CN109485913A - A kind of recovery method of polyphenylene sulfide fibre and its composite fiber filtering material - Google Patents
A kind of recovery method of polyphenylene sulfide fibre and its composite fiber filtering material Download PDFInfo
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- CN109485913A CN109485913A CN201811635049.9A CN201811635049A CN109485913A CN 109485913 A CN109485913 A CN 109485913A CN 201811635049 A CN201811635049 A CN 201811635049A CN 109485913 A CN109485913 A CN 109485913A
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- polyphenylene sulfide
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J11/00—Recovery or working-up of waste materials
- C08J11/04—Recovery or working-up of waste materials of polymers
- C08J11/06—Recovery or working-up of waste materials of polymers without chemical reactions
- C08J11/08—Recovery or working-up of waste materials of polymers without chemical reactions using selective solvents for polymer components
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2381/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing sulfur with or without nitrogen, oxygen, or carbon only; Polysulfones; Derivatives of such polymers
- C08J2381/02—Polythioethers; Polythioether-ethers
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/62—Plastics recycling; Rubber recycling
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- Chemical Kinetics & Catalysis (AREA)
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- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Polymers With Sulfur, Phosphorus Or Metals In The Main Chain (AREA)
- Filtering Materials (AREA)
Abstract
The invention belongs to the recovery technology fields of filtrate, and the present invention provides a kind of polyphenylene sulfide fibre and its recovery methods of composite fiber filtering material.The present invention is mixed by that will pre-process filtrate with solvent, in 150~250 DEG C of 20~40min of insulated and stirred, so that polyphenylene sulfide is dissolved in α-chloronaphthalene or N-Methyl pyrrolidone, if waste and old filtrate contains the waste product or leftover pieces of polyphenyl thioether composite material material, then compound material obtains non-polyphenylene sulfide solid insoluble in solvent, it is filtered using the device that filter opening aperture is 0.1~0.5mm, to realize the separation of polyphenylene sulfide and composite material, obtains the thick solution of polyphenylene sulfide；The thick solution of polyphenylene sulfide is filtered using the device that filter opening aperture is 10~50 μm, so as to the dust impurities removal that will be adhered on waste and old filtrate in the thick solution of polyphenylene sulfide, obtains polyphenylene sulfide solution；Polyphenylene sulfide solution is crystallized, pure polyphenylene sulfide is obtained.
Description
Technical field
The present invention relates to the recovery technology field of filtrate more particularly to a kind of polyphenylene sulfide fibres and its composite fiber filtering material
Recovery method.
Background technique
Bag-type dusting is the important technology approach for controlling industrial dust and high-temperature smoke, and filtrate is that core is played in bag-type dusting
The expendable material of filtration.In numerous areas such as coal-burning power plant, Industrial Boiler, garbage power, cement kiln, Ferrous Metallurgys
In main filtrate be the pure polyphenyl thioether filter material made of polyphenylene sulfide fibre, or it is fine with polyphenylene sulfide and other high efficiency
Tie up the polyphenylene sulfide composite filtering material of (such as polytetrafluoroethylene (PTFE), aramid fiber, polyimides, glass fibre) production.Filtrate uses the longevity
Life relies on concrete condition on site, just needs replacing to 3 years usual some months.Due to huge heavy industry scale and huge
Flue dust total amount, the waste and old filtrate occupied area that annual China generates reach more than one hundred million square meters, filter bag (dust settling pocket that filtrate is made into) number
Amount reaches 25,000,000, and volume reaches 300 ten thousand steres.The accumulation of waste and old filtrate not only creates a large amount of secondary pollution, and
And the filtrate for high-temperature smoke trapping, used fiber is high performance material, and the price is very expensive, even if becoming waste and old
The performance of filter bag, Fiber Materials is still fine, can recycle.In addition, can also be produced in the production of new filtrate and filter bag
Raw a large amount of leftover pieces, contained polyphenylene sulfide fibre amount are also very considerable.If can be by the waste and old filtrate after live use, filter
The leftover pieces generated in material manufacture recycle, and not only solve the secondary pollution problem in Environmental-protecting dust-removing field, but also realize high price
It is worth the multiplexing of material, embodies green circulatory.
Current existing filtrate recovery method is crushed to resin after mainly a live filter bag is heated, but due to waste and old filter
Bag attachment a large amount of dust still has micro dust even across washing on fiber, influence the quality of resin after hot melt, and many filters
Bag is largely to be made of polyphenylene sulfide fibre and polytetrafluoroethylene (PTFE) mixing, therefore it is also mixture that resin, which is made, in this method,
It can be only applied to require material not tight occasion, and the very high polyphenylene sulfide of value and the mixing of other high-performance fibers made
For usual resins use, its application value is greatly reduced, causes the cost of removal process can not filling-in.
Summary of the invention
The purpose of the present invention is to provide a kind of polyphenylene sulfide fibre and its recovery method of composite fiber filtering material, the present invention
Provided recovery method can separate polyphenylene sulfide with other composite materials, obtain pure polyphenylene sulfide, be equally also suitable
In extracting pure polyphenylene sulfide from polyphenyl thioether filter material.
In order to achieve the above-mentioned object of the invention, the present invention the following technical schemes are provided:
The present invention provides a kind of polyphenylene sulfide fibre and its recovery methods of composite fiber filtering material, include the following steps:
(1) waste and old filtrate is successively broken up and is chopped, obtain pretreatment filtrate；The waste and old filtrate is that polyphenylene sulfide is fine
Tie up the waste product of material, the leftover pieces of polyphenylene sulfide fibre material, the waste product of polyphenyl thioether complex fiber material and poly-
At least one of the leftover pieces of diphenyl sulfide composite fibre material；
(2) when the waste and old filtrate contain polyphenyl thioether complex fiber material waste product and/or polyphenylene sulfide it is compound
When the leftover pieces of Fiber Materials, the pretreatment filtrate is mixed with solvent, in 150~250 DEG C of 20~40min of insulated and stirred,
Then through the first filtering, non-polyphenylene sulfide solid and the thick solution of polyphenylene sulfide are obtained；Described first filters the filter opening of device used
Aperture is 0.1~0.5mm；
When the waste and old filtrate is free of the waste product and polyphenyl thioether complex fiber material of polyphenyl thioether complex fiber material
When the leftover pieces of matter, the pretreatment filtrate is mixed with solvent, in 150~250 DEG C of 20~40min of insulated and stirred, is gathered
The thick solution of diphenyl sulfide；
The solvent is α-chloronaphthalene or N-Methyl pyrrolidone；
(3) the polyphenylene sulfide solution is carried out to the second filtering under keeping warm mode, obtains polyphenylene sulfide solution；Described
The two filter opening apertures for filtering device used are 10~50 μm；
(4) the polyphenylene sulfide solution is successively carried out to crystallization and third filtering, obtains polyphenylene sulfide.
Preferably, the composite material in the polyphenyl thioether complex fiber is polytetrafluoroethylene (PTFE), aramid fiber, polyimides, glass
Glass fiber, PSA fiber, Powerleader synthetic fibre, terylene or acrylic.
Preferably, the step (1) further includes carrying out ash disposal and washing to waste and old filtrate.
Preferably, the washing carries out under conditions of mechanical stirring assisting ultrasonic.
Preferably, length≤10cm of the pretreatment filtrate in the step (1).
Preferably, the mass ratio of pretreatment filtrate and solvent is 1:50~100 in the step (2).
Preferably, the crystallization in the step (3) includes the following steps: for polyphenylene sulfide solution to be cooled to room temperature, and stands
10~20min.
It preferably, further include that successively polyphenylene sulfide particle is made through pressing and stripping and slicing in polyphenylene sulfide or described will be gathered
Successively polyphenylene sulfide powder is made through broken and milling in diphenyl sulfide.
It preferably, further include that the non-polyphenylene sulfide solid is obtained into the tree of non-polyphenylene sulfide successively through broken and milling
Cosmetics body.
Preferably, the third filtering gained filtrate in the step (3) continues to be recycled as solvent.
The present invention provides a kind of polyphenylene sulfide fibre and its recovery methods of composite fiber filtering material, include the following steps:
(1) waste and old filtrate is successively broken up and is chopped, obtain pretreatment filtrate；The waste and old filtrate is polyphenylene sulfide fibre material
Waste product, the leftover pieces of polyphenylene sulfide fibre material, the waste product of polyphenyl thioether complex fiber material and polyphenylene sulfide are multiple
At least one of the leftover pieces of condensating fiber material；(2) when the waste and old filtrate contains the useless of polyphenyl thioether complex fiber material
When old product and/or the leftover pieces of polyphenyl thioether complex fiber material, the pretreatment filtrate is mixed with solvent, 150~
250 DEG C of 20~40min of insulated and stirred obtain non-polyphenylene sulfide solid and the thick solution of polyphenylene sulfide then through the first filtering；It is described
The first filter opening aperture for filtering device used is 0.1~.5mm；When the waste and old filtrate is free of polyphenyl thioether complex fiber material
Waste product and polyphenyl thioether complex fiber material leftover pieces when, the pretreatment filtrate is mixed with solvent, 150~
250 DEG C of 20~40min of insulated and stirred, obtain polyphenylene sulfide solution；The solvent is α-chloronaphthalene or N-Methyl pyrrolidone；(3)
The thick solution of the polyphenylene sulfide is carried out to the second filtering under keeping warm mode, obtains polyphenylene sulfide solution；Second filtering institute
It is 10~50 μm with the filter opening aperture of device；(4) the polyphenylene sulfide solution is successively carried out to crystallization and third filtering, is gathered
Diphenyl sulfide.
The present invention is mixed by that will pre-process filtrate with solvent, in 150~250 DEG C of 20~40min of insulated and stirred, so that poly-
Diphenyl sulfide is dissolved in α-chloronaphthalene or N-Methyl pyrrolidone, if waste and old filtrate contains the useless of polyphenyl thioether composite material material
Old product or leftover pieces, then compound material obtains non-polyphenylene sulfide solid insoluble in solvent, using filter opening aperture be 0.1~
The device of 0.5mm filters, to realize the separation of polyphenylene sulfide and composite material, obtains the thick solution of polyphenylene sulfide；By polyphenyl
The thick solution of thioether is filtered using the device that filter opening aperture is 10~50 μm, waste and old so as to be adhered in the thick solution of polyphenylene sulfide
Dust impurities removal on filtrate, obtains polyphenylene sulfide solution；Polyphenylene sulfide solution is crystallized, pure polyphenylene sulfide is obtained
Ether.
Detailed description of the invention
The infrared spectrum of 1 gained polyphenylene sulfide powder of Fig. 1 embodiment；
The DSC of 1 gained polyphenylene sulfide powder of Fig. 2 embodiment schemes；
The heat stability testing result figure of 1 gained polyphenylene sulfide powder of Fig. 3 embodiment；
The infrared spectrum of 2 gained polyflon powder of Fig. 4 embodiment；
The DSC of 2 gained polyflon powder of Fig. 5 embodiment schemes；
The infrared spectrum of 3 gained polyimide resin powder body of Fig. 6 embodiment；
The DSC of 3 gained polyimide resin powder body of Fig. 7 embodiment schemes；
The infrared spectrum of 4 gained aramid fiber the tree powder body of Fig. 8 embodiment；
The DSC of 4 gained aramid fiber the tree powder body of Fig. 9 embodiment schemes.
Specific embodiment
The present invention provides a kind of polyphenylene sulfide fibre and its recovery methods of composite fiber filtering material, include the following steps:
(1) waste and old filtrate is successively broken up and is chopped, obtain pretreatment filtrate；The waste and old filtrate is that polyphenylene sulfide is fine
Tie up the waste product of material, the leftover pieces of polyphenylene sulfide fibre material, the waste product of polyphenyl thioether complex fiber material and poly-
At least one of the leftover pieces of diphenyl sulfide composite fibre material；
(2) when the waste and old filtrate contain polyphenyl thioether complex fiber material waste product and/or polyphenylene sulfide it is compound
When the leftover pieces of Fiber Materials, the pretreatment filtrate is mixed with solvent, in 150~250 DEG C of 20~40min of insulated and stirred,
Then through the first filtering, non-polyphenylene sulfide solid and the thick solution of polyphenylene sulfide are obtained；Described first filters the filter opening of device used
Aperture is 0.1~0.5mm；
When the waste and old filtrate is free of the waste product and polyphenyl thioether complex fiber material of polyphenyl thioether complex fiber material
When the leftover pieces of matter, the pretreatment filtrate is mixed with solvent, in 150~250 DEG C of 20~40min of insulated and stirred, is gathered
The thick solution of diphenyl sulfide；
The solvent is α-chloronaphthalene or N-Methyl pyrrolidone；
(3) the thick solution of the polyphenylene sulfide is carried out to the second filtering under keeping warm mode, obtains polyphenylene sulfide solution；It is described
The second filter opening aperture for filtering device used is 10~50 μm；
(4) the polyphenylene sulfide solution is successively carried out to crystallization and third filtering, obtains polyphenylene sulfide.
Waste and old filtrate is successively broken up and is chopped by the present invention, obtains pretreatment filtrate.
In the present invention, the waste and old filtrate is the waste product of polyphenylene sulfide fibre material, polyphenylene sulfide fibre material
Leftover pieces, in the waste product of polyphenyl thioether complex fiber material and the leftover pieces of polyphenyl thioether complex fiber material at least
It is a kind of.In the present invention, the waste product of the polyphenylene sulfide fibre material is preferably used polyphenylene sulfide fibre material
Filtrate；The waste product of the polyphenyl thioether complex fiber material is preferably used polyphenyl thioether complex fiber material
Filtrate；The leftover pieces of the polyphenylene sulfide fibre material are preferably prepared during the filtrate and filter bag of polyphenylene sulfide fibre material
The leftover pieces of generation；The leftover pieces of the polyphenyl thioether complex fiber material preferably prepare polyphenyl thioether complex fiber material
The leftover pieces generated during filtrate and filter bag.
In the present invention, the composite material in the polyphenyl thioether complex fiber is preferably polytetrafluoroethylene (PTFE), aramid fiber, polyamides
Imines, glass fibre, PSA fiber, Powerleader synthetic fibre, terylene or acrylic.
When the waste and old filtrate includes the waste product and/or polyphenyl thioether complex fiber material of polyphenylene sulfide fibre material
Waste product when, it is also preferable to include carry out ash disposal and washing to waste and old filtrate by the present invention；The ash disposal, wash, break up with it is short
The sequence cut preferably successively is broken up, ash disposal, is chopped and washs.
The present invention is not particularly limited the mode broken up, and waste and old filter bag can be torn, be broken up, obtained loose
Fiber or sheet filtrate.In the present invention, described break up can obtain loose fiber or sheet filtrate, be conducive to subsequent
Ash disposal in step.
In the present invention, the ash disposal is preferably mechanical vibrator ash disposal.
In the present invention, the mechanical vibrator ash disposal is preferably carried out in closed condition of negative pressure.The present invention is to the mechanical vibration
The design parameter for playing ash disposal is not particularly limited, and those skilled in the art can be using conventional rapping parameter.In this hair
In bright, by rapping, the most of dust being attached on filtrate and fiber can fall off, and fall under sieve, be located at sieve on
Fiber separation.
In the present invention, it is described pretreatment filtrate length preferably≤10cm；In the present invention, it is described be chopped obtain it is pre-
Processing filtrate is irregular shape, and the length is the extreme length by pretreatment filtrate center.
In the present invention, the washing is preferably water or added with the water of detergent with washing lotion；The present invention is to the washing
The dosage of agent is not particularly limited, and those skilled in the art can select to add or add less to wash according to the clean level of waste and old filtrate
Wash agent；The present invention is not particularly limited the type of the detergent, (is such as deoiled using conventional commercial detergent or similar product
Agent).
In the present invention, the washing is preferably carried out in the condition of mechanical stirring assisting ultrasonic；Described churned mechanically turn
Speed is preferably 100~500rpm, and supersonic frequency is preferably 30~80kHz, and ultrasonic power is preferably 1~5kW.
Preferably the waste and old filtrate after washing is dried by the present invention.The present invention does not have special limit to the mode of the drying
It is fixed, the waste and old filtrate of constant weight can be obtained.
When the waste and old filtrate contains the waste product and/or polyphenyl thioether complex fiber of polyphenyl thioether complex fiber material
When the leftover pieces of material, after obtaining pretreatment filtrate, the present invention mixes the pretreatment filtrate with solvent, it is warming up to 150~
250 DEG C, 20~40min of insulated and stirred, then through the first filtering, obtain non-polyphenylene sulfide solid and the thick solution of polyphenylene sulfide；Institute
The filter opening aperture for stating device used in the first filtering is 0.1~0.5mm.
In the present invention, the solvent is α-chloronaphthalene or N-Methyl pyrrolidone.In the present invention, when the solvent is α-
When chloronaphthalene, the target temperature of the heating is preferably 150~230 DEG C；When the solvent is N-Methyl pyrrolidone, the liter
The target temperature of temperature is preferably 200~250 DEG C.
The present invention is not particularly limited the rate of the heating.
In the present invention, in the mixed process of the pretreatment filtrate and solvent, stirring is preferably maintained.
In the present invention, the mass ratio of the pretreatment filtrate and solvent is preferably 1:50~100, and more preferably 1:70~
85。
The present invention is not particularly limited the concrete mode of first filtering, using filtering side commonly used in the art
Formula.In embodiments of the present invention, for the ease of the separation of non-polyphenylene sulfide solid, preferably by the waste and old filtrate be placed in by
It is then that stainless steel cloth container is soaked in solvent in stainless steel cloth container, it is warming up to required temperature, insulated and stirred is completed
Afterwards, directly stainless steel cloth container is taken out, the separation of solid and liquid of unlike material fiber in filtrate can be completed.
Preferably the first filtering obtained solid is dried by the present invention, obtains non-polyphenylene sulfide solid.The present invention is to described
Dry mode is not particularly limited.
It is also preferable to include the non-polyphenylene sulfide solid successively through broken and milling, is obtained non-polyphenylene sulfide by the present invention
The tree powder body.The present invention is not particularly limited described broken and milling method, using conventional broken of art technology and
Milling operation.In the present invention, the tree powder body of the non-polyphenylene sulfide and primary non-polyphenylene sulfide powder property
Quite, it can be used as the raw material of industry to continue to use.
When the waste and old filtrate is free of the waste product and polyphenyl thioether complex fiber material of polyphenyl thioether complex fiber material
When the leftover pieces of matter, after obtaining pretreatment filtrate, the present invention mixes the pretreatment filtrate with solvent, is warming up to 150~250
DEG C, 20~40min of insulated and stirred obtains the thick solution of polyphenylene sulfide.In the present invention, to contain polyphenylene sulfide with waste and old filtrate compound
The case where when waste products of Fiber Materials or the leftover pieces of polyphenyl thioether complex fiber material, is compared, and the waste and old filtrate is free of
Have polyphenyl thioether complex fiber material waste product and polyphenyl thioether complex fiber material leftover pieces when operating method not
It needs to carry out the first filter operation, other are all the same, and details are not described herein.
After obtaining the thick solution of polyphenylene sulfide, the thick solution of the polyphenylene sulfide is carried out the second mistake by the present invention under keeping warm mode
Filter, obtains polyphenylene sulfide solution；The described second filter opening aperture for filtering device used is 10~50 μm.In the present invention, pass through
The trace solid dust being adhered on polyphenylene sulfide fibre can be removed, play removal of impurities by the filtering of the thick solution of poly-p-phenylene sulfide ether
Effect.
The present invention filters device used to described second and is not particularly limited, and filter opening aperture is in 10~50 μ ms
It can.
After obtaining polyphenylene sulfide solution, the polyphenylene sulfide solution is successively carried out crystallization and third filtering by the present invention, is obtained
To polyphenylene sulfide.
In the present invention, the crystallization preferably includes following steps: polyphenylene sulfide solution is cooled to room temperature, standing 10~
20min.In the present invention, when the temperature of polyphenylene sulfide solution is down to 100 DEG C, polyphenylene sulfide starts to be precipitated, and is cooled to room temperature,
A period of time is stood again, polyphenylene sulfide can be made sufficiently to be precipitated.
The present invention is not particularly limited the speed of the cooling, can be any cooling rate.In the embodiment of the present invention
In, the cooling is preferably natural cooling.
After the completion of third filtering, the present invention is preferably dry by obtained solid product, obtains polyphenylene sulfide.
The mode that the present invention filters the third is not particularly limited, and can isolate the polyphenylene sulfide that crystallization obtains
Come.
In the present invention, the filtrate that the third is obtained by filtration preferably continues to be recycled as solvent.
After obtaining polyphenylene sulfide, preferably polyphenylene sulfide successively is made through pressing and stripping and slicing in polyphenylene sulfide by the present invention
Grain, or successively polyphenylene sulfide powder preferably is made through broken and milling in the polyphenylene sulfide.In the present invention, described poly-
Diphenyl sulfide the tree powder body and the property of primary polyphenylene sulfide powder are essentially identical, can substitute primary polyphenylene sulfide resin cosmetics
Body is used in mixed way with primary polyphenylene sulfide powder.
The present invention is not particularly limited the concrete operations of the pressing and stripping and slicing, prepares polyphenylene sulfide resin using conventional
The pressing of rouge particle and dicing operation.
The present invention is not particularly limited the broken and milling mode of the polyphenylene sulfide, and those skilled in the art are using normal
The broken and milling operation of rule.
Below with reference to embodiment to the recycling side of a kind of polyphenylene sulfide fibre provided by the invention and its composite fiber filtering material
Method is described in detail, but they cannot be interpreted as limiting the scope of the present invention.
Embodiment 1
It is 130~180 DEG C that the recovery processing object of the present embodiment, which is for treatment temperature, corrosivity is lesser conventional coal-fired
The filter bag of flue gas, i.e. 100% polyphenylene sulfide fibre surface layer/polyphenylene sulfide base fabric are handled as follows:
In closed negative pressure space, slabbing is disassembled by cloth shredding equipment, then remove filter with mechanical vibrator
Then bag surface and internal dust use cloth chopped device, be cut into 10cm fritter below, put into industrial washing, add
The degreaser and detergent for adding 5%, start rinsing maching, speed of agitator be 150rpm, supersonic frequency 40kHz, ultrasonic power
It is after the completion of washing, the filter bag centrifugal drying dry doubling after washing is dry to wash filter bag under conditions of 1.5kw, obtain the pre- of cleaning
Handle filtrate；The water of washing removes the greasy dirt on surface by standing overflow, is left the sludge of bottom after precipitation, upper water can
With reuse, the greasy dirt liquid and precipitating gained sludge of spilling are handled according to rule；
Pretreatment filtrate investment is filled into α-chloronaphthalene, in the reaction kettle with fluid agitation, pretreatment filtrate and α-chlorine
The mass ratio of naphthalene is 1:100, is heated to 220 DEG C, start liquid agitating device to accelerate the dissolution of polyphenylene sulfide, after 30 minutes to
Polyphenyl thioether filter material all dissolves, and the liquid in reaction kettle is poured into heat preserving type filter press at 220 DEG C and is filtered, filter used
The filter opening aperture of cloth is 50 μm, is the micro dust for being adhered on waste and old filtrate, not cleaning thoroughly above filter cloth, is below filter cloth
Pure polyphenylene sulfide solution is cooled to room temperature polyphenylene sulfide solution pure under filter cloth, stands 10 minutes, and polyphenylene sulfide is in
Floccule is precipitated, and liquid is poured into filter press and is filtered, is α-chloronaphthalene liquid below filter cloth, can continue reuse, on strainer
It is polyphenylene sulfide solid, after the drying of polyphenylene sulfide solid, polyphenylene sulfide particle is made by pressing, stripping and slicing.
Infrared spectroscopy and DSC combination are carried out to the resulting polyphenylene sulfide particle of the present embodiment and pure polyphenylene sulfide sample
Technology detects its ingredient and correlation properties, and gained infrared spectrum is as shown in Figure 1.As shown in Figure 1, polyphenylene sulfide obtained by the present embodiment
The skeletal vibration peak of resin particle is 1560cm-1、1470cm-1、1387cm-1、735cm-1, it is identical as pure polyphenylene sulfide sample,
There is not any other characteristic peak, illustrates the polyphenylene sulfide powder purity with higher that the present embodiment recycles.
Polyphenylene sulfide particle and pure polyphenylene sulfide sample obtained by the present embodiment are tested using differential scanning calorimetry
Fusing point, as a result as shown in Fig. 2, as shown in Figure 2, the fusing point of polyphenylene sulfide particle obtained by the present embodiment near 285 DEG C, with
The fusing point of pure polyphenylene sulfide sample is identical, and the holding of higher melt illustrate the obtained polyphenylene sulfide particle of recycling still have compared with
Big molecular weight, recycling quality are higher.
The thermal stability of polyphenylene sulfide particle obtained by the present embodiment and pure polyphenylene sulfide sample is tested, as a result
As shown in figure 3, polyphenylene sulfide particle corresponding temperature when thermal weight loss rate is 5% is 516 DEG C or so, slightly below pure polyphenyl
518 DEG C of thioether sample, i.e. the thermal stability of recovery product decreases, but still has preferable thermal stability on the whole.
Embodiment 2
The recovery processing object of the present embodiment is the filter bag for handling the higher coal smoke of sulfur corrosion, i.e. 50% polyphenyl
+ 50% polytetrafluoroethylene fibre surface layer of sulfide fibers/polytetrafluoroethylene (PTFE) base fabric is handled as follows:
In closed negative pressure space, slabbing is disassembled by cloth shredding equipment, then remove filter with mechanical vibrator
Then bag surface and internal dust use cloth chopped device, be cut into 10cm fritter below, put into industrial washing, add
The degreaser and detergent for adding 10%, start rinsing maching, speed of agitator be 200rpm, supersonic frequency 50kHz, ultrasonic power
It is after the completion of washing, the filter bag centrifugal drying dry doubling after washing is dry to wash filter bag under conditions of 3.5kW, obtain the pre- of cleaning
Handle filtrate；The water of washing removes the greasy dirt on surface by standing overflow, is left the sludge of bottom after precipitation, upper water can
With reuse, the greasy dirt liquid and precipitating gained sludge of spilling are handled according to rule；
The pretreatment filtrate is fitted into stainless steel cloth container, the mesh aperture of stainless steel cloth container is 0.5mm,
Stainless steel cloth container investment is filled into α-chloronaphthalene, in the reaction kettle with fluid agitation, pretreatment filtrate and α-chloronaphthalene quality
Than for 1:50, being heated to 230 DEG C, start liquid agitating device is poly- in filtrate after twenty minutes to accelerate the dissolution of polyphenylene sulfide
Sulfide fibers can all dissolve, and stainless steel cloth container is taken out, and polytetrafluoroethylene (PTFE) is filled in stainless steel cloth container, reaction
Liquid in kettle is polyphenylene sulfide solution；
Liquid in reaction kettle is poured into heat preserving type filter press at 230 DEG C to be filtered, the filter opening aperture of filter cloth is 50 μ
M, be above filter cloth be adhered on waste and old filtrate, not thorough clean micro dust, be that pure polyphenylene sulfide is molten below filter cloth
Liquid is cooled to room temperature polyphenylene sulfide solution pure under filter cloth, stands 10 minutes, and polyphenylene sulfide is precipitated in floccule, liquid
Body pours into filter press and is filtered, and is α-chloronaphthalene liquid below filter cloth, can continue reuse, is polyphenylene sulfide solid on strainer,
After the drying of polyphenylene sulfide solid, spinning is carried out after mixing with primary polyphenylene sulfide according to the ratio of mass ratio 1:1, is prepared
Polyphenylene sulfide fibre, and then reproduction filter bag, realize recycling for polyphenylene sulfide；Polytetrafluoroethyl-ne in stainless steel cloth container
Alkene clear water is cleaned dry after, by broken, milling, 60 mesh powder below, i.e. polyflon powder is made, is used as
The raw material of polytetrafluoroethyltubing tubing, wire rod, anti-corrosion part etc..
Infrared spectroscopy and DSC combination are carried out to the resulting polyphenylene sulfide powder of the present embodiment and polytetrafluoroethylpowder powder
Technology detects its ingredient and correlation properties, and wherein the infrared spectrum of polyphenylene sulfide powder is same as Example 1, illustrates this reality
Apply the polyphenylene sulfide powder purity with higher that example recycles；The infrared spectrum of gained polyflon powder
As shown in figure 4, as shown in Figure 4, the main characteristic peak 1219cm of polytetrafluoroethylene (PTFE)-1And 1158cm-1It still has, and it is pure
Polytetrafluoroethylene (PTFE) spectrum is compared, and not new characteristic peak occurs, it was demonstrated that the purity of the polyflon of recycling.
The fusing point of polyphenylene sulfide powder and polyflon powder obtained by the present embodiment is tested, wherein polyphenylene sulfide
The result figure of ether resin powder is same as Example 1, and the fusing point of polyphenylene sulfide powder obtained by the present embodiment is attached at 285 DEG C
Closely, identical as the fusing point of pure polyphenylene sulfide sample；The result figure of polyflon powder is as shown in figure 5, polytetrafluoroethylene (PTFE)
The fusing point of the tree powder body is 347 DEG C or so, close with pure polytetrafluoroethylene (PTFE), illustrates that polyflon powder purity is higher.
The thermal stability of polyphenylene sulfide powder obtained by the present embodiment and polyflon powder is tested,
Wherein the result figure of polyphenylene sulfide powder is same as Example 1, polyphenylene sulfide powder thermal weight loss rate be 5% when pair
The temperature answered is 516 DEG C or so；Polyflon powder corresponding temperature when thermal weight loss rate is 5% is 546 DEG C or so,
It is substantially identical as pure polytetrafluoroethylene (PTFE).
Embodiment 3
The recovery processing object of the present embodiment is for handling dust concentration 100g/m3More than or 190 DEG C of flue-gas temperature with
On flue dust filter bag, i.e. 80%+20% polyimides of polyphenylene sulfide/polyimides base fabric handles as follows:
In closed negative pressure space, slabbing is disassembled by cloth shredding equipment, then remove filter with mechanical vibrator
Then bag surface and internal dust use cloth chopped device, be cut into 10cm fritter below, put into industrial washing, add
The degreaser and detergent for adding 5%, start rinsing maching, speed of agitator be 200rpm, supersonic frequency 35kHz, ultrasonic power
It is after the completion of washing, the filter bag centrifugal drying dry doubling after washing is dry to wash filter bag under conditions of 1.8kW, obtain the pre- of cleaning
Handle filtrate；The water of washing removes the greasy dirt on surface by standing overflow, is left the sludge of bottom after precipitation, upper water can
With reuse, the greasy dirt liquid and precipitating gained sludge of spilling are handled according to rule；
The pretreatment filtrate is fitted into stainless steel cloth container, the mesh aperture of stainless steel cloth container is 0.5mm,
Stainless steel cloth container investment is filled into α-chloronaphthalene, in the reaction kettle with fluid agitation, pretreatment filtrate and α-chloronaphthalene quality
Than for 1:90, being heated to 230 DEG C, start liquid agitating device is to accelerate the dissolution of polyphenylene sulfide, polyphenyl in filtrate after 30 minutes
Sulfide fibers all dissolve, and stainless steel cloth container is taken out, and fill polyimides in stainless steel cloth container, in reaction kettle
Liquid is polyphenylene sulfide solution；
Liquid in reaction kettle is poured into heat preserving type filter press at 230 DEG C to be filtered, the filter opening aperture of filter cloth is 50 μ
M, be above filter cloth be adhered on waste and old filtrate, not thorough clean micro dust, be that pure polyphenylene sulfide is molten below filter cloth
Liquid is cooled to room temperature polyphenylene sulfide solution pure under filter cloth, stands 10 minutes, and polyphenylene sulfide is precipitated in floccule, liquid
Body pours into filter press and is filtered, and is α-chloronaphthalene liquid below filter cloth, can continue reuse, is polyphenylene sulfide solid on strainer,
After the drying of polyphenylene sulfide solid, polyphenylene sulfide is obtained；Polyimides clear water in stainless steel cloth container is cleaned dry after,
By broken, milling, 100 mesh powder below, i.e. polyimide resin powder body is made, is used as the raw material of industry.
Infrared spectroscopy and the inspection of DSC joint technology are carried out to the resulting polyphenylene sulfide of the present embodiment and polyimide resin powder body
Its ingredient and correlation properties are surveyed, wherein the infrared spectrum of polyphenylene sulfide is same as Example 1, illustrates what the present embodiment recycled
Polyphenylene sulfide purity with higher；The infrared spectrum of gained polyimide resin powder body as shown in fig. 6, it will be appreciated from fig. 6 that
1780cm-1、1725cm-1、1702cm-1For cyclic imide characteristic peak；1661cm-1For the characteristic peak of second level amide groups；
1579cm-1、1507cm-1、1423cm-1For the vibration peak of phenyl ring, compared with pure polyimide resin, not new vibration
Peak generates, it was demonstrated that the degree of purity of recycling resin polyimides.
The fusing point of polyphenylene sulfide powder and polyimide resin powder body obtained by the present embodiment is tested, wherein polyphenylene sulfide
The result figure of the tree powder body is same as Example 1, the fusing point of polyphenylene sulfide powder obtained by the present embodiment near 285 DEG C,
It is identical as the fusing point of pure polyphenylene sulfide sample；The result figure of polyimide resin powder body is as shown in fig. 7, polyimide resin powder body
There is no the appearance of feature melting peak, meets the feature of polyimides.
The thermal stability of polyphenylene sulfide powder obtained by the present embodiment and polyimide resin powder body is tested,
The result figure of middle polyphenylene sulfide powder is same as Example 1, and polyphenylene sulfide powder is 5% corresponding in thermal weight loss rate
Temperature is 516 DEG C or so；It is 429 DEG C or so that polyimide resin powder body, which is 10% corresponding temperature in thermal weight loss rate, is gathered with pure
Acid imide is essentially identical.
Embodiment 4
The recovery processing object of the present embodiment is the filter bag for 210 DEG C of temperature or so of cement kiln head flue gas, i.e., 50%
+ 50% aramid fiber of polyphenylene sulfide/polyphenylene sulfide base fabric is handled as follows:
In closed negative pressure space, slabbing is disassembled by cloth shredding equipment, then remove filter with mechanical vibrator
Then bag surface and internal dust use cloth chopped device, be cut into 10cm fritter below, put into industrial washing, add
The degreaser and detergent for adding 5%, start rinsing maching, speed of agitator be 350rpm, supersonic frequency 60kHz, ultrasonic power
It is after the completion of washing, the filter bag centrifugal drying dry doubling after washing is dry to wash filter bag under conditions of 5kW, obtain clean pre- place
Manage filtrate；The water of washing removes the greasy dirt on surface by standing overflow, is left the sludge of bottom after precipitation, and upper water can be with
Reuse, the greasy dirt liquid and precipitating gained sludge of spilling are handled according to rule；
The pretreatment filtrate is fitted into stainless steel cloth container, the mesh aperture of stainless steel cloth container is 0.5mm,
Stainless steel cloth container investment is filled into N-Methyl pyrrolidone, in the reaction kettle with fluid agitation, pretreatment filtrate and N- first
The mass ratio of base pyrrolidones is 1:50, is heated to 218 DEG C, and start liquid agitating device is to accelerate the dissolution of polyphenylene sulfide, 30
Polyphenylene sulfide fibre after minute in filtrate can all dissolve, and stainless steel cloth container is taken out, is contained in stainless steel cloth container
There is aramid fiber, the liquid in reaction kettle is polyphenylene sulfide solution；
Liquid in reaction kettle is poured into heat preserving type filter press at 218 DEG C to be filtered, the filter opening aperture of filter cloth used
It is 50 μm, is the micro dust for being adhered on waste and old filtrate, not cleaning thoroughly above filter cloth, is pure polyphenylene sulfide below filter cloth
Ethereal solution is cooled to room temperature polyphenylene sulfide solution pure under filter cloth, stands 10 minutes, and polyphenylene sulfide is precipitated in floccule,
Liquid is poured into filter press to be filtered, is N-Methyl pyrrolidone below filter cloth, reuse can be continued, is polyphenylene sulfide on strainer
Ether solid is milled to obtain 60 mesh polyphenylene sulfide powder below, with primary polyphenyl after the drying of polyphenylene sulfide solid
Thioether carries out spinning after mixing according to 1:1.5 ratio, manufactures filtrate again；Aramid fiber in stainless steel cloth container is cleaned with clear water
After drying, by broken, milling, 80 mesh powder below, i.e. aramid fiber the tree powder body is made, is used as the raw material of industry.
Infrared spectroscopy is carried out to the resulting polyphenylene sulfide powder of the present embodiment and aramid fiber the tree powder body and DSC is combined skill
Art detects its ingredient and correlation properties, and wherein the infrared spectrum of polyphenylene sulfide is same as Example 1, illustrates that the present embodiment recycles
The polyphenylene sulfide arrived purity with higher；The infrared spectrum of gained aramid fiber the tree powder body is as shown in figure 8, as shown in Figure 8, amide
Base stretching vibration peak 1648cm-1, the stretching vibration peak 1599cm of phenyl ring-1、1515cm-1、1470cm-1, the flexible vibration of phenyl ring meta position
Dynamic peak 682cm-1Still exist, and compared with pure aramid fiber spectrum, occur without others new feature peak, illustrates gained aramid fiber resin
Powder is more pure.
The fusing point of polyphenylene sulfide powder and aramid fiber the tree powder body obtained by the present embodiment is tested, wherein polyphenylene sulfide
The result figure of powder is same as Example 1, and the fusing point of polyphenylene sulfide powder obtained by the present embodiment is and pure near 285 DEG C
The fusing point of polyphenylene sulfide sample is identical；The result figure of aramid fiber the tree powder body is as shown in figure 9, fusing point is near 440 DEG C, for aramid fiber
Fusing point illustrates aramid fiber purity with higher.
The thermal stability of polyphenylene sulfide powder obtained by the present embodiment and aramid fiber the tree powder body is tested, wherein gathering
The result figure of diphenyl sulfide the tree powder body is same as Example 1, and polyphenylene sulfide powder is 5% corresponding temperature in thermal weight loss rate
It is 516 DEG C or so；It is 457 DEG C or so that aramid fiber the tree powder body, which is 10% corresponding temperature in thermal weight loss rate, with the basic phase of pure aramid fiber
Together.
Embodiment 5
The recovery processing object of the present embodiment is the filter bag for temperature in 180 DEG C of coal-fired plant flue gas below, i.e.,
80%+20% acrylic of polyphenylene sulfide/polyphenylene sulfide base fabric is handled as follows:
In closed negative pressure space, slabbing is disassembled by cloth shredding equipment, then remove filter with mechanical vibrator
Then bag surface and internal dust use cloth chopped device, be cut into 10cm fritter below, put into industrial washing, add
The degreaser and detergent for adding 5%, start rinsing maching, speed of agitator be 230rpm, supersonic frequency 50kHz, ultrasonic power
It is after the completion of washing, the filter bag centrifugal drying dry doubling after washing is dry to wash filter bag under conditions of 4.5kW, obtain the pre- of cleaning
Handle filtrate；The water of washing removes the greasy dirt on surface by standing overflow, is left the sludge of bottom after precipitation, upper water can
With reuse, the greasy dirt liquid and precipitating gained sludge of spilling are handled according to rule；
The pretreatment filtrate is fitted into stainless steel cloth container, the mesh aperture of stainless steel cloth container is 0.2mm,
Stainless steel cloth container investment is filled into α-chloronaphthalene, in the reaction kettle with fluid agitation, pretreatment filtrate and α-chloronaphthalene quality
Than for 1:100, being heated to 150 DEG C, start liquid agitating device is poly- in filtrate after forty minutes to accelerate the dissolution of polyphenylene sulfide
Sulfide fibers can all dissolve, and stainless steel cloth container is taken out, and fill acrylic in stainless steel cloth container, in reaction kettle
Liquid be polyphenylene sulfide solution；
Liquid in reaction kettle is poured into heat preserving type filter press at 150 DEG C to be filtered, the filter opening aperture of filter cloth used
It is 50 μm, is the micro dust for being adhered on waste and old filtrate, not cleaning thoroughly above filter cloth, is pure polyphenylene sulfide below filter cloth
Ethereal solution is cooled to room temperature polyphenylene sulfide solution pure under filter cloth, stands 10 minutes, and polyphenylene sulfide is precipitated in floccule,
Liquid is poured into filter press to be filtered, is α-chloronaphthalene below filter cloth, reuse can be continued, is polyphenylene sulfide solid on strainer,
After the drying of polyphenylene sulfide solid, it is milled to obtain 325 mesh polyphenylene sulfide powder below, can be used for 3D printing；No
Acrylic clear water in rust steel wire container is cleaned dry after, by broken, milling, 80 mesh powder below is made, i.e., it is sub-
Gram force the tree powder body, uses as the raw material of industry.
To the resulting polyphenylene sulfide powder of the present embodiment carry out infrared spectroscopy and DSC joint technology detect its ingredient and
Correlation properties, wherein the infrared spectrum of polyphenylene sulfide is same as Example 1.Test polyphenylene sulfide powder obtained by the present embodiment
Fusing point and thermal stability, it is as a result same as Example 1.
Embodiment 6
The recovery processing object of the present embodiment is the filter bag for temperature in 130~150 DEG C of coal-fired plant flue gas, i.e.,
80%+20% terylene of polyphenylene sulfide/polyphenylene sulfide base fabric is handled as follows:
In closed negative pressure space, slabbing is disassembled by cloth shredding equipment, then remove filter with mechanical vibrator
Then bag surface and internal dust use cloth chopped device, be cut into 10cm fritter below, put into industrial washing, add
The degreaser and detergent for adding 5%, start rinsing maching, speed of agitator be 230rpm, supersonic frequency 45kHz, ultrasonic power
It is after the completion of washing, the filtrate centrifugal drying dry doubling after washing is dry to wash filter bag under conditions of 4.0kW, obtain the pre- of cleaning
Handle filtrate；The water of washing removes the greasy dirt on surface by standing overflow, is left the sludge of bottom after precipitation, upper water can
With reuse, the greasy dirt liquid and precipitating gained sludge of spilling are handled according to rule；
The pretreatment filtrate is fitted into stainless steel cloth container, the mesh aperture of stainless steel cloth container is 0.2mm,
Stainless steel cloth container investment is filled into α-chloronaphthalene, in the reaction kettle with fluid agitation, pretreatment filtrate and α-chloronaphthalene quality
Than for 1:100, being heated to 180 DEG C, start liquid agitating device is poly- in filtrate after 25 minutes to accelerate the dissolution of polyphenylene sulfide
Diphenyl sulfide filtrate can all dissolve, and stainless steel cloth container is taken out, and fill terylene in stainless steel cloth container, in reaction kettle
Liquid is polyphenylene sulfide solution；
Liquid in reaction kettle is poured into heat preserving type filter press at 180 DEG C to be filtered, the filter opening aperture of filter cloth used
It is 50 μm, is the micro dust for being adhered on waste and old filtrate, not cleaning thoroughly above filter cloth, is pure polyphenylene sulfide below filter cloth
Ethereal solution is cooled to room temperature polyphenylene sulfide solution pure under filter cloth, stands 10 minutes, and polyphenylene sulfide is precipitated in floccule,
Liquid is poured into filter press to be filtered, is α-chloronaphthalene below filter cloth, reuse can be continued, is polyphenylene sulfide solid on strainer,
After the drying of polyphenylene sulfide solid, through broken and milling, obtains polyphenylene sulfide powder and be molded for polyphenylene sulfide；Stainless steel
Terylene clear water in silk screen container is cleaned dry after, by broken, milling, 16 mesh powder below, i.e. polyester resin is made
Powder makes polyester fiber after mixing with primary terylene according to 1:1.5 mass ratio, is re-used for production filtrate.
To the resulting polyphenylene sulfide powder of the present embodiment carry out infrared spectroscopy and DSC joint technology detect its ingredient and
Correlation properties, wherein the infrared spectrum of polyphenylene sulfide is same as Example 1.Test polyphenylene sulfide powder obtained by the present embodiment
Fusing point and thermal stability, it is as a result same as Example 1.
Embodiment 7
The recovery processing object of the present embodiment is small for the high temperature and corrosivity for steel and 180 DEG C of cement kiln or more
The filter bag of flue dust, i.e. 60%+40% glass fibre of polyphenylene sulfide/glass fibre base fabric are handled as follows:
In closed negative pressure space, slabbing is disassembled by cloth shredding equipment, then remove filter with mechanical vibrator
Then bag surface and internal dust use cloth chopped device, be cut into 10cm fritter below, put into industrial washing, add
The degreaser and detergent for adding 10%, start rinsing maching, speed of agitator be 200rpm, supersonic frequency 45kHz, ultrasonic power
It is after the completion of washing, the filtrate centrifugal drying dry doubling after washing is dry to wash filter bag under conditions of 5.0kW, obtain the pre- of cleaning
Handle filtrate；The water of washing removes the greasy dirt on surface by standing overflow, is left the sludge of bottom after precipitation, upper water can
With reuse, the greasy dirt liquid and precipitating gained sludge of spilling are handled according to rule；
The pretreatment filtrate is fitted into stainless steel cloth container, the mesh aperture of stainless steel cloth container is 0.1mm,
Stainless steel cloth container investment is filled into N-Methyl pyrrolidone, in the reaction kettle with fluid agitation, pretreatment filtrate and N- first
The mass ratio of base pyrrolidones is 1:50, is heated to 230 DEG C, and start liquid agitating device is to accelerate the dissolution of polyphenylene sulfide, 20
Polyphenylene sulfide fibre after minute in filtrate can all dissolve, and stainless steel cloth container is taken out, is contained in stainless steel cloth container
There is glass fibre, the liquid in reaction kettle is polyphenylene sulfide solution；
Liquid in reaction kettle is poured into heat preserving type filter press at 230 DEG C to be filtered, the filter opening aperture of filter cloth used
It is 50 μm, is the micro dust for being adhered on waste and old filtrate, not cleaning thoroughly above filter cloth, is pure polyphenylene sulfide below filter cloth
Ethereal solution is cooled to room temperature polyphenylene sulfide solution pure under filter cloth, stands 10 minutes, and polyphenylene sulfide is precipitated in floccule,
Liquid is poured into filter press to be filtered, is N-Methyl pyrrolidone below filter cloth, reuse can be continued, is polyphenylene sulfide on strainer
Ether solid is granulated after the drying of polyphenylene sulfide solid, is used for braking automobile tablet raw material；Glass fibers in stainless steel cloth container
Wesy's clear water clean dry after, used as the raw material of industry.
To the resulting polyphenylene sulfide powder of the present embodiment carry out infrared spectroscopy and DSC joint technology detect its ingredient and
Correlation properties, wherein the infrared spectrum of polyphenylene sulfide is same as Example 1.Test polyphenylene sulfide powder obtained by the present embodiment
Fusing point and thermal stability, it is as a result same as Example 1.
Embodiment 8
The recovery processing object of the present embodiment is 50%+50% polytetrafluoroethylene fibre of polyphenylene sulfide/PTFE base
The corner virgin material of cloth is handled as follows:
In closed negative pressure space, slabbing is disassembled by cloth shredding equipment, is then chopped and is filled using cloth
It sets, is cut into 10cm fritter below, obtain pretreatment filtrate；
The pretreatment filtrate is fitted into stainless steel cloth container, the mesh aperture of stainless steel cloth container is 0.1mm,
Stainless steel cloth container investment is filled into α-chloronaphthalene, in the reaction kettle with fluid agitation, pretreatment filtrate and α-chloronaphthalene quality
Than for 1:50, being heated to 230 DEG C, start liquid agitating device is poly- in filtrate after twenty minutes to accelerate the dissolution of polyphenylene sulfide
Sulfide fibers can all dissolve, and stainless steel cloth container is taken out, and polytetrafluoroethylene (PTFE) is filled in stainless steel cloth container, reaction
Liquid in kettle is polyphenylene sulfide solution；
Liquid in reaction kettle is poured into heat preserving type filter press at 230 DEG C to be filtered, the filter opening aperture of filter cloth used
It is 50 μm, is the micro dust for being adhered on waste and old filtrate, not cleaning thoroughly above filter cloth, is pure polyphenylene sulfide below filter cloth
Ethereal solution is cooled to room temperature polyphenylene sulfide solution pure under filter cloth, stands 10 minutes, and polyphenylene sulfide is precipitated in floccule,
Liquid is poured into filter press to be filtered, is α-chloronaphthalene below filter cloth, reuse can be continued, is polyphenylene sulfide solid on strainer,
After the drying of polyphenylene sulfide solid, successively through granulation and spinning, filtrate is manufactured again；Polytetrafluoroethyl-ne in stainless steel cloth container
Alkene clear water is cleaned dry after, by broken, milling, 60 mesh powder below is made, is used for polytetrafluoroethylene (PTFE) spinning, uses again
In production filtrate.
To the resulting polyphenylene sulfide powder of the present embodiment carry out infrared spectroscopy and DSC joint technology detect its ingredient and
Correlation properties, wherein the infrared spectrum of polyphenylene sulfide is same as Example 1.Test polyphenylene sulfide powder obtained by the present embodiment
Fusing point and thermal stability, it is as a result same as Example 1.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (10)
1. the recovery method of a kind of polyphenylene sulfide fibre and its composite fiber filtering material, includes the following steps:
(1) waste and old filtrate is successively broken up and is chopped, obtain pretreatment filtrate；The waste and old filtrate is polyphenylene sulfide fibre material
The waste product of matter, the leftover pieces of polyphenylene sulfide fibre material, polyphenyl thioether complex fiber material waste product and polyphenylene sulfide
At least one of the leftover pieces of ether composite fibre material；
(2) when the waste and old filtrate contains the waste product and/or polyphenyl thioether complex fiber of polyphenyl thioether complex fiber material
When the leftover pieces of material, the pretreatment filtrate is mixed with solvent, kept the temperature at 150~250 DEG C and stir 20~40min, so
By the first filtering, non-polyphenylene sulfide solid and the thick solution of polyphenylene sulfide are obtained；Described first filters the filter opening hole of device used
Diameter is 0.1~0.5mm；
When the waste and old filtrate waste product and polyphenyl thioether complex fiber material without polyphenyl thioether complex fiber material
When leftover pieces, the pretreatment filtrate is mixed with solvent, kept the temperature at 150~250 DEG C and stir 20~40min, obtains polyphenyl
The thick solution of thioether；
The solvent is α-chloronaphthalene or N-Methyl pyrrolidone；
(3) the thick solution of the polyphenylene sulfide is carried out to the second filtering under keeping warm mode, obtains polyphenylene sulfide solution；Described second
The filter opening aperture for filtering device used is 10~50 μm；
(4) the polyphenylene sulfide solution is successively carried out to crystallization and third filtering, obtains polyphenylene sulfide.
2. recovery method according to claim 1, which is characterized in that the composite material in the polyphenyl thioether complex fiber
For polytetrafluoroethylene (PTFE), aramid fiber, polyimides, glass fibre, PSA fiber, Powerleader synthetic fibre, terylene or acrylic.
3. recovery method according to claim 1, which is characterized in that the step (1) further includes carrying out to waste and old filtrate
Ash disposal and washing.
4. recovery method according to claim 3, which is characterized in that condition of the washing in mechanical stirring assisting ultrasonic
Lower progress.
5. recovery method according to claim 1, which is characterized in that the length of the pretreatment filtrate in the step (1)
≤10cm。
6. recovery method according to claim 1, which is characterized in that pretreatment filtrate and solvent in the step (2)
Mass ratio is 1:50~100.
7. recovery method according to claim 1, which is characterized in that the crystallization in the step (3) includes the following steps:
Polyphenylene sulfide solution is cooled to room temperature, 10~20min is stood.
8. recovery method according to claim 1 or claim 7, which is characterized in that further include by the polyphenylene sulfide successively through pressing
It closes and polyphenylene sulfide particle is made in stripping and slicing, or successively polyphenylene sulfide is made through broken and milling in the polyphenylene sulfide
Powder.
9. recovery method according to claim 1, which is characterized in that further include successively passing through the non-polyphenylene sulfide solid
Broken and milling, obtains the tree powder body of non-polyphenylene sulfide.
10. recovery method according to claim 1, which is characterized in that the third filtering gained filtrate in the step (3)
Continue to be recycled as solvent.
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Application publication date: 20190319 |
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