CN116288778A - Manufacturing and preparing method for PTFE (polytetrafluoroethylene) membranous split filament synthetic fibers - Google Patents
Manufacturing and preparing method for PTFE (polytetrafluoroethylene) membranous split filament synthetic fibers Download PDFInfo
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- CN116288778A CN116288778A CN202310254052.0A CN202310254052A CN116288778A CN 116288778 A CN116288778 A CN 116288778A CN 202310254052 A CN202310254052 A CN 202310254052A CN 116288778 A CN116288778 A CN 116288778A
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/44—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds
- D01F6/48—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds of polymers of halogenated hydrocarbons
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
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- Chemical Kinetics & Catalysis (AREA)
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Abstract
The invention discloses a method for manufacturing and preparing PTFE (polytetrafluoroethylene) membrane split filament synthetic fibers, which particularly relates to the field of fiber manufacturing and comprises the following steps: step one: PVDF, PVP, DMAc and PTFE are added into a reaction tank and stirred at room temperature for about 6 to 10 hours to form a homogeneous solution; step two: introducing the homogeneous solution into a vacuum deaeration machine for defoaming; step three: adding a coagulating liquid into the bubble-removed liquid, completely coagulating for 48 hours, and calendaring to form a film at the time end of twenty-four hours; step four: and drying the fiber membrane at normal temperature, heating, stretching and shaping after cooling to normal temperature, and finally forming a fiber rope shape. According to the invention, the fiber membrane prepared by PVDF, PVP, DMAc and PTFE in proportion is arranged, so that the hydrophilia and colorability of raw materials are ensured, the strength of the fiber is also increased, and the stable and difficult destruction of gaps between behaviors is ensured.
Description
Technical Field
The invention relates to the technical field of fiber manufacturing, in particular to a manufacturing and preparing method of PTFE (polytetrafluoroethylene) membrane split filament synthetic fibers.
Background
The existing PTFE fiber sold on the market is mainly white and brown (prepared by a sintering process), and the reason is that PTFE has poor compatibility with other substances, extremely small dissolution parameters and cannot be dyed by adopting a conventional dyeing method.
The invention patent of patent application publication No. CN110424061B discloses a polytetrafluoroethylene colored film-broken filament and a preparation method thereof, wherein inorganic high-temperature resistant pigment fine powder and PTFE dispersion resin are taken as raw materials, fully mixed, stirred and blended by a lubricant, and prepared by the working procedures of prepressing, pushing, calendaring to form a film, drying and degreasing, heating and stretching, heat setting and twisting, and winding a finished product. The PTFE colored film-broken filament has rich color, bright color and good color fastness. Solves the problem of difficult coloring of PTFE, improves the service performance and added value of PTFE, and expands the application range of high-technology PTFE fibers.
The main problems about PTFE fibers in the comparison document are that the coloring is easy to cause the increase of the hydrophilic performance of the PTFE fibers, the side effects are that the anti-fouling capability of the material is reduced and the decoloring condition when the PTFE fibers are in contact with water is serious, and the main reasons are that the molecular gaps of the material are increased due to the influence of the temperature on the effect of the lubricant in the degreasing process of the material, so that the toughness and the tensile strength of the material are greatly influenced.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention provides a manufacturing and preparing method of PTFE membrane split filament synthetic fibers, which solves the problems in the prior art by setting a new raw material ratio.
In order to achieve the above purpose, the present invention provides the following technical solutions: a preparation method of PTFE membrane split filament synthetic fiber comprises the following steps:
step one: PVDF, PVP, DMAc and PTFE are added into a reaction tank and stirred at room temperature for about 6 to 10 hours to form a homogeneous solution;
step two: introducing the homogeneous solution into a vacuum deaeration machine for defoaming;
step three: adding a coagulating liquid into the bubble-removed liquid, completely coagulating for 48 hours, and calendaring to form a film at the time end of twenty-four hours;
step four: and drying the fiber membrane at normal temperature, heating, stretching and shaping after cooling to normal temperature, and finally forming a fiber rope shape.
In a preferred embodiment, the ratio of PVDF, PVP, DMAc to PTFE is 1:3:0.5:80.
In a preferred embodiment, the PVDF is in powder form, having a molecular weight of 30 ten thousand, a melting point of 173 degrees Celsius, and a crystallization temperature of 140 degrees Celsius.
In a preferred embodiment, the degreasing temperature in the drying degreasing is 400 ℃.
In a preferred embodiment, the step four heating process is performed by placing the feedstock in a 30% glycerol aqueous solution and heating to 70 degrees celsius for 12 hours, followed by conventional heat stretching.
In a preferred embodiment, the pure water flux test is performed prior to conventional heat stretching during the fourth step, with the following test formula:
wherein m2 is the mass (g) of the container together with water at the end of the test after time t; m1 is the mass of the container at the beginning of the experiment (g: p is the density of pure water (1000 g/L), d is the inner diameter (m) of the stretched fiber membrane, L is the effective filtration length (m) of the stretched fiber membrane, t is the filtration test time (h), and the specific steps are as follows:
a1, taking a stretched fiber membrane with an effective filtering length of l, measuring the inner diameter of the stretched fiber membrane by using an optical microscope with a scale, and fixing the stretched fiber membrane on a testing device to be tested;
a2, measuring the mass m1 of the container;
a3, controlling the water inlet pressure at 0.1MPa, and starting the experiment after prepressing for 5 minutes. Collecting the pure water on the permeation side in a container, and measuring m2 after running for 5 minutes;
and A4, calculating by the formula to obtain pure water flux, and measuring three samples at the same time at each point to obtain the average value.
In a preferred embodiment, the hole gap test is performed prior to conventional heat stretching during step four, with the test formula:
wherein m is the mass (g) of the stretched fiber membrane before drying, and m2 is the mass (g) of the stretched fiber membrane after drying; density of ethanol (0.78 g/ml); the testing steps are as follows:
b1 soaking the stretched fiber membrane to be tested in ethanol for 24 hours, so that the membrane holes are completely filled with the ethanol. B2, taking out a certain length of soaked stretched fiber film, sucking the ethanol on the surface of the stretched fiber film by using filter paper, and blowing out the ethanol on the inner surface of the stretched fiber by using an ear ball;
b3, rapidly putting the stretched fiber membrane in the B2 into a micro-scale graduated cylinder which is prepared by 1ml of ethanol, and reading out the volume difference V before and after, namely the apparent volume of the stretched fiber membrane;
b4, taking out the stretched fiber membrane, repeating the operation of the step B2 again, and weighing the mass m;
b5 the stretched fiber film was put into a vacuum drying oven, dried at 80℃under an absolute pressure of 100mmHg for 8 hours, and then the mass m2 thereof was weighed.
The invention has the technical effects and advantages that:
according to the invention, the fiber membrane prepared by PVDF, PVP, DMAc and PTFE in proportion is arranged, so that the hydrophilia and colorability of raw materials are ensured, the strength of the fiber is also increased, and the stable and difficult destruction of gaps between behaviors is ensured.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described in the following in conjunction with the embodiments of the present invention, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Examples
The invention provides a method for manufacturing and preparing PTFE membrane split filament synthetic fibers, which is characterized in that: comprises the following steps:
step one: PVDF, PVP, DMAc and PTFE are added into a reaction tank and stirred at room temperature for about 6 to 10 hours to form a homogeneous solution;
step two: introducing the homogeneous solution into a vacuum deaeration machine for defoaming;
step three: adding a coagulating liquid into the bubble-removed liquid, completely coagulating for 48 hours, and calendaring to form a film at the time end of twenty-four hours;
step four: and drying the fiber membrane at normal temperature, heating, stretching and shaping after cooling to normal temperature, and finally forming a fiber rope shape.
The ratio of PVDF, PVP, DMAc to PTFE is 1:3:0.5:80, the PVDF is powder, the molecular weight is 30 ten thousand, the melting point is 173 ℃, the crystallization temperature is 140 ℃, the degreasing temperature in drying degreasing is 400 ℃, the raw materials are placed in 30% glycerol aqueous solution in the heating process for heating to 70 ℃ for 12 hours, and then conventional heating stretching is carried out.
Experimental example 1
A method for manufacturing and preparing PTFE membrane split filament synthetic fibers is characterized in that: comprises the following steps:
step one: PVDF, PVP, DMAc and PTFE are added into a reaction tank and stirred at room temperature for about 6 to 10 hours to form a homogeneous solution;
step two: introducing the homogeneous solution into a vacuum deaeration machine for defoaming;
step three: adding a coagulating liquid into the bubble-removed liquid, completely coagulating for 48 hours, and calendaring to form a film at the time end of twenty-four hours;
step four: and drying the fiber membrane at normal temperature, heating, stretching and shaping after cooling to normal temperature, and finally forming a fiber rope shape.
The ratio of PVDF, PVP, DMAc to PTFE is 1:3:0.5:80, the PVDF is powder, the molecular weight is 30 ten thousand, the melting point is 173 ℃, the crystallization temperature is 140 ℃, the degreasing temperature in drying degreasing is 400 ℃, the raw materials are placed in 30% glycerol aqueous solution in the heating process for heating to 70 ℃ for 12 hours, and then conventional heating stretching is carried out.
And in the fourth step, pure water flux test is carried out before conventional heating and stretching, and the test formula is as follows:
wherein m2 is the mass (g) of the container together with water at the end of the test after time t; m1 is the mass of the vessel at the beginning of the experiment (g: p is the density of pure water (1000 g/L), d is the inner diameter (m) of the drawn fiber film, L is the effective filtration length (m) of the drawn fiber filmThe method comprises the steps of carrying out a first treatment on the surface of the t is the filtration test time (h);
the method comprises the following specific steps:
a1, taking a stretched fiber membrane with an effective filtering length of l, measuring the inner diameter of the stretched fiber membrane by using an optical microscope with a scale, and fixing the stretched fiber membrane on a testing device to be tested;
a2, measuring the mass m1 of the container;
a3, controlling the water inlet pressure at 0.1MPa, and starting the experiment after prepressing for 5 minutes. Collecting the pure water on the permeation side in a container, and measuring m2 after running for 5 minutes;
and A4, calculating by the formula to obtain pure water flux, and measuring three samples at the same time at each point to obtain the average value.
Experimental example 2
A method for manufacturing and preparing PTFE membrane split filament synthetic fibers is characterized in that: comprises the following steps:
step one: PVDF, PVP, DMAc and PTFE are added into a reaction tank and stirred at room temperature for about 6 to 10 hours to form a homogeneous solution;
step two: introducing the homogeneous solution into a vacuum deaeration machine for defoaming;
step three: adding a coagulating liquid into the bubble-removed liquid, completely coagulating for 48 hours, and calendaring to form a film at the time end of twenty-four hours;
step four: and drying the fiber membrane at normal temperature, heating, stretching and shaping after cooling to normal temperature, and finally forming a fiber rope shape.
The ratio of PVDF, PVP, DMAc to PTFE is 1:3:0.5:80, the PVDF is powder, the molecular weight is 30 ten thousand, the melting point is 173 ℃, the crystallization temperature is 140 ℃, the degreasing temperature in drying degreasing is 400 ℃, the raw materials are placed in 30% glycerol aqueous solution in the heating process for heating to 70 ℃ for 12 hours, and then conventional heating stretching is carried out.
A method for manufacturing and preparing PTFE membrane split filament synthetic fibers is characterized in that: comprises the following steps:
step one: PVDF, PVP, DMAc and PTFE are added into a reaction tank and stirred at room temperature for about 6 to 10 hours to form a homogeneous solution;
step two: introducing the homogeneous solution into a vacuum deaeration machine for defoaming;
step three: adding a coagulating liquid into the bubble-removed liquid, completely coagulating for 48 hours, and calendaring to form a film at the time end of twenty-four hours;
step four: and drying the fiber membrane at normal temperature, heating, stretching and shaping after cooling to normal temperature, and finally forming a fiber rope shape.
The ratio of PVDF, PVP, DMAc to PTFE is 1:3:0.5:80, the PVDF is powder, the molecular weight is 30 ten thousand, the melting point is 173 ℃, the crystallization temperature is 140 ℃, the degreasing temperature in drying degreasing is 400 ℃, the raw materials are placed in 30% glycerol aqueous solution in the heating process for heating to 70 ℃ for 12 hours, and then conventional heating stretching is carried out.
And in the fourth step, hole gap testing is carried out before conventional heating stretching, and the testing formula is as follows:
wherein m is the mass (g) of the stretched fiber membrane before drying, and m2 is the mass (g) of the stretched fiber membrane after drying; density of ethanol (0.78 g/ml); the testing steps are as follows:
b1 soaking the stretched fiber membrane to be tested in ethanol for 24 hours, so that the membrane holes are completely filled with the ethanol. B2, taking out a certain length of soaked stretched fiber film, sucking the ethanol on the surface of the stretched fiber film by using filter paper, and blowing out the ethanol on the inner surface of the stretched fiber by using an ear ball;
b3, rapidly putting the stretched fiber membrane in the B2 into a micro-scale graduated cylinder which is prepared by 1ml of ethanol, and reading out the volume difference V before and after, namely the apparent volume of the stretched fiber membrane;
b4, taking out the stretched fiber membrane, repeating the operation of the step B2 again, and weighing the mass m;
b5 the stretched fiber film was put into a vacuum drying oven, dried at 80℃under an absolute pressure of 100mmHg for 8 hours, and then the mass m2 thereof was weighed.
Finally: the foregoing description of the preferred embodiments of the invention is not intended to limit the invention to the precise form disclosed, and any such modifications, equivalents, and alternatives falling within the spirit and principles of the invention are intended to be included within the scope of the invention.
Claims (7)
1. A method for manufacturing and preparing PTFE membrane split filament synthetic fibers is characterized in that: comprises the following steps:
step one: PVDF, PVP, DMAc and PTFE are added into a reaction tank and stirred at room temperature for about 6 to 10 hours to form a homogeneous solution;
step two: introducing the homogeneous solution into a vacuum deaeration machine for defoaming;
step three: adding a coagulating liquid into the bubble-removed liquid, completely coagulating for 48 hours, and calendaring to form a film at the time end of twenty-four hours;
step four: and drying the fiber membrane at normal temperature, heating, stretching and shaping after cooling to normal temperature, and finally forming a fiber rope shape.
2. The method for producing a PTFE membrane-broken filament synthetic fiber according to claim 1, characterized in that: the dosage ratio of PVDF, PVP, DMAc to PTFE is 1:3:0.5:80.
3. The method for producing a PTFE membrane-broken filament synthetic fiber according to claim 1, characterized in that: the PVDF is powder, the molecular weight is 30 ten thousand, the melting point is 173 ℃, and the crystallization temperature is 140 ℃.
4. The method for producing a PTFE membrane-broken filament synthetic fiber according to claim 1, characterized in that: the oil removal temperature in the drying degreasing is 400 ℃.
5. The method for producing a PTFE membrane-broken filament synthetic fiber according to claim 1, characterized in that: and in the heating process of the step four, the raw materials are placed in 30% glycerol water solution and heated to 70 ℃ for 12 hours, and then conventional heating stretching is carried out.
6. The method for producing a synthetic fiber of a split filament of PTFE according to claim 4, wherein: and in the fourth step, pure water flux test is carried out before conventional heating and stretching, and the test formula is as follows:
wherein m2 is the mass (g) of the container together with water at the end of the test after time t; m1 is the mass of the container at the beginning of the experiment (g: p is the density of pure water (1000 g/L), d is the inner diameter (m) of the stretched fiber membrane, L is the effective filtration length (m) of the stretched fiber membrane, t is the filtration test time (h), and the specific steps are as follows:
a1, taking a stretched fiber membrane with an effective filtering length of l, measuring the inner diameter of the stretched fiber membrane by using an optical microscope with a scale, and fixing the stretched fiber membrane on a testing device to be tested;
a2, measuring the mass m1 of the container;
a3, controlling the water inlet pressure at 0.1MPa, and starting the experiment after prepressing for 5 minutes. Collecting the pure water on the permeation side in a container, and measuring m2 after running for 5 minutes;
and A4, calculating by the formula to obtain pure water flux, and measuring three samples at the same time at each point to obtain the average value.
7. The method for producing a synthetic fiber of a split filament of PTFE according to claim 4, wherein: and in the fourth step, hole gap testing is carried out before conventional heating stretching, and the testing formula is as follows:
wherein m is the mass (g) of the stretched fiber membrane before drying, and m2 is the mass (g) of the stretched fiber membrane after drying; density of ethanol (0.78 g/ml); the testing steps are as follows:
b1 soaking the stretched fiber membrane to be tested in ethanol for 24 hours, so that the membrane holes are completely filled with the ethanol. B2, taking out a certain length of soaked stretched fiber film, sucking the ethanol on the surface of the stretched fiber film by using filter paper, and blowing out the ethanol on the inner surface of the stretched fiber by using an ear ball;
b3, rapidly putting the stretched fiber membrane in the B2 into a micro-scale graduated cylinder which is prepared by 1ml of ethanol, and reading out the volume difference V before and after, namely the apparent volume of the stretched fiber membrane;
b4, taking out the stretched fiber membrane, repeating the operation of the step B2 again, and weighing the mass m;
b5 the stretched fiber film was put into a vacuum drying oven, dried at 80℃under an absolute pressure of 100mmHg for 8 hours, and then the mass m2 thereof was weighed.
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| CN115110168A (en) * | 2022-06-24 | 2022-09-27 | 苏州大学 | Method for manufacturing polytetrafluoroethylene fibers with high mass density uniformity |
| CN115352104A (en) * | 2022-08-24 | 2022-11-18 | 江苏华跃纺织新材料科技股份有限公司 | Preparation method of graphene/polytetrafluoroethylene nano composite split fibers |
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2023
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Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| KR20130049626A (en) * | 2011-11-04 | 2013-05-14 | 웅진케미칼 주식회사 | Manufacturing method of separation membrane for water treatment and separation membrane for water treatment thereby |
| CN106637680A (en) * | 2016-12-30 | 2017-05-10 | 青岛大学 | Polytetrafluoroethylene filament non-woven fabric based on film tearing method and preparation technology thereof |
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