CN106751202A - A kind of mining electrostatic resistance flame retardant PVC and preparation method thereof - Google Patents
A kind of mining electrostatic resistance flame retardant PVC and preparation method thereof Download PDFInfo
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- CN106751202A CN106751202A CN201611183844.XA CN201611183844A CN106751202A CN 106751202 A CN106751202 A CN 106751202A CN 201611183844 A CN201611183844 A CN 201611183844A CN 106751202 A CN106751202 A CN 106751202A
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- graphene oxide
- nano imvite
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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
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F292/00—Macromolecular compounds obtained by polymerising monomers on to inorganic materials
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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
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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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
- C08L2201/00—Properties
- C08L2201/04—Antistatic
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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
- C08L2203/00—Applications
- C08L2203/18—Applications used for pipes
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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
- 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 Kinetics & Catalysis (AREA)
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- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Inorganic Chemistry (AREA)
- Materials Engineering (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a kind of mining electrostatic resistance flame retardant PVC and preparation method thereof, it is made up of the raw material of following weight portion：Polyvinyl chloride 74 88, montmorillonite 32 46, pentaerythrite diphosphate melamine salt 8 16, graphene oxide 18 30, Ethylhexyl stearate 5 10, basic nickel carbonate 37, brominated paraffin 6 11, glycerin zinc 24, magnesium stearate 12, zirconium hydroxide 10 15, chloromethoxy fatty acid methyl ester 12 19, pandermite powder 14 22.The present invention is carried out flame-retardant modified using the organic fire-retardant that basic nickel carbonate, zirconium hydroxide, the inorganic combustion inhibitor compounding pentaerythrite diphosphate melamine salt of pandermite powder composition, brominated paraffin, poly- aminopropyl/phenyl silsesquioxane micro mist, chloromethoxy fatty acid methyl ester are constituted to PVC, the oxygen index (OI) of material can be not only significantly improved, mechanical strength, resistance to ag(e)ing and the weatherability of material can also be improved.
Description
Technical field
The present invention relates to a kind of PVC and preparation method thereof, and in particular to a kind of mining electrostatic resistance flame retardant PVC and
Its preparation method.
Background technology
Montmorillonite is a kind of typical natural clay mineral, with reserves it is high, species is various, cheap, structure etc.
Advantage.Montmorillonite also has good dispersive property, can be extensively using macromolecular material industry as nanometer polymer high score
The additive of sub- material, improves mechanical property, dimensional stability, thermal stability and gas barrier property etc., so as to play increasing
The effect of strength polymer comprehensive physical performance, while improving materiel machining performance, has a extensive future.
Zheng Yuying, Peng Chao are at it《The development of PVC-U/ montmorillonite Nanocomposite Pipes》With montmorillonite as main former in one text
Material, is modified to it by suitable organic intercalation agent and have developed organo montmorillonite, then using the lipophile of polyvinyl chloride, fortune
With intercalation technique by between the PVC solutions organic cheating engaging layer of insertion, montmorillonite layer is set to peel off and with nano-size dispersion in PVC phases
In, the compound of nano lamellar montmorillonite and PVC is realized, there is obtained PVC-U/ montmorillonite Nanocomposite Pipes excellent
Physical and mechanical property.But composite pipe obtained in above-mentioned document has sheet resistance greatly, the shortcoming of antistatic behaviour difference, tubing
Surface will produce electrostatic once friction, and be gathered in tube surfaces, if being applied to coal production operation, just have during static discharge
Can fire hazard and gas explosion, it is impossible to meet the use requirement of mining pipes, limit its range of application.In addition, above-mentioned
The fire resistance of composite pipe obtained in document is also unsatisfactory.
Graphene oxide is the oxide of Graphene, is a kind of important derivatives of Graphene, is had to Graphene similar
Structure, with excellent optics, thermodynamics, mechanics and electric property, improving electric conductivity, thermal conductivity, the mechanical property of material
The combination properties such as energy aspect plays very important effect.
Therefore, the present invention first carries out ammonia using N- (β-aminoethyl)-γ-aminopropyltriethoxy dimethoxysilane to montmorillonite
Baseization is modified, and is then lived using 1- ethyls-(3- dimethylaminopropyls) carbodiimide hydrochloride and N-hydroxy-succinamide
Change the carboxyl of surface of graphene oxide, the carboxyl of such surface of graphene oxide can carry out acid amides with the amino on montmorillonite surface
Condensation, and then graphene oxide layer is coated on montmorillonite surface, graphene oxide cladding nano imvite is obtained, then adopt
Graft modification is carried out to it with butyl acrylate, its compatibility and dispersion stabilization with PVC matrix is improved, polyacrylic acid is obtained
The graphene oxide cladding nano imvite of butyl ester graft modification, is applied in PVC as conductive filler, is improving PVC
On the basis of the thermal stability and mechanical property of tubing, the sheet resistance of PVC is reduced, have obtained PVC
There is excellent antistatic behaviour.The present invention is also answered using the inorganic combustion inhibitor of basic nickel carbonate, zirconium hydroxide, pandermite powder composition
With pentaerythrite diphosphate melamine salt, brominated paraffin, poly- aminopropyl/phenyl silsesquioxane micro mist, chloromethoxy aliphatic acid
The organic fire-retardant of methyl esters composition carries out flame-retardant modified to PVC, can not only significantly improve the oxygen index (OI) of material, can be with
Improve mechanical strength, resistance to ag(e)ing and the weatherability of material.
The content of the invention
It is an object of the invention to provide a kind of antistatic property it is excellent, that oxygen index (OI) is high, mechanical property is good is mining anti-quiet
Resistance combustion PVC and preparation method thereof.
To achieve the above object, the present invention is adopted the following technical scheme that：
A kind of mining electrostatic resistance flame retardant PVC, is made up of the raw material of following weight portion：Polyvinyl chloride 74-88, montmorillonite
32-46, pentaerythrite diphosphate melamine salt 8-16, graphene oxide 18-30, Ethylhexyl stearate 5-10, basic nickel carbonate 3-
7th, brominated paraffin 6-11, glycerin zinc 2-4, magnesium stearate 1-2, poly- aminopropyl/phenyl silsesquioxane micro mist 7-13, zirconium hydroxide
10-15, chloromethoxy fatty acid methyl ester 12-19, pandermite powder 14-22.
A kind of preparation method of mining electrostatic resistance flame retardant PVC, comprises the following steps：
(1) according to solid-to-liquid ratio 1:Be added in 95% absolute ethyl alcohol for montmorillonite by 10-12, stirs, Ran Houjia
Enter N- (β-aminoethyl)-γ-aminopropyltriethoxy dimethoxysilane equivalent to montmorillonite quality 2-4%, oil bath heating to 50-
60 DEG C, 2-3h is stirred, be cooled to room temperature, respectively cleaned three times with ethanol, deionized water respectively, freeze-drying is crushed to nanoparticle
Footpath, sieving, obtains final product amination nano imvite；
(2) add water graphene oxide the graphene oxide dispersion for stirring and being made that mass concentration is 0.5-1mg/mL, so
Add afterwards 1- ethyls-(3- dimethylaminopropyls) carbodiimide hydrochloride equivalent to graphene oxide quality 35-45% and
The N-hydroxy-succinamide of 20-30%, adds amination nanometer obtained in step (1) to cover de- after ultrasonically treated 20-30min
Soil, stirs 10-15h under the rotating speed of 400-600r/min, filtering, and is respectively cleaned three times with methyl alcohol, deionized water respectively, freezes
Dry, 450-490 DEG C of calcining 1-2h is cooled to room temperature, obtains final product graphene oxide cladding nano imvite；
(3) according to solid-to-liquid ratio 1:25-35 by graphene oxide cladding nano imvite be added to the water, add equivalent to
The lauryl sodium sulfate of graphene oxide cladding nano imvite quality 3-5%, ultrasonic disperse 1-2h, then heating water bath,
It is heated to being passed through nitrogen at 50-60 DEG C, when heating 60-70 DEG C, adds and coat nano imvite quality equivalent to graphene oxide
The ammonium persulfate of 0.4-0.8%, when being heated to 70-80 DEG C, adds equivalent to graphene oxide cladding nano imvite quality 50-
60% butyl acrylate, stirring reaction 3-5h, filtering, washing, drying, air-flow crushing obtains final product butyl polyacrylate grafting and changes
Property graphene oxide cladding nano imvite；
(4) polyvinyl chloride, brominated paraffin, glycerin zinc, basic nickel carbonate, pentaerythrite diphosphate melamine salt are added to height
In speed heating mixer, be heated to 80-90 DEG C, mix 14-18min, add poly- aminopropyl/phenyl silsesquioxane micro mist,
Zirconium hydroxide, pandermite powder, are heated to 95-105 DEG C, mix 8-12min, and polypropylene is added when material temperature is down to 75-85 DEG C
Graphene oxide cladding nano imvite and remaining raw material of acid butyl ester graft modification, mix 10-15min, obtain final product compound；
(5) compound obtained in step (4) is added in double screw extruder and is extruded, double screw extruder barrel zone temperature
It is 170-190 DEG C, die head temperature is 160-180 DEG C, and screw speed is 30-50r/min, then through trombone slide, cooling, cutting, system
Into tubing.
Beneficial effects of the present invention：
(1) present invention first carries out amino using N- (β-aminoethyl)-γ-aminopropyltriethoxy dimethoxysilane to montmorillonite
Change and be modified, then activated using 1- ethyls-(3- dimethylaminopropyls) carbodiimide hydrochloride and N-hydroxy-succinamide
The carboxyl of surface of graphene oxide, the carboxyl of such surface of graphene oxide can carry out acid amides contracting with the amino on montmorillonite surface
Close, and then graphene oxide layer is coated on montmorillonite surface, graphene oxide cladding nano imvite is obtained, then use
Butyl acrylate carries out graft modification to it, improves its compatibility and dispersion stabilization with PVC matrix, and polyacrylic acid fourth is obtained
The graphene oxide cladding nano imvite of ester graft modification, is applied in PVC as conductive filler, is improving pvc pipe
On the basis of the thermal stability and mechanical property of material, the sheet resistance of PVC is reduced, there is obtained PVC
Excellent antistatic behaviour；
(2) present invention compounds Ji Wusi using the inorganic combustion inhibitor of basic nickel carbonate, zirconium hydroxide, pandermite powder composition
Alcohol bis phosphoric acid melamine salt, brominated paraffin, poly- aminopropyl/phenyl silsesquioxane micro mist, chloromethoxy fatty acid methyl ester composition
Organic fire-retardant PVC is carried out flame-retardant modified, can not only significantly improve the oxygen index (OI) of material, material can also be improved
Mechanical strength, resistance to ag(e)ing and weatherability.
Specific embodiment
A kind of mining electrostatic resistance flame retardant PVC, is made up of the raw material of following weight (kg)：Polyvinyl chloride 81, montmorillonite
39th, pentaerythrite diphosphate melamine salt 12, graphene oxide 24, Ethylhexyl stearate 8, basic nickel carbonate 5, brominated paraffin 8, sweet
Oily zinc 3, magnesium stearate 1.5, poly- aminopropyl/phenyl silsesquioxane micro mist 10, zirconium hydroxide 12, chloromethoxy fatty acid methyl
Ester 16, pandermite powder 18；
A kind of preparation method of mining electrostatic resistance flame retardant PVC, comprises the following steps：
(1) according to solid-to-liquid ratio 1:Be added in 95% absolute ethyl alcohol for montmorillonite by 10-12, stirs, Ran Houjia
Enter N- (β-aminoethyl)-γ-aminopropyltriethoxy dimethoxysilane equivalent to montmorillonite quality 2-4%, oil bath heating to 50-
60 DEG C, 2-3h is stirred, be cooled to room temperature, respectively cleaned three times with ethanol, deionized water respectively, freeze-drying is crushed to nanoparticle
Footpath, sieving, obtains final product amination nano imvite；
(2) add water graphene oxide the graphene oxide dispersion for stirring and being made that mass concentration is 0.5-1mg/mL, so
Add afterwards 1- ethyls-(3- dimethylaminopropyls) carbodiimide hydrochloride equivalent to graphene oxide quality 35-45% and
The N-hydroxy-succinamide of 20-30%, adds amination nanometer obtained in step (1) to cover de- after ultrasonically treated 20-30min
Soil, stirs 10-15h under the rotating speed of 400-600r/min, filtering, and is respectively cleaned three times with methyl alcohol, deionized water respectively, freezes
Dry, 450-490 DEG C of calcining 1-2h is cooled to room temperature, obtains final product graphene oxide cladding nano imvite；
(3) according to solid-to-liquid ratio 1:25-35 by graphene oxide cladding nano imvite be added to the water, add equivalent to
The lauryl sodium sulfate of graphene oxide cladding nano imvite quality 3-5%, ultrasonic disperse 1-2h, then heating water bath,
It is heated to being passed through nitrogen at 50-60 DEG C, when heating 60-70 DEG C, adds and coat nano imvite quality equivalent to graphene oxide
The ammonium persulfate of 0.4-0.8%, when being heated to 70-80 DEG C, adds equivalent to graphene oxide cladding nano imvite quality 50-
60% butyl acrylate, stirring reaction 3-5h, filtering, washing, drying, air-flow crushing obtains final product butyl polyacrylate grafting and changes
Property graphene oxide cladding nano imvite；
(4) polyvinyl chloride, brominated paraffin, glycerin zinc, basic nickel carbonate, pentaerythrite diphosphate melamine salt are added to height
In speed heating mixer, be heated to 80-90 DEG C, mix 14-18min, add poly- aminopropyl/phenyl silsesquioxane micro mist,
Zirconium hydroxide, pandermite powder, are heated to 95-105 DEG C, mix 8-12min, and polypropylene is added when material temperature is down to 75-85 DEG C
Graphene oxide cladding nano imvite and remaining raw material of acid butyl ester graft modification, mix 10-15min, obtain final product compound；
(5) compound obtained in step (4) is added in double screw extruder and is extruded, double screw extruder barrel zone temperature
It is 170-190 DEG C, die head temperature is 160-180 DEG C, and screw speed is 30-50r/min, then through trombone slide, cooling, cutting, system
Into tubing.
The main performance testing result of PVC obtained in above-described embodiment is as shown in the table：
| Detection project | Unit | Testing result |
| Tensile strength | MPa | 58 |
| Longitudinal welds | % | 3.1 |
| Oxygen index (OI) | % | 44 |
| Sheet resistance | Ω | 2.8×106 |
| Aging coefficient (70 DEG C, 144h) | — | 0.85 |
Claims (2)
1. a kind of mining electrostatic resistance flame retardant PVC, it is characterised in that be made up of the raw material of following weight portion：Polyvinyl chloride 74-
88th, montmorillonite 32-46, pentaerythrite diphosphate melamine salt 8-16, graphene oxide 18-30, Ethylhexyl stearate 5-10, alkali formula
Nickelous carbonate 3-7, brominated paraffin 6-11, glycerin zinc 2-4, magnesium stearate 1-2, poly- aminopropyl/phenyl silsesquioxane micro mist 7-13,
Zirconium hydroxide 10-15, chloromethoxy fatty acid methyl ester 12-19, pandermite powder 14-22.
2. a kind of preparation method of mining electrostatic resistance flame retardant PVC as claimed in claim 1, it is characterised in that including with
Lower step：
（1）According to solid-to-liquid ratio 1:Be added in 95% absolute ethyl alcohol for montmorillonite by 10-12, stirs, and is subsequently adding quite
In the N- of montmorillonite quality 2-4%（β-aminoethyl）- γ-aminopropyltriethoxy dimethoxysilane, oil bath heating is stirred to 50-60 DEG C
2-3h is mixed, room temperature is cooled to, is respectively cleaned three times with ethanol, deionized water respectively, freeze-drying is crushed to nanometer particle size, sieved,
Obtain final product amination nano imvite；
（2）Graphene oxide is added water the graphene oxide dispersion for stirring and being made that mass concentration is 0.5-1mg/mL, Ran Houjia
Enter 1- ethyls equivalent to graphene oxide quality 35-45%-（3- dimethylaminopropyls）Carbodiimide hydrochloride and 20-30%
N-hydroxy-succinamide, add step after ultrasonically treated 20-30min（1）Obtained amination nano imvite, in 400-
10-15h is stirred under the rotating speed of 600r/min, is filtered, and respectively cleaned three times with methyl alcohol, deionized water respectively, freeze-drying, 450-
490 DEG C of calcining 1-2h, are cooled to room temperature, obtain final product graphene oxide cladding nano imvite；
（3）According to solid-to-liquid ratio 1:Be added to the water for graphene oxide cladding nano imvite by 25-35, adds equivalent to oxidation
The lauryl sodium sulfate of graphene coated nano imvite quality 3-5%, ultrasonic disperse 1-2h, then heating water bath, is heated to
Nitrogen is passed through at 50-60 DEG C, when heating 60-70 DEG C, is added equivalent to graphene oxide cladding nano imvite quality 0.4-
0.8% ammonium persulfate, when being heated to 70-80 DEG C, adds equivalent to graphene oxide cladding nano imvite quality 50-60%'s
Butyl acrylate, stirring reaction 3-5h, filtering, washing, drying, air-flow crushing obtains final product the oxygen of butyl polyacrylate graft modification
Graphite alkene coats nano imvite；
（4）Polyvinyl chloride, brominated paraffin, glycerin zinc, basic nickel carbonate, pentaerythrite diphosphate melamine salt are added to and are added at a high speed
In Hot mixer, 80-90 DEG C is heated to, mixes 14-18min, add poly- aminopropyl/phenyl silsesquioxane micro mist, hydrogen-oxygen
Change zirconium, pandermite powder, be heated to 95-105 DEG C, mix 8-12min, polyacrylic acid fourth is added when material temperature is down to 75-85 DEG C
Graphene oxide cladding nano imvite and remaining raw material of ester graft modification, mix 10-15min, obtain final product compound；
（5）By step（4）Obtained compound is extruded in being added to double screw extruder, and double screw extruder barrel zone temperature is
170-190 DEG C, die head temperature is 160-180 DEG C, and screw speed is 30-50r/min, and then through trombone slide, cooling, cutting is made
Tubing.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201611183844.XA CN106751202A (en) | 2016-12-20 | 2016-12-20 | A kind of mining electrostatic resistance flame retardant PVC and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201611183844.XA CN106751202A (en) | 2016-12-20 | 2016-12-20 | A kind of mining electrostatic resistance flame retardant PVC and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107603058A (en) * | 2017-08-29 | 2018-01-19 | 三峡大学 | A kind of PVC/CPE composite pipes of graphene oxide enhancing and preparation method thereof |
| NL2032179B1 (en) * | 2022-06-15 | 2023-12-21 | Zhejiang Xidamen New Mat Co Ltd | Method for preparing inorganic component reinforced high-weather-resistance pvc film |
-
2016
- 2016-12-20 CN CN201611183844.XA patent/CN106751202A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107603058A (en) * | 2017-08-29 | 2018-01-19 | 三峡大学 | A kind of PVC/CPE composite pipes of graphene oxide enhancing and preparation method thereof |
| CN107603058B (en) * | 2017-08-29 | 2018-09-28 | 三峡大学 | A kind of PVC/CPE composite pipes and preparation method thereof of graphene oxide enhancing |
| NL2032179B1 (en) * | 2022-06-15 | 2023-12-21 | Zhejiang Xidamen New Mat Co Ltd | Method for preparing inorganic component reinforced high-weather-resistance pvc film |
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