CN110283411A - A kind of low cold flow polytetrafluoroethylene (PTFE) moulded board and preparation method thereof - Google Patents
A kind of low cold flow polytetrafluoroethylene (PTFE) moulded board and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to a kind of low cold flow polytetrafluoroethylene (PTFE) moulded boards and preparation method thereof, raw material is poured into mixing machine high speed to stir 2 ~ 3 times, mixing 15min every time, after mixing to raw material, mixed raw material is uniformly sprinkled into pressing mold at room temperature, carry out forming operation, control cold pressing forming process parameter is briquetting pressure 40Mpa ~ 60Mpa, compacting rate is 3 ~ 7Mpa/min, 10 ~ 20min of dwell time, gained sample is sintered solidification, sintering is since 100 DEG C, 30min is kept the temperature at 2 DEG C/min to 320 DEG C of heating rate of control, 350 ~ 380 DEG C are sintered to again with the rate of 3 DEG C/min, after keep the temperature 60min, after naturally cooling to 320 DEG C, keep the temperature 60min, naturally cool to room temperature, it carries out afterwards normal Rule processing has low compacted property and hypotoxicity to get low cold flow polytetrafluoroethylene (PTFE) moulded board, gained polytetrafluoroethylene (PTFE) moulded board.
Description
Technical field
The present invention relates to a kind of polytetrafluoroethylene (PTFE) moulded boards and preparation method thereof, particularly with regard to a kind of low cold flow
(low creep) polytetrafluoroethylene (PTFE) moulded board and preparation method thereof.
Background technique
Polytetrafluoroethylene (PTFE) (Poly tetra fluoroethylene, be abbreviated as PTFE), commonly referred to as " non-sticking lining " or
" material easy to clean ".This material has the characteristics that antiacid alkali resistant, resists various organic solvents, is practically insoluble in all solvents.
Meanwhile polytetrafluoroethylene (PTFE) has the characteristics that resistant to high temperature, its coefficient of friction is extremely low, so also becoming after can making lubricating action
The ideal coating of water pipe internal layer easy to clean.
High temperature resistant --- using operating temperature up to 250 DEG C；It is low temperature resistant --- there is good mechanical tenacity；At a temperature of even if
- 196 DEG C are dropped to, 5% elongation can also be kept；It is corrosion-resistant --- to most of chemicals and solvent, show inertia, energy
Strong alkali-acid resistance, water and various organic solvents.
Polytetrafluoroethylene (PTFE) relative molecular mass is larger, low to be hundreds of thousands of, high up to 10,000,000 or more, generally millions of
(degree of polymerization in the 10^4 order of magnitude, and polyethylene is only in 10^3).General crystallinity is 90~95%, and melting temperature is 327~342
℃.CF2 unit is arranged by zigzag fashion in polytetrafluoroethylene (PTFE) molecule, since fluorine atom radius is slightly larger compared with carbon, so adjacent CF2
Unit cannot press trans- crossed orientation completely, but form a spiral helicine twisting chain, and fluorine atom almost covers entire height
The surface of strand.This molecular structure explains the various performances of polytetrafluoroethylene (PTFE).When temperature is lower than 19 DEG C, 13/6 spiral shell is formed
Rotation；It is undergone phase transition at 19 DEG C, molecule is slightly unlocked, and 15/7 spiral is formed.
Polyfluortetraethylene plate (being also tetrafluoro plate, Teflon plate, Teflon plate) be divided to molding and two kinds of turning, moulded board be by
Polyflon is formed with die pressing at normal temperature, then is made through sintering, cooling.PTFE lathed plates are by poly- four
Fluoroethylene resin is formed through green compact, sintering, rotary-cut.Its product-use is wide, with extremely superior comprehensive performance: high-low temperature resistant (-
192 DEG C -260 DEG C), corrosion-resistant (strong acid, highly basic, chloroazotic acid etc.), weatherability, high insulation, it is high lubricate, do not adhere to, nonhazardous etc. it is excellent
Good characteristic.Polytetrafluoroethylene (PTFE) (english abbreviation is Teflon or [PTFE, F4]), be/is commonly called as " King ", Chinese commodity by good reputation
Name " Teflon ", " teflon " (teflon), " Teflon ", " Te Fulong ", " safe fluorine dragon " etc..
It is as tetrafluoroethene it is aggregated made of high-molecular compound, skeleton symbol be-[- CF2-CF2-] n-,
With excellent chemical stability, corrosion resistance, (polytetrafluoroethylene (PTFE) abbreviation PTFE or F4 are the world today's most corrosion-resistant materials
One of, " King " is being commonly called as polytetrafluoroethylene (PTFE), it is a kind of plastics that corrosion resistance is best.It not by known acid, alkali,
The corrosion of salt, oxidant, chloroazotic acid also have no way out to it, and hence obtain one's name King, in addition to molten metal sodium and liquid fluorine, energy
All resistance to other chemicals, be widely used in it is various need antiacid alkali and organic solvent, leakproofness, high lubrication and non-stickiness,
Electrical insulating property and good anti-aging endurance, heatproof are excellent (can+250 DEG C to -180 DEG C of at a temperature of long-term work).Poly- four
Vinyl fluoride itself does not have toxicity to people, but one of raw material used in process of production perfluorooctanoic acid (PFOA) is considered
There may be carcinogenesis.
Polytetrafluoroethylene (PTFE) has " cold flow properties ".That is material product plastic deformation for occurring under the effect of long-time continuous load
(creep), this brings certain limitation to its application.
Patent of invention 201610437341.4 discloses a kind of carbon nanotube-teflon valve sealing of low creep
Circle, is prepared by the component of following parts by weight: 8-10 parts of the copolymer of 100 parts of polytetrafluoroethylene (PTFE), polyethylene and tetrafluoroethene,
5-8 parts of carbon nanotube, 1-2 parts of molybdenum disulfide, 8-10 parts of phenol, 8-10 parts of p-methylbenzoic acid, 1-2 parts of graphite powder, diphenyl ether
5-8 parts, 1-3 parts of butyl titanate, 20-25 parts of 60-70% sodium hypochlorite, 20-25 parts of EDTA, 40-50 parts of ammonium hydroxide, dehydrated alcohol
80-100 parts, 1-2 parts of bauxite corundum, 1-3 parts of silane coupling agent kh550,9-10 parts of ammonium chloride, 30-35 parts of urea, water 30-35
Part.Carbon nanometer-teflon valve sealing ring of low creep disclosed by the invention has the smallest creep relaxation rate, so that its
The features such as tensile strength is higher, and chemical inertness is good, and creep-resistant property is stronger, after tested: drawing high intensity 18MPa；Extension at break
Rate 210%；Impact strength 21.5KJ/m；Bending strength 28MPa；Wear away 4.2mm3(250N, linear velocity 2m/s are loaded, the time 3 divides
Clock).
Chinese patent discloses a kind of fluorine plastics combined gasket seal of filled-type and washer (publication number CN 1109088A),
Using filled-type fluorine composite material, proportion be (: 1) with the copolymer of perfluoroethylene-propylene or ethylene and tetrafluoroethene be mainly at
Part, account for the 30-90%(of total stuff amount；2) polytetrafluoroethylene (PTFE) is added, accounts for the 8-50%(of total stuff amount；3) inorfil element is added, Zhan is total
The 2-20% of doses, inorfil element can be the mixture of carbon fiber, calcium and magnesium silicate and glass fibre；Also wherein two be can be used
Kind is a kind of.But there is creep relaxation and cold flow in the material of the sealing element of the patent disclosure, make it in sealing position
Used time deformation, loss of seal ability.
Summary of the invention
Present invention aims to overcome that the existing modeling occurred under the effect of long-time continuous load of polytetrafluoroethylene (PTFE) template
Property deformation (creep) and the substitute of fluorine ammonium caprylate that uses of production process, the performance of Lai Tigao polytetrafluoroethylene (PTFE) template, this hair
The bright plastic deformation for enhancing its long-time continuous load again using reinforcing agent, astringent and cold-resistant agent, using substance A replacement fluorine
Ammonium caprylate (perfluorooctanoic acid), reduces the toxicity of product.
A kind of low cold flow polytetrafluoroethylene (PTFE) moulded board and preparation method thereof, which is characterized in that the group of the following parts by weight
Divide and be prepared: 90 parts of polytetrafluoroethylene (PTFE), 7-9 parts of nano zircite, 2-3 parts of nano-titanium dioxide, 1-4 parts of sodium citrate, lemon
1-3 parts of lemon acid amide, 2-7 parts of 4- methoxysalicylic amide, 8-10 parts of iminodiacetic acid, 1-5 parts of graphite powder, maleic anhydride 3-
8 parts, 1-4 parts of butyl titanate, 7-16 parts of aminotriacetic acid, 1-6 parts of iso-octyl trichlorosilane, 1 ~ 5 part of reinforcing agent, astringent 0.5
~ 2 parts, 1-2 parts of cold-resistant agent, 0.6 ~ 1.1 part of substance A.
Preparation method is that the component by right 1 is uniformly mixed, pretreatment, mixing, molding, sintering, cooling, post-processing
After obtain the low cold flow polytetrafluoroethylene (PTFE) moulded board；Detailed process is that the material of claim 1 is poured into mixing machine high speed to stir
It mixes 2 ~ 3 times, mixes 15min every time, after mixing to raw material, be at room temperature uniformly sprinkled into mixed raw material in pressing mold,
Forming operation is carried out, control cold pressing forming process parameter is briquetting pressure 40Mpa ~ 60Mpa, and compacting rate is 3 ~ 7Mpa/min,
Gained sample is sintered solidification, is sintered since 100 DEG C by 10 ~ 20min of dwell time, and control 2 DEG C/min of heating rate is arrived
30min is kept the temperature at 320 DEG C, then is sintered to 350 ~ 380 DEG C with the rate of 3 DEG C/min, is kept the temperature 60min afterwards, is naturally cooled to 320 DEG C
Afterwards, 60min is kept the temperature, room temperature is naturally cooled to, the rear conventional treatment that carries out is to get low cold flow polytetrafluoroethylene (PTFE) moulded board.
Reinforcing agent the preparation method comprises the following steps: by 10 parts of bentonite, 1-2 parts of methyltriethoxysilane, 0.5 part of boric acid, carboxylic first
2.1 parts and 10 parts of water of base sodium cellulosate are uniformly mixed, and 1.3 parts of hexamethylolmelamine is added at 60 ~ 80 DEG C and span comes
1.7 parts of acid imide, it is stirred to react 1 ~ 2h, cooling and drying obtains the reinforcing agent.
The astringent the preparation method comprises the following steps: 15 parts of citric acid and aluminum sulfate 2-3 parts are added in 10 parts of water, add
1-3.1 parts and tannic acid 1-2 parts of maleic acid (purchase is in Wuhan far at for creating Science and Technology Ltd.) stirs anti-at 70 ~ 90 DEG C
1 ~ 2h is answered, cooling filter is dried to obtain the astringent.
The cold-resistant agent the preparation method comprises the following steps: by 10 parts of ethyl acrylate, 3 parts of D-sorbite, 1 ~ 2 part of aluminum acetate, 12
0.5 part and 10 parts water of sodium alkyl sulfate are stirred to react 1 ~ 2h at 60 ~ 70 DEG C, 1 part of trishydroxymethylaminomethane are added, in this
Temperature the reaction was continued 1h, it is cooling, remove moisture, obtains cold-resistant agent.
The cold-resistant agent the preparation method comprises the following steps: substance A be carbotriamine, N, N- dicyclohexylcarbodiimide any one.
Present invention has an advantage that
(1) reinforcing effect of reinforcing agent is improved using hexamethylolmelamine and bismaleimide；
(2) the anti-astringent and low creep properties of maleic acid and tannic acid raising material；
(3) trishydroxymethylaminomethane and aluminum acetate improve low creep properties of the material again under cryogenic conditions；
(4) carbotriamine, N, N- dicyclohexylcarbodiimide reduces the toxicity of product, instead of perfluorooctanoic acid.
(5) unmentioned technological parameter influences less performance in step, therefore does not refer in hello prolixity.
Specific implementation method
Example one
A kind of low cold flow polytetrafluoroethylene (PTFE) moulded board and preparation method thereof, which is characterized in that the component system of the following parts by weight
It is standby to form: 90 parts of polytetrafluoroethylene (PTFE), 7 parts of nano zircite, 2 parts of nano-titanium dioxide, 1 part of sodium citrate, citric mide 1
Part, 2 parts of 4- methoxysalicylic amide, 8 parts of iminodiacetic acid, 1 part of graphite powder, 3 parts of maleic anhydride, 1 part of butyl titanate, amino
7 parts of triacetic acid, 1 part of iso-octyl trichlorosilane, 1 part of reinforcing agent, 0.5 part of astringent, 1 part of cold-resistant agent, 0.6 ~ part of carbotriamine.
Preparation method is for above-mentioned component to be uniformly mixed, pretreatment, mixing, molding, sintering, cooling, post-processing
After obtain the low cold flow polytetrafluoroethylene (PTFE) moulded board；Detailed process is that above-mentioned raw material is poured into mixing machine high speed to stir 2 times,
Mixed raw material after mixing to raw material is uniformly sprinkled into pressing mold at room temperature, is formed by mixing 15min every time
Operation, control cold pressing forming process parameter are briquetting pressure 40Mpa, and compacting rate is 3Mpa/min, dwell time 10min, are incited somebody to action
Gained sample is sintered solidification, is sintered since 100 DEG C, keeps the temperature 30min at 2 DEG C/min to 320 DEG C of heating rate of control, then
350 DEG C are sintered to the rate of 3 DEG C/min, keeps the temperature 60min afterwards, after naturally cooling to 320 DEG C, 60min is kept the temperature, naturally cools to
Room temperature, the rear conventional treatment that carries out is to get low cold flow polytetrafluoroethylene (PTFE) moulded board.
Reinforcing agent the preparation method comprises the following steps: by 10 parts of bentonite, 1 part of methyltriethoxysilane, 0.5 part of boric acid, carboxymethyl
2.1 parts and 10 parts of water of sodium cellulosate are uniformly mixed, and 1.3 parts of hexamethylolmelamine and bismaleimide are added at 60 DEG C
1.7 parts, it is stirred to react 1h, cooling and drying obtains the reinforcing agent.
The astringent the preparation method comprises the following steps: 15 parts of citric acid and 2 parts of aluminum sulfate are added in 10 parts of water, add suitable
1 part of butene dioic acid and 1 part of tannic acid (purchase is in Wuhan far at for creating Science and Technology Ltd.) are stirred to react 1h at 70 DEG C, cooling to take out
Filter is dried to obtain the astringent.
The cold-resistant agent the preparation method comprises the following steps: by 10 parts of ethyl acrylate, 3 parts of D-sorbite, 1 part of aluminum acetate, dodecane
0.5 part and 10 parts water of base sodium sulphate are stirred to react 1h at 60 DEG C, add 1 part of trishydroxymethylaminomethane, in this temperature after
Continuous reaction 1h, it is cooling, remove moisture, obtains cold-resistant agent.
Example two
A kind of low cold flow polytetrafluoroethylene (PTFE) moulded board and preparation method thereof, which is characterized in that the component system of the following parts by weight
It is standby to form: 90 parts of polytetrafluoroethylene (PTFE), 9 parts of nano zircite, 3 parts of nano-titanium dioxide, 4 parts of sodium citrate, citric mide 3
Part, 7 parts of 4- methoxysalicylic amide, 10 parts of iminodiacetic acid, 5 parts of graphite powder, 8 parts of maleic anhydride, 4 parts of butyl titanate, ammonia
16 parts of base triacetic acid, 6 parts of iso-octyl trichlorosilane, 5 parts of reinforcing agent, 2 parts of astringent, 2 parts of cold-resistant agent, N, N- dicyclohexyl carbon two
1.1 parts of imines.
Preparation method is for the component of above-mentioned raw materials to be uniformly mixed, pretreatment, mixing, molding, sintering, cooling, after
The low cold flow polytetrafluoroethylene (PTFE) moulded board is obtained after processing；Detailed process is that above-mentioned raw materials are poured into mixing machine high speed stirring 3
It is secondary, mix 15min every time, after mixing to raw material, be at room temperature uniformly sprinkled into mixed raw material in pressing mold, carry out at
Type operation, control cold pressing forming process parameter be briquetting pressure 60Mpa, compacting rate be 7Mpa/min, dwell time 20min,
Gained sample is sintered solidification, is sintered since 100 DEG C, control 2 DEG C/min of heating rate, which is warming up at 320 DEG C, to be kept the temperature
30min, then 380 DEG C are sintered to the rate heating of 3 DEG C/min, 60min is kept the temperature afterwards, after naturally cooling to 320 DEG C, heat preservation
60min naturally cools to room temperature, and the rear conventional treatment that carries out is to get low cold flow polytetrafluoroethylene (PTFE) moulded board.
Reinforcing agent the preparation method comprises the following steps: by 10 parts of bentonite, 2 parts of methyltriethoxysilane, 0.5 part of boric acid, carboxymethyl
2.1 parts and 10 parts of water of sodium cellulosate are uniformly mixed, and 1.3 parts of hexamethylolmelamine and bismaleimide are added at 80 DEG C
1.7 parts, it is stirred to react 2h, cooling and drying obtains the reinforcing agent.
The astringent the preparation method comprises the following steps: 15 parts of citric acid and 3 parts of aluminum sulfate are added in 10 parts of water, add suitable
1-3.1 parts and tannic acid 1-2 parts of butene dioic acid (purchase is in Wuhan far at for creating Science and Technology Ltd.) is stirred to react 2h at 90 DEG C,
Cooling filter is dried to obtain the astringent.
The cold-resistant agent the preparation method comprises the following steps: by 10 parts of ethyl acrylate, 3 parts of D-sorbite, 2 parts of aluminum acetate, dodecane
0.5 part and 10 parts water of base sodium sulphate are stirred to react 2h at 70 DEG C, add 1 part of trishydroxymethylaminomethane, in this temperature after
Continuous reaction 1h, it is cooling, remove moisture, obtains cold-resistant agent.
Example three
A kind of low cold flow polytetrafluoroethylene (PTFE) moulded board and preparation method thereof, which is characterized in that the component system of the following parts by weight
It is standby to form: 90 parts of polytetrafluoroethylene (PTFE), 8 parts of nano zircite, 2.5 parts of nano-titanium dioxide, 2.5 parts of sodium citrate, citric acid acyl
2 parts of amine, 4.5 parts of 4- methoxysalicylic amide, 9 parts of iminodiacetic acid, 3 parts of graphite powder, 5.5 parts of maleic anhydride, butyl titanate
2.5 parts, 11.5 parts of aminotriacetic acid, 3.5 parts of iso-octyl trichlorosilane, 3 parts of reinforcing agent, 1.25 parts of astringent, cold-resistant agent 1.5
Part, 0.85 part of carbotriamine.
Preparation method is for the component of above-mentioned raw materials to be uniformly mixed, pretreatment, mixing, molding, sintering, cooling, after
The low cold flow polytetrafluoroethylene (PTFE) moulded board is obtained after processing；Detailed process is that above-mentioned raw materials are poured into mixing machine high speed stirring 3
It is secondary, mix 15min every time, after mixing to raw material, be at room temperature uniformly sprinkled into mixed raw material in pressing mold, carry out at
Type operation, control cold pressing forming process parameter be briquetting pressure 50Mpa, compacting rate be 5Mpa/min, dwell time 15min,
Gained sample is sintered solidification, is sintered since 100 DEG C, control 2 DEG C/min of heating rate, which is warming up at 320 DEG C, to be kept the temperature
30min, then 60min is kept the temperature for 365 DEG C with the rate heating sintering temperature of 3 DEG C/min afterwards, after naturally cooling to 320 DEG C, heat preservation
60min naturally cools to room temperature, and the rear conventional treatment that carries out is to get low cold flow polytetrafluoroethylene (PTFE) moulded board.
Reinforcing agent the preparation method comprises the following steps: by 10 parts of bentonite, 1.5 parts of methyltriethoxysilane, 0.5 part of boric acid, carboxylic first
2.1 parts and 10 parts of water of base sodium cellulosate are uniformly mixed, and 1.3 parts of hexamethylolmelamine and bismaleimide are added at 70 DEG C
1.7 parts of amine, it is stirred to react 1.5h, cooling and drying obtains the reinforcing agent.
The astringent the preparation method comprises the following steps: 15 parts of citric acid and 2.5 parts of aluminum sulfate are added in 10 parts of water, add
2 parts and tannic acid 1-2 parts of maleic acid (purchase is in Wuhan far at for creating Science and Technology Ltd.) is stirred to react 1.5h at 80 DEG C,
Cooling filter is dried to obtain the astringent.
The cold-resistant agent the preparation method comprises the following steps: by 10 parts of ethyl acrylate, 3 parts of D-sorbite, 1.5 parts of aluminum acetate, 12
0.5 part and 10 parts water of sodium alkyl sulfate are stirred to react 1.5h at 65 DEG C, add 1 part of trishydroxymethylaminomethane, in this temperature
Degree the reaction was continued 1h, it is cooling, remove moisture, obtains cold-resistant agent.
Example four
A kind of low cold flow polytetrafluoroethylene (PTFE) moulded board and preparation method thereof, which is characterized in that the component system of the following parts by weight
It is standby to form: 90 parts of polytetrafluoroethylene (PTFE), 7 parts of nano zircite, 2 parts of nano-titanium dioxide, 4 parts of sodium citrate, citric mide 3
Part, 7 parts of 4- methoxysalicylic amide, 8- parts of iminodiacetic acid, 2 parts of graphite powder, 4 parts of maleic anhydride, 2 parts of butyl titanate, ammonia
8 parts of base triacetic acid, 3 parts of iso-octyl trichlorosilane, 2 parts of reinforcing agent, 1 part of astringent, 1.5 parts of cold-resistant agent, N, N- dicyclohexyl carbon
0.7 part of diimine.
Preparation method is for the component of above-mentioned raw materials to be uniformly mixed, pretreatment, mixing, molding, sintering, cooling, after
The low cold flow polytetrafluoroethylene (PTFE) moulded board is obtained after processing；Detailed process is that above-mentioned raw materials are poured into mixing machine high speed stirring 2
It is secondary, mix 15min every time, after mixing to raw material, be at room temperature uniformly sprinkled into mixed raw material in pressing mold, carry out at
Type operation, control cold pressing forming process parameter be briquetting pressure 60Mpa, compacting rate be 4Mpa/min, dwell time 10min,
Gained sample is sintered solidification, is sintered since 100 DEG C, control 2 DEG C/min of heating rate, which is warming up at 320 DEG C, to be kept the temperature
30min, then 60min is kept the temperature to 370 DEG C with the rate heating sintering temperature of 3 DEG C/min afterwards, after naturally cooling to 320 DEG C, heat preservation
60min naturally cools to room temperature, and the rear conventional treatment that carries out is to get low cold flow polytetrafluoroethylene (PTFE) moulded board.
Reinforcing agent the preparation method comprises the following steps: by 10 parts of bentonite, 1.5 parts of methyltriethoxysilane, 0.5 part of boric acid, carboxylic first
2.1 parts and 10 parts of water of base sodium cellulosate are uniformly mixed, and 1.3 parts of hexamethylolmelamine and bismaleimide are added at 70 DEG C
1.7 parts of amine, it is stirred to react 1h, cooling and drying obtains the reinforcing agent.
The astringent the preparation method comprises the following steps: 15 parts of citric acid and 2 parts of aluminum sulfate are added in 10 parts of water, add suitable
2 parts of butene dioic acid and 1 part of tannic acid (purchase is in Wuhan far at for creating Science and Technology Ltd.) are stirred to react 1.5h at 80 DEG C, cooling
Suction filtration is dried to obtain the astringent.
The cold-resistant agent the preparation method comprises the following steps: by 10 parts of ethyl acrylate, 3 parts of D-sorbite, 1 part of aluminum acetate, dodecane
0.5 part and 10 parts water of base sodium sulphate are stirred to react 2h at 70 DEG C, add 1 part of trishydroxymethylaminomethane, in this temperature after
Continuous reaction 1h, it is cooling, remove moisture, obtains cold-resistant agent.
Example five
A kind of low cold flow polytetrafluoroethylene (PTFE) moulded board and preparation method thereof, which is characterized in that the component system of the following parts by weight
It is standby to form: 90 parts of polytetrafluoroethylene (PTFE), 8 parts of nano zircite, 2.5 parts of nano-titanium dioxide, 3 parts of sodium citrate, citric mide 3
Part, 4 parts of 4- methoxysalicylic amide, 8 parts of iminodiacetic acid, 5 parts of graphite powder, 8 parts of maleic anhydride, 4 parts of butyl titanate, amino
7 parts of triacetic acid, 3 parts of iso-octyl trichlorosilane, 2 parts of reinforcing agent, 1 part of astringent, 1 part of cold-resistant agent, 1.1 parts of carbotriamine.
Preparation method is for the component of raw material to be uniformly mixed, pretreatment, mixing, molding, sintering, cooling, post-processing
After obtain the low cold flow polytetrafluoroethylene (PTFE) moulded board；Detailed process is that above-mentioned raw materials are poured into mixing machine high speed stirring 3 times, often
Mixed raw material after mixing to raw material is uniformly sprinkled into pressing mold by secondary mixing 15min at room temperature, carries out molding behaviour
Make, control cold pressing forming process parameter is briquetting pressure 50Mpa, and compacting rate is 4Mpa/min, dwell time 10min, by institute
It obtaining sample and is sintered solidification, be sintered since 100 DEG C, control 2 DEG C/min of heating rate, which is warming up at 320 DEG C, keeps the temperature 30min,
Sintering temperature is improved to 370 DEG C with the rate of 3 DEG C/min again, keeps the temperature 60min afterwards, after naturally cooling to 320 DEG C, keeps the temperature 60min,
Room temperature is naturally cooled to, the rear conventional treatment that carries out is to get low cold flow polytetrafluoroethylene (PTFE) moulded board.
Reinforcing agent the preparation method comprises the following steps: by 10 parts of bentonite, 2 parts of methyltriethoxysilane, 0.5 part of boric acid, carboxymethyl
2.1 parts and 10 parts of water of sodium cellulosate are uniformly mixed, and 1.3 parts of hexamethylolmelamine and bismaleimide are added at 80 DEG C
1.7 parts, it is stirred to react 2h, cooling and drying obtains the reinforcing agent.
The astringent the preparation method comprises the following steps: 15 parts of citric acid and 2.2 parts of aluminum sulfate are added in 10 parts of water, add
2 parts of maleic acid and 1.5 parts of tannic acid (purchase is in Wuhan far at for creating Science and Technology Ltd.) are stirred to react 1h at 80 DEG C, cold
But it filters and is dried to obtain the astringent.
The cold-resistant agent the preparation method comprises the following steps: by 10 parts of ethyl acrylate, 3 parts of D-sorbite, 2 parts of aluminum acetate, dodecane
0.5 part and 10 parts water of base sodium sulphate are stirred to react 1h at 70 DEG C, add 1 part of trishydroxymethylaminomethane, in this temperature after
Continuous reaction 1h, it is cooling, remove moisture, obtains cold-resistant agent.
The creep of use with reference to the Master's thesis " research of polytetrafluoroethylene (PTFE) croop property " of Chen Bibo testing standard, with
Compression ratio and response rate characterize material creep.
The creep properties of 1 teflon gasket of table
As it can be seen from table 1 the gasket has stronger compression ratio and response rate, show that the material has good low creep
Property.
The creep properties (not plus reinforcing agent) of 2 teflon gasket of table
From table 2 it can be seen that reinforcing agent is not added to show that the gasket has poor creep properties.
The creep properties (add reinforcing agent, not plus hexamethylolmelamine) of 3 teflon gasket of table
From table 3 it can be seen that plus reinforcing agent and plus hexamethylolmelamine show the gasket have poor creep properties.
The creep properties (add reinforcing agent, not plus bismaleimide) of 4 teflon gasket of table
From table 4, it can be seen that plus reinforcing agent and plus hexamethylolmelamine show the gasket have poor creep properties.
The creep properties (not plus astringent) of 5 teflon gasket of table
As can be seen from Table 5, not plus reinforcing agent show the gasket have poor astringent.
The creep properties (add astringent, not plus tannic acid) of 6 teflon gasket of table
As can be seen from Table 5, add astringent, not plus tannic acid shows that the gasket has poor astringent.
The creep properties (not plus cold-resistant agent) of 7 teflon gasket of table
As can be seen from Table 7, not plus the cold-resistant agent gasket have stronger compression ratio and response rate, show the material have creep
Property decline.
The creep properties (not plus aluminum acetate, add cold-resistant agent) of 8 teflon gasket of table
As can be seen from Table 8, add cold-resistant agent, not plus the aluminum acetate gasket has stronger compression ratio and response rate, shows the material
Expecting, there is creep properties, which to compare, does not add the performance of cold-resistant agent to increase.
The creep properties (not plus aluminum acetate, add cold-resistant agent) of 9 teflon gasket of table
| Example one | Example two | Example three | Example four | Example five | |
| Compression ratio/% | 10.17 | 9.01 | 8.54 | 7.99 | 8.79 |
| Response rate/% | 68.35 | 67.88 | 67.56 | 65.99 | 68.77 |
As can be seen from Table 7, not plus aluminum acetate, add the cold-resistant agent gasket that there is stronger compression ratio and response rate, show the material
Expecting to have to compare does not add the performance of cold-resistant agent to increase.
With Cytotoxic evaluation result (cell proliferation rate, 96h, with reference to Tang Zhuping, king and jade etc., Cell culture invitro skill
Toxicity [J] Chinese experimental zoology magazine of art evaluation experimental animal plastics cage tool), in 96h, example one arrives example five
Cell proliferation rate be 845%, 895%, 912%, 932% and 877%, if keep fluorine ammonium caprylate (perfluorooctanoic acid) substitute
The cell proliferation rate of matter A is respectively 215%, 189%, 277%, 266% and 175%.
The compression ratio of documents 201610437341.4 and the example one of publication number CN 1109088A is respectively 9.31%
With 10.55%, response rate is respectively 68.21% and 64.78%.
Claims (6)
1. a kind of low cold flow polytetrafluoroethylene (PTFE) moulded board and preparation method thereof, which is characterized in that the component of the following parts by weight
It is prepared: 90 parts of polytetrafluoroethylene (PTFE), 7-9 parts of nano zircite, 2-3 parts of nano-titanium dioxide, 1-4 parts of sodium citrate, lemon
Sour amide 1-3 parts, 2-7 parts of 4- methoxysalicylic amide, 8-10 parts of iminodiacetic acid, 1-5 parts of graphite powder, maleic anhydride 3-8
Part, 1-4 parts of butyl titanate, 7-16 parts of aminotriacetic acid, 1-6 parts of iso-octyl trichlorosilane, 1 ~ 5 part of reinforcing agent, astringent 0.5 ~
2 parts, 1-2 parts of cold-resistant agent, 0.6 ~ 1.1 part of substance A.
2. low cold flow polytetrafluoroethylene (PTFE) moulded board as described in claim 1 and preparation method thereof, which is characterized in that its preparation side
Method is that the component by right 1 is uniformly mixed, and it is poly- that the low cold flow is obtained after pretreatment, mixing, molding, sintering, cooling, post-processing
Tetrafluoroethene moulded board；Detailed process is that the material of claim 1 is poured into mixing machine high speed to stir 2 ~ 3 times, is mixed every time
Mixed raw material after mixing to raw material is uniformly sprinkled into pressing mold by 15min at room temperature, carries out forming operation, control
Cold pressing forming process parameter be briquetting pressure 40Mpa ~ 60Mpa, compacting rate be 3 ~ 7Mpa/min, 10 ~ 20min of dwell time,
Gained sample is sintered solidification, is sintered since 100 DEG C, keeps the temperature 30min at 2 DEG C/min to 320 DEG C of heating rate of control,
350 ~ 380 DEG C are sintered to the rate of 3 DEG C/min again, keeps the temperature 60min afterwards, after naturally cooling to 320 DEG C, keeps the temperature 60min, it is natural
It is cooled to room temperature, the rear conventional treatment that carries out is to get low cold flow polytetrafluoroethylene (PTFE) moulded board.
3. a kind of low cold flow polytetrafluoroethylene (PTFE) moulded board as described in claim 1 and preparation method thereof, which is characterized in that described
Reinforcing agent the preparation method comprises the following steps: by 10 parts of bentonite, 1-2 parts of methyltriethoxysilane, 0.5 part of boric acid, carboxymethyl cellulose
2.1 parts and 10 parts of water of sodium are uniformly mixed, and 1.3 parts of hexamethylolmelamine and bismaleimide 1.7 are added at 60 ~ 80 DEG C
Part, it is stirred to react 1 ~ 2h, cooling and drying obtains the reinforcing agent.
4. a kind of low cold flow polytetrafluoroethylene (PTFE) moulded board as described in claim 1 and preparation method thereof, which is characterized in that described
Astringent the preparation method comprises the following steps: 15 parts of citric acid and aluminum sulfate 2-3 parts are added in 10 parts of water, add maleic acid 1-
1 ~ 2h is stirred to react at 70 ~ 90 DEG C for 3.1 parts and tannic acid 1-2 parts (purchase is in Wuhan far at for creating Science and Technology Ltd.), it is cooling
Suction filtration is dried to obtain the astringent.
5. a kind of low cold flow polytetrafluoroethylene (PTFE) moulded board as described in claim 1 and preparation method thereof, which is characterized in that described
Cold-resistant agent the preparation method comprises the following steps: by 10 parts of ethyl acrylate, 3 parts of D-sorbite, 1 ~ 2 part of aluminum acetate, lauryl sodium sulfate 0.5
Part and 10 parts of water are stirred to react 1 ~ 2h at 60 ~ 70 DEG C, add 1 part of trishydroxymethylaminomethane, the reaction was continued in this temperature
1h, it is cooling, remove moisture, obtains cold-resistant agent.
6. a kind of low cold flow polytetrafluoroethylene (PTFE) moulded board as described in claim 1 and preparation method thereof, which is characterized in that described
Cold-resistant agent the preparation method comprises the following steps: substance A be carbotriamine, N, N- dicyclohexylcarbodiimide any one.
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| CN111040347A (en) * | 2019-12-20 | 2020-04-21 | 佛山科学技术学院 | Polytetrafluoroethylene composite material and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106084582A (en) * | 2016-06-20 | 2016-11-09 | 安徽荣达阀门有限公司 | A kind of CNT teflon valve sealing ring of low creep |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106084582A (en) * | 2016-06-20 | 2016-11-09 | 安徽荣达阀门有限公司 | A kind of CNT teflon valve sealing ring of low creep |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111040347A (en) * | 2019-12-20 | 2020-04-21 | 佛山科学技术学院 | Polytetrafluoroethylene composite material and preparation method thereof |
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