CN107213880A - A kind of preparation method of cellular PVC graphene composite material - Google Patents
A kind of preparation method of cellular PVC graphene composite material Download PDFInfo
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- CN107213880A CN107213880A CN201710419593.9A CN201710419593A CN107213880A CN 107213880 A CN107213880 A CN 107213880A CN 201710419593 A CN201710419593 A CN 201710419593A CN 107213880 A CN107213880 A CN 107213880A
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- graphene
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- composite material
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- graphene composite
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/26—Synthetic macromolecular compounds
- B01J20/261—Synthetic macromolecular compounds obtained by reactions only involving carbon to carbon unsaturated bonds
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/285—Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/40—Devices for separating or removing fatty or oily substances or similar floating material
Abstract
The invention discloses a kind of preparation method of cellular PVC graphene composite material, by the method for high-energy ball milling by hydrophobically modified nano-graphene and the N of polyvinyl chloride, N dimethyl formamide solutions, sodium chloride is mixed, finally mixture is instilled cellular PVC graphene particles are formed in distilled water, pore-foaming agent is compatible with water in water, form the less top layer of pore structure, and slowed inside ball because the barrier on top layer is compatible with water, the effect of pore is served during slowly dissolution, the pore size distribution of formation is uniform, aperture is homogeneous, with good through hole and perforate performance；Simultaneously because the addition of hydrophobically modified nano-graphene, so that the composite being made has good hydrophobic performance, loose structure can be used for the processing of the water-oil separatings such as water pollution processing, and present invention process is easy to Industry Control, has widened the application field of polyvinyl chloride.
Description
Technical field
The present invention relates to polyvinyl chloride technical field, more particularly to a kind of system of cellular PVC graphene composite material
Preparation Method.
Background technology
Polyvinyl chloride（PVC）It is the usage amount maximum plastic products raw material after polyethylene polypropylene, there is its uniqueness
Physical chemistry advantage, is widely used in every field, but its heat endurance is poor, and easy degradation and decomposition reduces it using scope and made
With value.In addition country's PVC industries face production capacity surplus, energy prices rise, Market competition, environmental protection pressure in recent years
The baptism of the problems such as increasing.There are many researchers to be directed to the modification to PVC materials at present to improve its machinery
Performance and heat resistance.Common modified filler mainly has clay, wood powder, wood-fibred, crops residue, cellulose, calcium carbonate
Deng but either for the mechanical performance and heat resistance of modified polyvinyl chloride, there is certain modified effect, but
It is that effect is limited.Graphene can improve the heat endurance and tensile strength of polyvinyl chloride due to its excellent physico-chemical property
Deng, it is considered to be the best material of modified polyvinyl chloride.Graphene is as brand-new material, with excellent physical and chemical performance,
Furtherd investigate by numerous scholars, but graphene is the problem of preparation and application aspect still have a lot, such as difficult batch
Large area produces the graphene of structural integrity, and graphite has larger Van der Waals force, and easily reunion is scattered uneven in polymeric matrix
It is even etc..Cellular PVC has good absorption property, and preparing the main method of porous PVC material has improvement suspension polymerisation
Method, pore-foaming agent percolation and breathing pattern method.But or cellular PVC apparent density prepared by these methods is big, hole
Rate is undesirable；Porosity is low, and absorption property is limited；Control condition is difficult Industry Control, yields poorly, and cost is high.This
It is accomplished by carrying out a series of modification to the production technology of cellular PVC, be modified using graphene etc., expand poly-
The use scope of vinyl chloride, improves value.
The content of the invention
The object of the invention is exactly that there is provided a kind of cellular PVC graphene composite wood in order to make up the defect of prior art
The preparation method of material.
The present invention is achieved by the following technical solutions：
A kind of preparation method of cellular PVC graphene composite material, including step in detail below：
（1）Nano-graphene and dimethyl silicone polymer are put into closed measuring cup, is put into Muffle furnace, is heated to 230-
240 DEG C are incubated 60-80 minutes, are taken out after cooling, obtain modified nano graphite alkene；
（2）By sodium chloride be placed in baking oven with 100-110 DEG C dry 20-24 hours it is stand-by, by step（1）Obtained modified Nano stone
Black alkene is added in polyvinyl chloride solution, magnetic agitation 30-40 minutes so that modified nano graphite alkene is tentatively dispersed in polychlorostyrene second
In alkene solution；
（3）By step（2）Product is mixed with the sodium chloride dried, and is put into ball mill, with 600-800 revs/min of speed ball milling
60-90 minutes；Then the mixture after ball milling is added dropwise in distilled water and be molded, until turned with 500-600 after dripping off completely/
The speed agitator treating divided 4-5 hours, until cleaning up completely；
（4）By the above-mentioned product filtering cleaned up, it is put into refrigerator after being freezed 8-12 hours at -20--18 DEG C and inserts freezing
Dried 12-24 hours in drying machine.
A kind of preparation method of cellular PVC graphene composite material, step（1）Described nano-graphene is with gathering
The mass ratio of dimethyl siloxane is 10:1.
A kind of preparation method of cellular PVC graphene composite material, step（2）Described polyvinyl chloride solution is
Refer to polyvinyl chloride and be dissolved in the solution formed in DMF, and mass concentration is 0.075g/mL.
A kind of preparation method of cellular PVC graphene composite material, it is characterised in that step（2）Described modification
The addition of nano-graphene is the 1wt% of polyvinyl chloride, and the addition of the sodium chloride is 4 times of polyvinyl chloride.
A kind of preparation method of cellular PVC graphene composite material, step（3）Ball milling in described mechanical milling process
Medium is zirconia ball, and addition is 3-5 times of total material.
A kind of preparation method of cellular PVC graphene composite material, step（3）Described washing, specific steps are such as
Under：First water was changed every 40-60 minutes, the chlorion in cleaning solution is then detected, until chlorion is can't detect, depending on
To clean up.
It is an advantage of the invention that：The present invention to nano-graphene first by being modified, by Pintsch process, poly- diformazan
The long-chain of radical siloxane fragments into silicon oxygen bond, deposits to nano-graphene surface, strengthens its hydrophobicity；Then high energy ball is passed through
The method of mill is mixed modified nano graphite alkene with DMF solution, the cause sodium chloride of polyvinyl chloride, into
Distribution ratio is scientific and reasonable, realizes polyvinyl chloride, DMF and pore-foaming agent sodium chloride dispersed while
Between mixing and progress to pore-foaming agent particle diameter effective control, finally mixture is instilled and form porous poly- in distilled water
Vinyl chloride graphene particles, pore-foaming agent is compatible with water in water, forms the less top layer of pore structure, and due to the resistance on top layer inside ball
Slowed every compatible with water, the effect of pore is served during slowly dissolution, the pore size distribution of formation is uniform, and aperture is equal
One, with good through hole and perforate performance；Simultaneously because the addition of hydrophobically modified nano-graphene so that the composite wood being made
Material has good hydrophobic performance, and loose structure can be used for the processing of the water-oil separatings such as water pollution processing, and present invention process
It is easy to Industry Control, has widened the application field of polyvinyl chloride.
Embodiment
A kind of preparation method of cellular PVC graphene composite material, including step in detail below：
（1）0.9g nano-graphenes and 0.09g dimethyl silicone polymers are put into closed measuring cup, are put into Muffle furnace,
It is heated to 230 DEG C and is incubated 60 minutes, is taken out after cooling, obtain modified nano graphite alkene；
（2）By sodium chloride be placed in baking oven with 100 DEG C dry 20 hours it is stand-by, 90g polyvinyl chloride is dissolved into 1200mLN, N diformazans
In base formamide solution, then by step（1）Obtained modified nano graphite alkene is added thereto, magnetic agitation 30 minutes so that
Modified nano graphite alkene is tentatively dispersed in polyvinyl chloride solution；
（3）By step（2）Product is mixed with the 360g sodium chloride dried, and is put into ball mill, and ball-milling medium is 3000g oxidation
Zirconium ball, with 600 revs/min of speed ball milling 60 minutes；Then the mixture after ball milling is added dropwise in distilled water and be molded, until
With 500 revs/min of speed agitator treating 4 hours after dripping off completely, first water was changed every 40 minutes, then detection washing
Chlorion in liquid, until can't detect chlorion, is considered as and cleans up completely；
（4）By the above-mentioned product filtering cleaned up, it is put into refrigerator after being freezed 10 hours at -18 DEG C and inserts freeze drier
Middle drying 12 hours.
Claims (6)
1. a kind of preparation method of cellular PVC graphene composite material, it is characterised in that including step in detail below：
（1）Nano-graphene and dimethyl silicone polymer are put into closed measuring cup, is put into Muffle furnace, is heated to 230-
240 DEG C are incubated 60-80 minutes, are taken out after cooling, obtain modified nano graphite alkene；
（2）By sodium chloride be placed in baking oven with 100-110 DEG C dry 20-24 hours it is stand-by, by step（1）Obtained modified Nano stone
Black alkene is added in polyvinyl chloride solution, magnetic agitation 30-40 minutes so that modified nano graphite alkene is tentatively dispersed in polychlorostyrene second
In alkene solution；
（3）By step（2）Product is mixed with the sodium chloride dried, and is put into ball mill, with 600-800 revs/min of speed ball milling
60-90 minutes；Then the mixture after ball milling is added dropwise in distilled water and be molded, until turned with 500-600 after dripping off completely/
The speed agitator treating divided 4-5 hours, until cleaning up completely；
（4）By the above-mentioned product filtering cleaned up, it is put into refrigerator after being freezed 8-12 hours at -20--18 DEG C and inserts freezing
Dried 12-24 hours in drying machine.
2. a kind of preparation method of cellular PVC graphene composite material according to claim 1, it is characterised in that
Step（1）Described nano-graphene and the mass ratio of dimethyl silicone polymer are 10:1.
3. a kind of preparation method of cellular PVC graphene composite material according to claim 1, it is characterised in that
Step（2）Described polyvinyl chloride solution refers to that polyvinyl chloride is dissolved in the solution formed in DMF, and quality
Concentration is 0.075g/mL.
4. a kind of preparation method of cellular PVC graphene composite material according to claim 1, it is characterised in that
Step（2）The addition of described modified nano graphite alkene is the 1wt% of polyvinyl chloride, and the addition of the sodium chloride is polychlorostyrene
4 times of ethene.
5. a kind of preparation method of cellular PVC graphene composite material according to claim 1, it is characterised in that
Step（3）Ball-milling medium is zirconia ball in described mechanical milling process, and addition is 3-5 times of total material.
6. a kind of preparation method of cellular PVC graphene composite material according to claim 1, it is characterised in that
Step（3）Described washing, is comprised the following steps that：First water was changed every 40-60 minutes, is then detected in cleaning solution
Chlorion, until can't detect chlorion, is considered as and cleans up.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710419593.9A CN107213880A (en) | 2017-06-06 | 2017-06-06 | A kind of preparation method of cellular PVC graphene composite material |
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| CN201710419593.9A CN107213880A (en) | 2017-06-06 | 2017-06-06 | A kind of preparation method of cellular PVC graphene composite material |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111994893A (en) * | 2020-07-24 | 2020-11-27 | 盐城工学院 | Preparation method of nitrogen-doped carbon material |
| CN112940411A (en) * | 2021-01-29 | 2021-06-11 | 大连理工大学 | Graphene/polyvinyl chloride composite packaging material and preparation method thereof |
Citations (3)
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|---|---|---|---|---|
| CN103146024A (en) * | 2013-03-19 | 2013-06-12 | 苏州格瑞丰纳米科技有限公司 | Porous graphene/polymer composite structure and preparation method and application thereof |
| CN105233335A (en) * | 2015-11-06 | 2016-01-13 | 四川大学 | Porous polyaryletherketone material with bioactivity, and preparation method and application thereof |
| CN105735047A (en) * | 2016-02-01 | 2016-07-06 | 东南大学 | Preparation method of conductive and super-hydrophobic functional graphene paper |
-
2017
- 2017-06-06 CN CN201710419593.9A patent/CN107213880A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103146024A (en) * | 2013-03-19 | 2013-06-12 | 苏州格瑞丰纳米科技有限公司 | Porous graphene/polymer composite structure and preparation method and application thereof |
| CN105233335A (en) * | 2015-11-06 | 2016-01-13 | 四川大学 | Porous polyaryletherketone material with bioactivity, and preparation method and application thereof |
| CN105735047A (en) * | 2016-02-01 | 2016-07-06 | 东南大学 | Preparation method of conductive and super-hydrophobic functional graphene paper |
Non-Patent Citations (2)
| Title |
|---|
| 秦晓娟: ""改性石墨烯的制备及其超疏水性能研究"", 《中国优秀硕士学位论文全文数据库工程科技I辑》 * |
| 陈韩莉: ""两种聚氯乙烯/石墨烯复合材料的制备及其性能研究"", 《中国优秀硕士学位论文全文数据库工程科技I辑》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111994893A (en) * | 2020-07-24 | 2020-11-27 | 盐城工学院 | Preparation method of nitrogen-doped carbon material |
| CN112940411A (en) * | 2021-01-29 | 2021-06-11 | 大连理工大学 | Graphene/polyvinyl chloride composite packaging material and preparation method thereof |
| CN112940411B (en) * | 2021-01-29 | 2022-08-05 | 大连理工大学 | Graphene/polyvinyl chloride composite packaging material and preparation method thereof |
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Application publication date: 20170929 |