared using hydro-thermal method Anti-flaming smoke-inhibiting agent phosphomolybdic acid iron (Fe [PMo12O40]).Phosphomolybdic acid iron anti-flaming smoke-inhibiting agent can improve the oxygen index (OI) of PVC board, suppression The smoke amount of PVC board processed, and it is with obvious effects.The PVC board for adding anti-flaming smoke-inhibiting agent phosphomolybdic acid iron has simple production process, Yield is high, and product flame-retardant smoke inhibition is with obvious effects.
Specific implementation mode
Technical scheme of the present invention is described further below, however, it is not limited to this, all using to the technology of the present invention Scheme on an equal basis replace or modification, without departing from the technology of the present invention principle and purport, should all cover the present invention claims protection model It encloses.
Embodiment 1
Respectively by 100 mass parts of SG-5 resins, 2.2 mass parts of Ca-Zn composite heat stabilizer, 2.5 matter of acrylate copolymer Measure part, 0.5 mass parts of paraffin, 0.3 mass parts of stearic acid, 4 matter of methyl methacrylate-butadiene-styrene terpolymer Amount part, 1250 mesh calcium carbonate, 12 mass parts, 5 mass parts of phosphomolybdic acid iron pour into homogenizer, start blender stirring, work as temperature It when reaching 120 DEG C or so, stirs 2 minutes, discharges it and be added in extruder when into 60 DEG C or so of cold blender.
The wherein temperature setting in extruder transportation section, compression section, melt zone and each area of head：
Ⅰ160℃ Ⅱ170℃ Ⅲ180℃ Ⅳ175℃
The temperature of each roller of calender is set：
Ⅰ185℃ Ⅱ190℃ Ⅲ195℃ Ⅳ190℃
By the sheet material that calender comes out, the PVC sheet of flame-retardant smoke inhibition can be prepared by by removing, being cooled to room temperature.
The PVC board of acquisition is subjected to flame-proof smoke-suppressing test, as a result obtains oxygen index (OI) 40.37, maximum smoke density (MSD) 72.64, smoke density grade (SDR) 53.98.
Embodiment 2
Respectively by 100 mass parts of SG-5 resins, 3 mass parts of Ca-Zn composite heat stabilizer, 2 mass of acrylate copolymer Part, 0.6 mass parts of paraffin, 0.4 mass parts of stearic acid, 3 mass of methyl methacrylate-butadiene-styrene terpolymer Part, 1250 mesh calcium carbonate, 11 mass parts, 4 mass parts of phosphomolybdic acid iron pour into homogenizer, start blender stirring, when temperature reaches It when to 120 DEG C or so, stirs 2 minutes, discharges it and be added in extruder when into 60 DEG C or so of cold blender.
The wherein temperature setting in extruder transportation section, compression section, melt zone and each area of head：
Ⅰ160℃ Ⅱ170℃ Ⅲ180℃ Ⅳ175℃
The temperature of each roller of calender is set：
Ⅰ185℃ Ⅱ190℃ Ⅲ195℃ Ⅳ190℃
By the sheet material that calender comes out, the PVC sheet of flame-retardant smoke inhibition can be prepared by by removing, being cooled to room temperature.
The PVC board of acquisition is subjected to flame-proof smoke-suppressing test, as a result obtains oxygen index (OI) 42.43, maximum smoke density (MSD) 74.06, smoke density grade (SDR) 54.45.
Embodiment 3
Respectively by 100 mass parts of SG-5 resins, 2 mass parts of Ca-Zn composite heat stabilizer, 2.7 mass of acrylate copolymer Part, 0.7 mass parts of paraffin, 0.5 mass parts of stearic acid, 5 mass of methyl methacrylate-butadiene-styrene terpolymer Part, 1250 mesh calcium carbonate, 10 mass parts, 5 mass parts of phosphomolybdic acid iron pour into homogenizer, start blender stirring, when temperature reaches It when to 120 DEG C or so, stirs 2 minutes, discharges it and be added in extruder when into 60 DEG C or so of cold blender.
The wherein temperature setting in extruder transportation section, compression section, melt zone and each area of head：
Ⅰ160℃ Ⅱ170℃ Ⅲ180℃ Ⅳ175℃
The temperature of each roller of calender is set：
Ⅰ185℃ Ⅱ190℃ Ⅲ195℃ Ⅳ190℃
By the sheet material that calender comes out, the PVC sheet of flame-retardant smoke inhibition can be prepared by by removing, being cooled to room temperature.
The PVC board of acquisition is subjected to flame-proof smoke-suppressing test, as a result obtains oxygen index (OI) 42.92, maximum smoke density (MSD) 73.33, smoke density grade (SDR) 55.12.
Embodiment 4
Respectively by 100 mass parts of SG-5 resins, 2.5 mass parts of Ca-Zn composite heat stabilizer, 2.6 matter of acrylate copolymer Measure part, 0.3 mass parts of paraffin, 0.3 mass parts of stearic acid, 5 matter of methyl methacrylate-butadiene-styrene terpolymer Amount part, 1250 mesh calcium carbonate, 15 mass parts, 4 mass parts of phosphomolybdic acid iron pour into homogenizer, start blender stirring, work as temperature It when reaching 120 DEG C or so, stirs 2 minutes, discharges it and be added in extruder when into 60 DEG C or so of cold blender.
The wherein temperature setting in extruder transportation section, compression section, melt zone and each area of head：
Ⅰ160℃ Ⅱ170℃ Ⅲ180℃ Ⅳ175℃
The temperature of each roller of calender is set：
Ⅰ185℃ Ⅱ190℃ Ⅲ195℃ Ⅳ190℃
By the sheet material that calender comes out, the PVC sheet of flame-retardant smoke inhibition can be prepared by by removing, being cooled to room temperature.
The PVC board of acquisition is subjected to flame-proof smoke-suppressing test, as a result obtains oxygen index (OI) 39.65, maximum smoke density (MSD) 73.35, smoke density grade (SDR) 53.87.
Embodiment 5
Respectively by 100 mass parts of SG-5,2.3 mass parts of Ca-Zn composite heat stabilizer, 2.5 mass of acrylate copolymer Part, 0.4 mass parts of paraffin, 0.3 mass parts of stearic acid, 3 mass of methyl methacrylate-butadiene-styrene terpolymer Part, 1250 mesh calcium carbonate, 8 mass parts, 6 mass parts of phosphomolybdic acid iron pour into homogenizer, start blender stirring, when temperature reaches It when to 120 DEG C or so, stirs 2 minutes, discharges it and be added in extruder when into 60 DEG C or so of cold blender.
The wherein temperature setting in extruder transportation section, compression section, melt zone and each area of head：
Ⅰ160℃ Ⅱ170℃ Ⅲ180℃ Ⅳ175℃
The temperature of each roller of calender is set：
Ⅰ185℃ Ⅱ190℃ Ⅲ195℃ Ⅳ190℃
By the sheet material that calender comes out, the PVC sheet of flame-retardant smoke inhibition can be prepared by by removing, being cooled to room temperature.
The PVC board of acquisition is subjected to flame-proof smoke-suppressing test, as a result obtains oxygen index (OI) 44.28, maximum smoke density (MSD) 73.42, smoke density grade (SDR) 55.20.
Comparative example
Respectively by 100 mass parts of SG-5 resins, 2 mass parts of Ca-Zn composite heat stabilizer, 2.7 mass of acrylate copolymer Part, 0.9 mass parts of paraffin, 5 mass parts of toughener, 1250 mesh calcium carbonate, 10 mass parts, 5 mass parts of anti-flaming smoke-inhibiting agent pour into high speed Blender uses molybdenum trioxide and ammonium octamolybdate in mass ratio 3:2 be used as composite flame-proof smoke suppressants, according to Examples 1 to 5 phase It is prepared by same method.
Blank sample
Respectively by 100 mass parts of SG-5 resins, 2 mass parts of Ca-Zn composite heat stabilizer, 2.7 mass of acrylate copolymer Part, 0.9 mass parts of paraffin, 5 mass parts of toughener, 1250 mesh calcium carbonate, 10 mass parts pour into homogenizer, according to implementation It is prepared by 1~5 identical method of example.
The above-mentioned plank being prepared is tested for the property, the results are shown in Table 1.
1 flame retarding and smoke suppressing properties test result of table
Oxygen index (OI) % Smoke density MSD Smoke density grade SDR
Blank sample 36.61 92.33 79.56
Embodiment 1 40.37 72.64 53.98
Embodiment 2 42.43 74.06 54.45
Embodiment 3 42.92 73.33 55.12
Embodiment 4 39.65 73.35 53.87
Embodiment 5 44.28 73.42 55.20
Comparative example 39.55 79.53 58.22
Above-described embodiment and blank sample and comparative example relatively find out that the application of phosphomolybdic acid iron is than molybdenum trioxide and eight molybdenums Sour ammonium in mass ratio 3:2 as composite flame-proof smoke suppressant oxygen index (OI) is larger, smoke density is smaller.

Claims (9)

1. a kind of phosphomolybdic acid iron smoke-inhibiting PVC plank, which is characterized in that its component and its parts by weight are：100 mass of PVC resin powder Part, 3~5 mass parts of toughener, is filled out at 2~3 mass parts of stabilizer, 2~3 mass parts of processing aid, 0.5~1 mass parts of lubricant Expect 8~15 mass parts, 4~6 mass parts of anti-flaming smoke-inhibiting agent.
2. phosphomolybdic acid iron smoke-inhibiting PVC plank according to claim 1, it is characterised in that：The PVC resin powder is SG-5 Resin.
3. phosphomolybdic acid iron smoke-inhibiting PVC plank according to claim 1, it is characterised in that：The stabilizer is that calcium zinc is multiple Close heat stabilizer.
4. phosphomolybdic acid iron smoke-inhibiting PVC plank according to claim 1, it is characterised in that：The processing aid is propylene Acid ester copolymer.
5. phosphomolybdic acid iron smoke-inhibiting PVC plank according to claim 1, it is characterised in that：The lubricant be paraffin and Stearic acid.
6. phosphomolybdic acid iron smoke-inhibiting PVC plank according to claim 1, it is characterised in that：The toughener is methyl-prop E pioic acid methyl ester-butadiene-styrene terpolymer.
7. phosphomolybdic acid iron smoke-inhibiting PVC plank according to claim 1, it is characterised in that：The filler is 1250 mesh carbon Sour calcium.
8. phosphomolybdic acid iron smoke-inhibiting PVC plank according to claim 1, it is characterised in that：The anti-flaming smoke-inhibiting agent is phosphorus Iron molybdate is prepared using phosphomolybdic acid and iron hydroxide as raw material using hydro-thermal method.
9. according to the preparation method of claim 1~8 any one of them phosphomolybdic acid iron smoke-inhibiting PVC plank, it is characterised in that：Packet Include following steps：
1) PVC resin powder and processing aid are added to homogenizer and are mixed, after temperature reaches 100~130 DEG C, stirring 2 It~5 minutes, discharges it and is added in extruder when being cooled to 40~60 DEG C；
2) it is squeezed out through parallel double-screw extruder, screw zones temperature is：140~170 DEG C of transportation section, compression section 150~180 DEG C, 160~190 DEG C of melt zone, 160~180 DEG C of head；
3) pass through the plank that calender comes out, can be prepared by the PVC board of flame-retardant smoke inhibition by removing, being cooled to room temperature.
CN201810135998.4A 2018-02-09 2018-02-09 A kind of phosphomolybdic acid iron smoke-inhibiting PVC plank and preparation method thereof Pending CN108456374A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111548581A (en) * 2020-06-11 2020-08-18 安徽奥凯材料股份有限公司 Flame-retardant smoke suppressant and preparation method of flame-retardant smoke suppressant for PVC (polyvinyl chloride) sheet
CN111548582A (en) * 2020-06-11 2020-08-18 安徽奥凯材料股份有限公司 Ferric phosphotungstate flame-retardant smoke-suppression semi-rigid PVC (polyvinyl chloride) sheet and preparation method thereof
CN112876787A (en) * 2021-01-28 2021-06-01 安徽奥凯材料股份有限公司 Flame-retardant smoke-suppression PVC (polyvinyl chloride) plate containing zinc and molybdate ion complexes and preparation method thereof

Citations (1)

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CN107286494A (en) * 2016-03-31 2017-10-24 苏州奥凯高分子材料股份有限公司 Phosphomolybdic acid zinc fire-resistant smoke-inhibiting PVC sheet material

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CN107286494A (en) * 2016-03-31 2017-10-24 苏州奥凯高分子材料股份有限公司 Phosphomolybdic acid zinc fire-resistant smoke-inhibiting PVC sheet material

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111548581A (en) * 2020-06-11 2020-08-18 安徽奥凯材料股份有限公司 Flame-retardant smoke suppressant and preparation method of flame-retardant smoke suppressant for PVC (polyvinyl chloride) sheet
CN111548582A (en) * 2020-06-11 2020-08-18 安徽奥凯材料股份有限公司 Ferric phosphotungstate flame-retardant smoke-suppression semi-rigid PVC (polyvinyl chloride) sheet and preparation method thereof
CN112876787A (en) * 2021-01-28 2021-06-01 安徽奥凯材料股份有限公司 Flame-retardant smoke-suppression PVC (polyvinyl chloride) plate containing zinc and molybdate ion complexes and preparation method thereof
CN112876787B (en) * 2021-01-28 2023-05-02 安徽奥凯材料股份有限公司 Flame-retardant smoke-suppressing PVC (polyvinyl chloride) plate containing zinc and molybdate ion complex and preparation method thereof

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Application publication date: 20180828