CN106432869A - Environment-friendly flame-retardant PE material and preparation method thereof - Google Patents
Environment-friendly flame-retardant PE material and preparation method thereof Download PDFInfo
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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
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions 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
- C08L23/04—Homopolymers or copolymers of ethene
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/25—Component parts, details or accessories; Auxiliary operations
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C2948/00—Indexing scheme relating to extrusion moulding
- B29C2948/92—Measuring, controlling or regulating
- B29C2948/92504—Controlled parameter
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C2948/00—Indexing scheme relating to extrusion moulding
- B29C2948/92—Measuring, controlling or regulating
- B29C2948/92819—Location or phase of control
- B29C2948/92857—Extrusion unit
- B29C2948/92876—Feeding, melting, plasticising or pumping zones, e.g. the melt itself
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C2948/00—Indexing scheme relating to extrusion moulding
- B29C2948/92—Measuring, controlling or regulating
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- C08L2201/02—Flame or fire retardant/resistant
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- C08L2203/14—Applications used for foams
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Abstract
The invention discloses an environment-friendly flame-retardant PE material and a preparation method thereof. High density polyethylene, hydroxyethyl acrylate, triphenyl phosphite and polyvinylidene fluoride are used as main ingredients, dicumyl peroxide, maleic anhydride, sucrose acetoisobutyrate, isophorone diisocyanate, attapulgite, expanded perlite, hydrated zinc borate, vanadium diboride, aluminum titanate, bamboo charcoal powder, dithio-salicylic acid, an auxiliary agent and a silane coupler are added, processes of ball-milling, ultrasonic treatment, calcining, hot blending, foaming, curing, extruding and the like are carried out, so that the prepared environment-friendly flame-retardant PE material has excellent flame retardance, is environment-friendly, and meanwhile is high in strength, and application level of the material is increased.
Description
Technical field
The present invention relates to environment-friendly materials technical field, particularly to a kind of environmental-protection flame-retardant PE material and preparation method thereof.
Background technology
PE is polyethylene, is a kind of aggregated prepared thermoplastic resin of ethene.Industrially, also include ethene with a small amount of
The copolymer of alpha-olefin.Polyethylene odorless, nontoxic, feel ceraceous, there is excellent resistance to low temperature.Meanwhile, polyethylene have excellent
Different chemical stability, the various chemistry such as resistance to hydrochloric acid, hydrofluoric acid, phosphoric acid, formic acid, amine, NaOH, potassium hydroxide under room temperature
Material corrosiveness.Common solvent is not dissolved in, water imbibition is little, and electrical insulating property is excellent under normal temperature.Polyethylene can be made into various
Application material, the especially main material of packaging material.It has advantages below as packaging material：Polyethylene resists multiple organic
Solvent, anti-multiple acid and alkali corrosions, and moisture absorption is little, is not necessary to fully be dried.Polyethylene can be divided into high density according to the difference of density
Polyethylene, medium density polyethylene and low density polyethylene (LDPE).Wherein, high density polyethylene (HDPE) has rigidity, hardness and mechanical strength greatly,
Low-temperature impact resistance is good, and anti-stress cracking is good, and wearability is good, ageing-resistant characteristic.High-density polyethylene resin price is low
Honest and clean, processing characteristics is excellent, and physics and chemical property are all good, has good barrier to water polar solvent simultaneously, therefore high
Density polyethylene is more widely used in packaging material compared to medium density polyethylene and low density polyethylene (LDPE).
But as packaging material, polyethylene has the shortcomings that to meet fire inflammable, and to need it to have fire-retardant for many application scenarios
Property.The flame-retardant system of traditional fire-retardant polyethylene material is using bromine antimony flame-retardant system, affects the mankind however as environmental pollution
The problem of health has become the focus of global concern, and bromine antimony flame-retardant system is providing the environment danger brought while flame-retarding characteristic
Evil significantly limit the application of polythene material, particularly must so developing a kind of environmental-protection flame-retardant polythene material and just seeming
Will.
Content of the invention
For solving above-mentioned technical problem, the present invention provides a kind of environmental-protection flame-retardant PE material, by using specific raw material
It is combined, coordinates specific production technology, the environmental-protection flame-retardant PE material obtaining possesses excellent anti-flammability, and to environment friend
Good, intensity is high simultaneously, disclosure satisfy that the requirement of industry, has preferable application prospect.
The purpose of the present invention can be achieved through the following technical solutions：
A kind of environmental-protection flame-retardant PE material, is prepared by the raw materials in：High density polyethylene (HDPE) 65-75 part, acrylic acid hydroxyl
Ethyl ester 50-60 part, triphenyl phosphite 35-45 part, Kynoar 30-40 part, cumyl peroxide 15-20 part, Malaysia
Acid anhydrides 12-18 part, Sucrose acetoisobutyrate 10-15 part, IPDI 8-12 part, attapulgite 6-8 part, swollen
Swollen perlite 5-7 part, hydration zinc borate 4-6 part, vanadium diboride 4-6 part, aluminium titanates 2-4 part, bamboo charcoal powder 2-4 part, two thio water
Poplar acid 1-3 part, auxiliary agent 3-5 part, silane coupler 3-5 part.
Preferably, described auxiliary agent by etc. the polyisobutene of quality and carbon tetrachloride proportioning form.
Preferably, described silane coupler is selected from Silane coupling agent KH550, silane coupler KH792, silane coupler
Any one in A187.
The preparation method of described environmental-protection flame-retardant PE material, comprises the following steps：
（1）By attapulgite, expanded perlite, hydration zinc borate, vanadium diboride, aluminium titanates, bamboo charcoal powder mixing, put into ball grinder
In, with 200 revs/min of rotating speed, in ball mill, ball milling 90 minutes, obtain powder mixture；
（2）The powder of cumyl peroxide, Sucrose acetoisobutyrate, IPDI and step 1 is mixed
The concentration that compound is added to 30 times of its weight jointly is in 75% ethanol solution, ultrasonic disperse 25-35 minute, is subsequently added horse
Come acid anhydrides, magnetic agitation 10 minutes, suction filtration, the product after suction filtration be dried 4 hours at 135-145 DEG C, send in Muffle furnace,
Calcine 3 hours at 660-680 DEG C, cooling, obtain preconditioned mixture；
（3）By high density polyethylene (HDPE), hydroxy-ethyl acrylate, triphenyl phosphite, Kynoar, dithio-salicylic acid, auxiliary agent,
The preconditioned mixture of silane coupler and step 2 adds in the mixed machine of heat, carries out mixed at high speed with 950 revs/min of speed, mixing
Time is 20 minutes, subsequently feeds the mixture into reactor and stirs 1.5 hours, subsequently with dilute hydrochloric acid solution by pH in 85 DEG C
Adjust to 5.0-5.5, then at 90 DEG C of stirring 5-7 hours, then pH is adjusted to neutrality and filters, obtain modified compound；
(4) by the blank that foams to obtain in the modified compound injection mould of step 3；Then blank is sent in tunnel type baking oven, point
Duan Shengwen：At 70-80 DEG C, react 18-20 minute；Again at 90-100 DEG C, react 12-15 minute；Last ripe at 120 DEG C
Change 2-3 hour；
(5) blank after curing in step 4 is sent into double screw extruder to melt extrude, the product of extrusion is cold through circulator bath
But and pelletizing, obtain finished product.
Preferably, described step（2）In, the temperature of ultrasonic disperse is 60 DEG C, and ultrasonic power is 700W.
Preferably, described step（5）In, the temperature control of double screw extruder is 125-135 DEG C of feeding section, melt zone
175-185 DEG C, 230-240 DEG C of homogenizing zone, 185-195 DEG C of head, 195-205 DEG C of die orifice, screw speed is 45-55 rev/min.
Compared with prior art, its advantage is the present invention：
（1）The environmental-protection flame-retardant PE material of the present invention with high density polyethylene (HDPE), hydroxy-ethyl acrylate, triphenyl phosphite, poly- partially
PVF is main component, by adding cumyl peroxide, maleic anhydride, Sucrose acetoisobutyrate, isophorone two
Isocyanates, attapulgite, expanded perlite, hydration zinc borate, vanadium diboride, aluminium titanates, bamboo charcoal powder, dithio-salicylic acid,
Auxiliary agent, silane coupler, are aided with the techniques such as ball milling, ultrasonic, calcining, heat is mixed, foaming, curing, extrusion so that the ring that is prepared from
Guarantor's type fire-retardant PE material possesses excellent anti-flammability, and environmentally friendly, and intensity is high simultaneously, improves materials application level.
（2）The environmental-protection flame-retardant PE material feedstock of the present invention is cheap, process is simple, is suitable to heavy industrialization and uses, real
Strong with property.
Specific embodiment
With reference to specific embodiment, the technical scheme of invention is described in detail.
Embodiment 1
Accurately weigh 65 parts of high density polyethylene (HDPE), 50 parts of hydroxy-ethyl acrylate, 35 parts of triphenyl phosphite, gather according to parts by weight
30 parts of vinylidene, 15 parts of cumyl peroxide, 12 parts of maleic anhydride, 10 parts of Sucrose acetoisobutyrate, isophorone two
8 parts of isocyanates, 6 parts of attapulgite, 5 parts of expanded perlite, 4 parts of hydration zinc borate, 4 parts of vanadium diboride, 2 parts of aluminium titanates, bamboo
2 parts of powdered carbon, 1 part of dithio-salicylic acid, 3 parts of auxiliary agent, 3 parts of Silane coupling agent KH550.Described auxiliary agent by etc. quality poly- isobutyl
Alkene and carbon tetrachloride proportioning form.
（1）By attapulgite, expanded perlite, hydration zinc borate, vanadium diboride, aluminium titanates, bamboo charcoal powder mixing, put into ball
In grinding jar, with 200 revs/min of rotating speed, in ball mill, ball milling 90 minutes, obtain powder mixture；
（2）The powder of cumyl peroxide, Sucrose acetoisobutyrate, IPDI and step 1 is mixed
The concentration that compound is added to 30 times of its weight jointly is in 75% ethanol solution, ultrasonic disperse 25 minutes, the temperature of ultrasonic disperse
For 60 DEG C, ultrasonic power is 700W, is subsequently added maleic anhydride, magnetic agitation 10 minutes, suction filtration, the product after suction filtration is existed
It is dried 4 hours at 135 DEG C, send in Muffle furnace, calcine 3 hours at 660 DEG C, cooling, obtain preconditioned mixture；
（3）By high density polyethylene (HDPE), hydroxy-ethyl acrylate, triphenyl phosphite, Kynoar, dithio-salicylic acid, auxiliary agent,
The preconditioned mixture of Silane coupling agent KH550 and step 2 adds in the mixed machine of heat, is carried out mixed at a high speed with 950 revs/min of speed
Close, incorporation time is 20 minutes, subsequently feed the mixture into reactor and stir 1.5 hours in 85 DEG C, subsequently use watery hydrochloric acid molten
Liquid adjusts pH to 5.0, stirs 5 hours then at 90 DEG C, then pH is adjusted to neutrality and filters, obtain modified compound；
(4) by the blank that foams to obtain in the modified compound injection mould of step 3；Then blank is sent in tunnel type baking oven, point
Duan Shengwen：At 70 DEG C, react 18 minutes；Again at 90 DEG C, react 12 minutes；Last curing 2 hours at 120 DEG C；
(5) blank after curing in step 4 is sent into double screw extruder to melt extrude, the temperature control of double screw extruder is
125 DEG C of feeding section, 175 DEG C of melt zone, 230 DEG C of homogenizing zone, 185 DEG C of head, 195 DEG C of die orifice, screw speed is 45 revs/min, squeezes
The product going out, through circulator bath cooling and pelletizing, obtains finished product
The performance test results of prepared environmental-protection flame-retardant PE material are as shown in table 1.
Embodiment 2
Accurately weigh 70 parts of high density polyethylene (HDPE), 55 parts of hydroxy-ethyl acrylate, 40 parts of triphenyl phosphite, gather according to parts by weight
35 parts of vinylidene, 17 parts of cumyl peroxide, 15 parts of maleic anhydride, 12 parts of Sucrose acetoisobutyrate, isophorone two
10 parts of isocyanates, 7 parts of attapulgite, 6 parts of expanded perlite, 5 parts of hydration zinc borate, 5 parts of vanadium diboride, 3 parts of aluminium titanates, bamboo
3 parts of powdered carbon, 2 parts of dithio-salicylic acid, 4 parts of auxiliary agent, 4 parts of silane coupler KH792.Described auxiliary agent by etc. quality poly- isobutyl
Alkene and carbon tetrachloride proportioning form.
（1）By attapulgite, expanded perlite, hydration zinc borate, vanadium diboride, aluminium titanates, bamboo charcoal powder mixing, put into ball
In grinding jar, with 200 revs/min of rotating speed, in ball mill, ball milling 90 minutes, obtain powder mixture；
（2）The powder of cumyl peroxide, Sucrose acetoisobutyrate, IPDI and step 1 is mixed
The concentration that compound is added to 30 times of its weight jointly is in 75% ethanol solution, ultrasonic disperse 30 minutes, the temperature of ultrasonic disperse
For 60 DEG C, ultrasonic power is 700W, is subsequently added maleic anhydride, magnetic agitation 10 minutes, suction filtration, the product after suction filtration is existed
It is dried 4 hours at 140 DEG C, send in Muffle furnace, calcine 3 hours at 670 DEG C, cooling, obtain preconditioned mixture；
（3）By high density polyethylene (HDPE), hydroxy-ethyl acrylate, triphenyl phosphite, Kynoar, dithio-salicylic acid, auxiliary agent,
The preconditioned mixture of silane coupler KH792 and step 2 adds in the mixed machine of heat, is carried out mixed at a high speed with 950 revs/min of speed
Close, incorporation time is 20 minutes, subsequently feed the mixture into reactor and stir 1.5 hours in 85 DEG C, subsequently use watery hydrochloric acid molten
Liquid adjusts pH to 5.3, stirs 6 hours then at 90 DEG C, then pH is adjusted to neutrality and filters, obtain modified compound；
(4) by the blank that foams to obtain in the modified compound injection mould of step 3；Then blank is sent in tunnel type baking oven, point
Duan Shengwen：At 75 DEG C, react 19 minutes；Again at 95 DEG C, react 14 minutes；Last curing 2.5 hours at 120 DEG C；
(5) blank after curing in step 4 is sent into double screw extruder to melt extrude, the temperature control of double screw extruder is
130 DEG C of feeding section, 180 DEG C of melt zone, 235 DEG C of homogenizing zone, 190 DEG C of head, 200 DEG C of die orifice, screw speed is 50 revs/min, squeezes
The product going out, through circulator bath cooling and pelletizing, obtains finished product
The performance test results of prepared environmental-protection flame-retardant PE material are as shown in table 1.
Embodiment 3
Accurately weigh 75 parts of high density polyethylene (HDPE), 60 parts of hydroxy-ethyl acrylate, 45 parts of triphenyl phosphite, gather according to parts by weight
40 parts of vinylidene, 20 parts of cumyl peroxide, 18 parts of maleic anhydride, 15 parts of Sucrose acetoisobutyrate, isophorone two
12 parts of isocyanates, 8 parts of attapulgite, 7 parts of expanded perlite, 6 parts of hydration zinc borate, 6 parts of vanadium diboride, 4 parts of aluminium titanates, bamboo
4 parts of powdered carbon, 3 parts of dithio-salicylic acid, 5 parts of auxiliary agent, 187 5 parts of silane coupling A.Described auxiliary agent by etc. quality polyisobutene
Form with carbon tetrachloride proportioning.
（1）By attapulgite, expanded perlite, hydration zinc borate, vanadium diboride, aluminium titanates, bamboo charcoal powder mixing, put into ball
In grinding jar, with 200 revs/min of rotating speed, in ball mill, ball milling 90 minutes, obtain powder mixture；
（2）The powder of cumyl peroxide, Sucrose acetoisobutyrate, IPDI and step 1 is mixed
The concentration that compound is added to 30 times of its weight jointly is in 75% ethanol solution, ultrasonic disperse 35 minutes, the temperature of ultrasonic disperse
For 60 DEG C, ultrasonic power is 700W, is subsequently added maleic anhydride, magnetic agitation 10 minutes, suction filtration, the product after suction filtration is existed
It is dried 4 hours at 145 DEG C, send in Muffle furnace, calcine 3 hours at 680 DEG C, cooling, obtain preconditioned mixture；
（3）By high density polyethylene (HDPE), hydroxy-ethyl acrylate, triphenyl phosphite, Kynoar, dithio-salicylic acid, auxiliary agent,
The preconditioned mixture of silane coupling A 187 and step 2 adds in the mixed machine of heat, carries out mixed at high speed with 950 revs/min of speed,
Incorporation time is 20 minutes, subsequently feeds the mixture into reactor and stirs 1.5 hours in 85 DEG C, subsequently will with dilute hydrochloric acid solution
PH is adjusted to 5.5, stirs 7 hours then at 90 DEG C, then pH is adjusted to neutrality and filters, obtain modified compound；
(4) by the blank that foams to obtain in the modified compound injection mould of step 3；Then blank is sent in tunnel type baking oven, point
Duan Shengwen：At 80 DEG C, react 20 minutes；Again at 100 DEG C, react 15 minutes；Last curing 3 hours at 120 DEG C；
(5) blank after curing in step 4 is sent into double screw extruder to melt extrude, the temperature control of double screw extruder is
135 DEG C of feeding section, 185 DEG C of melt zone, 240 DEG C of homogenizing zone, 195 DEG C of head, 205 DEG C of die orifice, screw speed is 55 revs/min, squeezes
The product going out, through circulator bath cooling and pelletizing, obtains finished product
The performance test results of prepared environmental-protection flame-retardant PE material are as shown in table 1.
Embodiment 4
Accurately weigh 65 parts of high density polyethylene (HDPE), 60 parts of hydroxy-ethyl acrylate, 35 parts of triphenyl phosphite, gather according to parts by weight
40 parts of vinylidene, 15 parts of cumyl peroxide, 18 parts of maleic anhydride, 10 parts of Sucrose acetoisobutyrate, isophorone two
12 parts of isocyanates, 6 parts of attapulgite, 7 parts of expanded perlite, 4 parts of hydration zinc borate, 6 parts of vanadium diboride, 2 parts of aluminium titanates, bamboo
4 parts of powdered carbon, 1 part of dithio-salicylic acid, 5 parts of auxiliary agent, 3 parts of silane coupler KH792.Described auxiliary agent by etc. quality poly- isobutyl
Alkene and carbon tetrachloride proportioning form.
（1）By attapulgite, expanded perlite, hydration zinc borate, vanadium diboride, aluminium titanates, bamboo charcoal powder mixing, put into ball
In grinding jar, with 200 revs/min of rotating speed, in ball mill, ball milling 90 minutes, obtain powder mixture；
（2）The powder of cumyl peroxide, Sucrose acetoisobutyrate, IPDI and step 1 is mixed
The concentration that compound is added to 30 times of its weight jointly is in 75% ethanol solution, ultrasonic disperse 35 minutes, the temperature of ultrasonic disperse
For 60 DEG C, ultrasonic power is 700W, is subsequently added maleic anhydride, magnetic agitation 10 minutes, suction filtration, the product after suction filtration is existed
It is dried 4 hours at 135 DEG C, send in Muffle furnace, calcine 3 hours at 680 DEG C, cooling, obtain preconditioned mixture；
（3）By high density polyethylene (HDPE), hydroxy-ethyl acrylate, triphenyl phosphite, Kynoar, dithio-salicylic acid, auxiliary agent,
The preconditioned mixture of silane coupler KH792 and step 2 adds in the mixed machine of heat, is carried out mixed at a high speed with 950 revs/min of speed
Close, incorporation time is 20 minutes, subsequently feed the mixture into reactor and stir 1.5 hours in 85 DEG C, subsequently use watery hydrochloric acid molten
Liquid adjusts pH to 5.0, stirs 7 hours then at 90 DEG C, then pH is adjusted to neutrality and filters, obtain modified compound；
(4) by the blank that foams to obtain in the modified compound injection mould of step 3；Then blank is sent in tunnel type baking oven, point
Duan Shengwen：At 70 DEG C, react 20 minutes；Again at 90 DEG C, react 15 minutes；Last curing 2 hours at 120 DEG C；
(5) blank after curing in step 4 is sent into double screw extruder to melt extrude, the temperature control of double screw extruder is
135 DEG C of feeding section, 175 DEG C of melt zone, 240 DEG C of homogenizing zone, 185 DEG C of head, 205 DEG C of die orifice, screw speed is 45 revs/min, squeezes
The product going out, through circulator bath cooling and pelletizing, obtains finished product
The performance test results of prepared environmental-protection flame-retardant PE material are as shown in table 1.
Comparative example 1
Accurately weigh 70 parts of high density polyethylene (HDPE), 55 parts of hydroxy-ethyl acrylate, 40 parts of triphenyl phosphite, gather according to parts by weight
35 parts of vinylidene, 17 parts of cumyl peroxide, 15 parts of maleic anhydride, 12 parts of Sucrose acetoisobutyrate, attapulgite 7
Part, 6 parts of expanded perlite, 5 parts of hydration zinc borate, 5 parts of vanadium diboride, 3 parts of aluminium titanates, 3 parts of bamboo charcoal powder, 4 parts of auxiliary agent, silane are even
4 parts of agent KH792 of connection.Described auxiliary agent by etc. the polyisobutene of quality and carbon tetrachloride proportioning form.
（1）By attapulgite, expanded perlite, hydration zinc borate, vanadium diboride, aluminium titanates, bamboo charcoal powder mixing, put into ball
In grinding jar, with 200 revs/min of rotating speed, in ball mill, ball milling 90 minutes, obtain powder mixture；
（2）The powder mixture of cumyl peroxide, Sucrose acetoisobutyrate and step 1 is added to its weight jointly
30 times of concentration is in 75% ethanol solution, ultrasonic disperse 30 minutes, and the temperature of ultrasonic disperse is 60 DEG C, and ultrasonic power is
700W, is subsequently added maleic anhydride, magnetic agitation 10 minutes, suction filtration, the product after suction filtration is dried 4 hours at 140 DEG C, send
Enter in Muffle furnace, calcine 3 hours at 670 DEG C, cooling, obtain preconditioned mixture；
（3）By high density polyethylene (HDPE), hydroxy-ethyl acrylate, triphenyl phosphite, Kynoar, auxiliary agent, silane coupler
The preconditioned mixture of KH792 and step 2 adds in the mixed machine of heat, carries out mixed at high speed, incorporation time with 950 revs/min of speed
For 20 minutes, subsequently feed the mixture into reactor and stir 1.5 hours in 85 DEG C, subsequently with dilute hydrochloric acid solution, pH is adjusted
To 5.3, stir 6 hours then at 90 DEG C, then pH is adjusted to neutrality and filters, obtain modified compound；
(4) by the blank that foams to obtain in the modified compound injection mould of step 3；Then blank is sent in tunnel type baking oven, point
Duan Shengwen：At 75 DEG C, react 19 minutes；Again at 95 DEG C, react 14 minutes；Last curing 2.5 hours at 120 DEG C；
(5) blank after curing in step 4 is sent into double screw extruder to melt extrude, the temperature control of double screw extruder is
130 DEG C of feeding section, 180 DEG C of melt zone, 235 DEG C of homogenizing zone, 190 DEG C of head, 200 DEG C of die orifice, screw speed is 50 revs/min, squeezes
The product going out, through circulator bath cooling and pelletizing, obtains finished product
The performance test results of prepared environmental-protection flame-retardant PE material are as shown in table 1.
Comparative example 2
Accurately weigh 65 parts of high density polyethylene (HDPE), 60 parts of hydroxy-ethyl acrylate, 35 parts of triphenyl phosphite, gather according to parts by weight
40 parts of vinylidene, 15 parts of cumyl peroxide, 18 parts of maleic anhydride, 12 parts of IPDI, attapulgite 6
Part, 7 parts of expanded perlite, 6 parts of vanadium diboride, 2 parts of aluminium titanates, 4 parts of bamboo charcoal powder, 1 part of dithio-salicylic acid, 5 parts of auxiliary agent, silane
3 parts of coupling agent KH792.Described auxiliary agent by etc. the polyisobutene of quality and carbon tetrachloride proportioning form.
（1）Put into attapulgite, expanded perlite, vanadium diboride, aluminium titanates, bamboo charcoal powder mixing in ball grinder, with
200 revs/min of rotating speed, in ball mill, ball milling 90 minutes, obtain powder mixture；
（2）The powder mixture of cumyl peroxide, IPDI and step 1 is added to it jointly heavy
The concentration of 30 times of amount is in 75% ethanol solution, ultrasonic disperse 35 minutes, and the temperature of ultrasonic disperse is 60 DEG C, and ultrasonic power is
700W, is subsequently added maleic anhydride, magnetic agitation 10 minutes, suction filtration, the product after suction filtration is dried 4 hours at 135 DEG C, send
Enter in Muffle furnace, calcine 3 hours at 680 DEG C, cooling, obtain preconditioned mixture；
（3）By high density polyethylene (HDPE), hydroxy-ethyl acrylate, triphenyl phosphite, Kynoar, dithio-salicylic acid, auxiliary agent,
The preconditioned mixture of silane coupler KH792 and step 2 adds in the mixed machine of heat, is carried out mixed at a high speed with 950 revs/min of speed
Close, incorporation time is 20 minutes, subsequently feed the mixture into reactor and stir 1.5 hours in 85 DEG C, subsequently use watery hydrochloric acid molten
Liquid adjusts pH to 5.0, stirs 7 hours then at 90 DEG C, then pH is adjusted to neutrality and filters, obtain modified compound；
(4) by the blank that foams to obtain in the modified compound injection mould of step 3；Then blank is sent in tunnel type baking oven, point
Duan Shengwen：At 70 DEG C, react 20 minutes；Again at 90 DEG C, react 15 minutes；Last curing 2 hours at 120 DEG C；
(5) blank after curing in step 4 is sent into double screw extruder to melt extrude, the temperature control of double screw extruder is
135 DEG C of feeding section, 175 DEG C of melt zone, 240 DEG C of homogenizing zone, 185 DEG C of head, 205 DEG C of die orifice, screw speed is 45 revs/min, squeezes
The product going out, through circulator bath cooling and pelletizing, obtains finished product
The performance test results of prepared environmental-protection flame-retardant PE material are as shown in table 1.
The environmental-protection flame-retardant PE material of embodiment 1-4 and comparative example 1-2 is carried out fire rating test, burning gases respectively
Evaluation, tension test, melt flows measure this several performance tests.
Table 1
| Fire-protection rating UL94 | Combustion generated gas environmental evaluation | Tensile strength（MPa） | Melt flow rate (MFR)（g/10min） | |
| Embodiment 1 | V-0 | No pernicious gas | 30.7 | 2.6 |
| Embodiment 2 | V-0 | No pernicious gas | 32.4 | 2.1 |
| Embodiment 3 | V-0 | No pernicious gas | 31.9 | 2.4 |
| Embodiment 4 | V-0 | No pernicious gas | 31.3 | 2.5 |
| Comparative example 1 | V-1 | No pernicious gas | 24.8 | 3.3 |
| Comparative example 2 | V-1 | No pernicious gas | 23.6 | 3.5 |
The environmental-protection flame-retardant PE material of the present invention is with high density polyethylene (HDPE), hydroxy-ethyl acrylate, triphenyl phosphite, polyvinylidene fluoride
Alkene is main component, by adding cumyl peroxide, maleic anhydride, Sucrose acetoisobutyrate, isophorone two isocyanide
Acid esters, attapulgite, expanded perlite, hydration zinc borate, vanadium diboride, aluminium titanates, bamboo charcoal powder, dithio-salicylic acid, auxiliary agent,
Silane coupler, is aided with the techniques such as ball milling, ultrasonic, calcining, heat is mixed, foaming, curing, extrusion so that the environment-friendly type that is prepared from
Fire-retardant PE material possesses excellent anti-flammability, and environmentally friendly, and intensity is high simultaneously, improves materials application level.The present invention
Environmental-protection flame-retardant PE material feedstock is cheap, process is simple, be suitable to heavy industrialization and use, practical.
The foregoing is only embodiments of the invention, not thereby limit the present invention the scope of the claims, every using this
Equivalent structure or equivalent flow conversion that bright description is made, or directly or indirectly it is used in other related technology necks
Domain, is included within the scope of the present invention.
Claims (6)
1. a kind of environmental-protection flame-retardant PE material it is characterised in that：It is prepared by the raw materials in：High density polyethylene (HDPE) 65-
75 parts, hydroxy-ethyl acrylate 50-60 part, triphenyl phosphite 35-45 part, Kynoar 30-40 part, cumyl peroxide
15-20 part, maleic anhydride 12-18 part, Sucrose acetoisobutyrate 10-15 part, IPDI 8-12 part, concavo-convex
Rod soil 6-8 part, expanded perlite 5-7 part, hydration zinc borate 4-6 part, vanadium diboride 4-6 part, aluminium titanates 2-4 part, bamboo charcoal powder 2-4
Part, dithio-salicylic acid 1-3 part, auxiliary agent 3-5 part, silane coupler 3-5 part.
2. environmental-protection flame-retardant PE material according to claim 1 it is characterised in that：Described auxiliary agent by etc. quality poly- isobutyl
Alkene and carbon tetrachloride proportioning form.
3. environmental-protection flame-retardant PE material according to claim 1 it is characterised in that：It is even that described silane coupler is selected from silane
Any one in connection agent KH550, silane coupler KH792, silane coupling A 187.
4. the preparation method according to the arbitrary described environmental-protection flame-retardant PE material of claim 1-3 is it is characterised in that include following
Step：
（1）By attapulgite, expanded perlite, hydration zinc borate, vanadium diboride, aluminium titanates, bamboo charcoal powder mixing, put into ball grinder
In, with 200 revs/min of rotating speed, in ball mill, ball milling 90 minutes, obtain powder mixture；
（2）The powder of cumyl peroxide, Sucrose acetoisobutyrate, IPDI and step 1 is mixed
The concentration that compound is added to 30 times of its weight jointly is in 75% ethanol solution, ultrasonic disperse 25-35 minute, is subsequently added horse
Come acid anhydrides, magnetic agitation 10 minutes, suction filtration, the product after suction filtration be dried 4 hours at 135-145 DEG C, send in Muffle furnace,
Calcine 3 hours at 660-680 DEG C, cooling, obtain preconditioned mixture；
（3）By high density polyethylene (HDPE), hydroxy-ethyl acrylate, triphenyl phosphite, Kynoar, dithio-salicylic acid, auxiliary agent,
The preconditioned mixture of silane coupler and step 2 adds in the mixed machine of heat, carries out mixed at high speed with 950 revs/min of speed, mixing
Time is 20 minutes, subsequently feeds the mixture into reactor and stirs 1.5 hours, subsequently with dilute hydrochloric acid solution by pH in 85 DEG C
Adjust to 5.0-5.5, then at 90 DEG C of stirring 5-7 hours, then pH is adjusted to neutrality and filters, obtain modified compound；
(4) by the blank that foams to obtain in the modified compound injection mould of step 3；Then blank is sent in tunnel type baking oven, point
Duan Shengwen：At 70-80 DEG C, react 18-20 minute；Again at 90-100 DEG C, react 12-15 minute；Last ripe at 120 DEG C
Change 2-3 hour；
(5) blank after curing in step 4 is sent into double screw extruder to melt extrude, the product of extrusion is cold through circulator bath
But and pelletizing, obtain finished product.
5. the preparation method of environmental-protection flame-retardant PE material according to claim 4 is it is characterised in that described step（2）In,
The temperature of ultrasonic disperse is 60 DEG C, and ultrasonic power is 700W.
6. the preparation method of environmental-protection flame-retardant PE material according to claim 4 is it is characterised in that described step（5）In,
The temperature control of double screw extruder is 125-135 DEG C of feeding section, 175-185 DEG C of melt zone, 230-240 DEG C of homogenizing zone, head
185-195 DEG C, 195-205 DEG C of die orifice, screw speed is 45-55 rev/min.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107868385A (en) * | 2017-12-01 | 2018-04-03 | 周昭金 | The preparation method and applications of anti-flammability environment-friendly materials |
| CN108912370A (en) * | 2018-08-01 | 2018-11-30 | 苏州环亚软管塑业有限公司 | A kind of preparation method of acrylic glass fiber composite hose material |
| CN109181057A (en) * | 2018-08-01 | 2019-01-11 | 苏州环亚软管塑业有限公司 | A kind of preparation method of impact resistance plastic flexible pipe |
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| CN104311968A (en) * | 2014-11-05 | 2015-01-28 | 安徽恒晶电缆集团有限公司 | Modified polyethylene material for aerial cables |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107868385A (en) * | 2017-12-01 | 2018-04-03 | 周昭金 | The preparation method and applications of anti-flammability environment-friendly materials |
| CN108912370A (en) * | 2018-08-01 | 2018-11-30 | 苏州环亚软管塑业有限公司 | A kind of preparation method of acrylic glass fiber composite hose material |
| CN109181057A (en) * | 2018-08-01 | 2019-01-11 | 苏州环亚软管塑业有限公司 | A kind of preparation method of impact resistance plastic flexible pipe |
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