CN110157068A - A kind of ultra-high molecular weight polyethylene special graphite alkene microballoon mother material and preparation method - Google Patents
A kind of ultra-high molecular weight polyethylene special graphite alkene microballoon mother material and preparation method Download PDFInfo
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- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/20—Compounding polymers with additives, e.g. colouring
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- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/20—Compounding polymers with additives, e.g. colouring
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- C08J3/226—Compounding polymers with additives, e.g. colouring using masterbatch techniques using a polymer as a carrier
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- C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2323/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2323/04—Homopolymers or copolymers of ethene
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- C08J2483/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
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- C08K3/34—Silicon-containing compounds
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/16—Solid spheres
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- C08K7/00—Use of ingredients characterised by shape
- C08K7/22—Expanded, porous or hollow particles
- C08K7/24—Expanded, porous or hollow particles inorganic
Abstract
The present invention relates to a kind of ultra-high molecular weight polyethylene special graphite alkene microballoon mother material and preparation method thereof, graphene microballoon mother material includes filling kernel, graphene.Preparation method are as follows: graphite solution preparation；The preparation of graphene microspheres solution；The preparation of graphene microsphere powder.Graphene is wrapped in outside common filler particle by the present invention, graphene is set to be easier to save, it avoids reuniting, graphene can be effectively distributed in High molecular weight polyethylene, improving ultra-high molecular weight polyethylene has preferable melt-processed mobility, and utilize the high surface energy of graphene, moreover it is possible to guarantee that modified ultra high molecular polyethylene has excellent impact strength.
Description
Technical field
The present invention relates to ultra-high molecular weight polyethylene special graphite alkene preparation method fields, and in particular to a kind of supra polymer
Weight northylen special graphite alkene microballoon mother material and preparation method.
Background technique
Ultra-high molecular weight polyethylene English name ultra-high molecular weight polyethylene is (referred to as
It UHMWPE), is the unbranched linear polyethylene of 1,500,000 or more molecular weight.Molecular formula :-(- CH2-CH2 -)-n-, it is close
Degree: 0.920~0.964g/cm3.85 DEG C of heat distortion temperature (0.46MPa), 130~136 DEG C of fusing point.Ultra-high molecular weight polyethylene
It is a kind of high-molecular compound, is difficult to process, and wearability with super strength, self-lubrication, intensity is relatively high, chemical property
Stabilization, anti-aging property are strong.Since the viscosity of ultra-high molecular weight polyethylene (UHMW-PE) molten condition is up to 108Pa*s, flowing
Property it is very poor, compared with other engineering plastics, ultra-high molecular weight polyethylene (UHMW-PE) have surface hardness and heat distortion temperature
Low, the disadvantages of bending strength and croop property are poor.This is because the molecular structure of ultra-high molecular weight polyethylene (UHMW-PE)
With caused by molecule accumulation shape, can be improved by the method filled and be crosslinked.General filling glass microballoon, glass fibers
Dimension, mica, talcum powder, silica, aluminum oxide, molybdenum disulfide, carbon black etc., to ultra-high molecular weight polyethylene (UHMW-
PE it) is filled modification, surface hardness, rigidity, creep properties, bending strength, heat distortion temperature can be enable preferably to improve.With
After coupling agent treatment, effect is more obvious.Such as filling treated glass microballoon, heat distortion temperature can be made to improve 30 DEG C.Filling
Hardness, rigidity and temperature tolerance can be improved in glass microballoon, glass fibre, mica, talcum powder etc.；Molybdenum disulfide, silicone oil and Wax special
Friction factor can be reduced, to further increase self-lubrication；Carbon black or metal powder can be improved antistatic property and electric conductivity and
Conductivity of heat etc..But filler modified rear impact strength is declined slightly.
Graphene have excellent optics, electricity, mechanical characteristic, materialogy, micro-nano technology, the energy, biomedicine and
Drug delivery etc. is with important application prospects, excellent surface area, and can improve ultra-high molecular weight polyethylene has
Preferable melt-processed mobility, but graphene itself is easy to produce reunion, is not easy to disperse, cannot criticize since surface can be big
Amount is for producing.
Summary of the invention
To overcome the deficiency, the purpose of the present invention is to provide a kind of ultra-high molecular weight polyethylene special graphite alkene microballoons
Masterbatch and preparation method.
The technical solution adopted by the present invention to solve the technical problems is: a kind of ultra-high molecular weight polyethylene special graphite alkene
Microballoon mother material, including filling kernel, graphene.
Specifically, the filling kernel uses glass microballoon, mica, talcum powder, molybdenum disulfide, silicone oil, carbon black or metal
One of powder, wherein for improving hardness, rigidity and temperature tolerance, molybdenum disulfide, silicone oil are mentioned for glass microballoon, mica, talcum powder
High-wearing feature, carbon black or metal powder improve antistatic property, electric conductivity and heat transfer property.
Specifically, the partial size of the filling kernel is less than 2 microns.
Preparation method are as follows:
Step 1: prepared by graphite solution
The high-purity natural crystalline flake graphite of 100mg80 mesh is weighed in 250mL polytetrafluoroethylene (PTFE) autoclave, the N methyl of 100mL is added
Pyrrolidones (NMP) organic solvent, 140-160 DEG C of reaction 3-5h, obtained graphite dispersing solution is poured into Ultrasound Instrument, setting
Certain ultrasonic power, ultrasound are taken out after a certain period of time；
Step 2: prepared by graphene microspheres solution
The filling kernel of 2000-3000mg is added in graphite dispersing solution obtained in step 1, in the revolving speed of 2000r/min
Under, it is centrifuged 30min, takes upper liquid up to graphene/carrier solution, the graphene generated under high-speed rotation is wrapped in filling
Outside core；
Step 3: prepared by graphene microsphere powder
Graphene microspheres solution obtained in step 2 filters the NMP in removal graphene microspheres solution using cellulose membrane, uses
Deionized water is cleaned three times, then graphene microballoon is placed in the deionized water of 100mL, it is water-soluble that ultrasound obtains graphene microballoon
Graphene microballoon mother material powder is made by being freeze-dried in liquid.
Specifically, particles of fluoropolymer is added in the filling kernel, the partial size of particles of fluoropolymer is less than 2um, filling
The fineness ratio of kernel and particles of fluoropolymer is 1:(0.01-0.1).
Specifically, the graphene microballoon mother material powder that the step 3 obtains is coupled with 3- aminopropyl triethoxysilane
Agent flows back 2 hours in ethanol, obtain it is coupling agent modified after hungry graphene microballoon mother material.
The invention has the following advantages: graphene is wrapped in outside common filler particle, hold that graphene more
It is easy to maintain, it avoids reuniting, graphene can be effectively distributed in High molecular weight polyethylene, improve ultra-high molecular weight polyethylene
With preferable melt-processed mobility, and utilize the high surface energy of graphene, moreover it is possible to guarantee the poly- second of modified supra polymer
Alkene has excellent impact strength.
Specific embodiment
The present invention is described in further detail now.
Embodiment one
A kind of ultra-high molecular weight polyethylene special graphite alkene microballoon mother material, including filling kernel, graphene.
Specifically, the filling kernel uses glass microballoon, mica, talcum powder.
Specifically, the partial size of the filling kernel is less than 2 microns.
Preparation method are as follows:
Step 1: prepared by graphite solution
The high-purity natural crystalline flake graphite of 100mg80 mesh is weighed in 250mL polytetrafluoroethylene (PTFE) autoclave, the N methyl of 100mL is added
Pyrrolidones (NMP) organic solvent, 140-160 DEG C of reaction 4h, obtained graphite dispersing solution is poured into Ultrasound Instrument, setting one
Fixed ultrasonic power, ultrasound are taken out after a certain period of time；
Step 2: prepared by graphene microspheres solution
The filling kernel of 2000mg, under the revolving speed of 2000r/min, centrifugation is added in graphite dispersing solution obtained in step 1
30min takes upper liquid up to graphene/carrier solution, and the graphene generated under high-speed rotation is wrapped in outside filling kernel；
Step 3: prepared by graphene microsphere powder
Graphene microspheres solution obtained in step 2 filters the NMP in removal graphene microspheres solution using cellulose membrane, uses
Deionized water is cleaned three times, then graphene microballoon is placed in the deionized water of 100mL, it is water-soluble that ultrasound obtains graphene microballoon
Graphene microballoon mother material powder is made by being freeze-dried in liquid.
Specifically, particles of fluoropolymer is added in the filling kernel, the partial size of particles of fluoropolymer is less than 2um, filling
The fineness ratio of kernel and particles of fluoropolymer is 1:0.01.
Specifically, the graphene microballoon mother material powder that the step 3 obtains is coupled with 3- aminopropyl triethoxysilane
Agent flows back 2 hours in ethanol, obtain it is coupling agent modified after hungry graphene microballoon mother material.
Embodiment two
A kind of ultra-high molecular weight polyethylene special graphite alkene microballoon mother material, including filling kernel, graphene.
Specifically, the filling kernel uses one kind of molybdenum disulfide, silicone oil.
Specifically, the partial size of the filling kernel is less than 2 microns.
Preparation method are as follows:
Step 1: prepared by graphite solution
The high-purity natural crystalline flake graphite of 100mg80 mesh is weighed in 250mL polytetrafluoroethylene (PTFE) autoclave, the N methyl of 100mL is added
Pyrrolidones (NMP) organic solvent, 140-160 DEG C of reaction 5h, obtained graphite dispersing solution is poured into Ultrasound Instrument, setting one
Fixed ultrasonic power, ultrasound are taken out after a certain period of time；
Step 2: prepared by graphene microspheres solution
The filling kernel of 2200mg, under the revolving speed of 2000r/min, centrifugation is added in graphite dispersing solution obtained in step 1
30min takes upper liquid up to graphene/carrier solution, and the graphene generated under high-speed rotation is wrapped in outside filling kernel；
Step 3: prepared by graphene microsphere powder
Graphene microspheres solution obtained in step 2 filters the NMP in removal graphene microspheres solution using cellulose membrane, uses
Deionized water is cleaned three times, then graphene microballoon is placed in the deionized water of 100mL, it is water-soluble that ultrasound obtains graphene microballoon
Graphene microballoon mother material powder is made by being freeze-dried in liquid.
Specifically, particles of fluoropolymer is added in the filling kernel, the partial size of particles of fluoropolymer is less than 2um, filling
The fineness ratio of kernel and particles of fluoropolymer is 1:0.03.
Specifically, the graphene microballoon mother material powder that the step 3 obtains is coupled with 3- aminopropyl triethoxysilane
Agent flows back 2 hours in ethanol, obtain it is coupling agent modified after hungry graphene microballoon mother material.
Embodiment three
A kind of ultra-high molecular weight polyethylene special graphite alkene microballoon mother material, including filling kernel, graphene.
Specifically, the filling kernel uses one of carbon black or metal powder.
Specifically, the partial size of the filling kernel is less than 2 microns.
Preparation method are as follows:
Step 1: prepared by graphite solution
The high-purity natural crystalline flake graphite of 100mg80 mesh is weighed in 250mL polytetrafluoroethylene (PTFE) autoclave, the N methyl of 100mL is added
Pyrrolidones (NMP) organic solvent, 140-160 DEG C of reaction 4h, obtained graphite dispersing solution is poured into Ultrasound Instrument, setting one
Fixed ultrasonic power, ultrasound are taken out after a certain period of time；
Step 2: prepared by graphene microspheres solution
The filling kernel of 2500mg, under the revolving speed of 2000r/min, centrifugation is added in graphite dispersing solution obtained in step 1
30min takes upper liquid up to graphene/carrier solution, and the graphene generated under high-speed rotation is wrapped in outside filling kernel；
Step 3: prepared by graphene microsphere powder
Graphene microspheres solution obtained in step 2 filters the NMP in removal graphene microspheres solution using cellulose membrane, uses
Deionized water is cleaned three times, then graphene microballoon is placed in the deionized water of 100mL, it is water-soluble that ultrasound obtains graphene microballoon
Graphene microballoon mother material powder is made by being freeze-dried in liquid.
Specifically, particles of fluoropolymer is added in the filling kernel, the partial size of particles of fluoropolymer is less than 2um, filling
The fineness ratio of kernel and particles of fluoropolymer is 1:0.05.
Specifically, the graphene microballoon mother material powder that the step 3 obtains is coupled with 3- aminopropyl triethoxysilane
Agent flows back 2 hours in ethanol, obtain it is coupling agent modified after hungry graphene microballoon mother material.
Example IV
A kind of ultra-high molecular weight polyethylene special graphite alkene microballoon mother material, including filling kernel, graphene.
Specifically, the filling kernel uses mica.
Specifically, the partial size of the filling kernel is less than 2 microns.
Preparation method are as follows:
Step 1: prepared by graphite solution
The high-purity natural crystalline flake graphite of 100mg80 mesh is weighed in 250mL polytetrafluoroethylene (PTFE) autoclave, the N methyl of 100mL is added
Pyrrolidones (NMP) organic solvent, 140-160 DEG C of reaction 3h, obtained graphite dispersing solution is poured into Ultrasound Instrument, setting one
Fixed ultrasonic power, ultrasound are taken out after a certain period of time；
Step 2: prepared by graphene microspheres solution
The filling kernel of 2800mg, under the revolving speed of 2000r/min, centrifugation is added in graphite dispersing solution obtained in step 1
30min takes upper liquid up to graphene/carrier solution, and the graphene generated under high-speed rotation is wrapped in outside filling kernel；
Step 3: prepared by graphene microsphere powder
Graphene microspheres solution obtained in step 2 filters the NMP in removal graphene microspheres solution using cellulose membrane, uses
Deionized water is cleaned three times, then graphene microballoon is placed in the deionized water of 100mL, it is water-soluble that ultrasound obtains graphene microballoon
Graphene microballoon mother material powder is made by being freeze-dried in liquid.
Specifically, particles of fluoropolymer is added in the filling kernel, the partial size of particles of fluoropolymer is less than 2um, filling
The fineness ratio of kernel and particles of fluoropolymer is 1:0.08.
Specifically, the graphene microballoon mother material powder that the step 3 obtains is coupled with 3- aminopropyl triethoxysilane
Agent flows back 2 hours in ethanol, obtain it is coupling agent modified after hungry graphene microballoon mother material.
Embodiment five
A kind of ultra-high molecular weight polyethylene special graphite alkene microballoon mother material, including filling kernel, graphene.
Specifically, the filling kernel uses glass microballoon, mica, talcum powder, molybdenum disulfide, silicone oil, carbon black or metal
One of powder, wherein for improving hardness, rigidity and temperature tolerance, molybdenum disulfide, silicone oil are mentioned for glass microballoon, mica, talcum powder
High-wearing feature, carbon black or metal powder improve antistatic property, electric conductivity and heat transfer property.
Specifically, the partial size of the filling kernel is less than 2 microns.
Preparation method are as follows:
Step 1: prepared by graphite solution
The high-purity natural crystalline flake graphite of 100mg80 mesh is weighed in 250mL polytetrafluoroethylene (PTFE) autoclave, the N methyl of 100mL is added
Pyrrolidones (NMP) organic solvent, 140-160 DEG C of reaction 4h, obtained graphite dispersing solution is poured into Ultrasound Instrument, setting one
Fixed ultrasonic power, ultrasound are taken out after a certain period of time；
Step 2: prepared by graphene microspheres solution
The filling kernel of 3000mg, under the revolving speed of 2000r/min, centrifugation is added in graphite dispersing solution obtained in step 1
30min takes upper liquid up to graphene/carrier solution, and the graphene generated under high-speed rotation is wrapped in outside filling kernel；
Step 3: prepared by graphene microsphere powder
Graphene microspheres solution obtained in step 2 filters the NMP in removal graphene microspheres solution using cellulose membrane, uses
Deionized water is cleaned three times, then graphene microballoon is placed in the deionized water of 100mL, it is water-soluble that ultrasound obtains graphene microballoon
Graphene microballoon mother material powder is made by being freeze-dried in liquid.
Specifically, particles of fluoropolymer is added in the filling kernel, the partial size of particles of fluoropolymer is less than 2um, filling
The fineness ratio of kernel and particles of fluoropolymer is 1:0.1.
Specifically, the graphene microballoon mother material powder that the step 3 obtains is coupled with 3- aminopropyl triethoxysilane
Agent flows back 2 hours in ethanol, obtain it is coupling agent modified after hungry graphene microballoon mother material.
The present invention is not limited to the embodiment, anyone should learn that the structure made under the inspiration of the present invention becomes
Change, the technical schemes that are same or similar to the present invention are fallen within the scope of protection of the present invention.
Technology not described in detail in the present invention, shape, construction portion are well-known technique.
Claims (6)
1. a kind of ultra-high molecular weight polyethylene special graphite alkene microballoon mother material, it is characterised in that: including filling kernel, graphene.
2. a kind of ultra-high molecular weight polyethylene special graphite alkene microballoon mother material according to claim 1, it is characterised in that: institute
Filling kernel is stated using one of glass microballoon, mica, talcum powder, molybdenum disulfide, silicone oil, carbon black or metal powder.
3. a kind of ultra-high molecular weight polyethylene special graphite alkene microballoon mother material according to claim 1, it is characterised in that: institute
The partial size of filling kernel is stated less than 2 microns.
4. a kind of preparation method of ultra-high molecular weight polyethylene special graphite alkene microballoon mother material, it is characterised in that: including following step
Suddenly,
Step 1: prepared by graphite solution
The high-purity natural crystalline flake graphite of 100mg80 mesh is weighed in 250mL polytetrafluoroethylene (PTFE) autoclave, the N methyl of 100mL is added
Pyrrolidones organic solvent, 140-160 DEG C of reaction 3-5h, obtained graphite dispersing solution is poured into Ultrasound Instrument, and setting is certain
Ultrasonic power, ultrasound take out after a certain period of time；
Step 2: prepared by graphene microspheres solution
The filling kernel of 2000-3000mg is added in graphite dispersing solution obtained in step 1, in the revolving speed of 2000r/min
Under, it is centrifuged 30min, takes upper liquid up to graphene/carrier solution, the graphene generated under high-speed rotation is wrapped in filling
Outside core；
Step 3: prepared by graphene microsphere powder
Graphene microspheres solution obtained in step 2 filters the N methyl in removal graphene microspheres solution using cellulose membrane
Pyrrolidones is cleaned three times with deionized water, then graphene microballoon is placed in the deionized water of 100mL, ultrasound obtains stone
Graphene microballoon mother material powder is made by being freeze-dried in black alkene microballoon aqueous solution.
5. a kind of preparation method of ultra-high molecular weight polyethylene special graphite alkene microballoon mother material, it is characterised in that: in the filling
Particles of fluoropolymer is added in core, the partial size of particles of fluoropolymer is less than 2um, fills the fineness ratio of kernel and particles of fluoropolymer
For 1:(0.01-0.1).
6. a kind of preparation method of ultra-high molecular weight polyethylene special graphite alkene microballoon mother material, it is characterised in that: the step 3
Obtained graphene microballoon mother material powder, flows back 2 hours in ethanol with 3- aminopropyl triethoxysilane coupling agent, obtains idol
Join the modified hungry graphene microballoon mother material of agent.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110862577A (en) * | 2019-11-22 | 2020-03-06 | 北京航天凯恩化工科技有限公司 | Preparation method and application of unsaturated polyolefin loaded graphene master batch |
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| CN107022114A (en) * | 2017-05-26 | 2017-08-08 | 成都新柯力化工科技有限公司 | A kind of ultra-high molecular weight polyethylene special graphite alkene microballoon mother material and preparation method |
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| CN107151364A (en) * | 2017-05-22 | 2017-09-12 | 成都新柯力化工科技有限公司 | A kind of microballoon graphene enhancing masterbatch and preparation method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110862577A (en) * | 2019-11-22 | 2020-03-06 | 北京航天凯恩化工科技有限公司 | Preparation method and application of unsaturated polyolefin loaded graphene master batch |
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