CN107236224A - A kind of preparation method of graphene modified polyvinyl-chloride composite material - Google Patents
A kind of preparation method of graphene modified polyvinyl-chloride composite material Download PDFInfo
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- CN107236224A CN107236224A CN201710608748.3A CN201710608748A CN107236224A CN 107236224 A CN107236224 A CN 107236224A CN 201710608748 A CN201710608748 A CN 201710608748A CN 107236224 A CN107236224 A CN 107236224A
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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
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/24—Crosslinking, e.g. vulcanising, of macromolecules
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2327/00—Characterised by the use 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; Derivatives of such polymers
- C08J2327/02—Characterised by the use 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; Derivatives of such polymers not modified by chemical after-treatment
- C08J2327/04—Characterised by the use 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; Derivatives of such polymers not modified by chemical after-treatment containing chlorine atoms
- C08J2327/06—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
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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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
- C08L2312/00—Crosslinking
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Abstract
The invention discloses a kind of preparation method of graphene modified polyvinyl-chloride composite material, the present invention distinguishes graphene and polyvinyl chloride to be crosslinked again after organic-treating, is enhanced dispersiveness of the graphene between polymer, is improved the stability_intensity of finished-product material.
Description
Technical field
The invention belongs to Material Field, and in particular to a kind of preparation method of graphene modified polyvinyl-chloride composite material.
Background technology
Polyvinyl chloride is VCM in initiators such as peroxide, azo-compounds；Or pressed certainly under light, heat effect
The polymer being polymerized by base polymerization reaction mechanism.Ryuron and vinyl chloride copolymer system are referred to as vinyl chloride tree
Fat.PVC is the white powder of impalpable structure, and the degree of branching is smaller, relative density 1.4 or so, 77~90 DEG C of glass transition temperature,
170 DEG C or so start to decompose, and the stability to light and heat is poor, more than 100 DEG C or through long-time exposure in sunshine, will decompose and
Hydrogen chloride is produced, and further autocatalysis is decomposed, and causes discoloration, physical and mechanical properties also declines rapidly, in actual applications
Stabilizer is must be added to improve the stability to light and heat.Industrial PVC molecular weight is general in 50,000~110,000 scopes
It is interior, with larger polydispersity, the reduction of molecular weight with polymerisation temperature and increase；Without definite melting point, 80~85 DEG C of beginnings are soft
Change, 130 DEG C are changed into viscoelastic state, and 160~180 DEG C start to be changed into viscous state；There are preferable mechanical performance, tensile strength 60MPa
Left and right, 5~10kJ/m2 of impact strength；There are excellent dielectric properties.PVC was once the general-purpose plastics of yield maximum in the world, application
Widely.In construction material, industrial product, commodity, flooring laminate, floor tile, artificial leather, tubing, electric wire, packaging
It is widely used in terms of film, bottle, expanded material, encapsulant, fiber.Then in order to improve the mechanical property of polyvinyl chloride
Can, a variety of inorganic additives are often added wherein, then the poor compatibility of inorganic additive and polymer, the group of easily causing
It is poly-, reduce the stability_intensity of finished product.
The content of the invention
In view of the defects and deficiencies of the prior art, the present invention intends to provide a kind of graphene modified polyvinyl chloride is multiple
The preparation method method of condensation material.
To achieve the above object, the present invention uses following technical scheme：
A kind of preparation method of graphene modified polyvinyl-chloride composite material, comprises the following steps：
(1) graphene of 13-20 parts by weight is taken, in the mixed acid solution for being added to 30-40 times of its weight, rise temperature is
50-60 DEG C, ultrasonic 1-2 hours, precipitation is washed, mixed with the octylisothiazolinone of 0.7-1 parts by weight by filtering, and stirring is equal
Even, air drying obtains graphene oxide；
(2) aluminum stearate of 2-4 parts by weight is taken, in the tetrahydrofuran for being added to 6-9 times of its weight, is stirred, is added
Above-mentioned graphene oxide, 2-3 hours are incubated at 65-70 DEG C, and distillation removes tetrahydrofuran, are mixed with the stearic acid of 1-2 parts by weight
Close, stir to normal temperature, obtain carboxylated graphene；
(3) octyl phenyl cyclotetrasiloxane, castor oil acid mixing are taken, the N- methyl pyrroles of 3-4 times of compound weight are added to
In pyrrolidone, stir, rise temperature is 50-60 DEG C, adds barium stearate, and insulated and stirred 10-20 minutes obtains organic silica
Alkane dispersion liquid；
(4) polyvinyl chloride is taken, in the dimethyl carbonate for being added to 1.7-2 times of its weight, stirs, is sent to reactor
In, rise temperature is 130-140 DEG C, insulated and stirred 20-30 minutes, and discharging is mixed with above-mentioned triethanolamine borate, and stirring is extremely
Normal temperature, obtains modified polyvinyl chloride dispersion liquid；
(5) triethylamine of 1-2 parts by weight is taken, in the absolute ethyl alcohol for being added to 3-5 times of its weight, is stirred, it is and above-mentioned
Modified polyvinyl chloride dispersion liquid, it is ultrasonic 10-15 minutes, ethanol is distilled off, the organic polyvinyl chloride of amination is obtained；
(6) the organic polyvinyl chloride mixing of above-mentioned carboxylated graphene, amination is taken, is added in organosiloxane dispersion liquid,
Stir, be sent in reactor, in 86-90 DEG C of insulated and stirred 40-50 minutes, discharge, filtering will precipitation washing, vacuum
Dried 1-2 hours at 100-105 DEG C, be cooled to normal temperature, obtained acid amides and organise graphene cross-linked polrvinyl chloride；
(7) above-mentioned acid amides is taken to organise graphene cross-linked polrvinyl chloride, polyvinyl chloride, 2-3 weights with 120-130 parts by weight
The melamine mixing of part is measured, is sent in extruder, melting extrusion, cools down, the graphene modified polyvinyl chloride is produced and answers
Condensation material.
Advantages of the present invention：
The present invention by the oxidation processes in mixed acid solution, then organises graphene by aluminum stearate, stearic acid
Acidifying, obtains carboxylated graphene, then disperses octyl phenyl cyclotetrasiloxane in pyrrolidones, while introducing castor oil
Acid, obtains the organosiloxane dispersion liquid of acidity, and polyvinyl chloride then is passed through into triethanolamine borate modification, enhancing again
Plasticity and weather resistance, then by the alcoholic solution amination of triethylamine, finally by the polyvinyl chloride of amination and carboxylated graphene
Mixing, the cross-linking reaction in acid organosiloxane dispersion liquid obtains acid amides and organised graphene cross-linked polrvinyl chloride, enters one
Step melting, obtains finished-product material；
The present invention distinguishes graphene and polyvinyl chloride to be crosslinked again after organic-treating, enhances graphene between polymer
Dispersiveness, improve the stability_intensity of finished-product material.
Embodiment
Embodiment 1
A kind of preparation method of graphene modified polyvinyl-chloride composite material, comprises the following steps：
(1) graphene of 20 parts by weight is taken, in the mixed acid solution for being added to 40 times of its weight, rise temperature is 60 DEG C, is surpassed
Precipitation is washed, mixes, stir with the octylisothiazolinone of 1 parts by weight, air drying obtains oxygen by sound 2 hours, filtering
Graphite alkene；
(2) aluminum stearate of 4 parts by weight is taken, in the tetrahydrofuran for being added to 9 times of its weight, is stirred, is added above-mentioned
Graphene oxide, 3 hours are incubated at 70 DEG C, and distillation removes tetrahydrofuran, mixed with the stearic acid of 2 parts by weight, stirs to normal
Temperature, obtains carboxylated graphene；
(3) octyl phenyl cyclotetrasiloxane, castor oil acid mixing are taken, the N- methylpyrroles of 4 times of compound weight are added to
In alkanone, stir, rise temperature is 60 DEG C, add barium stearate, insulated and stirred 20 minutes obtains organosiloxane and disperseed
Liquid；
(4) polyvinyl chloride is taken, in the dimethyl carbonate for being added to 2 times of its weight, stirs, is sent in reactor,
It is 140 DEG C to raise temperature, insulated and stirred 30 minutes, and discharging is mixed with above-mentioned triethanolamine borate, is stirred to normal temperature, must be changed
Property PVC dispersion；
(5) triethylamine of 2 parts by weight is taken, in the absolute ethyl alcohol for being added to 5 times of its weight, is stirred, with above-mentioned modification
PVC dispersion, ultrasound 15 minutes, is distilled off ethanol, obtains the organic polyvinyl chloride of amination；
(6) the organic polyvinyl chloride mixing of above-mentioned carboxylated graphene, amination is taken, is added in organosiloxane dispersion liquid,
Stir, be sent in reactor, in 90 DEG C of insulated and stirreds 50 minutes, discharge, filtering, will precipitation washing, at 105 DEG C of vacuum
Dry 2 hours, be cooled to normal temperature, obtain acid amides and organise graphene cross-linked polrvinyl chloride；
(7) above-mentioned acid amides is taken to organise graphene cross-linked polrvinyl chloride, the polyvinyl chloride, 3 parts by weight with 130 parts by weight
Melamine is mixed, and is sent in extruder, melting extrusion, is cooled down, is produced the graphene modified polyvinyl-chloride composite material.
Embodiment 2
(1) graphene of 13 parts by weight is taken, in the mixed acid solution for being added to 30 times of its weight, rise temperature is 50 DEG C, is surpassed
Precipitation is washed, mixes, stir with the octylisothiazolinone of 0.7 parts by weight by sound 1-2 hours, filtering, air drying,
Obtain graphene oxide；
(2) aluminum stearate of 2 parts by weight is taken, in the tetrahydrofuran for being added to 6 times of its weight, is stirred, is added above-mentioned
Graphene oxide, 2 hours are incubated at 65 DEG C, and distillation removes tetrahydrofuran, mixed with the stearic acid of 1 parts by weight, stirs to normal
Temperature, obtains carboxylated graphene；
(3) octyl phenyl cyclotetrasiloxane, castor oil acid mixing are taken, the N- methylpyrroles of 3 times of compound weight are added to
In alkanone, stir, rise temperature is 50 DEG C, add barium stearate, insulated and stirred 10 minutes obtains organosiloxane and disperseed
Liquid；
(4) polyvinyl chloride is taken, in the dimethyl carbonate for being added to 1.7 times of its weight, stirs, is sent to reactor
In, rise temperature is 130 DEG C, insulated and stirred 20 minutes, and discharging is mixed with above-mentioned triethanolamine borate, is stirred to normal temperature, is obtained
Modified polyvinyl chloride dispersion liquid；
(5) triethylamine of 1 parts by weight is taken, in the absolute ethyl alcohol for being added to 3 times of its weight, is stirred, with above-mentioned modification
PVC dispersion, ultrasound 10 minutes, is distilled off ethanol, obtains the organic polyvinyl chloride of amination；
(6) the organic polyvinyl chloride mixing of above-mentioned carboxylated graphene, amination is taken, is added in organosiloxane dispersion liquid,
Stir, be sent in reactor, in 86 DEG C of insulated and stirreds 40 minutes, discharge, filtering, will precipitation washing, at 100 DEG C of vacuum
Dry 1 hour, be cooled to normal temperature, obtain acid amides and organise graphene cross-linked polrvinyl chloride；
(7) above-mentioned acid amides is taken to organise graphene cross-linked polrvinyl chloride, the polyvinyl chloride, 2 parts by weight with 120 parts by weight
Melamine is mixed, and is sent in extruder, melting extrusion, is cooled down, is produced the graphene modified polyvinyl-chloride composite material.
Performance test：
The polyvinyl chloride composite materials of the present invention：
Hardness (Shao A) is that 91-93, tensile strength are that 27.3-28.4MPa, elongation at break are 330.5-340.4%, lacked
Mouth impact strength (kJ/m2) it is 9-11；
Traditional polyvinyl chloride：
Hardness (Shao A) is that 70-74, tensile strength are that 15-20MPa, elongation at break are that 230-273%, notch shock are strong
Spend (kJ/m2) it is 6-7.
Claims (1)
1. a kind of preparation method of graphene modified polyvinyl-chloride composite material, it is characterised in that comprise the following steps：
(1) graphene of 13-20 parts by weight is taken, in the mixed acid solution for being added to 30-40 times of its weight, rise temperature is 50-60
DEG C, precipitation is washed, mixes, stir with the octylisothiazolinone of 0.7-1 parts by weight, often by ultrasonic 1-2 hours, filtering
Temperature is dried, and obtains graphene oxide；
(2) aluminum stearate of 2-4 parts by weight is taken, in the tetrahydrofuran for being added to 6-9 times of its weight, is stirred, is added above-mentioned
Graphene oxide, 2-3 hours are incubated at 65-70 DEG C, and distillation removes tetrahydrofuran, mixed with the stearic acid of 1-2 parts by weight,
Stirring obtains carboxylated graphene to normal temperature；
(3) octyl phenyl cyclotetrasiloxane, castor oil acid mixing are taken, the N- crassitudes of 3-4 times of compound weight are added to
In ketone, stir, rise temperature is 50-60 DEG C, add barium stearate, insulated and stirred 10-20 minutes obtains organosiloxane point
Dispersion liquid；
(4) polyvinyl chloride is taken, in the dimethyl carbonate for being added to 1.7-2 times of its weight, stirs, is sent in reactor,
It is 130-140 DEG C to raise temperature, insulated and stirred 20-30 minutes, and discharging is mixed with above-mentioned triethanolamine borate, is stirred to normal
Temperature, obtains modified polyvinyl chloride dispersion liquid；
(5) triethylamine of 1-2 parts by weight is taken, in the absolute ethyl alcohol for being added to 3-5 times of its weight, is stirred, with above-mentioned modification
PVC dispersion, it is ultrasonic 10-15 minutes, ethanol is distilled off, the organic polyvinyl chloride of amination is obtained；
(6) the organic polyvinyl chloride mixing of above-mentioned carboxylated graphene, amination is taken, is added in organosiloxane dispersion liquid, stirs
Uniformly, it is sent in reactor, in 86-90 DEG C of insulated and stirred 40-50 minutes, discharges, filtering will precipitation washing, vacuum 100-
Dried 1-2 hours at 105 DEG C, be cooled to normal temperature, obtained acid amides and organise graphene cross-linked polrvinyl chloride；
(7) above-mentioned acid amides is taken to organise graphene cross-linked polrvinyl chloride, polyvinyl chloride, 2-3 parts by weight with 120-130 parts by weight
Melamine mixing, be sent in extruder, melting extrusion, cool down, produce the graphene modified polyvinyl chloride composite wood
Material.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109265856A (en) * | 2018-08-05 | 2019-01-25 | 梅敉萌 | A kind of environmental protection crosslinking pvc automotive interior material and preparation method thereof |
| CN111334133A (en) * | 2020-04-02 | 2020-06-26 | 汉中木头人科技信息咨询有限公司 | Graphene antistatic coating and preparation method thereof |
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| CN104327405A (en) * | 2014-10-16 | 2015-02-04 | 广州合成材料研究院有限公司 | Thermal conductive PVC composite material and preparation method thereof |
| CN104710709A (en) * | 2015-03-04 | 2015-06-17 | 聊城大学 | Polyvinyl chloride/graphene nanocomposite and preparation method thereof |
| CN105295255A (en) * | 2015-12-01 | 2016-02-03 | 济南大学 | Graphene oxide and glass-fiber reinforced polyvinyl chloride composite material and preparation method thereof |
| CN106977843A (en) * | 2017-04-11 | 2017-07-25 | 商立华 | A kind of phosphatization cross-linked graphene flame-proof composite material and preparation method thereof |
| CN108239358A (en) * | 2018-02-26 | 2018-07-03 | 杭州乐守科技有限公司 | A kind of zinc oxide/graphene composite material modified PVC section bar and preparation method thereof |
| CN108752794A (en) * | 2018-06-12 | 2018-11-06 | 台州学院 | A kind of carbon fiber and graphite alkene plastics pipe of high-strength light |
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2017
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Patent Citations (7)
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|---|---|---|---|---|
| CN102775700A (en) * | 2012-08-17 | 2012-11-14 | 西安科技大学 | PVC (Polyvinyl Chloride)/graphite alkene antistatic composite material and preparation method thereof |
| CN104327405A (en) * | 2014-10-16 | 2015-02-04 | 广州合成材料研究院有限公司 | Thermal conductive PVC composite material and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109265856A (en) * | 2018-08-05 | 2019-01-25 | 梅敉萌 | A kind of environmental protection crosslinking pvc automotive interior material and preparation method thereof |
| CN111334133A (en) * | 2020-04-02 | 2020-06-26 | 汉中木头人科技信息咨询有限公司 | Graphene antistatic coating and preparation method thereof |
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