CN101363142A - Technology for covering polyphenyl thioether fabric surface with silicon coating - Google Patents
Technology for covering polyphenyl thioether fabric surface with silicon coating Download PDFInfo
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- CN101363142A CN101363142A CNA2007100497086A CN200710049708A CN101363142A CN 101363142 A CN101363142 A CN 101363142A CN A2007100497086 A CNA2007100497086 A CN A2007100497086A CN 200710049708 A CN200710049708 A CN 200710049708A CN 101363142 A CN101363142 A CN 101363142A
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- polyphenylene sulfide
- silicon coating
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Abstract
The invention discloses a technique for covering silicon coating on the surface of polyphenylene fiber. Sodium sulfide and santochlor are taken as raw materials and then synthesized to obtain polyphenylene fiber protofilament after the melt spinning; heat drawing treatment is applied to the fiber protofilament so as to get finished fiber; after the protofilament finished fiber is precoated with film material solution which contains at least one of the components of phenol silicone resin, hydroxy-polyorganosiloxanem and PPTA, the heat treatment is carried out under the condition of normal atmosphere air of 20-360 DEG C or nitrogen protection so as to get the polyphenylene fiber products with the thickness of 1-100 micron silicon coating. The obtained polyphenylene composite fiber is especially suitable for serving as filter materials in thermal power generation, garbage incinerators, chemical filters, and the like.
Description
Affiliated technical field
The invention belongs to production, the Application Areas of special fibre.
Background technology
High-performance polyphenylene sulfide has the heat endurance under excellent chemical proofing and the high temperature, and has fire-retardant, insulation, radiation hardness and favorable mechanical performance.For enlarging the scope of application of this material, the researchers of various countries make it the new method that fibration is used in searching always.
PPS fiber chemical-resistant stability is good, and it has outstanding chemical stability extremely still keeping its original performance under the harsh conditions, is only second to polytetrafluoroethylene fibre.At high temperature, be placed in the different inorganic reagents and can keep original tensile strength after the week.It also has the performance of good organic solvent-resistant, except 93 ℃ toluene to its intensity slightly influential, in organic solvents such as carbon tetrachloride, chloroform, even its intensity still can not change place a week under boiling point after, temperature is that 93 ℃ formic acid, acetic acid does not influence its intensity yet.The nonwoven fabric filter fabric of being made by polyphenylene sulfide fibre has good corrosion resistance in 93 ℃ 50% sulfuric acid, strength retention does not make significant difference.Placed for two weeks in 93 ℃, 10% sodium hydroxide solution after, its intensity does not have obvious variation yet.
PPS fiber good heat stability, it has outstanding heat-resisting quantity, and fusing point reaches 285 ℃, is higher than other melt-spun fibres of present suitability for industrialized production, so dimensionally stable.Its limited oxygen index can reach 35% one 45%, can not burn under normal atmospheric conditions.The heat resistance of polyphenylene sulfide fibre also shows: its strength retention in the time of 200 ℃ is about 40% when being 60%, 250 ℃.Below 250 ℃ the time, its extension at break remains unchanged substantially.If its multifilament is placed 200 ℃ high temperature furnace, fracture strength remains unchanged substantially after 54 days, and extension at break is reduced to 50% of initial collapse elongation; Under 260 ℃ after 48 hours, still can keep 60% of fiber initial strength, extension at break is reduced to 50% of initial collapse elongation.Go out outside this, the PPS fiber has good textile processibility energy, can be processed into the fibre of all size, different shape.
But in some extreme occasion, elevated temperature strength conservation rate to fiber has higher requirement, for example when temperature is higher, can occur because of the polyphenylene sulfide fibre vitrifying and reach the polyphenylene sulfide fusing point causing filtering material softening, stop up and reduction production efficiency thereby make filtering material that the space take place.
U.S. Pat: introduce in 6280880 and use nitrogen and oxygen as carrier, the fluorine gas that adds 1-5% then therein, in the potassium hydroxide solution of 30-38%, handle polyphenylene sulfide fibre or PPSS fiber then, obtain that fiber surface is fluorine-containing to be the fiber after treatment of 0.01-0.2%.With the ability that has just improved the chemicals-resistant of fiber behind this method processing fiber, can't improve the oxygen index (OI) and the resistant to elevated temperatures ability of fiber.
United States Patent (USP): introduced the processing method of the fine fiber of polypropylene being carried out face coat among the US:5030509, after this kind fiber being carried out the face coat processing, improved the oxygen index (OI) and the resistant to elevated temperatures ability of fiber.
Up to the present, do not see that poly-this thioether fiber surface coating of concrete manufacturing makes it to improve the relevant report of fiber high temperature strength retention.
The objective of the invention is to study a kind of process at covering polyphenyl thioether fabric surface with silicon coating, solve the problem that polyphenylene sulfide fibre can occur under higher temperature, as: its mechanical performance reduces, the fiber heat-resisting ability is improved simultaneously, can remain on temperature in the time of long (more than 200 hours, even longer time) is 200-265
0In the environment of C, its polyphenylene sulfide fibre mechanical property remains unchanged substantially.
Summary of the invention
Adopting vulcanized sodium and paracide is that raw material is synthetic after the polyphenylene sulfide fibre precursor that the melt spinning weaving obtains; Fiber precursor carries out hot drawing-off and is processed into finished fiber; Described polyphenylene sulfide finished fiber with the film forming matter solution pre-coated that one of contains in phenol silicone resin, hydroxyl-polyorganosiloxane resin, the PPTA at least after, be 20-360 in temperature
0Heat treatment obtains the polyphenylene sulfide fibre product that applied thickness is a 1-100 micron silicon coating under the condition of C atmospheric air or nitrogen protection.
The film-forming process that uses in invention is: the polyphenylene sulfide finished fiber is equipped with the solution tank of film forming matter speed impregnation of fibers with 0.1-0.6m/min from 3 or 5 long 3-6m, thereby the time that makes fiber pass through 3 or 5 solution tanks is not hanged down 15 minutes (min), will be impregnated with the polyphenylene sulfide fibre of film forming matter then at 20-600
0Heat-treat under the temperature of C, the processing time of this moment is no more than 60min, is not less than 10 seconds (s) simultaneously, has just obtained having in the polyphenylene sulfide fibre surface-coated polyphenylene sulfide fibre of silicon coating through such processing.
Annealer of the present invention is cylindrical or plate shaped electric heater, according to the needs of coating many heaters of can connecting.To guarantee the processing time of polyphenylene sulfide fibre in heater.
Improved much through its resistant to elevated temperatures degree of check through the polyphenylene sulfide fibre after handling like this, under 200-260 ℃ high temperature, used after 200 hours, its fibre strength conservation rate is about 90%, and its oxygen index (OI) can reach 50 or higher.
What deserves to be mentioned is organosilicon polymer here, heat treatment time can not be higher than 30min when temperature is 300 ℃, be certain to reduce a lot when the high more processing time of temperature, but can cause polyphenylene sulfide fibre that to a certain degree fracture is arranged, therefore grasp suitable temperature and the appropriate time is very important.
Polyamide solution of the present invention comprises the diamines constituent structure, as: PPTA.Behind the polyphenylene sulfide fibre dipping, wash neutralize away acid flux material and then 200-600
0Heat treatment of fibre under the temperature of C is at the film of polyphenylene sulfide fibre surface formation one deck high-compactness.
The present invention adopts the method for dipping or wet-spraying, make the inorganic or polysiloxane film of material formation of having the ability to constitute film, heat-treat at polyphenylene sulfide fibre subsequently, or react with catalyst mutagenesis, or make it to take place crosslinked, form the organic or inorganic compound silicon thin film of one deck high-compactness, but the film here produces under heat treated condition.
The detection method of the polyphenylene sulfide fibre that the present invention obtains is consistent with the detection method of general fiber.The detection of the coating layer thickness on polyphenylene sulfide fibre surface is measured with single fiber.
Description of drawings:
Accompanying drawing 1: be polyphenylene sulfide fibre impregnation technology flow process
Accompanying drawing 2: be the Technology for Heating Processing flow process behind the polyphenylene sulfide fibre dipping
Accompanying drawing 3: the performance characteristic tables of data that is polyphenylene sulfide fibre after treatment
What figure one represented is that polyphenylene sulfide fibre is from front end (or left end) the pressure roller traction of ship shape groove Enter the ship shape groove, at five pressure rollers through the ship shape groove, it is molten that fiber can be immersed in well In the liquid, the rear end (or right-hand member) from the ship shape groove goes out groove then, and is again through the pressure roller of rear end, defeated Deliver to heat treatment step.
What figure two represented is to import the cylindrical of heating through the polyphenylene sulfide fibre of dipping solution Electric furnace or dull and stereotyped electric heater are heat-treated.
The specific embodiment
Example 1:
It with the dilution with toluene solids content 0.5% phenol silicone resin, and add the toluene solution that trimethyl-trimethoxy silane of 3.5% is made resin, polyphenylene sulfide fibre is flooded 120min by the impregnation technology flow process of accompanying drawing one, by the 20C air drying, be transported to 220 then
0Handle 60min in the cylindrical high temperature furnace of C, polyphenylene sulfide fibre has just been coated the silicone resin film like this, therefore smears structure and the character of handling the front and back polyphenylene sulfide and shows in the table of accompanying drawing three.
Example 2:
Add the sulfuric acid solution that 99.5% concentrated sulfuric acid solution is mixed with 3.5% PPTA resin with the PPTA resin, adopt the technological process dipping 15min of accompanying drawing one, use 50-80 then
0The deionized water washing polyphenylene sulfide strand of C is 20
0The air drying of C is transported to 600
0The cylindrical electric furnace of C, under protection of nitrogen gas, heat treatment 15s, polyphenylene sulfide fibre has just been coated polyamide resin like this, therefore smears structure and the character of handling the front and back polyphenylene sulfide and shows in the table of accompanying drawing three.
Example 3:
With the isopropanol solids content is the solution of 3.5% hydroxyl-polyorganosiloxane resin, adds 0.5% dimethyl-dimethoxy silane, adopts the technological process of accompanying drawing one to flood the 15min that films with the solution that makes, before this by 20
0The air drying of C is transported to 220
0Handle 60min in the cylindrical high temperature furnace of C, polyphenylene sulfide fibre has just been coated the layer of silicon dioxide film like this, therefore smears structure and the character of handling the front and back polyphenylene sulfide and shows in the table of accompanying drawing three.
Example 4:
It with the dilution with toluene solids content 3.5% phenol silicone resin, with the dimethyl-dimethoxy silane that adds 0.5%, and make resin solution, polyphenylene sulfide fibre is flooded 15min by the impregnation technology flow process of figure one, by the 20C air drying, be transported to 220 then
0Handle 60min in the cylindrical high temperature furnace of C, polyphenylene sulfide fibre has just been coated silicone resin like this, therefore smears structure and the character of handling the front and back polyphenylene sulfide and shows in the table of accompanying drawing three.
Example 5:
With the isopropanol solids content is 0.5% can constitute SiO
2The solution of film (hydroxyl-polyorganosiloxane resin) adds 3.5% trimethyl-trimethoxy silane, adopts the technological process of accompanying drawing one to flood the 120min that films with the solution that makes, before this by 20
0The air drying of C is transported to 220
0Handle 60min in the cylindrical high temperature furnace of C, polyphenylene sulfide fibre has just been coated the layer of silicon dioxide film like this, therefore smears structure and the character of handling the front and back polyphenylene sulfide and shows in the table of accompanying drawing three.
More than utilize the polyphenylene sulfide fibre long filament to handle, if when handling staple fibre, the compound method of above solution and concentration do not have any variation, but, no longer adopt the continuous processing flow process in the impregnation technology flow process, can only adopt mode intermittently polyphony thioether short fiber to be immersed in the solution for preparing, adopt air drying equally, heat treatment can only adopt flat electric heater to come heat treatment of fibre.Its result is also similar with the performance characteristic of handling long filament.
Claims (6)
1. the process of covering polyphenyl thioether fabric surface with silicon coating, adopting vulcanized sodium and paracide is that raw material is synthetic after the polyphenylene sulfide fibre precursor that melt spinning is weaved and obtained; Fiber precursor carries out hot drawing-off and is processed into finished fiber; Described polyphenylene sulfide finished fiber with one of at least film forming matter solution pre-coated in the PPTA that contains phenol silicone resin, hydroxyl-polyorganosiloxane resin, polyamide after, be that heat treatment obtains the polyphenylene sulfide fibre product that applied thickness is a 1-100 micron silicon coating under the 20-600 ℃ of atmospheric air condition in temperature.
2. according to the process of the described covering polyphenyl thioether fabric surface with silicon coating of claim 1, it is characterized in that described coating can adopt modes such as solution impregnation and spraying to carry out.
3. according to the manufacture method of claim 1 or 2 described polyphenylene sulfide fibre surface applied coatings, it is characterized in that described fiber flooded 15-120 minute in film forming matter solution.
4. according to the process of claim 1 or 2 or 3 described covering polyphenyl thioether fabric surface with silicon coating, it is characterized in that described different coating heat treatment time was generally 10 seconds-60 minutes.
5. according to the process of the described covering polyphenyl thioether fabric surface with silicon coating of claim 2, the solution concentration that it is characterized in that described dipping polyphenylene sulfide fibre is 0.5-3.5%.
6. according to the process of the described covering polyphenyl thioether fabric surface with silicon coating of claim 1, it is characterized in that heat treatment is carried out under the condition of nitrogen protection.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CNA2007100497086A CN101363142A (en) | 2007-08-09 | 2007-08-09 | Technology for covering polyphenyl thioether fabric surface with silicon coating |
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| Application Number | Priority Date | Filing Date | Title |
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| CNA2007100497086A CN101363142A (en) | 2007-08-09 | 2007-08-09 | Technology for covering polyphenyl thioether fabric surface with silicon coating |
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| CN101363142A true CN101363142A (en) | 2009-02-11 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102560718A (en) * | 2012-01-04 | 2012-07-11 | 四川华通特种工程塑料研究中心有限公司 | Preparation method of surface coating type anti-oxidation polyphenylene sulfide fiber |
| CN102888779A (en) * | 2011-07-18 | 2013-01-23 | 四川得阳科技股份有限公司 | Process method of coating aramid fiber resin protective layer on surface of polyphenylene sulfide fiber |
| CN103397526A (en) * | 2013-08-02 | 2013-11-20 | 泰山体育产业集团有限公司 | Airport-use instantaneous-high-temperature-resistant man-made grass filament fiber and preparation technology thereof |
| CN105625042A (en) * | 2014-11-04 | 2016-06-01 | 厦门三维丝环保股份有限公司 | High temperature resistant filter cartridge substrate filter material stiffening finishing method |
-
2007
- 2007-08-09 CN CNA2007100497086A patent/CN101363142A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102888779A (en) * | 2011-07-18 | 2013-01-23 | 四川得阳科技股份有限公司 | Process method of coating aramid fiber resin protective layer on surface of polyphenylene sulfide fiber |
| CN102560718A (en) * | 2012-01-04 | 2012-07-11 | 四川华通特种工程塑料研究中心有限公司 | Preparation method of surface coating type anti-oxidation polyphenylene sulfide fiber |
| CN102560718B (en) * | 2012-01-04 | 2013-10-02 | 四川华通特种工程塑料研究中心有限公司 | Preparation method of surface coating type anti-oxidation polyphenylene sulfide fiber |
| CN103397526A (en) * | 2013-08-02 | 2013-11-20 | 泰山体育产业集团有限公司 | Airport-use instantaneous-high-temperature-resistant man-made grass filament fiber and preparation technology thereof |
| CN103397526B (en) * | 2013-08-02 | 2015-08-19 | 泰山体育产业集团有限公司 | One the airport artificial turf fiber of resistance to TRANSIENT HIGH TEMPERATURE and preparation technology thereof |
| CN105625042A (en) * | 2014-11-04 | 2016-06-01 | 厦门三维丝环保股份有限公司 | High temperature resistant filter cartridge substrate filter material stiffening finishing method |
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Open date: 20090211 |