CN104448074A - Special modified graphene for polymerization of vinyl chloride - Google Patents
Special modified graphene for polymerization of vinyl chloride Download PDFInfo
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- CN104448074A CN104448074A CN201410745546.XA CN201410745546A CN104448074A CN 104448074 A CN104448074 A CN 104448074A CN 201410745546 A CN201410745546 A CN 201410745546A CN 104448074 A CN104448074 A CN 104448074A
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Abstract
The invention belongs to the technical field of graphene materials and particularly relates to special modified graphene for polymerization of vinyl chloride. The special modified graphene for polymerization of vinyl chloride comprises graphene powder and multiple surface modifiers, wherein the weight ratio of the surface modifiers is 0.5-5wt% and the surface and edges of graphene are uniformly coated with the surface modifiers. The preparation method is simple, efficient and environment-friendly, industrialized mass production can be achieved, the obtained product is particularly suitable for a vinyl chloride suspension polymerization system, the properties including thermal property, mechanical property and electrical property of polyvinyl chloride (PVC) can be significantly improved and thus the market application range of PVC is expanded.
Description
Technical field
The invention belongs to grapheme material technical field, the modified graphene that particularly a kind of chloroethylene polymerization is special.
Background technology
Graphene, with the electricity of the specific surface area of the physical strength of its superelevation, super large and excellence, calorifics and optical property, is considered to the ideal filler strengthening polymer performance.Research shows, adds some performance that a small amount of Graphene series material significantly can promote traditional material, such as electroconductibility, thermal conductivity, photocatalysis characteristic, thermostability, hardness, modulus etc.Graphene-based polymer composites is the focus of domestic and international expert research, is considered to the important directions of Graphene industrialization, has broad application prospects.But the research of Graphene reinforced composite performance faces huge challenge, the maximum 'bottleneck' restrictions of its industrialization be Graphene reunion-scattering problem and with polymer interface in conjunction with problem.The preparation method of current matrix material mainly contains solution mixing, melting mixing and in-situ polymerization.Solution blending technique needs a large amount of solvent, bring severe environmental issue, and its energy consumption is high, process is long, yield is low, almost cannot industrialization.The subject matter of melt-blending process is that Graphene is difficult to reach nano-scale dispersion.Situ aggregation method can realize the dispersed of nano particle, and can make again filler and matrix In-situ reaction, the feasibility of suitability for industrialized production is higher.
At home and abroad under economic overall situation, polyvinyl chloride (PVC) industry faces that the energy rises steadily, the situation of downstream dull sale, especially by the impact of national regulation and control policy of real estate, real estate causes PVC industry to continue decline tendency for the slump in demand of PVC and door and window, PVC industry is in heavy losses state, the management mode that PVC price around the narrow oscillatory operation of lower rail below cost average line, defines always " mending chlorine with alkali ".The four major contradictions of the one three large pressure that face of restriction, two large impacts of raw material route, enterprise operation and the industrial structure greatly of long-standing problem PVC industry survival and development more manifests and gives prominence to.Current Chinese PVC production capacity is expanded a road and is sung heartily, but kind is single, production capacity surplus, cost up, dog-eat-dog become the potential problems that its industry development faces.The breach addressed these problems is foreign company mode, take user as guiding, makes polyvinyl chloride resin specialized and differentiation on specification, goods kind and applicating category, in high-end product, seeks new growth point.
Adopt in-situ suspension polymerization, Graphene is added in polyvinyl chloride resin, preparation PVC-Graphene Special Resin, the matrix material that available can be excellent.But, at present Graphene mostly on the market be general, mass product, the special graphite alkene for a certain field, a certain product development is also fewer, only in battery, coating etc., has certain progress.Be directed to matrix material, particularly the general-purpose plastics such as PVC, the exploitation of special graphite alkene product have not been reported.The present invention is according to the feature of suspension polymerization of VC, take into full account the over-all properties of the safety factorss such as polymerization system compatibility, kinetics of polymerization reaction, heat transfer process and products obtained therefrom, be intended to exploitation and be a kind ofly suitable for the special modified graphene of suspension polymerization of VC.
Summary of the invention
The technical problem to be solved in the present invention is exactly the modified graphene providing a kind of chloroethylene polymerization special for above-mentioned the deficiencies in the prior art.
This modified graphene is particularly suitable for suspension polymerization of VC system, on kinetics of polymerization reaction and heat transfer process without impact, can comprehensively improve polyvinyl chloride performance, is to aim at the product innovation that chloroethylene polymerization provides.
The preparation method of the modified graphene that the present invention also provides a kind of chloroethylene polymerization special, its technological process is simple, can industrial volume production, high-efficiency environment friendly.
In order to solve above technical problem, solution of the present invention is:
The modified graphene that chloroethylene polymerization is special, described modified graphene is made up of graphene powder and kinds of surface properties-correcting agent, and wherein weight ratio shared by surface-modifying agent is 0.5-5wt%, and is evenly coated on graphenic surface and edge.
Described Graphene is of a size of 0.01-2 μm, and thickness is less than 5nm.
The a large amount of defect of marginal existence of described Graphene, has greater activity, easily carries out modification.
Described kinds of surface properties-correcting agent is the specific auxiliary agent of chloroethylene polymerization or the water-soluble surface modifier fully compatible with polymerization system.
Described kinds of surface properties-correcting agent is Walocel MT 20.000PV, Vltra tears, Sodium dodecylbenzene sulfonate, sodium lauryl sulphate, polyvinyl alcohol, the binary of sodium stearate or multiplexed combination.
Described properties-correcting agent is evenly coated on graphenic surface and edge is completed by reactive forces such as physical adsorption, chemisorption, electrostatic adhesion, covalent linkage.
A preparation method for the modified graphene that chloroethylene polymerization is special, preparation process is as follows:
(1) join in strong base solution by graphite raw material, 150 DEG C of water-baths 2 hours, take out, washing suction filtration is to neutral, and obtain graphite slurry, the proportion that wherein in solution, highly basic accounts for is 2-10wt%, and the proportion that graphite accounts for is 1-5%;
(2) be fully dissolved in water by surface-modifying agent, wiring solution-forming, the proportion that wherein in solution, surface-modifying agent accounts for is 0.005-0.25wt%;
(3) joined in the solution in step (2) by the graphite slurry in step (1), fully mix, obtain uniform graphite dispersing solution, the proportion wherein in dispersion liquid shared by graphite is 1-5wt%;
(4) join in nanometer sand mill by the graphite dispersing solution in step (3), fully grind, rotating speed is 2000-2500rpm, and the time is 5-15 hour, obtains modified graphene slurries;
(5) modified graphene slurries are taken out, dry modified graphene powder.
Described graphite raw material is crystalline flake graphite, expanded graphite, synthetic graphite, amorphous graphite.
Described strong base solution is the aqueous solution of potassium hydroxide, sodium hydroxide, calcium hydroxide, hydrated barta, sodium carbonate, sodium bicarbonate, salt of wormwood, saleratus etc.
Described drying process is lyophilize, microwave drying, critical point drying, spraying dry.
Feature of the present invention and beneficial effect:
The modified graphene that a kind of chloroethylene polymerization provided by the invention is special, is particularly suitable for suspension polymerization of VC system, on kinetics of polymerization reaction and heat transfer process without impact; This modified graphene possesses the general property of Graphene, as high conductivity, high thermal conductivity, high strength, high-modulus, high heat resistance etc., can comprehensively improve polyvinyl chloride performance, simultaneously it has done and has specially modified and design in particle diameter, properties-correcting agent, dispersiveness, local edge etc., is to aim at the product innovation that chloroethylene polymerization provides.
It possesses following advantage: (1) properties-correcting agent is the dispersion agent of chloroethylene polymerization or the material similar with dispersion agent, is conducive to the dispersed of Graphene; (2) particle diameter is less than the primary particle diameter of polyvinyl chloride (PVC) RESINS, can be completely coated by resin particle, is beneficial to enhancing resin property; (3) edge defect is many, and active high, being modified under dry powder, agent is coated, passivation, and after being made into dispersion liquid, active site exposes, and can interact with polyvinyl chloride molecular chain, strengthens the performance of resin; (4) preparation method is simple, can industrial volume production, high-efficiency environment friendly.
Accompanying drawing explanation
Accompanying drawing 1: the scanning electron microscope diagram (SEM) of the modified graphene that chloroethylene polymerization is special
Embodiment
For a better understanding of the present invention, illustrate content of the present invention further below in conjunction with embodiment, but content of the present invention is not only confined to following specific embodiment.
Embodiment 1
(1) take 30g sodium hydroxide and 300g water is made into sodium hydroxide solution, add 5g amorphous graphite, water-bath 2 hours at 150 DEG C; Taken out by mixed solution and filter, washing suction filtration, to neutral, obtains graphite slurry.
(2) by 0.15g Sodium dodecylbenzene sulfonate, 0.1g Vltra tears is fully dissolved in 600g water, is made into composite modified agent solution.
(3) graphite slurry in step (1) is joined in the composite modified agent solution in step (2), fully mix, obtain uniform graphite dispersing solution.
(4) join in nanometer sand mill by the graphite dispersing solution in step (3), fully grind, rotating speed is 2500rpm, and the time is 5 hours, obtains modified graphene slurries.
(5) take out modified graphene slurries, spraying dry obtains modified graphene powder.
Embodiment 2
(1) take 30g sodium hydroxide and 300g water is made into sodium hydroxide solution, add 5g amorphous graphite, water-bath 2 hours at 150 DEG C; Taken out by mixed solution and filter, washing suction filtration, to neutral, obtains graphite slurry.
(2) by 0.1g Sodium dodecylbenzene sulfonate, 0.1g Vltra tears, 0.05g sodium stearate is fully dissolved in 600g water, is made into composite modified agent solution.
(3) graphite slurry in step (1) is joined in the composite modified agent solution in step (2), fully mix, obtain uniform graphite dispersing solution.
(4) join in nanometer sand mill by the graphite dispersing solution in step (3), fully grind, rotating speed is 2500rpm, and the time is 5 hours, obtains modified graphene slurries.
(5) take out modified graphene slurries, spraying dry obtains modified graphene powder.
Embodiment 3
(1) take 10g potassium hydroxide and 200g water is made into potassium hydroxide solution, add 4g amorphous graphite, water-bath 2 hours at 150 DEG C; Taken out by mixed solution and filter, washing suction filtration, to neutral, obtains graphite slurry.
(2) by 0.1g Sodium dodecylbenzene sulfonate, 0.1g Vltra tears, is fully dissolved in 400g water, is made into composite modified agent solution.
(3) graphite slurry in step (1) is joined in the composite modified agent solution in step (2), fully mix, obtain uniform graphite dispersing solution.
(4) join in nanometer sand mill by the graphite dispersing solution in step (3), fully grind, rotating speed is 2000rpm, and the time is 8 hours, obtains modified graphene slurries.
(5) take out modified graphene slurries, spraying dry obtains modified graphene powder.
Embodiment 4
(1) take 10g potassium hydroxide and 200g water is made into potassium hydroxide solution, add 4g crystalline flake graphite, water-bath 2 hours at 150 DEG C; Taken out by mixed solution and filter, washing suction filtration, to neutral, obtains graphite slurry.
(2) by 0.1g sodium lauryl sulphate, 0.1g polyvinyl alcohol, is fully dissolved in 400g water, is made into composite modified agent solution.
(3) graphite slurry in step (1) is joined in the composite modified agent solution in step (2), fully mix, obtain uniform graphite dispersing solution.
(4) join in nanometer sand mill by the graphite dispersing solution in step (3), fully grind, rotating speed is 2000rpm, and the time is 8 hours, obtains modified graphene slurries.
(5) take out modified graphene slurries, spraying dry obtains modified graphene powder.
Embodiment 5
(1) take 10g potassium hydroxide and 200g water is made into potassium hydroxide solution, add 9.5g amorphous graphite, water-bath 2 hours at 150 DEG C; Taken out by mixed solution and filter, washing suction filtration, to neutral, obtains graphite slurry.
(2) by 0.2g sodium lauryl sulphate, 0.25g polyvinyl alcohol, is fully dissolved in 200g water, is made into composite modified agent solution.
(3) graphite slurry in step (1) is joined in the composite modified agent solution in step (2), fully mix, obtain uniform graphite dispersing solution.
(4) join in nanometer sand mill by the graphite dispersing solution in step (3), fully grind, rotating speed is 2500rpm, and the time is 7 hours, obtains modified graphene slurries.
(5) take out modified graphene slurries, spraying dry obtains modified graphene powder.
Embodiment 6
(1) take 10g potassium hydroxide and 200g water is made into potassium hydroxide solution, add 9.5g amorphous graphite, water-bath 2 hours at 150 DEG C; Taken out by mixed solution and filter, washing suction filtration, to neutral, obtains graphite slurry.
(2) 0.2g sodium lauryl sulphate, 0.25g polyvinyl alcohol, 0.05 Walocel MT 20.000PV are fully dissolved in 200g water, are made into composite modified agent solution.
(3) graphite slurry in step (1) is joined in the composite modified agent solution in step (2), fully mix, obtain uniform graphite dispersing solution.
(4) join in nanometer sand mill by the graphite dispersing solution in step (3), fully grind, rotating speed is 2500rpm, and the time is 7 hours, obtains modified graphene slurries.
(5) take out modified graphene slurries, spraying dry obtains modified graphene powder.
Embodiment 7
(1) take 10g potassium hydroxide and 200g water is made into potassium hydroxide solution, add 9.5g synthetic graphite, water-bath 2 hours at 150 DEG C; Taken out by mixed solution and filter, washing suction filtration, to neutral, obtains graphite slurry.
(2) 0.2g sodium lauryl sulphate, 0.25g polyvinyl alcohol, 0.05 Walocel MT 20.000PV are fully dissolved in 200g water, are made into composite modified agent solution.
(3) graphite slurry in step (1) is joined in the composite modified agent solution in step (2), fully mix, obtain uniform graphite dispersing solution.
(4) join in nanometer sand mill by the graphite dispersing solution in step (3), fully grind, rotating speed is 2500rpm, and the time is 7 hours, obtains modified graphene slurries.
(5) take out modified graphene slurries, spraying dry obtains modified graphene powder.
Embodiment 8
(1) take 10g potassium hydroxide and 200g water is made into potassium hydroxide solution, add 9.5g expanded graphite, water-bath 2 hours at 150 DEG C; Taken out by mixed solution and filter, washing suction filtration, to neutral, obtains graphite slurry.
(2) by 0.2g sodium lauryl sulphate, 0.25g polyvinyl alcohol, is fully dissolved in 200g water, is made into composite modified agent solution.
(3) graphite slurry in step (1) is joined in the composite modified agent solution in step (2), fully mix, obtain uniform graphite dispersing solution.
(4) join in nanometer sand mill by the graphite dispersing solution in step (3), fully grind, rotating speed is 2500rpm, and the time is 7 hours, obtains modified graphene slurries.
(5) take out modified graphene slurries, spraying dry obtains modified graphene powder.
Embodiment 9
(1) take 10g potassium hydroxide and 200g water is made into potassium hydroxide solution, add 9.5g crystalline flake graphite, water-bath 2 hours at 150 DEG C; Taken out by mixed solution and filter, washing suction filtration, to neutral, obtains graphite slurry.
(2) by 0.2g sodium lauryl sulphate, 0.25g polyvinyl alcohol, is fully dissolved in 200g water, is made into composite modified agent solution.
(3) graphite slurry in step (1) is joined in the composite modified agent solution in step (2), fully mix, obtain uniform graphite dispersing solution.
(4) join in nanometer sand mill by the graphite dispersing solution in step (3), fully grind, rotating speed is 2500rpm, and the time is 7 hours, obtains modified graphene slurries.
(5) take out modified graphene slurries, spraying dry obtains modified graphene powder.
Selected embodiment is typical embodiments above, and above-mentioned explanation just understands method of the present invention and core concept thereof for helping.It should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention, can also carry out some improvement and modification to the present invention, these improve and modify and also fall in the protection domain of the claims in the present invention.
Claims (8)
1. the modified graphene that chloroethylene polymerization is special, it is characterized in that described modified graphene is made up of graphene powder and kinds of surface properties-correcting agent, wherein weight ratio shared by surface-modifying agent is 0.5-5wt%, and is evenly coated on graphenic surface and edge.
2. the modified graphene that a kind of chloroethylene polymerization according to claim 1 is special, is characterized in that, described Graphene is of a size of 0.01-2 μm, and thickness is less than 5nm.
3. the modified graphene that a kind of chloroethylene polymerization according to claim 1 is special, is characterized in that, a large amount of defect of marginal existence of described Graphene, has greater activity.
4. the modified graphene that a kind of chloroethylene polymerization according to claim 1 is special, is characterized in that, described kinds of surface properties-correcting agent is the specific auxiliary agent of chloroethylene polymerization or the water-soluble surface modifier fully compatible with polymerization system.
5. the modified graphene that a kind of chloroethylene polymerization according to claim 1 is special, it is characterized in that, described kinds of surface properties-correcting agent is Walocel MT 20.000PV, Vltra tears, Sodium dodecylbenzene sulfonate, sodium lauryl sulphate, polyvinyl alcohol, the binary of sodium stearate or multiplexed combination.
6. the preparation method of the modified graphene that a kind of chloroethylene polymerization according to any one of claim 1-5 is special, it is characterized in that, preparation process is as follows:
(1) join in strong base solution by graphite raw material, 150 DEG C of water-baths 2 hours, take out, washing suction filtration is to neutral, and obtain graphite slurry, the proportion that wherein in solution, highly basic accounts for is 2-10wt%, and the proportion that graphite accounts for is 1-5%;
(2) be fully dissolved in water by surface-modifying agent, wiring solution-forming, the proportion that wherein in solution, surface-modifying agent accounts for is 0.005-0.25wt%;
(3) joined in the solution in step (2) by the graphite slurry in step (1), fully mix, obtain uniform graphite dispersing solution, the proportion wherein in dispersion liquid shared by graphite is 1-5wt%;
(4) join in nanometer sand mill by the graphite dispersing solution in step (3), fully grind, rotating speed is 2000-2500rpm, and the time is 5-15 hour, obtains modified graphene slurries;
(5) modified graphene slurries are taken out, dry modified graphene powder.
7., according to the preparation method of the special modified graphene of a kind of chloroethylene polymerization described in claim 6, it is characterized in that, described graphite raw material is crystalline flake graphite, expanded graphite, synthetic graphite, amorphous graphite.
8., according to the preparation method of the special modified graphene of a kind of chloroethylene polymerization described in claim 6, it is characterized in that, described drying process is lyophilize, microwave drying, critical point drying, spraying dry.
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| CN106589701A (en) * | 2016-12-19 | 2017-04-26 | 山东霞光实业有限公司 | Environmental-friendly and anti-aging outdoor wood plastic material and preparation method thereof |
| CN113462202A (en) * | 2021-06-24 | 2021-10-01 | 浙江工业大学 | Method for improving dispersion effect of graphene in acrylic emulsion |
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