CN105014982A - Preparation method of graphene and polytetrafluoroethylene osmotic distillation film - Google Patents
Preparation method of graphene and polytetrafluoroethylene osmotic distillation film Download PDFInfo
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Abstract
The invention relates to a preparation method of a graphene and polytetrafluoroethylene osmotic distillation film. According to the preparation method, a nano graphene solution or an oxidized graphene aqueous solution and ultra-high molecular polytetrafluoroethylene dispersion resin powder are mixed, and the graphene and polytetrafluoroethylene osmotic distillation film is prepared through the processes of mixing, blank forming, extruding, rolling, longitudinal drawing after degreasing treatment, sintering solidification after transverse drawing, rewinding, secondary sintering solidification and demolding. The average pore size of the prepared hollow tubular film is 0.05 micron-1 micron, the porosity of the prepared hollow tubular film is larger than 80%, and the salt rejection rate of the prepared hollow tubular film is larger than 99%. The film has good chemical stability, self-lubrication performance and high-low temperature tolerance characteristics, and the temperature ranges from minus 240 DEG C to 260 DEG C. The film cannot be hardened or embrittled as time goes. The cold flow property of pure polytetrafluoroethylene sealing materials is overcome. The PH value ranges from 0 to 14. Sewage blocking is prevented. Surface lubrication is good. The aperture ratio reaches over 85%. The film is suitable for various types of high-corrosivity sewage treatment, salty alkaline water distillation desalination, liquid-solid separation, gas-water separation and oil-water separation.
Description
Technical field:
The invention belongs to water environment protection technical field, more specifically to a kind of preparation method of Graphene polytetrafluoroethylene (PTFE) osmotic distillation film.
Background technology:
In recent years, due to the fast development of industry, becoming increasingly conspicuous of shortage of water resources and pollution problem, having higher requirement to water treatment, is also that water technology is faced with new challenges and opportunity to develop.The fields such as the sewage disposal that various corrosivity is strong, the distillation of salty buck desalination, solid-liquor separation, gas-water separation, water-oil separating all need to face water treatment problems.
Membrane Materials is the one of low temperature distillation technology, is the innovation based on conventional film isolation technics.Current reverse osmosis membrane technology replaces traditional ion-exchange, electrodialysis desalination technology gradually, become the one preferred technique of pure water manufacture, city, industrial wastewater pollution degree of depth Treatment for Reuse, but the theoretical producing water ratio of reverse osmosis membrane technology only has 75%, reality only about 60%, desalination is only limited to less than 8%, and energy consumption is higher.Some problems such as current existing above Membrane Materials mode all exists moisture film hydrophiling leakage problems, solute substance fouling and clogging microporous barrier, and energy consumption is high simultaneously, efficiency is low, reliability is low.Therefore study new membrane technology particularly important, be reduce investment and operating cost, reduce concentrated water discharge move towards the industrialization use inevitable choice.
Summary of the invention:
The object of this invention is to provide a kind of preparation method of Graphene polytetrafluoroethylene (PTFE) osmotic distillation film, be applicable to the strong sewage disposal of various corrosivity, the distillation of salty buck desalination, solid-liquor separation, gas-water separation, water-oil separating etc.The present invention is economic and practical.
As follows for realizing the technology solution that object of the present invention adopts:
The preparation method of Graphene polytetrafluoroethylene (PTFE) osmotic distillation film, it comprises the following steps:
1. batch mixing: the nano-graphene solution of ketones solvent or graphene oxide water solution are mixed with polytetrafluoroethyldispersion dispersion resin powder, add hydro carbons extrusion aid, 24 hours are left standstill at 50 ~ 70 DEG C, make extrusion aid fully infiltrate through the nano-graphene solution of ketones solvent and the mixture of polytetrafluoroethyldispersion dispersion resin powder, form material.
2. base: cylindrical base material being pressed at 40 ~ 50 DEG C Φ 120mm in advance.
3. extrude: cylindrical base is placed on pushing machine, under 55 ~ 60 DEG C of conditions, be forced into the round bar of Φ 12 ~ Φ 22mm.
4. roll: circle bar is placed on calender, under 70 DEG C of conditions, is rolled into oil-containing base band.
5. longitudinal stretching after ungrease treatment: by the degreasing at 260 DEG C ~ 280 DEG C of oil-containing base band, remove extrusion aid, and carry out first time longitudinal stretching, draw ratio is become degreasing base band after 3 ~ 6 times; At 280 DEG C ~ 300 DEG C, carry out second time longitudinal stretching, stretching ratio is 4 ~ 8 times, obtains longitudinal stretching Ranvier's membrane.
6. sintering curing after cross directional stretch: by longitudinal stretching Ranvier's membrane, cross directional stretch at 120 DEG C ~ 200 DEG C, then 350 DEG C ~ 380 DEG C sintering curings 50 seconds, namely preparing thickness is 20 ~ 40 microns, and aperture is at the Graphene polytetrafluoroethylene (PTFE) microwell plate Ranvier's membrane of 0.05 ~ 0.5 micron.
7. rewinding: be that the microporous teflon membran of 0.5 micron carries out tight multireel and oppositely unreels by conventional aperture, and roll up again to desired thickness, or to cut after membrane coat or dipping and to carry out screw-type wrapped to desired thickness, rolling is on the core rod scribbling high-temperature mold lubricant, and the thickness of the microporous teflon membran of the periosteum after rolling is 50 ~ 500 microns; Then to reel outward Graphene polytetrafluoroethylene (PTFE) microwell plate Ranvier's membrane at described periosteum, the thickness of the Graphene polytetrafluoroethylene (PTFE) microwell plate Ranvier's membrane of winding is 50-200 micron, forms pipe rod after rolling.
8. double sintering solidification: in the excellent high temperature sintering furnace putting into 327 DEG C-360 DEG C of the pipe wound, sintering makes the polytetrafluoroethylbulked bulked pipe rod of Graphene for 20 ~ 180 minutes.
9. the demoulding: by step 8. in obtained Graphene polytetrafluoroethylbulked bulked pipe rod be cooled to room temperature after the demoulding obtain the hydrophobic hollow periosteum of Graphene polytetrafluoroethylene (PTFE), hollow periosteum diameter is 4 ~ 30 millimeters, hollow periosteum average pore size 0.05 ~ 1 micron.
As preferably, the weight ratio of the nano-graphene solution of ketones solvent or graphene oxide water solution, polytetrafluoroethyldispersion dispersion resin powder and hydro carbons extrusion aid is 0.003 ~ 0.1:1:0.25 ~ 0.3.
As preferably, in the nano-graphene solution of described ketones solvent, Graphene is black liquor, and ketone is as solvent, and the average grain diameter of the nano-graphene solution of ketones solvent is 10-100nm.
As preferably, in the nano-graphene solution of described ketones solvent, the concentration of ketones solvent is less than 1mg/ml, and thickness is 0.7-1.2nm, individual layer rate >90%, and particle diameter 100-1000nm, Fe content is less than 100PPM.
As preferably, the solvent of described graphene oxide water solution is deionized water, and the pH value of graphene oxide water solution is 5 ~ 7, concentration 0.001 ~ 10mg/ml, individual layer rate >98%, and thickness is 0.6-1.0nm, lamella diameter 10 ~ 50 μm.
Adopt preparation method's preparation-obtained Graphene polytetrafluoroethylene (PTFE) microporous hydrophobic hollow periosteum of nano-graphene microporous teflon membran.
Beneficial effect of the present invention is:
The present invention using nano-graphene liquid (nitrogen methyl pyrrolidone is as solvent) or graphene oxide water solution and the mixing of supra polymer polytetrafluoroethyldispersion dispersion resin powder, through batch mixing, base, extrude, roll, after longitudinal stretching, cross directional stretch, the processes of sintering curing, rewinding (core rod winding is combined into pipe), double sintering solidification, the demoulding is made after ungrease treatment.Graphene polytetrafluoroethylene (PTFE) osmotic distillation film prepared by the present invention, technique is simple, economic and practical.The nano-graphene polytetrafluoroethylene (PTFE) osmotic distillation film utilizing the present invention to prepare, average pore size 0.05 ~ 1 micron, porosity more than 80%, salt rejection rate more than 99%.Use the hollow periosteum that the present invention prepares, there is good chemical stability, self lubricity, overcome the cold flow properties (creep) of pure PTFE stuffing materials, electric conductivity, can not harden along with the time or the characteristic of brittle (good springiness) and high-low temperature resistant-240 DEG C ~ 260 DEG C, pH value 0-14, antifouling stifled, surface lubrication is outstanding, and percent opening is up to more than 85%.Be applicable to the strong sewage disposal of various corrosivity, the distillation of salty buck desalination, solid-liquor separation, gas-water separation, water-oil separating etc.
Detailed description of the invention:
Below in conjunction with embodiment, the invention will be further described, but the present invention's scope required for protection is not limited to the scope described by embodiment.
Embodiment 1, the preparation method of Graphene polytetrafluoroethylene (PTFE) osmotic distillation film, it comprises the following steps:
1. batch mixing: the polytetrafluoroethyldispersion dispersion resin powder of the nano-graphene solution of ketones solvent (nitrogen methyl pyrrolidone) with middle vast and boundless morning twilight chemicals 216G is mixed, wherein Graphene is black liquor, nitrogen methyl pyrrolidone is as solvent, the preparation method of the nano-graphene solution of ketones solvent is: first adopt the Hummers method of improvement to prepare graphene oxide, cationic surfactant modification is utilized to obtain modified graphene on this basis, stable graphene dispersing solution is obtained through ultrasonic process in ketones solvent, graphene dispersing solution average grain diameter is 50nm, concentration is less than 1mg/ml, in the preparation process of the nano-graphene solution of ketones solvent, the concentration of ketones solvent is less than 1mg/ml, thickness is 0.7-1.2nm, individual layer rate >90%, particle diameter 100-1000nm, Fe content is less than 100PPM.Then aviation kerosine is added as hydro carbons cosolvent, the weight ratio of the nano-graphene solution of ketones solvent, polytetrafluoroethyldispersion dispersion resin powder and hydro carbons extrusion aid is 0.005:1:0.25,24 hours are left standstill at 50 DEG C, make extrusion aid fully infiltrate through the nano-graphene solution of ketones solvent and the mixture of polytetrafluoroethyldispersion dispersion resin powder, form material.
2. base: cylindrical base material being pressed at 40 DEG C Φ 120mm in advance;
3. extrude: cylindrical base is placed on pushing machine, under 55 DEG C of conditions, be forced into the round bar of Φ 12mm;
4. roll: circle bar is placed on calender, under 70 DEG C of conditions, is rolled into oil-containing base band;
5. longitudinal stretching after ungrease treatment: by the degreasing at 260 DEG C of oil-containing base band, remove extrusion aid, and carry out first time longitudinal stretching, draw ratio is become degreasing base band after 4 times; At 280 DEG C, carry out second time longitudinal stretching, stretching ratio is 5 times, obtains longitudinal stretching Ranvier's membrane;
6. sintering curing after cross directional stretch: by longitudinal stretching Ranvier's membrane, cross directional stretch at 150 DEG C, then sintering curing 50 seconds at 360 DEG C, namely preparing thickness is 25 microns, and aperture is the Graphene polytetrafluoroethylene (PTFE) microwell plate Ranvier's membrane of 0.1 micron;
7. rewinding: be that the microporous teflon membran of 0.5 micron carries out tight multireel and oppositely unreels by conventional aperture, and roll up again to desired thickness, rolling is on the core rod scribbling high-temperature mold lubricant, and the thickness of the microporous teflon membran of the periosteum after rolling is 200 microns; Then to reel outward Graphene polytetrafluoroethylene (PTFE) microwell plate Ranvier's membrane at described periosteum, the thickness of the Graphene polytetrafluoroethylene (PTFE) microwell plate Ranvier's membrane of winding is 100 microns, forms pipe rod after rolling;
8. double sintering solidification: in the excellent high temperature sintering furnace putting into 330 DEG C of the pipe wound, sintering makes the polytetrafluoroethylbulked bulked pipe rod of Graphene after 50 minutes;
9. the demoulding: by step 8. in the obtained polytetrafluoroethylbulked bulked pipe rod of Graphene be cooled to room temperature after the demoulding obtain Graphene polytetrafluoroethylene (PTFE) microporous hydrophobic hollow periosteum, hollow periosteum diameter is 10 millimeters.
The Graphene polytetrafluoroethylene (PTFE) microporous hydrophobic hollow periosteum adopting above-mentioned technique to prepare, wherein hollow periosteum average pore size 0.2 micron, porosity is 85%, salt rejection rate 99.5%.
Embodiment 2, the preparation method of Graphene polytetrafluoroethylene (PTFE) osmotic distillation film, it comprises the following steps:
1. batch mixing: graphene oxide water solution is mixed with the F1065 polytetrafluoroethyldispersion dispersion resin powder of Daikin chemicals production, the solvent of graphene oxide water solution is deionized water, the pH value of graphene oxide water solution is 5 ~ 7, concentration 0.001 ~ 10mg/ml, individual layer rate >98%, thickness is 0.6-1.0nm, lamella diameter 10 ~ 50 μm, and graphene oxide water solution is black liquor.Then the ISOPARK of Exxon Mobil Corporation is added as hydro carbons extrusion aid, the weight ratio of graphene oxide water solution, polytetrafluoroethyldispersion dispersion resin powder and hydro carbons extrusion aid is 0.1:1:0.3,24 hours are left standstill at 70 DEG C, make extrusion aid fully infiltrate through the mixture of graphene oxide water solution and polytetrafluoroethyldispersion dispersion resin powder, form material;
2. base: cylindrical base material being pressed at 50 DEG C Φ 120mm in advance;
3. extrude: cylindrical base is placed on pushing machine, under 60 DEG C of conditions, be forced into the round bar of Φ 20mm;
4. roll: circle bar is placed on calender, under 70 DEG C of conditions, is rolled into oil-containing base band;
5. longitudinal stretching after ungrease treatment: by the degreasing at 280 DEG C of oil-containing base band, remove extrusion aid, and carry out first time longitudinal stretching, draw ratio is become degreasing base band after 5 times; At 300 DEG C, carry out second time longitudinal stretching, stretching ratio is 8 times, obtains longitudinal stretching Ranvier's membrane;
6. sintering curing after cross directional stretch: by longitudinal stretching Ranvier's membrane, cross directional stretch at 200 DEG C, then 380 DEG C of sintering curings 50 seconds, namely preparing thickness is 40 microns, and aperture is at the Graphene polytetrafluoroethylene (PTFE) microwell plate Ranvier's membrane of 0.5 micron;
7. rewinding: be that the microporous teflon membran of 0.5 micron carries out tight multireel and oppositely unreels by conventional aperture, and roll up again to desired thickness, or to cut after membrane coat or dipping and to carry out screw-type wrapped to desired thickness, rolling is on the core rod scribbling high-temperature mold lubricant, and the thickness of the microporous teflon membran of the periosteum after rolling is 400 microns; Then to reel outward Graphene polytetrafluoroethylene (PTFE) microwell plate Ranvier's membrane at described periosteum, the thickness of the Graphene polytetrafluoroethylene (PTFE) microwell plate Ranvier's membrane of winding is 200 microns, forms pipe rod after rolling;
8. double sintering solidification: in the excellent high temperature sintering furnace putting into 360 DEG C of the pipe wound, sintering makes the polytetrafluoroethylbulked bulked pipe rod of Graphene for 150 minutes;
9. the demoulding: by step 8. in obtained Graphene polytetrafluoroethylbulked bulked pipe rod be cooled to room temperature after the demoulding obtain the hydrophobic hollow periosteum of Graphene polytetrafluoroethylene (PTFE), hollow periosteum diameter is 25 millimeters, hollow periosteum average pore size 1 micron.
The Graphene polytetrafluoroethylene (PTFE) micropore microporous hydrophobic hollow periosteum adopting above-mentioned technique to prepare, wherein hollow periosteum average pore size 0.5 micron, porosity is 90%, salt rejection rate 99.9%.
Claims (6)
1. the preparation method of Graphene polytetrafluoroethylene (PTFE) osmotic distillation film, it is characterized in that, it comprises the following steps:
1. batch mixing: the nano-graphene solution of ketones solvent or graphene oxide water solution are mixed with polytetrafluoroethyldispersion dispersion resin powder, add hydro carbons extrusion aid, 24 hours are left standstill at 50 ~ 70 DEG C, make extrusion aid fully infiltrate through the nano-graphene solution of ketones solvent and the mixture of polytetrafluoroethyldispersion dispersion resin powder, form material;
2. base: cylindrical base material being pressed at 40 ~ 50 DEG C Φ 120mm in advance;
3. extrude: cylindrical base is placed on pushing machine, under 55 ~ 60 DEG C of conditions, be forced into the round bar of Φ 12 ~ Φ 22mm;
4. roll: circle bar is placed on calender, under 70 DEG C of conditions, is rolled into oil-containing base band;
5. longitudinal stretching after ungrease treatment: by the degreasing at 260 DEG C ~ 280 DEG C of oil-containing base band, remove extrusion aid, and carry out first time longitudinal stretching, draw ratio is become degreasing base band after 3 ~ 6 times; At 280 DEG C ~ 300 DEG C, carry out second time longitudinal stretching, stretching ratio is 4 ~ 8 times, obtains longitudinal stretching Ranvier's membrane;
6. sintering curing after cross directional stretch: by longitudinal stretching Ranvier's membrane, cross directional stretch at 120 DEG C ~ 200 DEG C, then 350 DEG C ~ 380 DEG C sintering curings 50 seconds, namely preparing thickness is 20 ~ 40 microns, and aperture is at the Graphene polytetrafluoroethylene (PTFE) microwell plate Ranvier's membrane of 0.05 ~ 0.5 micron;
7. rewinding: be that the microporous teflon membran of 0.5 micron carries out tight multireel and oppositely unreels by conventional aperture, and roll up again to desired thickness, or to cut after membrane coat or dipping and to carry out screw-type wrapped to desired thickness, rolling is on the core rod scribbling high-temperature mold lubricant, and the thickness of the microporous teflon membran of the periosteum after rolling is 50 ~ 500 microns; Then to reel outward Graphene polytetrafluoroethylene (PTFE) microwell plate Ranvier's membrane at described periosteum, the thickness of the Graphene polytetrafluoroethylene (PTFE) microwell plate Ranvier's membrane of winding is 50-200 micron, forms pipe rod after rolling;
8. double sintering solidification: in the excellent high temperature sintering furnace putting into 327 DEG C-360 DEG C of the pipe wound, sintering makes the polytetrafluoroethylbulked bulked pipe rod of Graphene for 20 ~ 180 minutes;
9. the demoulding: by step 8. in obtained Graphene polytetrafluoroethylbulked bulked pipe rod be cooled to room temperature after the demoulding obtain the hydrophobic hollow periosteum of Graphene polytetrafluoroethylene (PTFE), hollow periosteum diameter is 4 ~ 30 millimeters, hollow periosteum average pore size 0.05 ~ 1 micron.
2. the preparation method of Graphene polytetrafluoroethylene (PTFE) osmotic distillation film according to claim 1, is characterized in that: the weight ratio of the nano-graphene solution of ketones solvent or graphene oxide water solution, polytetrafluoroethyldispersion dispersion resin powder and hydro carbons extrusion aid is 0.003 ~ 0.1:1:0.25 ~ 0.3.
3. the preparation method of Graphene polytetrafluoroethylene (PTFE) osmotic distillation film according to claim 1, it is characterized in that: in the nano-graphene solution of described ketones solvent, Graphene is black liquor, ketone is as solvent, and the average grain diameter of the nano-graphene solution of ketones solvent is 10-100nm.
4. the preparation method of Graphene polytetrafluoroethylene (PTFE) osmotic distillation film according to claim 3, it is characterized in that: in the nano-graphene solution of described ketones solvent, the concentration of ketones solvent is less than 1mg/ml, thickness is 0.7-1.2nm, individual layer rate >90%, particle diameter 100-1000nm, Fe content is less than 100PPM.
5. the preparation method of Graphene polytetrafluoroethylene (PTFE) osmotic distillation film according to claim 2, it is characterized in that: the solvent of described graphene oxide water solution is deionized water, the pH value of graphene oxide water solution is 5 ~ 7, concentration 0.001 ~ 10mg/ml, individual layer rate >98%, thickness is 0.6-1.0nm, lamella diameter 10 ~ 50 μm.
6. preparation method's preparation-obtained Graphene polytetrafluoroethylene (PTFE) microporous hydrophobic hollow periosteum of Graphene polytetrafluoroethylene (PTFE) osmotic distillation film according to claim 1.
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| CN109912924A (en) * | 2019-03-05 | 2019-06-21 | 深圳市驭晟新材料科技有限公司 | A kind of preparation of the composite modified filler of graphene-nanometer polytetrafluoroethylcomposite and its application method |
| CN109939571A (en) * | 2019-04-01 | 2019-06-28 | 江西师范大学 | A kind of graphene oxide frame composite membrane and its preparation method and application |
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| CN112745608A (en) * | 2020-12-29 | 2021-05-04 | 施柏德（厦门）科技有限公司 | PTFE composite material with excellent uniformity and manufacturing process and application thereof |
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| CN108332592A (en) * | 2018-03-13 | 2018-07-27 | 武汉工程大学 | Loop circuit heat pipe capable of fast starting |
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