CN108047527A - A kind of preparation method of high-strength halogen-free flame retardant polyolefine material - Google Patents

A kind of preparation method of high-strength halogen-free flame retardant polyolefine material Download PDF

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CN108047527A
CN108047527A CN201711246676.9A CN201711246676A CN108047527A CN 108047527 A CN108047527 A CN 108047527A CN 201711246676 A CN201711246676 A CN 201711246676A CN 108047527 A CN108047527 A CN 108047527A
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高产明
何少雄
陈可
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    • 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
    • C08L23/06Polyethene
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00Properties
    • C08L2201/02Flame or fire retardant/resistant
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00Properties
    • C08L2201/22Halogen free composition
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    • 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
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/14Polymer mixtures characterised by other features containing polymeric additives characterised by shape
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    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2207/00Properties characterising the ingredient of the composition
    • C08L2207/06Properties of polyethylene
    • C08L2207/062HDPE

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Abstract

The invention discloses a kind of preparation methods of high-strength halogen-free flame retardant polyolefine material, belong to polyolefine material preparing technical field.The present invention, which mixes magnalium hydrotalcite with ethanol water, to be disperseed to obtain hydrotacite suspension, reaction is heated with onodoidecyl phosphonic acid methyl esters salt and hydrotacite suspension in acid condition, mix lifeless thing fiber, obtain rubber compound, lignin reaches glassy state, soften and generate flowing under high pressure, lignin has very strong adhesive power at this time, is improved the mechanical property of polyolefine material;Hydrotalcite grain size is smaller in the present invention, it can reach nano-dispersion in the polymer, resulting materials are really a kind of hydrotalcite-Polyethylene Nanocomposites, make the hydrophobic immersion oil of magnalium hydrotalcite intercalation, form compact composite material, in combustion, these processes will all absorb the concentration of substantial amounts of heat and dilution oxygen, promote polymer into charcoal, form carbon net, so as to improve polyolefine material flame retardant property, have a extensive future.

Description

A kind of preparation method of high-strength halogen-free flame retardant polyolefine material
Technical field
The invention discloses a kind of preparation methods of high-strength halogen-free flame retardant polyolefine material, belong to polyolefine material preparation Technical field.
Background technology
Polyolefin refers to the polymer general name of ethylene, propylene or higher alkene, by ethylene, propylene, 1- butylene, 1- amylenes, 1- The alpha-olefins such as hexene, 1- octenes, 4-methyl-1-pentene and some cycloolefins be polymerized alone or combined polymerization and obtain.
It is cheap due to abundant raw material, shaping, high comprehensive performance are easily worked, therefore be that a kind of yield is maximum, Using very extensive high molecular material.It is wherein mostly important with polyethylene, polypropylene.Principal item has polyethylene and with second The copolymer of some copolymers based on alkene, such as ethylene-vinyl acetate copolymer, ethylene-acrylic acid or acrylate also has Polypropylene and some propylene copolymers, poly 1-butene, poly(4-methyl-1-pentene), cyclic olefin polymer.
Separately there is the smaller higher olefin polymer of yield such as:Poly 1-butene, the polymer of 1- butylene.Mainly with gas-phase polymerization It prepares.135 DEG C of melting temperature, crystal transfer can occur for room temperature.Can with squeeze out, blowing and injection etc. techniques be processed into pipe, Plate, film and fiber.Since its creep resistance and stress crack resistance performance protrude, often make the pipeline material used at -25~100 DEG C Material.Poly(4-methyl-1-pentene), the polymer of 4-methyl-1-pentene.It is prepared in stereospecfic polymerization method.About 240 DEG C of melting temperature, For most light macromolecule, transparency is high, insulating properties, good corrosion resistance, and air penetrability is high(For 10 times of polyethylene), but impact resistance, Stress cracking and photooxidative aging performance are poor.Injection and extrusion method can be used to process.For manufacturing optical instrument, chemistry and medical treatment Utensil, electronic device and insulating materials, gas separation membrane and packaging material, fiber etc..Polyolefine material common at present exists The defects of damaging polyolefine material mechanical strength after poor flame retardant properties, addition flame retardant effect ingredient.Therefore, a kind of intensity is invented High and good flame retardation effect polyolefine material has positive effect to polyolefine material preparing technical field.
The content of the invention
Present invention mainly solves the technical issues of, for polyolefine material poor flame retardant properties, addition with flame retardant effect The defects of mechanical strength of polyolefine material can be damaged after ingredient, provides a kind of system of high-strength halogen-free flame retardant polyolefine material Preparation Method.
In order to solve the above-mentioned technical problem, the technical solution adopted in the present invention is:
A kind of preparation method of high-strength halogen-free flame retardant polyolefine material, it is characterised in that specifically preparation process is:
(1)600~700mL ethanol waters are added in three-necked flask, three-necked flask is transferred in water-bath, heating rises Temperature adds in 30~35g magnalium hydrotalcites into three-necked flask, starts magnetic stirring apparatus, is stirred, obtains finely dispersed water Talc suspension;
(2)70~80g onodoidecyl phosphonic acid methyl esters potassium is put into above-mentioned hydrotacite suspension, is stirred, with hydrochloric acid tune Water-saving talc suspension pH, heat temperature raising are stirred to react, and obtain white slurries, and white slurries are placed in vacuum filtration machine and are taken out After filter, the isolated wet white powder of filtrate is removed, white powder with absolute ethyl alcohol is washed and is placed in baking oven, it is dry, Obtain organically-modified hydrotalcite;
(3)Reed is put into pulverizer and is crushed, sieving obtains reed powder, reed powder is placed in baking oven, heat temperature raising, It is dry, dried reed powder is obtained, dried reed powder, organically-modified hydrotalcite, ethyl acetate are mixed, are placed in High speed dispersor, high speed dispersion obtain dispersed paste;
(4)Dispersed paste is placed in vacuum filtration machine and is filtered, the isolated lifeless thing fiber of filtrate is removed, takes 150~170g high Density polyethylene masterbatch pellet is put into baking oven, heat temperature raising, after preheating, is put into melting in rubber mixing machine, is treated that polyethylene master batch is complete 60~65g lifeless thing fibers are mixed after full-fusing, obtain rubber compound;
(5)Rubber compound is transferred in mixer, 40~50g ethylene-vinyl acetate copolymers are mixed to rubber compound, after mixing It squeezes out into mold, mold is placed in compression molding agent and is vulcanized, demoulded after vulcanization postcooling to room temperature and obtain high intensity Halogen-free anti-flaming polyolefin material.
Step(1)The mass fraction of the ethanol water is 40%, is 70~80 to temperature after water-bath heat temperature raising DEG C, magnetic stirring apparatus rotating speed is 350~400r/min, is stirred the time as 1~2h.
Step(2)Described is stirred the time as 5~10min, and the mass fraction of hydrochloric acid is 15%, and hydrochloric acid adjusts neatly Stone pH of suspension is 4~5, and temperature is 80~90 DEG C after heat temperature raising, is stirred to react the time as 6~7h, baking oven design temperature is 90~100 DEG C, drying time is 7~8h.
Step(3)The grinding time is 3~4h, and specification of sieving is 100 mesh, is to temperature after baking oven heat temperature raising 70~80 DEG C, drying time be 10~12h, dried reed powder, organically-modified hydrotalcite, ethyl acetate mixing quality Than for 1 ︰, 3 ︰ 10, high speed dispersor rotating speed is 2000~2500r/min, the high speed dispersion time is 10~15min.
Step(4)Temperature is 120~130 DEG C after the heat temperature raising, and preheating time is 5~7min, and rubber mixing machine is set Temperature is 160~200 DEG C.
Step(5)The ethylene contents of the ethylene-vinyl acetate copolymer are 60~65%, control adding for mixer Work temperature is 140~160 DEG C, and head rotating speed is 60~80r/min, and mixing time is 20~25min, controls the curing temperature to be 120~150 DEG C, sulfide stress is 15~18MPa, and vulcanization time is 15~20min.
The beneficial effects of the invention are as follows:
(1)The present invention, which mixes magnalium hydrotalcite with ethanol water, to be disperseed to obtain hydrotacite suspension, with single dodecyl phosphorus Sour methyl esters salt heats reaction in acid condition with hydrotacite suspension, through being filtered by vacuum, being dried to obtain organically-modified hydrotalcite, Reed powder, organically-modified hydrotalcite, ethyl acetate are mixed, it, will through high speed dispersion, the isolated lifeless thing fiber of vacuum filtration High density polyethylene (HDPE) masterbatch pellet is put into melting in rubber mixing machine, mixes lifeless thing fiber, obtains rubber compound, rubber compound is transferred to close Mill, mixes ethylene-vinyl acetate copolymer, and extruded, die-filling, vulcanization, the demoulding obtain high-strength halogen-free fire retardant polyolefin Material, theoretical according to wooden powder warm-pressing formation, the present invention melts lifeless thing fiber incorporation polyethylene at 160~200 DEG C of temperature Body, lignin reach glassy state, soften and generate flowing under high pressure, lignin has very strong adhesive power, absorption at this time In fiber surface and hole, polyethylene is pressed closely, enhances the interface binding power between wood fibre and polyethylene, wooden fibre The tensile property of polythene material can longitudinally improved by tieing up, and in the shock loading of radially reinforced polythene material, improve stress punching Hit intensity, so that the mechanical property of polyolefine material is improved;
(2)Hydrotalcite grain size is smaller in the present invention, can reach nano-dispersion in the polymer, and resulting materials are really a kind of water Talcum-Polyethylene Nanocomposites, after onodoidecyl phosphonic acid methyl esters salt is modified magnalium hydrotalcite, onodoidecyl phosphonic acid Methyl esters salt can substitute the carbanion between magnalium hydrotalcite intercalation, make the hydrophobic immersion oil of magnalium hydrotalcite intercalation, and make between intercalation Away from increase, be conducive to polyethylene macromolecular chain insertion intercalation, form compact composite material, in combustion, make magnesium Aluminum hydrotalcite can lose interlayer hydrone and interlayer anion, it also occur that decarboxylation reaction, these processes will all absorb a large amount of Heat and dilution oxygen concentration, promote polymer into charcoal, so as to play the role of protecting polymer and air-isolation, mix The wood fibre entered can be expanded in burning in the condition of high temperature, form carbon net, and carbon yield rises, and exhaust smoke level declines, so as to carry High polyolefine material flame retardant property, has a extensive future.
Specific embodiment
The ethanol water that 600~700mL mass fractions are 40% is added in three-necked flask, three-necked flask is shifted Into water-bath, after being heated to 70~80 DEG C, 30~35g magnalium hydrotalcites are added in into three-necked flask, starts magnetic force and stirs Device is mixed, 1~2h is stirred with the rotating speed of 350~400r/min, obtains finely dispersed hydrotacite suspension;By 70~80g Onodoidecyl phosphonic acid methyl esters potassium is put into above-mentioned hydrotacite suspension, is stirred 5~10min, is 15% salt with mass fraction Acid adjusts hydrotacite suspension pH to 4~5, is heated to 80~90 DEG C, is stirred to react 6~7h, obtains white slurries, will be white Mill base liquid is placed in vacuum filtration machine filter after, the isolated wet white powder of filtrate is removed, by white powder with anhydrous second Alcohol washing is placed in the baking oven that design temperature is 90~100 DEG C, and dry 7~8h obtains organically-modified hydrotalcite;Reed is put Enter in pulverizer 3~4h of crushing, cross 100 mesh sieves and obtain reed powder, reed powder is placed in baking oven, it is heated to 70~ 80 DEG C, dry 10~12h obtains dried reed powder, by dried reed powder, organically-modified hydrotalcite, acetic acid Ethyl ester is mixed for 1 ︰, 3 ︰ 10 in mass ratio, is placed in high speed dispersor, with the rotating speed high speed dispersion 10 of 2000~2500r/min~ 15min obtains dispersed paste;Dispersed paste is placed in vacuum filtration machine and is filtered, the isolated lifeless thing fiber of filtrate is removed, takes 150~170g high density polyethylene (HDPE) masterbatch pellets are put into baking oven, are heated to 120~130 DEG C, after preheating 5~7min, are put Enter melting in the rubber mixing machine that design temperature is 160~200 DEG C, it is fine to mix 60~65g lifeless things after polyethylene master batch completely melting Dimension, obtains rubber compound;Rubber compound is transferred in mixer, the second that 40~50g ethylene contents are 60~65% is mixed to rubber compound Alkene-vinyl acetate co-polymer, controlling the processing temperature of mixer, head rotating speed is 60~80r/min, close for 140~160 DEG C Refine 20~25min after squeeze out into mold, mold is placed in compression molding agent and is vulcanized, control curing temperature be 120~ 150 DEG C, sulfide stress is 15~18MPa, and vulcanizing the demoulding after 15~20min postcoolings to room temperature, to obtain high-strength halogen-free fire-retardant poly- Olefin material.
Example 1
The ethanol water that 600mL mass fractions are 40% is added in three-necked flask, three-necked flask is transferred to water-bath In, after being heated to 70 DEG C, 30g magnalium hydrotalcites are added in into three-necked flask, start magnetic stirring apparatus, with 350r/min's Rotating speed is stirred 1h, obtains finely dispersed hydrotacite suspension;70g onodoidecyl phosphonic acid methyl esters potassium is put into above-mentioned water In talc suspension, 5min is stirred, hydrotacite suspension pH to 4 is adjusted for 15% hydrochloric acid with mass fraction, is heated to 80 DEG C, 6h is stirred to react, obtains white slurries, white slurries are placed in vacuum filtration machine after filtering, removal filtrate separates To wet white powder, white powder with absolute ethyl alcohol is washed and is placed in the baking oven that design temperature is 90 DEG C, dry 7h is obtained To organically-modified hydrotalcite;Reed is put into pulverizer and crushes 3h, 100 mesh sieves is crossed and obtains reed powder, reed powder is put In baking oven, 70 DEG C are heated to, dry 10h obtains dried reed powder, by dried reed powder, organic Modified hydrotalcite, ethyl acetate mix in mass ratio for 1 ︰, 3 ︰ 10, are placed in high speed dispersor, with the rotating speed of 2000r/min at a high speed Scattered 10min, obtains dispersed paste;Dispersed paste is placed in vacuum filtration machine and is filtered, the isolated lifeless thing of removal filtrate is fine Dimension, takes 150g high density polyethylene (HDPE) masterbatch pellets to be put into baking oven, is heated to 120 DEG C, after preheating 5min, is put into setting temperature Melting in the rubber mixing machine for 160 DEG C is spent, 60g lifeless thing fibers is mixed after polyethylene master batch completely melting, obtains rubber compound;It will be mixed Refining glue is transferred in mixer, the ethylene-vinyl acetate copolymer for being 60% to rubber compound incorporation 40g ethylene contents, and control is close The processing temperature of mill is 140 DEG C, and head rotating speed is 60r/min, squeezes out into mold, mold is placed on flat after mixing 20min Vulcanized on plate vulcanizing agent, control curing temperature as 120 DEG C, sulfide stress 15MPa, vulcanization 15min postcoolings to room temperature The demoulding obtains high-strength halogen-free flame retardant polyolefine material afterwards.
Example 2
The ethanol water that 650mL mass fractions are 40% is added in three-necked flask, three-necked flask is transferred to water-bath In, after being heated to 75 DEG C, 32g magnalium hydrotalcites are added in into three-necked flask, start magnetic stirring apparatus, with 375r/min's Rotating speed is stirred 1.5h, obtains finely dispersed hydrotacite suspension;75g onodoidecyl phosphonic acid methyl esters potassium is put into above-mentioned In hydrotacite suspension, 7min is stirred, hydrotacite suspension pH to 4, heat temperature raising are adjusted for 15% hydrochloric acid with mass fraction To 85 DEG C, 6.5h is stirred to react, obtains white slurries, white slurries are placed in vacuum filtration machine after filtering, removal filtrate point From wet white powder is obtained, white powder with absolute ethyl alcohol is washed and is placed in the baking oven that design temperature is 95 DEG C, it is dry 7.8h obtains organically-modified hydrotalcite;Reed is put into pulverizer and crushes 3.5h, 100 mesh sieves is crossed and obtains reed powder, by reed Reed powder is placed in baking oven, is heated to 75 DEG C, and dry 11h obtains dried reed powder, by dried reed powder Last, organically-modified hydrotalcite, ethyl acetate mix in mass ratio for 1 ︰, 3 ︰ 10, are placed in high speed dispersor, with turning for 2200r/min Fast high speed dispersion 12min, obtains dispersed paste;Dispersed paste is placed in vacuum filtration machine and is filtered, removal filtrate is isolated Lifeless thing fiber takes 160g high density polyethylene (HDPE) masterbatch pellets to be put into baking oven, is heated to 125 DEG C, after preheating 6min, is put into Melting in the rubber mixing machine that design temperature is 180 DEG C mixes 62g lifeless thing fibers after polyethylene master batch completely melting, is kneaded Glue;Rubber compound is transferred in mixer, the ethylene-vinyl acetate for being 62% to rubber compound incorporation 45g ethylene contents is copolymerized Object, controlling the processing temperature of mixer, head rotating speed is 70r/min, is squeezed out after mixing 22min into mold, by mould for 150 DEG C Tool, which is placed in compression molding agent, to be vulcanized, and controls curing temperature as 135 DEG C, sulfide stress 17MPa, cold after vulcanization 17min But high-strength halogen-free flame retardant polyolefine material is obtained to the demoulding after room temperature.
Example 3
The ethanol water that 700mL mass fractions are 40% is added in three-necked flask, three-necked flask is transferred to water-bath In, after being heated to 80 DEG C, 35g magnalium hydrotalcites are added in into three-necked flask, start magnetic stirring apparatus, with 400r/min's Rotating speed is stirred 2h, obtains finely dispersed hydrotacite suspension;80g onodoidecyl phosphonic acid methyl esters potassium is put into above-mentioned water In talc suspension, 10min is stirred, hydrotacite suspension pH to 5, heat temperature raising are adjusted for 15% hydrochloric acid with mass fraction To 90 DEG C, 7h is stirred to react, obtains white slurries, white slurries are placed in vacuum filtration machine after filtering, removal filtrate separation Wet white powder is obtained, white powder with absolute ethyl alcohol is washed and is placed in the baking oven that design temperature is 100 DEG C, it is dry 8h obtains organically-modified hydrotalcite;Reed is put into pulverizer and crushes 4h, 100 mesh sieves is crossed and obtains reed powder, by reed powder End is placed in baking oven, is heated to 80 DEG C, and dry 12h obtains dried reed powder, by dried reed powder, Organically-modified hydrotalcite, ethyl acetate mix in mass ratio for 1 ︰, 3 ︰ 10, high speed dispersor are placed in, with the rotating speed of 2500r/min High speed dispersion 15min, obtains dispersed paste;Dispersed paste is placed in vacuum filtration machine and is filtered, removes the isolated wood of filtrate Mineral wool takes 170g high density polyethylene (HDPE) masterbatch pellets to be put into baking oven, is heated to 130 DEG C, after preheating 7min, is put into and sets Melting in the rubber mixing machine that constant temperature degree is 200 DEG C mixes 65g lifeless thing fibers after polyethylene master batch completely melting, obtains rubber compound; Rubber compound is transferred in mixer, the ethylene-vinyl acetate copolymer for being 65% to rubber compound incorporation 50g ethylene contents, control The processing temperature of mixer processed is 160 DEG C, and head rotating speed is 80r/min, is squeezed out after mixing 25min into mold, mold is put Vulcanized in compression molding agent, control curing temperature as 150 DEG C, sulfide stress 18MPa, vulcanization 20min postcoolings are extremely The demoulding obtains high-strength halogen-free flame retardant polyolefine material after room temperature.
Comparative example
With the high-strength halogen-free flame retardant polyolefine material of Tianjin company production as a comparison case to high intensity produced by the present invention High-strength halogen-free flame retardant polyolefine material in halogen-free anti-flaming polyolefin material and comparative example carries out performance detection, and testing result is such as Shown in table 1:
1st, test method:
Tensile strength test is detected by the standard of GB/T1040;
Impact strength test is detected by the standard of GB/T1843;
Bending strength test is detected by the standard of GB/T9341;
Bending modulus test is detected by the standard of GB/T9341;
Oxygen index (OI) test is detected using oxygen index (OI) tester.
Table 1
High-strength halogen-free flame retardant polyolefine material intensity produced by the present invention is high according to above-mentioned middle data, and flame retardant property is good, It has broad application prospects.

Claims (6)

1. a kind of preparation method of high-strength halogen-free fire retardant polyolefin material, it is characterised in that specifically preparation process is:
(1)600~700mL ethanol waters are added in three-necked flask, three-necked flask is transferred in water-bath, heating rises Temperature adds in 30~35g magnalium hydrotalcites into three-necked flask, starts magnetic stirring apparatus, is stirred, obtains finely dispersed water Talc suspension;
(2)70~80g onodoidecyl phosphonic acid methyl esters potassium is put into above-mentioned hydrotacite suspension, is stirred, with hydrochloric acid tune Water-saving talc suspension pH, heat temperature raising are stirred to react, and obtain white slurries, and white slurries are placed in vacuum filtration machine and are taken out After filter, the isolated wet white powder of filtrate is removed, white powder with absolute ethyl alcohol is washed and is placed in baking oven, it is dry, Obtain organically-modified hydrotalcite;
(3)Reed is put into pulverizer and is crushed, sieving obtains reed powder, reed powder is placed in baking oven, heat temperature raising, It is dry, dried reed powder is obtained, dried reed powder, organically-modified hydrotalcite, ethyl acetate are mixed, are placed in High speed dispersor, high speed dispersion obtain dispersed paste;
(4)Dispersed paste is placed in vacuum filtration machine and is filtered, the isolated lifeless thing fiber of filtrate is removed, takes 150~170g high Density polyethylene masterbatch pellet is put into baking oven, heat temperature raising, after preheating, is put into melting in rubber mixing machine, is treated that polyethylene master batch is complete 60~65g lifeless thing fibers are mixed after full-fusing, obtain rubber compound;
(5)Rubber compound is transferred in mixer, 40~50g ethylene-vinyl acetate copolymers are mixed to rubber compound, after mixing It squeezes out into mold, mold is placed in compression molding agent and is vulcanized, demoulded after vulcanization postcooling to room temperature and obtain high intensity Halogen-free anti-flaming polyolefin material.
2. a kind of preparation method of high-strength halogen-free fire retardant polyolefin material according to claim 1, it is characterised in that:Step (1)The mass fraction of the ethanol water is 40%, is 70~80 DEG C to temperature after water-bath heat temperature raising, magnetic agitation Device rotating speed is 350~400r/min, is stirred the time as 1~2h.
3. a kind of preparation method of high-strength halogen-free fire retardant polyolefin material according to claim 1, it is characterised in that:Step (2)Described is stirred the time as 5~10min, and the mass fraction of hydrochloric acid is 15%, and it is 4 that hydrochloric acid, which adjusts hydrotacite suspension pH, ~5, temperature is 80~90 DEG C after heat temperature raising, is stirred to react the time as 6~7h, and baking oven design temperature is 90~100 DEG C, dry Time is 7~8h.
4. a kind of preparation method of high-strength halogen-free fire retardant polyolefin material according to claim 1, it is characterised in that:Step (3)The grinding time is 3~4h, and specification of sieving is 100 mesh, is 70~80 DEG C to temperature after baking oven heat temperature raising, does The dry time is 10~12h, and dried reed powder, organically-modified hydrotalcite, the mass ratio of ethyl acetate mixing are 1 ︰, 3 ︰ 10, High speed dispersor rotating speed is 2000~2500r/min, and the high speed dispersion time is 10~15min.
5. a kind of preparation method of high-strength halogen-free fire retardant polyolefin material according to claim 1, it is characterised in that:Step (4)Temperature is 120~130 DEG C after the heat temperature raising, and preheating time is 5~7min, rubber mixing machine design temperature for 160~ 200℃。
6. a kind of preparation method of high-strength halogen-free fire retardant polyolefin material according to claim 1, it is characterised in that:Step (5)The ethylene contents of the ethylene-vinyl acetate copolymer are 60~65%, control the processing temperature of mixer for 140~ 160 DEG C, head rotating speed is 60~80r/min, and mixing time is 20~25min, controls curing temperature as 120~150 DEG C, vulcanization Pressure is 15~18MPa, and vulcanization time is 15~20min.
CN201711246676.9A 2017-12-01 2017-12-01 A kind of preparation method of high-strength halogen-free flame retardant polyolefine material Pending CN108047527A (en)

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111100359A (en) * 2019-12-20 2020-05-05 周璇 Preparation method of high-flame-retardant insulated wire and cable
CN112812421A (en) * 2021-02-02 2021-05-18 浙江中聚材料有限公司 Modified polyolefin compound and preparation process and application thereof
CN112812421B (en) * 2021-02-02 2022-10-21 浙江中聚材料有限公司 Modified polyolefin compound and preparation process and application thereof

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