CN106283249A - Polytetrafluoroethylsuperfine superfine fiber - Google Patents
Polytetrafluoroethylsuperfine superfine fiber Download PDFInfo
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- CN106283249A CN106283249A CN201510275243.0A CN201510275243A CN106283249A CN 106283249 A CN106283249 A CN 106283249A CN 201510275243 A CN201510275243 A CN 201510275243A CN 106283249 A CN106283249 A CN 106283249A
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- directional stretch
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Abstract
The present invention relates to a kind of polytetrafluoroethylsuperfine superfine fiber.Be made up of following methods, in turn include the following steps: lubrication mixing, screening, modified mix, extrude, roll, except boat coal, stretch, solidify removing oil, score a goal, it is characterised in that interpolation silicone oil in modified mixed process;Encrypt comb when scoring a goal and accelerate combing such that it is able to make 1D and following fiber and possess good physical property.This superfine fibre can be used for the filtration of high-temperature flue gas after making Nomex, while ensureing filtration flux, the best to the interception result of PM2.5, even if the biggest discharge capacity also can control PM2.5 discharge capacity at below 10mg/m3.
Description
Technical field
The present invention relates to a kind of polytetrafluoroethylsuperfine superfine fiber.
Background technology
In view of in air, PM2.5 remains high, air problem is paid attention to by compatriots again.PM2.5
Mostly come from combustion
Burn, carry out the enterprise generated electricity especially with coal.If it is huge that generating set is all reconstructed obviously investment.Prior art is deposited
At a kind of coated filter material.Coated filter material prepared by full politef has good filter effect, can be by the PM2.5 in flue gas
It is retained down.PTFE membrane filter material is generally that one layer is politef screen cloth casing play, another layer by double-layer structure
It is to be attached on teflon membrane filter thereon.PTFE membrane filter material rejection effect in the market 99% with
On.But the flux of coated filter material is low, i.e. filter efficiency is poor.If coated filter material to be used for the smoke stack emission mouth in thermal power plant,
The situation of booster the most very likely occurs, there is serious potential safety hazard.Prior art there is also a kind of Nomex, but due to
Technical reason, not yet prepares the Nomex of full politef, the Nomex of other materials, such as terylene needled felt, no
Being suitable for the process to high-temperature flue gas, and the rejection effect of this Nomex is the most undesirable, PM2.5 discharge capacity reaches 50mg/m3.Nomex is a kind of special construction of non-woven fabrics, is to use needing machine superfine fibre acupuncture to be made on special base material on special base material.Prior art has dacron ultrafine fiber, but the difficulty of processing of politef is big, not yet prepares the superfine fibre of politef.The thinnest polytetrafluoroethylene fibre can prepared in prior art is at about 5D, and prepares the fiber required for having the Nomex of good filter effect and need as little as 1D.
Summary of the invention
For solving above-mentioned technical problem, the present invention provides a kind of polytetrafluoroethylsuperfine superfine fiber.
The scheme that the present invention solves above-mentioned technical problem is as follows:
Polytetrafluoroethylsuperfine superfine fiber, is made up of following methods:
(1) lubrication mixing: add aerial kerosene, mixing in ptfe micropowder;
(2) screening: sieve with 10~30 mesh sieves;
(3) modified mixing: add silicone oil again, then mix;
(4) extrusion: using the raw material extrusion that modification is mixed by extruder, squeezing parameter is as follows, extruded velocity 5~15mm/min, extrudes diameter 15~25mm, and die entrance angle L/D is 20~40, cone angle 30~50 °, compression ratio 140~160;
(5) calendering: use calender that the raw material after extrusion is rolled, during calendering, roller temperature controls is 140~180 DEG C,
Prepare raw material band;
(6) except boat coal: little to described raw material band dried 18~24 higher than at a temperature of the boiling point of described aerial kerosene
Time, remove described aerial kerosene;
(7) stretching: carry out longitudinal stretching while raw material band is removed aerial kerosene, then carry out a thermal finalization;Then enter
Row cross directional stretch first, second heat sizing, cross directional stretch again, three thermal finalization, prepare polytetrafluoroethylfiber fiber film;Stretching is fixed
During type control parameter as follows: longitudinal stretching speed 1%~
10%/s, draw ratio 2~6, a heat setting temperature 200~250 DEG C;First cross directional stretch speed 45~
50mm/s, draw ratio 20~25, second heat setting temperature 200~250 DEG C;Cross directional stretch is that the raw material band after cross directional stretch first is redrawn 180~200 times again, rate of extension 20~30mm/s, and three heat setting temperatures control to be 250~300 DEG C, obtain shaping membrane;
(8) solidification removing oil: multiple Concourse Division formulas that described shaping membrane gradually rises in temperature being processed, described stagewise processes
Initial temperature be 300~320 DEG C, until described shaping membrane is heated to transparence, obtain finished film;
(9) score a goal: process that described finished film is scored a goal, the chi of former comb is buckled encryption by cutting machine, the combing of comb
Speed is accelerated, and described encryption is specially encryption 50~100%, and described quickening is specially accelerates 50~200%.
Preferred as technique scheme, the addition of described aerial kerosene is ptfe micropowder quality
10~30%.
Preferred as technique scheme, the addition of described silicone oil is the 1~10% of ptfe micropowder quality.
Preferred as technique scheme, the particle diameter of selected ptfe micropowder be 0.215~
0.225μm。
The selected aerial kerosene of the present invention is as lubricating oil so that ptfe micropowder can preferably be mixed, be added
Work, lubricating oil are preferably removed.Such as use aerial kerosene to have worse detachability than gasoline, but have preferably calendering
Property;Than diesel oil, there is more preferable detachability.The raw material band quality that described calenderability rolls out after referring to enter calendaring processes
Quality.The quality of raw material band quality has following standard: such as tensile property, the uniform performance of stretching, the thickness uniformity of raw material band
The intensity etc. of the raw material band after, drawing high.
After superfine fibre makes Nomex, examining under a microscope, Nomex surface can form fine hair shape, significantly increases
Its interdiction capability to PM2.5.And dacron ultrafine fiber thermostability is poor, under the influence of the temperature of high-temperature flue gas, the fine hair on surface can deform, and then affects its interdiction capability.And the C-F bond of polytetrafluoroethylmaterial material is closed very firm, and fluorine atom shields the carbon atom on main chain get up, and therefore, it is resistant to elevated temperatures that polytetrafluoroethylmaterial material has the strongest acid-fast alkali-proof
Ability.But this is also it is difficult to processed reason, because politef participates in the poor ability of chemical reaction, it is again line
Property molecule, the intermolecular ability of entwining is the lowest, therefore be difficult to politef ethylene is made superfine fibre by spin processes,
Even if it is the lowest to process its intensity, industrial cannot use.Therefore can only use pulling method, and current pulling method can only
Accomplish about 5D.Therefore, polytetrafluoroethylsuperfine superfine fiber to be prepared it is necessary to manufacture can be drawn evenly, thinner after, hot strength can continue to maintain;And also the polytetrafluoroethylraw raw material that comb to be stood encryption and combing speed acceleration process
Band.This just toughness to it propose new requirement.The present inventor improves raw material after with the addition of silicone oil in the feed significantly
The tensile property of band and intensity so that after thin film is made in stretching, this thin film can encrypted combing and acceleration combing when scoring a goal
And continuous, and remain good fracture strength.The most therefore, at conventional equipment after transformation, it is possible to produce 1D and following polytetrafluoroethylsuperfine superfine fiber.The Nomex that 1D and following polytetrafluoroethylene fibre are produced not only has good flux, good heat resistanceheat resistant performance, it may have good strainability, it is possible to substantially reduce PM2.5 in discharge flue gas
Content, PM 2.5 discharge capacity is at 10mg/m3
Below.
The finished film of the present invention, compared with the polytetrafluoroethylfiber fiber film that prior art prepares, has thinner characteristic, and
And hot strength than the stretched polytetrafluoroethylene intensity of prior art double left and right.This superfine fibre can be used after making Nomex
In the filtration of high-temperature flue gas, while ensureing filtration flux, the best to the interception result of PM2.5, even if the biggest discharge capacity also can control PM2.5 discharge capacity at 10mg/m3
Below.
[in sum, the method have the advantages that
The polytetrafluoroethylfiber fiber film that the present invention prepares has more preferable toughness, it is possible to drawn the thinnest evenly, when scoring a goal
Comb encryption can be stood and acceleration processes.Thus, the polytetrafluoroethylfiber fiber film of the present invention can prepare superfine fibre.
This superfine fibre, after making Nomex, can effectively solve the problem of PTFE coated filter material in prior art, and the problem of dacron ultrafine fiber Nomex in prior art, it is possible to by the fume emission of coal-fired power plant, controls PM
2.5 discharge capacitys are at below 10mg/m3.
Detailed description of the invention
This specific embodiment is only explanation of the invention, and it is not limitation of the present invention, people in the art
The present embodiment can be made after reading this specification by member as required does not has the amendment of creative contribution, but as long as at this
All protected by Patent Law in the right of invention.
Embodiment one
Polytetrafluoroethylsuperfine superfine fiber, is made up of following methods:
(1) lubrication mixing: add aerial kerosene, mixing in ptfe micropowder;The addition of described aerial kerosene is poly-
The 10% of tetrafluoroethene micropowder quality;The particle diameter of selected ptfe micropowder is 0.215
~0.225 μm;
(2) screening: sieve with 10~30 mesh sieves;
(3) modified mixing: add silicone oil again, then mix;The addition of described silicone oil is the 1% of ptfe micropowder quality;
(4) extrusion: using the raw material extrusion that modification is mixed by extruder, squeezing parameter is as follows, extruded velocity 5~15mm/min,
Extrusion diameter 15~25mm, die entrance angle L/D is 20~40, cone angle 30~50 °, compression ratio 140~160;
(5) calendering: use calender that the raw material after extrusion is rolled, during calendering, roller temperature controls is 140~180 DEG C,
Prepare raw material band;
(6) except boat coal: little to described raw material band dried 18~24 higher than at a temperature of the boiling point of described aerial kerosene
Time, remove described aerial kerosene;
(7) stretching: carry out longitudinal stretching while raw material band is removed described aerial kerosene, then carry out a thermal finalization;Connect
And carry out cross directional stretch first, second heat is shaped, cross directional stretch again, three thermal finalization, prepares polytetrafluoroethylfiber fiber film;Parameter is controlled as follows: longitudinal stretching speed 1%/s, draw ratio 2, a heat setting temperature 200~250 DEG C during drawing and setting;Cross directional stretch speed 45mm/s first, draw ratio 20, second heat setting temperature 200~250 DEG C;Cross directional stretch is that the raw material band after cross directional stretch first is redrawn 180 times again, rate of extension 20 mm/s, and three heat setting temperatures control to be 250~300 DEG C, obtain shaping membrane;
(8) solidification removing oil: multiple Concourse Division formulas that described shaping membrane gradually rises in temperature being processed, described stagewise processes
Initial temperature be 300~320 DEG C, until described shaping membrane is heated to transparence, obtain finished film;Described finished film elongation at break 30%, hot strength 10Mpa
;
(9) score a goal: process that described finished film is scored a goal, the chi of former comb is buckled encryption by cutting machine, the combing of comb
Speed is accelerated, and described encryption is specially encryption 50%, and described quickening is specially quickening 50%.
The computational methods of elongation at break are as follows:
Elongation at break=△
L/L0*100% ;
(former long L0, under axial tension effect, the breaking length after deformation is L, then extension at break △ L=L-L0)
The computational methods of hot strength are as follows: σ t=p/(b × d)
σ t is hot strength (MPa);P is peak load (N);B is specimen width (mm);D is sample thickness (mm).
Embodiment two
Polytetrafluoroethylsuperfine superfine fiber, is made up of following methods:
(1) lubrication mixing: add aerial kerosene, mixing in ptfe micropowder;The addition of described aerial kerosene is poly-
The 13% of tetrafluoroethene micropowder quality;The particle diameter of selected ptfe micropowder is 0.215
~0.225 μm;
(2) screening: sieve with 10~30 mesh sieves;
(3) modified mixing: add silicone oil again, then mix;The addition of described silicone oil is the 2% of ptfe micropowder quality;
(4) extrusion: using the raw material extrusion that modification is mixed by extruder, squeezing parameter is as follows, extruded velocity 5~15mm/min, extrudes diameter 15~25mm, and die entrance angle L/D is 20~40, cone angle 30~50 °, compression ratio 140~160;
(5) calendering: use calender that the raw material after extrusion is rolled, during calendering, roller temperature controls is 140~180 DEG C,
Prepare raw material band;
(6) except boat coal: little to described raw material band dried 18~24 higher than at a temperature of the boiling point of described aerial kerosene
Time, remove described aerial kerosene;
(7) stretching: carry out longitudinal stretching while raw material band is removed described aerial kerosene, then carry out a thermal finalization;Connect
And carry out cross directional stretch first, second heat is shaped, cross directional stretch again, three thermal finalization, prepares polytetrafluoroethylfiber fiber film;Parameter is controlled as follows: longitudinal stretching speed 2%/s, draw ratio 2, a heat setting temperature 200~250 DEG C during drawing and setting;Cross directional stretch speed 45mm/s first, draw ratio 20, second heat setting temperature 200~250 DEG C;Cross directional stretch is that the raw material band after cross directional stretch first is redrawn 182 times again, rate of extension 21 mm/s, and three heat setting temperatures control to be 250~300 DEG C, obtain shaping membrane;
(8) solidification removing oil: multiple Concourse Division formulas that described shaping membrane gradually rises in temperature being processed, described stagewise processes
Initial temperature be 300~320 DEG C, until described shaping membrane is heated to transparence, obtain finished film;Elongation at break 30%, hot strength 10Mpa
;
(9) score a goal: process that described finished film is scored a goal, the chi of former comb is buckled encryption by cutting machine, the combing of comb
Speed is accelerated, and described encryption is specially encryption 50%, and described quickening is specially quickening 60%.
The computational methods of elongation at break are as follows:
Elongation at break=△
L/L0*100% ;
(former long L0, under axial tension effect, the breaking length after deformation is L, then extension at break △ L=L-L0)
The computational methods of hot strength are as follows: σ t=p/(b × d)
σ t is hot strength (MPa);P is peak load (N);B is specimen width (mm);D is sample thickness (mm).
Embodiment three
Polytetrafluoroethylsuperfine superfine fiber, is made up of following methods:
(1) lubrication mixing: add aerial kerosene, mixing in ptfe micropowder;The addition of described aerial kerosene is poly-
The 16% of tetrafluoroethene micropowder quality;The particle diameter of selected ptfe micropowder is 0.215
~0.225 μm;
(2) screening: sieve with 10~30 mesh sieves;
(3) modified mixing: add silicone oil again, then mix;The addition of described silicone oil is the 3% of ptfe micropowder quality;
(4) extrusion: using the raw material extrusion that modification is mixed by extruder, squeezing parameter is as follows, extruded velocity 5~15mm/min, extrudes diameter 15~25mm, and die entrance angle L/D is 20~40, cone angle 30~50 °, compression ratio 140~160;
(5) calendering: use calender that the raw material after extrusion is rolled, during calendering, roller temperature controls is 140~180 DEG C,
Prepare raw material band;
(6) except boat coal: little to described raw material band dried 18~24 higher than at a temperature of the boiling point of described aerial kerosene
Time, remove described aerial kerosene;
(7) stretching: carry out longitudinal stretching while raw material band is removed described aerial kerosene, then carry out a thermal finalization;Connect
And carry out cross directional stretch first, second heat is shaped, cross directional stretch again, three thermal finalization, prepares polytetrafluoroethylfiber fiber film;Parameter is controlled as follows: longitudinal stretching speed 13%/s, draw ratio 3, a heat setting temperature 200~250 DEG C during drawing and setting;Cross directional stretch speed 46mm/s first, draw ratio 21, second heat setting temperature 200~250 DEG C;Cross directional stretch is that the raw material band after cross directional stretch first is redrawn 184 times again, rate of extension 22 mm/s, and three heat setting temperatures control to be 250~300 DEG C, obtain shaping membrane;
(8) solidification removing oil: multiple Concourse Division formulas that described shaping membrane gradually rises in temperature being processed, described stagewise processes
Initial temperature be 300~320 DEG C, until described shaping membrane is heated to transparence, obtain finished film;Elongation at break 30%, hot strength 10Mpa
;
(9) score a goal: process that described finished film is scored a goal, the chi of former comb is buckled encryption by cutting machine, the combing of comb
Speed is accelerated, and described encryption is specially encryption 60%, and described quickening is specially quickening 70%.
The computational methods of elongation at break are as follows:
Elongation at break=△
L/L0*100% ;
(former long L0, under axial tension effect, the breaking length after deformation is L, then extension at break △ L=L-L0)
The computational methods of hot strength are as follows: σ t=p/(b × d)
σ t is hot strength (MPa);P is peak load (N);B is specimen width (mm);D is sample thickness (mm).
Embodiment four
Polytetrafluoroethylsuperfine superfine fiber, is made up of following methods:
(1) lubrication mixing: add aerial kerosene, mixing in ptfe micropowder;The addition of described aerial kerosene is poly-
The 19% of tetrafluoroethene micropowder quality;The particle diameter of selected ptfe micropowder is 0.215
~0.225 μm;
(2) screening: sieve with 10~30 mesh sieves;
(3) modified mixing: add silicone oil again, then mix;The addition of described silicone oil is the 4% of ptfe micropowder quality;
(4) extrusion: using the raw material extrusion that modification is mixed by extruder, squeezing parameter is as follows, extruded velocity 5~15mm/min,
Extrusion diameter 15~25mm, die entrance angle L/D is 20~40, cone angle 30~50 °, compression ratio 140~160;
(5) calendering: use calender that the raw material after extrusion is rolled, during calendering, roller temperature controls is 140~180 DEG C,
Prepare raw material band;
(6) except boat coal: little to described raw material band dried 18~24 higher than at a temperature of the boiling point of described aerial kerosene
Time, remove described aerial kerosene;
(7) stretching: carry out longitudinal stretching while raw material band is removed described aerial kerosene, then carry out a thermal finalization;Connect
And carry out cross directional stretch first, second heat is shaped, cross directional stretch again, three thermal finalization, prepares polytetrafluoroethylfiber fiber film;Parameter is controlled as follows: longitudinal stretching speed 4%/s, draw ratio 3, a heat setting temperature 200~250 DEG C during drawing and setting;Cross directional stretch speed 46mm/s first, draw ratio 21, second heat setting temperature 200~250 DEG C;Cross directional stretch is that the raw material band after cross directional stretch first is redrawn 186 times again, rate of extension 23mm/s, and three heat setting temperatures control to be 250~300 DEG C, obtain shaping membrane;
(8) solidification removing oil: multiple Concourse Division formulas that described shaping membrane gradually rises in temperature being processed, described stagewise processes
Initial temperature be 300~320 DEG C, until described shaping membrane is heated to transparence, obtain finished film;Elongation at break 31%, hot strength 10.2Mpa
;
(9) score a goal: process that described finished film is scored a goal, the chi of former comb is buckled encryption by cutting machine, the combing of comb
Speed is accelerated, and described encryption is specially encryption 60%, and described quickening is specially quickening 80%.
The computational methods of elongation at break are as follows:
Elongation at break=△
L/L0*100% ;
(former long L0, under axial tension effect, the breaking length after deformation is L, then extension at break △ L=L-L0)
The computational methods of hot strength are as follows: σ t=p/(b × d)
σ t is hot strength (MPa);P is peak load (N);B is specimen width (mm);D is sample thickness (mm).
Embodiment five
Polytetrafluoroethylsuperfine superfine fiber, is made up of following methods:
(1) lubrication mixing: add aerial kerosene, mixing in ptfe micropowder;The addition of described aerial kerosene is poly-
The 22% of tetrafluoroethene micropowder quality;The particle diameter of selected ptfe micropowder is 0.215
~0.225 μm;
(2) screening: sieve with 10~30 mesh sieves;
(3) modified mixing: add silicone oil again, then mix;The addition of described silicone oil is the 5% of ptfe micropowder quality;
(4) extrusion: using the raw material extrusion that modification is mixed by extruder, squeezing parameter is as follows, extruded velocity 5~15mm/min, extrudes diameter 15~25mm, and die entrance angle L/D is 20~40, cone angle 30~50 °, compression ratio 140~160;
(5) calendering: use calender that the raw material after extrusion is rolled, during calendering, roller temperature controls is 140~180 DEG C,
Prepare raw material band;
(6) except boat coal: little to described raw material band dried 18~24 higher than at a temperature of the boiling point of described aerial kerosene
Time, remove described aerial kerosene;
(7) stretching: carry out longitudinal stretching while raw material band is removed described aerial kerosene, then carry out a thermal finalization;Connect
And carry out cross directional stretch first, second heat is shaped, cross directional stretch again, three thermal finalization, prepares polytetrafluoroethylfiber fiber film;Parameter is controlled as follows: longitudinal stretching speed 5%/s, draw ratio 4, a heat setting temperature 200~250 DEG C during drawing and setting;Cross directional stretch speed 47mm/s first, draw ratio 22, second heat setting temperature 200~250 DEG C;Cross directional stretch is that the raw material band after cross directional stretch first is redrawn 188 times again, rate of extension 24 mm/s, and three heat setting temperatures control to be 250~300 DEG C, obtain shaping membrane;
(8) solidification removing oil: multiple Concourse Division formulas that described shaping membrane gradually rises in temperature being processed, described stagewise processes
Initial temperature be 300~320 DEG C, until described shaping membrane is heated to transparence, obtain finished film;Elongation at break 32%, hot strength 10.2Mpa
;
(9) score a goal: process that described finished film is scored a goal, the chi of former comb is buckled encryption by cutting machine, the combing of comb
Speed is accelerated, and described encryption is specially encryption 70%, and described quickening is specially quickening 90%.
The computational methods of elongation at break are as follows:
Elongation at break=△
L/L0*100% ;
(former long L0, under axial tension effect, the breaking length after deformation is L, then extension at break △ L=L-L0)
The computational methods of hot strength are as follows: σ t=p/(b × d)
σ t is hot strength (MPa);P is peak load (N);B is specimen width (mm);D is sample thickness (mm).
Embodiment six
Polytetrafluoroethylsuperfine superfine fiber, is made up of following methods:
(1) lubrication mixing: add aerial kerosene, mixing in ptfe micropowder;The addition of described aerial kerosene is poly-
The 25% of tetrafluoroethene micropowder quality;The particle diameter of selected ptfe micropowder is 0.215
~0.225 μm;
(2) screening: sieve with 10~30 mesh sieves;
(3) modified mixing: add silicone oil again, then mix;The addition of described silicone oil is the 6% of ptfe micropowder quality;
(4) extrusion: using the raw material extrusion that modification is mixed by extruder, squeezing parameter is as follows, extruded velocity 5~15mm/min, extrudes diameter 15~25mm, and die entrance angle L/D is 20~40, cone angle 30~50 °, compression ratio 140~160;
(5) calendering: use calender that the raw material after extrusion is rolled, during calendering, roller temperature controls is 140~180 DEG C,
Prepare raw material band;
(6) except boat coal: little to described raw material band dried 18~24 higher than at a temperature of the boiling point of described aerial kerosene
Time, remove described aerial kerosene;
(7) stretching: carry out longitudinal stretching while raw material band is removed described aerial kerosene, then carry out a thermal finalization;Connect
And carry out cross directional stretch first, second heat is shaped, cross directional stretch again, three thermal finalization, prepares polytetrafluoroethylfiber fiber film;Parameter is controlled as follows: longitudinal stretching speed 6%/s, draw ratio 4, a heat setting temperature 200~250 DEG C during drawing and setting;Cross directional stretch speed 47mm/s first, draw ratio 22, second heat setting temperature 200~250 DEG C;Cross directional stretch is that the raw material band after cross directional stretch first is redrawn 188 times again, rate of extension 25 mm/s, and three heat setting temperatures control to be 250~300 DEG C, obtain shaping membrane;
(8) solidification removing oil: multiple Concourse Division formulas that described shaping membrane gradually rises in temperature being processed, described stagewise processes
Initial temperature be 300~320 DEG C, until described shaping membrane is heated to transparence, obtain finished film;Elongation at break 32%, hot strength 10.5Mpa.;
(9) score a goal: process that described finished film is scored a goal, the chi of former comb is buckled encryption by cutting machine, the combing of comb
Speed is accelerated, and described encryption is specially encryption 70%, and described quickening is specially quickening 100%.
The computational methods of elongation at break are as follows:
Elongation at break=△
L/L0*100% ;
(former long L0, under axial tension effect, the breaking length after deformation is L, then extension at break △ L=L-L0)
The computational methods of hot strength are as follows: σ t=p/(b × d)
σ t is hot strength (MPa);P is peak load (N);B is specimen width (mm);D is sample thickness (mm).
Embodiment seven
Polytetrafluoroethylsuperfine superfine fiber, is made up of following methods:
(1) lubrication mixing: add aerial kerosene, mixing in ptfe micropowder;The addition of described aerial kerosene is poly-
The 28% of tetrafluoroethene micropowder quality;The particle diameter of selected ptfe micropowder is 0.215
~0.225 μm;
(2) screening: sieve with 10~30 mesh sieves;
(3) modified mixing: add silicone oil again, then mix;The addition of described silicone oil is the 7% of ptfe micropowder quality;
(4) extrusion: using the raw material extrusion that modification is mixed by extruder, squeezing parameter is as follows, extruded velocity 5~15mm/min, extrudes diameter 15~25mm, and die entrance angle L/D is 20~40, cone angle 30~50 °, compression ratio 140~160;
(5) calendering: use calender that the raw material after extrusion is rolled, during calendering, roller temperature controls is 140~180 DEG C,
Prepare raw material band;
(6) except boat coal: little to described raw material band dried 18~24 higher than at a temperature of the boiling point of described aerial kerosene
Time, remove described aerial kerosene;
(7) stretching: carry out longitudinal stretching while raw material band is removed described aerial kerosene, then carry out a thermal finalization;Connect
And carry out cross directional stretch first, second heat is shaped, cross directional stretch again, three thermal finalization, prepares polytetrafluoroethylfiber fiber film;Parameter is controlled as follows: longitudinal stretching speed 7%/s, draw ratio 5, a heat setting temperature 200~250 DEG C during drawing and setting;Cross directional stretch speed 48mm/s first, draw ratio 23, second heat setting temperature 200~250 DEG C;Cross directional stretch is that the raw material band after cross directional stretch first is redrawn 192 times again, rate of extension 26mm/s, and three heat setting temperatures control to be 250~300 DEG C, obtain shaping membrane;
(8) solidification removing oil: multiple Concourse Division formulas that described shaping membrane gradually rises in temperature being processed, described stagewise processes
Initial temperature be 300~320 DEG C, until described shaping membrane is heated to transparence, obtain finished film;Elongation at break 32%, hot strength 10.3Mpa
;
(9) score a goal: process that described finished film is scored a goal, the chi of former comb is buckled encryption by cutting machine, the combing of comb
Speed is accelerated, and described encryption is specially encryption 80%, and described quickening is specially quickening 110%.
The computational methods of elongation at break are as follows:
Elongation at break=△
L/L0*100% ;
(former long L0, under axial tension effect, the breaking length after deformation is L, then extension at break △ L=L-L0)
The computational methods of hot strength are as follows: σ t=p/(b × d)
σ t is hot strength (MPa);P is peak load (N);B is specimen width (mm);D is sample thickness (mm).
Embodiment eight
Polytetrafluoroethylsuperfine superfine fiber, is made up of following methods:
(1) lubrication mixing: add aerial kerosene, mixing in ptfe micropowder;The addition of described aerial kerosene is poly-
The 31% of tetrafluoroethene micropowder quality;The particle diameter of selected ptfe micropowder is 0.215
~0.225 μm;
(2) screening: sieve with 10~30 mesh sieves;
(3) modified mixing: add silicone oil again, then mix;The addition of described silicone oil is the 8% of ptfe micropowder quality;
(4) extrusion: using the raw material extrusion that modification is mixed by extruder, squeezing parameter is as follows, extruded velocity 5~15mm/min, extrudes diameter 15~25mm, and die entrance angle L/D is 20~40, cone angle 30~50 °, compression ratio 140~160;
(5) calendering: use calender that the raw material after extrusion is rolled, during calendering, roller temperature controls is 140~180 DEG C,
Prepare raw material band;
(6) except boat coal: little to described raw material band dried 18~24 higher than at a temperature of the boiling point of described aerial kerosene
Time, remove described aerial kerosene;
(7) stretching: carry out longitudinal stretching while raw material band is removed described aerial kerosene, then carry out a thermal finalization;Connect
And carry out cross directional stretch first, second heat is shaped, cross directional stretch again, three thermal finalization, prepares polytetrafluoroethylfiber fiber film;Parameter is controlled as follows: longitudinal stretching speed 8%/s, draw ratio 5, a heat setting temperature 200~250 DEG C during drawing and setting;Cross directional stretch speed 48mm/s first, draw ratio 23, second heat setting temperature 200~250 DEG C;Cross directional stretch is that the raw material band after cross directional stretch first is redrawn 192 times again, rate of extension 27mm/s, and three heat setting temperatures control to be 250~300 DEG C, obtain shaping membrane;
(8) solidification removing oil: multiple Concourse Division formulas that described shaping membrane gradually rises in temperature being processed, described stagewise processes
Initial temperature be 300~320 DEG C, until described shaping membrane is heated to transparence, obtain finished film;Elongation at break 30%, hot strength 10Mpa
;
(9) score a goal: process that described finished film is scored a goal, the chi of former comb is buckled encryption by cutting machine, the combing of comb
Speed is accelerated, and described encryption is specially encryption 80%, and described quickening is specially quickening 120%.
The computational methods of elongation at break are as follows:
Elongation at break=△
L/L0*100% ;
(former long L0, under axial tension effect, the breaking length after deformation is L, then extension at break △ L=L-L0)
The computational methods of hot strength are as follows: σ t=p/(b × d)
σ t is hot strength (MPa);P is peak load (N);B is specimen width (mm);D is sample thickness (mm).
Embodiment nine
Polytetrafluoroethylsuperfine superfine fiber, is made up of following methods:
(1) lubrication mixing: add aerial kerosene, mixing in ptfe micropowder;The addition of described aerial kerosene is poly-
The 34% of tetrafluoroethene micropowder quality;The particle diameter of selected ptfe micropowder is 0.215
~0.225 μm;
(2) screening: sieve with 10~30 mesh sieves;
(3) modified mixing: add silicone oil again, then mix;The addition of described silicone oil is the 9% of ptfe micropowder quality;
(4) extrusion: using the raw material extrusion that modification is mixed by extruder, squeezing parameter is as follows, extruded velocity 5~15mm/min, extrusion diameter 15~25mm, die entrance angle L/D is 20~40, _ _ _ _ _ _ _ _ _ _ cone angle 30~50 °, compression ratio 140~160;
(5) calendering: use calender that the raw material after extrusion is rolled, during calendering, roller temperature controls is 140~180 DEG C,
Prepare raw material band;
(6) except boat coal: little to described raw material band dried 18~24 higher than at a temperature of the boiling point of described aerial kerosene
Time, remove described aerial kerosene;
(7) stretching: carry out longitudinal stretching while raw material band is removed described aerial kerosene, then carry out a thermal finalization;Connect
And carry out cross directional stretch first, second heat is shaped, cross directional stretch again, three thermal finalization, prepares polytetrafluoroethylfiber fiber film;Parameter is controlled as follows: longitudinal stretching speed 9%/s, draw ratio 6, a heat setting temperature 200~250 DEG C during drawing and setting;Cross directional stretch speed 49mm/s first, draw ratio 24, second heat setting temperature 200~250 DEG C;Cross directional stretch is that the raw material band after cross directional stretch first is redrawn 196 times again, rate of extension 28 mm/s, and three heat setting temperatures control to be 250~300 DEG C, obtain shaping membrane;
(8) solidification removing oil: multiple Concourse Division formulas that described shaping membrane gradually rises in temperature being processed, described stagewise processes
Initial temperature be 300~320 DEG C, until described shaping membrane is heated to transparence, obtain finished film;Elongation at break 30%, hot strength 10Mpa
;
(9) score a goal: process that described finished film is scored a goal, the chi of former comb is buckled encryption by cutting machine, the combing of comb
Speed is accelerated, and described encryption is specially encryption 90%, and described quickening is specially quickening 130%.
The computational methods of elongation at break are as follows:
Elongation at break=△
L/L0*100% ;
(former long L0, under axial tension effect, the breaking length after deformation is L, then extension at break △ L=L-L0)
The computational methods of hot strength are as follows: σ t=p/(b × d)
σ t is hot strength (MPa);P is peak load (N);B is specimen width (mm);D is sample thickness (mm).
Embodiment ten
Polytetrafluoroethylsuperfine superfine fiber, is made up of following methods:
(1) lubrication mixing: add aerial kerosene, mixing in ptfe micropowder;The addition of described aerial kerosene is poly-
The 37% of tetrafluoroethene micropowder quality;The particle diameter of selected ptfe micropowder is 0.215
~0.225 μm;
(2) screening: sieve with 10~30 mesh sieves;
(3) modified mixing: add silicone oil again, then mix;The addition of described silicone oil is the 10% of ptfe micropowder quality;
(4) extrusion: using the raw material extrusion that modification is mixed by extruder, squeezing parameter is as follows, extruded velocity 5~15mm/min, extrudes diameter 15~25mm, and die entrance angle L/D is 20~40, cone angle 30~50 °, compression ratio 140~160;
(5) calendering: use calender that the raw material after extrusion is rolled, during calendering, roller temperature controls is 140~180 DEG C,
Prepare raw material band;
(6) except boat coal: little to described raw material band dried 18~24 higher than at a temperature of the boiling point of described aerial kerosene
Time, remove described aerial kerosene;
(7) stretching: carry out longitudinal stretching while raw material band is removed described aerial kerosene, then carry out a thermal finalization;Connect
And carry out cross directional stretch first, second heat is shaped, cross directional stretch again, three thermal finalization, prepares polytetrafluoroethylfiber fiber film;Parameter is controlled as follows: longitudinal stretching speed 10%/s, draw ratio 6, a heat setting temperature 200~250 DEG C during drawing and setting;
Cross directional stretch speed 49mm/s first, draw ratio 24, second heat setting temperature 200~250 DEG C;Cross directional stretch is that the raw material band after cross directional stretch first is redrawn 196 times again, rate of extension 29
Mm/s, three heat setting temperatures control is
250~300 DEG C, obtain shaping membrane;
(8) solidification removing oil: multiple Concourse Division formulas that described shaping membrane gradually rises in temperature being processed, described stagewise processes
Initial temperature be 300~320 DEG C, until described shaping membrane is heated to transparence, obtain finished film;Elongation at break 30%, hot strength 10Mpa
;
(9) score a goal: process that described finished film is scored a goal, the chi of former comb is buckled encryption by cutting machine, the combing of comb
Speed is accelerated, and described encryption is specially encryption 90%, and described quickening is specially quickening 140%.
The computational methods of elongation at break are as follows:
Elongation at break=△
L/L0*100% ;
(former long L0, under axial tension effect, the breaking length after deformation is L, then extension at break △ L=L-L0)
The computational methods of hot strength are as follows: σ t=p/(b × d)
σ t is hot strength (MPa);P is peak load (N);B is specimen width (mm);D is sample thickness (mm).
Embodiment 11
Polytetrafluoroethylsuperfine superfine fiber, is made up of following methods:
(1) lubrication mixing: add aerial kerosene, mixing in ptfe micropowder;The addition of described aerial kerosene is poly-
The 40% of tetrafluoroethene micropowder quality;The particle diameter of selected ptfe micropowder is 0.215
~0.225 μm;
(2) screening: sieve with 10~30 mesh sieves;
(3) modified mixing: add silicone oil again, then mix;The addition of described silicone oil is the 10% of ptfe micropowder quality;
(4) extrusion: using the raw material extrusion that modification is mixed by extruder, squeezing parameter is as follows, extruded velocity 5~15mm/min, extrudes diameter 15~25mm, and die entrance angle L/D is 20~40, cone angle 30~50 °, compression ratio 140~160;
(5) calendering: use calender that the raw material after extrusion is rolled, during calendering, roller temperature controls is 140~180 DEG C,
Prepare raw material band;
(6) except boat coal: little to described raw material band dried 18~24 higher than at a temperature of the boiling point of described aerial kerosene
Time, remove described aerial kerosene;
(7) stretching: carry out longitudinal stretching while raw material band is removed described aerial kerosene, then carry out a thermal finalization;Connect
And carry out cross directional stretch first, second heat is shaped, cross directional stretch again, three thermal finalization, prepares polytetrafluoroethylfiber fiber film;Parameter is controlled as follows: longitudinal stretching speed 10%/s, draw ratio 6, a heat setting temperature 200~250 DEG C during drawing and setting;Cross directional stretch speed 50mm/s first, draw ratio 25, second heat setting temperature 200~250 DEG C;Cross directional stretch is that the raw material band after cross directional stretch first is redrawn 200 times again, rate of extension 30 mm/s, and three heat setting temperatures control to be 250~300 DEG C, obtain shaping membrane;
(8) solidification removing oil: multiple Concourse Division formulas that described shaping membrane gradually rises in temperature being processed, described stagewise processes
Initial temperature be 300~320 DEG C, until described shaping membrane is heated to transparence, obtain finished film;Elongation at break 30%,
Hot strength 10Mpa;
(9) score a goal: process that described finished film is scored a goal, the chi of former comb is buckled encryption by cutting machine, the combing of comb
Speed is accelerated, and described encryption is specially encryption 100%, and described quickening is specially quickening 150%.
The computational methods of elongation at break are as follows:
Elongation at break=△
L/L0*100% ;
(former long L0, under axial tension effect, the breaking length after deformation is L, then extension at break △ L=L-L0)
The computational methods of hot strength are as follows: σ t=p/(b × d)
σ t is hot strength (MPa);P is peak load (N);B is specimen width (mm);D is sample thickness (mm).
Comparative example
1. mixing: being mixed into low surface tension lubricating oil in ptfe micropowder, addition is ptfe micropowder quality
10%;The particle diameter of selected ptfe micropowder is 0.215
~0.225 μm;
2. screening: above-mentioned batch mixing is sieved with 10~30 mesh sieves;
3. preforming: screened batch mixing is placed at a temperature of 20 DEG C 20 hours;
4. extrusion: using extruder to be extruded by the raw material of above-mentioned preforming, squeezing parameter is as follows, extruded velocity 5mm/min, squeezes
Going out diameter 15mm, membrana oralis draw ratio L/D is 20, cone angle 30 °, compression ratio 140;
5. calendering: use calender to roll the raw material after extrusion, during calendering, roller temperature controls is 140 DEG C;Prepare raw
Material strip;
6. except lubricant: to described raw material band dried at a temperature of the boiling point of a little higher than described low surface tension lubricating oil
18 hours, remove described low surface tension lubricating oil;
7. drawing and setting: carry out longitudinal stretching while raw material band is removed described low surface tension lubricating oil, then carry out
Secondary thermal finalization;Then carrying out cross directional stretch first, second heat is shaped, cross directional stretch again, prepares micropore filter after three thermal finalization
Film;Parameter is controlled as follows during drawing and setting;
8. scoring a goal, conventional comb density, conventional speeds scores a goal.
The technological parameter of drawing and setting step is as follows: longitudinal stretching speed 1%/s, longitudinal stretching multiple 2, heat setting temperature 200 DEG C, cross directional stretch speed 10mm/s first, first cross directional stretch multiple 2, second heat setting temperature 200 DEG C, again
Cross directional stretch speed 40mm/s, again cross directional stretch multiple 50, three heat setting temperatures 250 DEG C.
The elongation at break 10% of the film prepared, hot strength 5Mpa.
The computational methods of elongation at break are as follows:
Elongation at break=△
L/L0*100% ;
(former long L0, under axial tension effect, the breaking length after deformation is L, then extension at break △ L=L-L0)
The computational methods of hot strength are as follows: σ t=p/(b × d)
σ t is hot strength (MPa);P is peak load (N);B is specimen width (mm);D is sample thickness (mm).
The fiber of comparative example is the thinnest up to 3D, but more than 80% all at more than 5D.
Embodiment one~11 fibre fineness the most all at about 1D, and CV value is little.CV value i.e. fluctuates one
Individual value, in order to represent the stability of product.
Claims (5)
1. polytetrafluoroethylsuperfine superfine fiber, it is characterised in that represent chemical fibre fineness denier at below 1D, specifically by with
Lower section method is made:
(1) lubrication mixing: add aerial kerosene, mixing in ptfe micropowder;
(2) screening: sieve with 10~30 mesh sieves;
(3) modified mixing: add silicone oil again, then mix;
(4) extrusion: using the raw material extrusion that modification is mixed by extruder, squeezing parameter is as follows, extruded velocity 5~15mm/min, extrudes diameter 15~25mm, and die entrance angle L/D is 20~40, cone angle 30~50 °, compression ratio 140~160;
(5) calendering: use calender that the raw material after extrusion is rolled, during calendering, roller temperature controls is 140~180 DEG C,
Prepare raw material band;
(6) except boat coal: little to described raw material band dried 18~24 higher than at a temperature of the boiling point of described aerial kerosene
Time, remove described aerial kerosene;
(7) stretching: carry out longitudinal stretching while raw material band is removed aerial kerosene, then carry out a thermal finalization;Then enter
Row cross directional stretch first, second heat sizing, cross directional stretch again, three thermal finalization, prepare polytetrafluoroethylfiber fiber film;Parameter is controlled as follows: longitudinal stretching speed 1%~10%/s, draw ratio 2~6, a heat setting temperature 200~250 DEG C during drawing and setting;Cross directional stretch speed 45~50mm/s first, draw ratio 20~25, second heat setting temperature 200~250 DEG C;Cross directional stretch is that the raw material band after cross directional stretch first is redrawn 180~200 times again, rate of extension 20~30mm/s, and three heat setting temperatures control to be 250~300 DEG C, obtain shaping membrane;
(8) solidification removing oil: multiple Concourse Division formulas that described shaping membrane gradually rises in temperature being processed, described stagewise processes
Initial temperature be 300~320 DEG C, until described shaping membrane is heated to transparence, obtain finished film;
(9) score a goal: process that described finished film is scored a goal, the chi of former comb is buckled encryption by cutting machine, the combing of comb
Speed is accelerated, and described encryption is specially encryption 50
~100%, described quickening is specially accelerates 50~150%.
2. according to the polytetrafluoroethylsuperfine superfine fiber described in claim 1, it is characterised in that: the addition of described aerial kerosene
For ptfe micropowder quality 10~30%.
3. according to the polytetrafluoroethylsuperfine superfine fiber described in claim 1 or 2, it is characterised in that: the addition of described silicone oil
For ptfe micropowder quality 1~10%.
4. according to the polytetrafluoroethylsuperfine superfine fiber described in claim 1 or 2, it is characterised in that: selected polytetrafluoroethyl-ne
The particle diameter of alkene micropowder is 0.215~0.225 μm.
5. according to the polytetrafluoroethylsuperfine superfine fiber described in claim 3, it is characterised in that: selected politef is micro-
The particle diameter of powder is 0.215~0.225 μm.
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ID=57635376
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