CN107540978B - A kind of conduction flame-proof PVC composition and preparation method thereof - Google Patents
A kind of conduction flame-proof PVC composition and preparation method thereof Download PDFInfo
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- CN107540978B CN107540978B CN201610485013.1A CN201610485013A CN107540978B CN 107540978 B CN107540978 B CN 107540978B CN 201610485013 A CN201610485013 A CN 201610485013A CN 107540978 B CN107540978 B CN 107540978B
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Abstract
A kind of conduction flame-proof PVC composition and preparation method thereof, belongs to processing and the applied technical field of high molecular material.It is made of the raw material of following parts by weight: 100 parts of polyvinyl chloride resin, 1 ~ 10 part of MBS resin, 3 ~ 15 parts of modifier, 8 ~ 15 parts of the conductive black handled through acrylic ester monomer, 4 ~ 6 parts of calcium zinc stabilizer, 1 ~ 6 part of thermal-reversible cross-linking agent, 1 ~ 3 part of assistant crosslinking agent, 5 ~ 10 parts of flame-proof modifier, 1 ~ 4 part of lubricant；Through acrylic ester monomer handle conductive black the preparation method comprises the following steps: by acrylic ester monomer solubilization dilution agent, be uniformly mixed with conductive black, fling to solvent to get；Both acrylic ester monomer and conductive black mass ratio are 1 ~ 2:10.Conductive flame-proof PVC composition of the invention has preferable electric conductivity and mechanical property, solves the problems, such as that mechanical property caused by a large amount of conductive carbon black fillers of addition reduces.
Description
Technical field
The invention belongs to the processing of high molecular material and applied technical fields, and in particular to a kind of conduction flame-proof PVC combination
Object and preparation method thereof.
Background technique
Conductive plastics tubing development in recent years is very fast, wherein the dual anti-tubing for coal mine occupies larger proportion.Coal mine
There is high requirement to material with pipe, it is desirable that material resistance is less than 1 × 106Ω, it is fire-retardant to reach Ministry of Coal Industry's MT-181 standard
" plastic pipe for coal mine Safety Inspection specification " requirement.To reach standard requirements, a large amount of conductive blacks and resistance need to be added
Agent, but the addition of mass filler are fired, so that modified plastics system impact flexibility declines to a great extent, conductive black is easily poly- in material
Group, it is difficult to disperse, although carbon black is contributed less mostly by surface treatment to dispersibility and with plastic substrate binding performance,
Impact property still declines seriously, it has to add a large amount of anti-impact modifier to improve toughness.But it is a large amount of impact-resistant modified
The addition of agent not only increases material cost, and tensile strength of material is greatly reduced, and influences the service performance of material, is difficult
Reach preferable rigidity-toughness balanced.
National patent has many related PVC conductive materials, and carbon black processing therein all uses coupling agent, dispersing agent substantially
Method, such as application No. is a kind of 201310526520.1 processing of low compression set conductive shield silicon rubber conductive black
Method carries out hot kneading processing using the superconductive carbon black of addition coupling agent and low mass molecule alcohol mixed solution in kneader；State
Family patent CN102558749A, ABS resin/conductive black/asphalt base carbon fiber conducing composite material and preparation method thereof,
It is the method using coupling agent treatment.After handling in this way, although strengthening the interfacial adhesion between carbon black and polymeric matrix, material
The performance of material is still greatly reduced.Also have using cross-linking method, such as the patent No. 200910010679, carbon black filled polyvinyl chloride/
The preparation method of ethylene propylene rubber composite foam conductive NTC material uses spy to lead carbon black (HG-1P) as conductive filler, polychlorostyrene second
Dilute (PVC) and EP rubbers (EPR) are polymeric matrix, and dioctyl phthalate (DOP) is plasticizer, and stearic acid (ST) is
Lubricant, azodicarbonamide (AC) are foaming agent, and zinc stearate (ZN-ST) is foaming synergist, cumyl peroxide
It (DCP) is crosslinking agent, calcium/zinc Ca/Zn compound stabilizer is that heat stabilizer is prepared for using mill melt blending processing method
PVC/EPR foam conductive NTC material, but do not refer to carbon black filler dispersion therein and the influence situation to performance.
Summary of the invention
The technical problem to be solved by the present invention is being directed to the above-mentioned deficiency of the prior art, a kind of conductive flame-proof PVC group is provided
Object and preparation method thereof is closed, which has preferable electric conductivity and mechanical property, and it is big to solve addition
Measure the problem of mechanical property caused by conductive carbon black filler reduces.
The present invention is achieved by the following technical solutions: the conduction flame-proof PVC composition, which is characterized in that by following
The raw materials of parts by weight forms: 100 parts of polyvinyl chloride resin, 1 ~ 10 part of MBS resin, 3 ~ 15 parts of modifier, through acrylic ester monomer
It is 1 ~ 3 part of 1 ~ 6 part of 4 ~ 6 parts of 8 ~ 15 parts of conductive black, calcium zinc stabilizer, thermal-reversible cross-linking agent, the assistant crosslinking agent of processing, flame-retardant modified
5 ~ 10 parts of agent, 1 ~ 4 part of lubricant；.
The conduction flame-proof PVC composition, which is characterized in that be made of the raw material of following parts by weight: 100 parts of polyvinyl chloride resin,
3 ~ 7 parts of MBS resin, 3 ~ 10 parts of modifier, 10 ~ 14 parts of the conductive black handled through acrylic ester monomer, calcium zinc are stablized
4 ~ 6 parts of agent, 2 ~ 4 parts of thermal-reversible cross-linking agent, 1 ~ 2 part of assistant crosslinking agent, 6 ~ 8 parts of flame-proof modifier, 2 ~ 4 parts of lubricant.
The described conductive black handled through acrylic ester monomer the preparation method comprises the following steps: by acrylic ester monomer solubilization
Dilution agent is uniformly mixed with conductive black, fling to solvent to get.
The mass ratio of the acrylic ester monomer and solvent is 1:1 ~ 3, acrylic ester monomer and conductive black two
Person's mass ratio is 1 ~ 2:10.
The acrylic ester monomer is n-butyl acrylate, and solvent is dehydrated alcohol.
The polyvinyl chloride resin be use made from ethylene process or suspension method and the degree of polymerization for 800 ~ 1300 polyvinyl chloride resin.
The thermal-reversible cross-linking agent is dicyclopentadiene dicarboxylate, and assistant crosslinking agent is three isocyanuric acid of triolefin ylmethyl
Rouge；The calcium zinc stabilizer is calcium zinc stabilizer 9700.
The flame-proof modifier is phosphate and the antimony oxide mixture of 2:1, modifier in mass ratio are
Chlorinated paraffin.
The lubricant is polyethylene wax, stearic acid, any two or three of mixture in paraffin.
A kind of preparation method of above-described conductive flame-proof PVC composition, which comprises the steps of:
1) polyvinyl chloride resin, MBS resin, modifier, the conductive charcoal handled through acrylic ester monomer are weighed by weight
Black, calcium zinc stabilizer, thermal-reversible cross-linking agent, assistant crosslinking agent, flame-proof modifier and lubricant are put into high-speed mixer high together
Speed mixing, when mixed material is warming up to 100 ~ 110 DEG C, is discharged in low-speed mixer and mixes, when mixed material is cooled to 40 ~
It discharges at 50 DEG C, obtains mixed material；
2) mixed material is added in parallel double-screw extruder and squeezes out, is granulated, 110 ~ 175 DEG C of extrusion temperature, after pelletizing
To obtain the final product.
The present invention is described as follows: applicant is had found under study for action in conductive PVC composition, in order to improve its electric conductivity
It can need to add larger amount of conductive black, and add a large amount of conductive blacks as mechanical property problem caused by filler.Application
People devises the conductive black handled through acrylic ester monomer, is by the acrylic ester monomer dilution of liquid and conductive charcoal
It is black to be sufficiently mixed, it is evenly coated at acrylic ester monomer outside conductive black.Then in step 1 ~ 2) in: use acrylic acid
Esters monomer is reacted with PVC, MBS resin, thermal-reversible cross-linking agent, assistant crosslinking agent blended cross linking, and carbon black is closely tied with polyvinyl chloride resin
Merging evenly spread in polyvinyl chloride system so that the impact strength of material hardly reduce or reduce it is less；It is modified
The use of resin M BS resin maintains the resistance to low temperature of material while participating in crosslinking；The use of thermal-reversible cross-linking agent
So that cross-linking agent at high temperature can be with depolymerization, thus can be very good to reuse.Preferably, the step 2) in preparation method is adopted
With parallel double-screw extruder extruding pelletization；Parallel double-screw squeezes out extruder temperature (DEG C) successively are as follows: 1 120 DEG C of area, 2 areas 160
DEG C, 170 DEG C of 3rd area, 175 DEG C of 4th area, 175 DEG C of 5th area, 165 DEG C of head.
Preferably, through acrylic ester monomer handle conductive black the preparation method comprises the following steps: acrylic ester monomer is added
Solvent dilution, obtains acrylic ester monomer dilution；By in conductive black high-speed mixer, side high-speed stirred conductive black,
Side spray acrylic ester monomer dilution, be uniformly mixed, volatilization removal solvent to get.Third is sprayed when stirring conductive black
The mode of olefin(e) acid esters monomer dilution facilitates acrylic ester monomer and is evenly coated at conductive black outer surface；It is preferred that high
The mixing time of fast blender is 5 ~ 10 minutes.Preferably, it is sprayed when spraying acrylic ester monomer dilution using misty, with
Improve the covered effect to conductive black.The conductive black that applicant is handled by research discovery using acrylic ester monomer,
The promotion of its mechanical property is the most obvious, wherein preferred acrylic ester monomer is n-butyl acrylate, n-butyl acrylate is handed over
It is good to join effect, and n-butyl acrylate is liquid, has preferable mobility, and be soluble in dehydrated alcohol, is easily formed
The uniform coated with conductive carbon black of dilution.Solvent is wherein flung to, it is the idiomatic expression in this field that is referred to, which is volatilization removal solvent,
Mode.
In the raw material of composition: use ethylene process or suspension method obtained and the degree of polymerization for 800 ~ 1300 polyvinyl chloride resin,
It can guarantee that composition has preferable mechanical property, and easy to process.MBS resin is methyl methacrylate (M), fourth two
The terpolymer of alkene (B) and styrene (S), it has typical nucleocapsid structure.Calcium zinc stabilizer 9700 is that German bear board is raw
It produces, can make gained PVC composition that there is preferable thermal stability.Chlorinated paraffin can not only play processing flow modifier and make
With, and certain assisting flame-resistant effect played to system, cooperation flame-proof modifier (phosphate and antimony oxide in mass ratio 2:
1 mixture) it uses, it can be further improved the flame retardant property of composition.Three isocyanuric acid rouge of triolefin ylmethyl plays auxiliary
The effect of crosslinking.Dicyclopentadiene dicarboxylate (DCPD (COOM)2) n-butyl acrylate, MBS resin, polychlorostyrene second can be caused
Crosslinking between alkene, so that carbon black is evenly spread in mixed material.
Compared with prior art, beneficial possessed by a kind of conductive flame-proof PVC composition of the invention and preparation method thereof
Effect is:
1, the conduction flame-proof PVC composition conduction flame-proof PVC composition have preferable electric conductivity, flame retardant property and
Mechanical property solves the problems, such as that mechanical property caused by a large amount of conductive carbon black fillers of addition reduces.Applicant is in composition original
It is added to the conductive black handled through acrylic ester monomer in material, micro- cross-linking reaction occurs during preparing composition,
Solve the problems, such as that composition mechanical property caused by a large amount of additions of inorganic filler conductive black reduces, final resulting combination
Object can obtain preferable mechanical property and electric conductivity simultaneously.
2, conduction flame-proof PVC composition flame retardant property, impact strength, high temperature resistance and the lower temperature resistance with higher
Energy.Applicant uses phosphate and the antimony oxide mixture of 2:1 in mass ratio to match as flame-proof modifier in the composition
Chlorinated paraffin is closed as modifier and auxiliary flame retardant, shows composition in terms of resistance to flaming combustion and resistance to flameless combustion
It is excellent.Applicant is added to calcium zinc stabilizer 9700 in formula, to improve the Heat-resistant stable performance of composition.
Specific embodiment
Embodiment 1 ~ 10 is a kind of specific embodiment of conductive flame-proof PVC composition of the invention and preparation method thereof.
Wherein embodiment 1 is most preferred embodiment.
The proportion (in parts by weight) of 1 embodiment 1 ~ 6 of table
。
The proportion (in parts by weight) of 2 embodiment 7 ~ 10 of table and comparative example 1 ~ 2
。
Flame-proof modifier is phosphate and the antimony oxide mixture of 2:1 in mass ratio in table 1 ~ 2.1 ~ 2 institute of comparative example
With the carbon black that conductive black is without any surface treatment, belong to commercial product.Embodiment 1 ~ 10 is used through esters of acrylic acid
Monomer processing conductive black the preparation method comprises the following steps: according to n-butyl acrylate and dehydrated alcohol mass ratio 1:1, by acrylic acid
N-butyl adds dehydrated alcohol to dilute, and obtains dilution；According to 1 ~ 2:10 of mass ratio of n-butyl acrylate and conductive black, will lead
In electric carbon black high-speed mixer, dilution is sprayed when stirring conductive black, continues stirring after sprinkling 5 ~ 10 minutes,
Even mixing simultaneously volatilizees and removes dehydrated alcohol to get the conductive black handled through acrylic ester monomer.
The preparation method of embodiment 1 ~ 10 uses following steps:
1) polyvinyl chloride resin, MBS resin, modifier, the conductive charcoal handled through acrylic ester monomer are weighed by weight
Black, calcium zinc stabilizer, thermal-reversible cross-linking agent, assistant crosslinking agent, flame-proof modifier and lubricant are put into high-speed mixer high together
Speed mixing, when mixed material is warming up to 100 ~ 110 DEG C, is discharged in low-speed mixer and mixes, when mixed material is cooled to 40 ~
It discharges at 50 DEG C, obtains mixed material；
2) will mixed material be added parallel double-screw extruder in squeeze out, be granulated, pelletizing to get；Parallel double-screw squeezes out
Machine temperature (DEG C) is successively are as follows: 1 120 DEG C of area, 160 DEG C of 2nd area, 170 DEG C of 3rd area, 175 DEG C of 4th area, 175 DEG C of 5th area, 165 DEG C of head.
The preparation method is the same as that of Example 1 for comparative example 1 ~ 2 ~ and 10.
Performance test
By embodiment 1 ~ 10 and 1 ~ 2 resulting composition of comparative example using crowded plumber's skill as follows, tubing, performance test knot are obtained
Fruit typing following table.Squeeze plumber's skill: through by step 2 resulting composition pellet in dedicated single screw rod tube extruding machine extruding pipe material, and
Micro- cross-linking reaction occurs in extrusion process.Length of extruder die and extruding pipe material diameter ratio are 2:1, guarantee that extruding pipe material is micro-
Cross-linking reaction is gone on smoothly.Crowded pipe technological temperature: 1 130 DEG C of area, 2 170 DEG C of areas, 3 180 DEG C of areas, 4 180 DEG C of areas, 5 195 DEG C of areas,
190 DEG C of head.
The performance test results of 3 embodiment and comparative example of table
。
Embodiment 1 ~ 10 is all made of the conductive charcoal handled through acrylic ester monomer it can be seen from performance test table 2
It is black, and comparative example 1 ~ 2 uses the conductive black handled without monomer, no matter 1 ~ 10 resulting composition of acetonideexample stretches by force
Degree or impact strength are superior to comparative example, and resistance to low temperature improves a lot than comparative example.Add the carbon black of same number, this hair
Bright embodiment impact strength is much higher than comparative example, after illustrating the blended extrusion crosslinking of carbon black that the present invention is handled, composition tool
There is higher impact flexibility.And it can be seen from Table 1 that embodiment 1 ~ 10 is obtaining preferable electric conductivity and mechanical property
While, flame retardant property, impact strength, high temperature resistance and resistance to low temperature also with higher.
The above described is only a preferred embodiment of the present invention, be not the limitation for making other forms to invention, it is any
Those skilled in the art are changed or are modified as the equivalent of equivalent variations possibly also with the technology contents of the disclosure above
Embodiment.But without departing from the technical solutions of the present invention, above embodiments are made according to the technical essence of the invention
Any simple modification, equivalent variations and remodeling, still fall within the protection scope of technical solution of the present invention.
Claims (9)
1. a kind of conduction flame-proof PVC composition, which is characterized in that be made of the raw material of following parts by weight: 100 parts of polyvinyl chloride resin,
1 ~ 10 part of MBS resin, 3 ~ 15 parts of modifier, 8 ~ 15 parts of the conductive black handled through acrylic ester monomer, calcium zinc are stablized
4 ~ 6 parts of agent, 1 ~ 6 part of thermal-reversible cross-linking agent, 1 ~ 3 part of assistant crosslinking agent, 5 ~ 10 parts of flame-proof modifier, 1 ~ 4 part of lubricant；The warp
Acrylic ester monomer processing conductive black the preparation method comprises the following steps: by acrylic ester monomer solubilization dilution agent, with conductive charcoal
It is black be uniformly mixed, fling to solvent to get.
2. a kind of conductive flame-proof PVC composition according to claim 1, which is characterized in that by the raw material of following parts by weight
Composition: 100 parts of polyvinyl chloride resin, 3 ~ 7 parts of MBS resin, 3 ~ 10 parts of modifier, the conductive charcoal handled through acrylic ester monomer
Black 10 ~ 14 parts, 4 ~ 6 parts of calcium zinc stabilizer, 2 ~ 4 parts of thermal-reversible cross-linking agent, 1 ~ 2 part of assistant crosslinking agent, 6 ~ 8 parts of flame-proof modifier, profit
2 ~ 4 parts of lubrication prescription.
3. a kind of conductive flame-proof PVC composition according to claim 1, it is characterised in that: the esters of acrylic acid list
The mass ratio of body and solvent is 1:1 ~ 3, and both acrylic ester monomer and conductive black mass ratio are 1 ~ 2:10.
4. a kind of conductive flame-proof PVC composition according to claim 1, it is characterised in that: the esters of acrylic acid list
Body is n-butyl acrylate, and solvent is dehydrated alcohol.
5. a kind of conductive flame-proof PVC composition according to claim 1, it is characterised in that: the polyvinyl chloride resin is to use
The polyvinyl chloride resin that ethylene process or suspension method be obtained and the degree of polymerization is 800 ~ 1300.
6. a kind of conductive flame-proof PVC composition according to claim 1, it is characterised in that: the thermal-reversible cross-linking agent
For dicyclopentadiene dicarboxylate, assistant crosslinking agent is three isocyanuric acid rouge of triolefin ylmethyl；The calcium zinc stabilizer is calcium zinc
Stabilizer 9700.
7. a kind of conductive flame-proof PVC composition according to claim 1, it is characterised in that: the flame-proof modifier is
Phosphate and the antimony oxide mixture of 2:1 in mass ratio, modifier is chlorinated paraffin.
8. a kind of conductive flame-proof PVC composition according to claim 1, it is characterised in that: the lubricant is poly- second
Alkene wax, stearic acid, any two or three of mixture in paraffin.
9. a kind of described in any item preparation methods of conductive flame-proof PVC composition of claim 1 ~ 8, which is characterized in that including
Following steps:
1) weigh by weight polyvinyl chloride resin, MBS resin, modifier, through acrylic ester monomer handle conductive black,
Calcium zinc stabilizer, thermal-reversible cross-linking agent, assistant crosslinking agent, flame-proof modifier and lubricant are put into high-speed mixer high speed together
Mixing, when mixed material is warming up to 100 ~ 110 DEG C, is discharged in low-speed mixer and mixes, when mixed material is cooled to 40 ~ 50
DEG C when discharge, obtain mixed material；
2) mixed material is added in parallel double-screw extruder and squeezes out, be granulated, 110 ~ 175 DEG C of extrusion temperature, after pelletizing to obtain the final product.
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| CN108440871A (en) * | 2018-04-19 | 2018-08-24 | 温州市赢创新材料技术有限公司 | A kind of antistatic bamboo moulding material and preparation method thereof |
| CN114672108A (en) * | 2022-04-15 | 2022-06-28 | 浙江元通线缆制造有限公司 | Rubber sleeve cable three-layer co-extrusion external shielding strippable material and preparation method thereof |
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| CN1357567A (en) * | 2000-12-05 | 2002-07-10 | 中国石化集团齐鲁石油化工公司 | Antistatic polyvinyl chloride plastic composition and its prepn |
| CN1667052A (en) * | 2004-03-09 | 2005-09-14 | 华东理工大学 | Carbon microstrip and method for preparing same |
| CN101061174A (en) * | 2004-11-18 | 2007-10-24 | 兰科瑟斯有限公司 | Rubber compostion containing improved filler |
| CN101724241A (en) * | 2009-12-15 | 2010-06-09 | 上海新上化高分子材料有限公司 | Antistatic thermoplastic polycarbonate composition and preparation method thereof |
-
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1357567A (en) * | 2000-12-05 | 2002-07-10 | 中国石化集团齐鲁石油化工公司 | Antistatic polyvinyl chloride plastic composition and its prepn |
| CN1667052A (en) * | 2004-03-09 | 2005-09-14 | 华东理工大学 | Carbon microstrip and method for preparing same |
| CN101061174A (en) * | 2004-11-18 | 2007-10-24 | 兰科瑟斯有限公司 | Rubber compostion containing improved filler |
| CN101724241A (en) * | 2009-12-15 | 2010-06-09 | 上海新上化高分子材料有限公司 | Antistatic thermoplastic polycarbonate composition and preparation method thereof |
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