CN104178824B - Prepare purging system and the method for polyacrylonitrile fibril dry-jet wet-spinning spinneret - Google Patents
Prepare purging system and the method for polyacrylonitrile fibril dry-jet wet-spinning spinneret Download PDFInfo
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- CN104178824B CN104178824B CN201310194958.4A CN201310194958A CN104178824B CN 104178824 B CN104178824 B CN 104178824B CN 201310194958 A CN201310194958 A CN 201310194958A CN 104178824 B CN104178824 B CN 104178824B
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Abstract
The present invention relates to a kind of purging system and method for preparing polyacrylonitrile fibril dry-jet wet-spinning spinneret. This purging system comprises for spinneret being carried out to the pre-soaking device of pre-soaking, for spinneret being carried out to the circulation cleaning device of wash cycles, for spinneret being carried out to the equipment for steam treatment of steam treatment. Above-mentioned cleaning method comprises: spinneret is carried out to prerinse with DMSO; With desalted water to rinsing through the spinneret of pre-soaking; With DMSO to spinneret wash cycles; With desalted water to rinsing through the spinneret of wash cycles; Spinneret is carried out to steam treatment with steam; Spinneret through steam treatment is carried out to Ultrasonic Cleaning; To dry up through ultrasonic wave clear spinneret with compressed air; To detecting through the spinneret cleaning, process for underproof repeating, until qualified.
Description
Technical field
The present invention relates to a kind of purging system and method for preparing polyacrylonitrile fibril dry-jet wet-spinning spinneret, belong to highMolecular material stand-by equipment cleaning technique processed field.
Background technology
Dry-jet wet-spinning spinneret is the main portion that dry-jet wet-spinning is prepared the moulding of high-performance carbon fibre polyacrylonitrile (PAN) precursorPart, its Main Function is that PAN spinning solution is sprayed to uniform spinning solution thread vertically downward by spinneret, by a bit of airLayer enters coagulating bath coagulation forming, forms as-spun fibre.
In dry-jet wet-spinning spray silk process, because dry-jet wet-spinning spinning fluid viscosity used is high, molecular weight is high, spinning solution filtersThe impact of the factors such as bad, spinning solution homogeneity is poor, there is easy plug-hole, tear drop or unrestrained plate in spinneret, even cannot spinning etc. existingResemble, greatly affect spinnability and the fiber quality of spinning, therefore must carry out periodic cycle cleaning to spinneret.
The cleaning method of spinneret has various ways, and conventional have solvent clean method, ultrasonic cleaning process, an acid process etc.Because dry-jet wet-spinning spinneret is thicker, adopt single method all to have the drawbacks such as cleaning performance is poor, scavenging period is long, serious shadowRung spinning quality, therefore PAN precursor with being washed to of dry-jet wet-spinning spinneret be badly in need of solve a great problem.
Summary of the invention
For solving the problems of the technologies described above, the object of the present invention is to provide one to prepare polyacrylonitrile fibril dry-jet wet-spinningThe cleaning device of spinneret and method, it is by adopting dimethyl sulfoxide (DMSO) (DMSO) and steam etc. to carry out repeatedly clear to spinneretThe method of washing, adopts this device and method can thoroughly remove attachment and the impurity on spinneret, thereby increases substantially drySquirt the quality of spinning PAN precursor.
For achieving the above object, the invention provides a kind of cleaning of preparing polyacrylonitrile fibril dry-jet wet-spinning spinneretSystem, it comprises pre-soaking device, circulation cleaning device, equipment for steam treatment, wherein:
Described pre-soaking device comprises spinneret presoaking tank, and a side of this spinneret presoaking tank is established from high to low successivelyHave desalted water entrance, DMSO entrance, compressed air inlet, this spinneret presoaking tank inside is provided with the dividing plate of level, and, instituteStating compressed air inlet is connected with the nozzle that is positioned at described spinneret presoaking tank inside;
Described circulation cleaning device comprises DMSO solvent circulating slot, and a side of this DMSO solvent circulating slot is provided with DMSO entranceWith desalted water entrance, opposite side is provided with DMSO and exports and be connected with a liquid level gauge, and the top of this DMSO solvent circulating slot is provided with manyIndividual spinneret fixing seal chamber; Described DMSO outlet is connected with DMSO circulating pump by pipeline, and described DMSO circulating pump passed throughFilter is connected with described spinneret fixing seal chamber and its connecting pipe is provided with wash cycles pipeline drain; Described DMSOCirculating pump is also connected to by pipeline DMSO self loop head that is positioned at described DMSO solvent circulating slot inside; Described spinneretFixing seal chamber is connected with the wash cycles pipeline DMSO outlet that is positioned at described DMSO solvent circulating slot inside respectively;
Described equipment for steam treatment comprises spinneret steam treatment groove and desalted water recycle unit, this spinneret steam treatmentThe top of groove is provided with a spinneret fixing seal chamber, and this spinneret fixing seal chamber is provided with steam (vapor) outlet, and this spinneret is solidDetermine annular seal space and be connected with steam input pipe line, this steam input pipe line is provided with steam inlet and compressed air inlet, described steamingVapour entrance is connected with described spinneret fixing seal chamber by cylinder valve with compressed air inlet; Described spinneret steam treatment grooveA side be provided with successively from high to low the outlet of overfall, steam treatment groove desalted water, desalted water water supplement port; Described spinneret steamThe bottom for the treatment of trough is provided with steam treatment groove desalted water entrance;
Described desalted water recycle unit comprises plate type heat exchanger and temperature controller, and wherein, described plate type heat exchanger is provided withChilled water inlet and chilled water outlet, and described chilled water inlet place is provided with control valve group, and described plate type heat exchanger is also distinguishedIs connected with the outlet of described steam treatment groove desalted water entrance, described steam treatment groove desalted water, described plate type heat exchanger and described inConnecting pipe between the outlet of steam treatment groove desalted water is provided with desalted water circulating pump, described temperature controller and described adjustingValve group connects.
In the above-mentioned purging system of preparing polyacrylonitrile fibril dry-jet wet-spinning spinneret, pre-soaking device is used for needSpinneret to be processed carries out pre-soaking, and spinneret is placed on the dividing plate of spinneret presoaking tank in the time soaking, this spinneretDesalted water entrance, DMSO entrance, compressed air inlet that one side of presoaking tank sets gradually are from high to low respectively used to thisIn spinneret presoaking tank, input desalted water, DMSO solvent, compressed air, the nozzle of spinneret presoaking tank inside is used for spurtingCompressed air.
According to specific embodiment of the invention scheme, preferably, the steam that is internally connected with of described spinneret presoaking tank addsHot equipment, heats for the DMSO solvent to spinneret presoaking tank; This steam-heating apparatus is a steam-heating pipeLine, this Steam Heating pipeline is provided with steam inlet, control valve group, drain valve group, steam (vapor) outlet and temperature controller, this steamA part for heating pipeline is positioned at the inside (for DMSO solvent is heated) of described spinneret presoaking tank, described adjustingIn described steam inlet and between the pipeline of described spinneret presoaking tank inside, (control valve group is used for controlling steaming to valve groupThe flow of vapour), described drain valve group is at described steam (vapor) outlet and between the pipeline of described spinneret presoaking tank inside(drain valve group is for exhaust steam condensed water), described temperature controller (for controlling temperature) is connected with described control valve group.
In the above-mentioned purging system of preparing polyacrylonitrile fibril dry-jet wet-spinning spinneret, circulation cleaning device is for rightSpinneret through pre-soaking carries out wash cycles, and wherein, DMSO solvent circulating slot is used for storing DMSO solvent, and one side is provided withDMSO entrance and desalted water entrance be respectively used to input DMSO solvent and desalted water, the DMSO that opposite side is provided with exports for defeatedGo out DMSO solvent, liquid level gauge is used for the liquid level of the DMSO solvent that measures DMSO flux bath; Spinneret fixing seal chamber is usedNeed spinneret to be processed in placing; DMSO circulating pump is used to the DMSO solvent in pipeline that power is provided, and can circulateFlow; Filter is for filtering the DMSO solvent of pipeline; DMSO solvent self loop head is used for to DMSO solventIn groove, input DMSO solvent; Wash cycles pipeline DMSO outlet is for leaving the DMSO solvent row in spinneret fixing seal chamberEnter in DMSO flux bath; Wash cycles pipeline drain is for entering the DMSO solvent that does not enter spinneret fixing seal chamberIn DMSO flux bath; DMSO solvent circulating slot, DMSO outlet, DMSO circulating pump, filter, DMSO solvent self loop head,The compositions that link together such as spinneret fixing seal chamber, wash cycles pipeline DMSO outlet, wash cycles pipeline drainThe circulation of DMSO solvent.
According to specific embodiment of the invention scheme, preferably, described circulation cleaning device be internally connected with Steam HeatingEquipment (heating for the DMSO solvent to DMSO flux bath), this steam-heating apparatus is a Steam Heating pipeline, itsBe provided with steam inlet, control valve group, drain valve group, steam (vapor) outlet and temperature controller, a part for this Steam Heating pipelineBe positioned at the inside of described DMSO solvent circulating slot, described control valve group (for controlling flowing of steam) is positioned at described steam inletAnd between " being positioned at the pipeline of described DMSO solvent circulating slot inside ", described drain valve group is positioned at described steam (vapor) outlet and " is positioned atThe pipeline of described DMSO solvent circulating slot inside " between, described temperature controller (for controlling temperature) and described control valve groupConnect.
In the above-mentioned purging system of preparing polyacrylonitrile fibril dry-jet wet-spinning spinneret, equipment for steam treatment is for rightSpinneret through solvent circular treatment carries out steam treatment. Wherein, the spinneret fixing seal chamber of spinneret steam treatment grooveBe used for placing need spinneret to be processed; The steam (vapor) outlet in this spinneret fixing seal chamber steams for input in sealing chamberVapour, the steam inlet arranging on steam input pipe line and compressed air inlet are respectively used to input steam and compressed air, cylinderValve is for controlling the switching of pipeline; Overfall, steam treatment groove desalted water outlet that one side in spinneret fixing seal chamber arranges,Desalted water water supplement port is respectively used to discharge the liquid, the discharge desalted water, supplementary that in spinneret fixing seal chamber, exceed certain liquid levelDesalted water; The steam treatment groove desalted water entrance that the bottom in spinneret fixing seal chamber arranges is used for inputting through changing heat treatedDesalted water; Desalted water recycle unit is for realizing the circulation of desalted water, and wherein, plate type heat exchanger is used for realizing desalted water and freezingThe heat exchange of water, to reduce the temperature of desalted water, temperature controller is for controlling the temperature of desalted water; Chilled water inlet place arrangesControl valve group is for controlling the flow of chilled water.
According to specific embodiment of the invention scheme, preferably, the height of the dividing plate in spinneret presoaking tank is between desalinationBetween water inlet and DMSO entrance.
The present invention also provides a kind of cleaning method of preparing polyacrylonitrile fibril dry-jet wet-spinning spinneret, and the method isAdopt the above-mentioned purging system of preparing polyacrylonitrile fibril dry-jet wet-spinning spinneret to carry out, it comprises the following steps:
(1) with the prerinse of DMSO solvent
To injecting the DMSO solvent that is enough to submergence spinneret in spinneret presoaking tank, and in spinneret presoaking tank with0.5-1.0m3The flow of/h passes into compressed air, makes in groove DMSO solvent in dynamically;
Spinneret is placed in spinneret presoaking tank, in the DMSO solvent of 60 DEG C, soaks 12 hours;
The DMSO solvent that spinneret presoaking tank is included to polymer put clean after, the DMSO solvent that reinjects new;
Spinneret is soaked 12 hours in the new DMSO of 60 DEG C again;
(2) rinse with desalted water
Spinneret is taken out in spinneret presoaking tank, rinse 5min with desalted water, make its cleaning;
(3) by DMSO solvent wash cycles
Spinneret is placed in the spinneret sealing lock chamber of spinneret circulation cleaning washing trough top;
The import, the outlet that spinneret are sealed to import, outlet and the DMSO solvent circulation of lock chamber connect;
In DMSO solvent circulating slot, inject the DMSO solvent that is enough to submergence spinneret, liquid level is controlled at the circulation of DMSO solventIn the 60-70% of groove volume;
The temperature of the DMSO solvent in DMSO solvent circulating slot is controlled to 60 ± 1 DEG C;
Start DMSO solvent circulating pump, make DMSO solvent circulating pump outlet pressure reach 0.3-0.4MPa;
Inlet valve and the outlet valve of opening spinneret sealing lock chamber, the DMSO solvent that passes into 60 DEG C follows spinneretRing cleans at least 10 hours;
Then, steam off control valve, cuts out DMSO solvent circulating pump, and spinneret is cooled to room temperature, and solid from sealingDetermine to take out in chamber;
(4) desalted water rinses
Spinneret after wash cycles is put into flushed channel, rinse 5min with desalted water, make its cleaning;
(5) use steam treatment
Spinneret is placed in the spinneret sealing lock chamber on spinneret equipment for steam treatment top, and good seal;
To deliver to through the steam filtering, pressure is 0.3MPa before the cylinder valve of spinneret sealing lock chamber entrance;
In vapor absorption circulating slot, inject desalted water to overfall place;
The temperature that starts the desalted water of circulating pump controlled circulation is 40 ± 1 DEG C;
Start the steam cylinder valve of spinneret sealing lock chamber entrance, steam enters spinneret sealing lock chamber to spinneretProcess 3 hours;
Close the cylinder valve of spinneret sealing lock chamber steam inlet, close circulating pump, spinneret is cooled to after room temperatureFrom spinneret sealing lock chamber, take out;
(6) use Ultrasonic Cleaning spinneret
Spinneret face after steam treatment is placed in ultrasonic cleaner upward;
The water that is enough to submergence spinneret is added in ultrasonic cleaner;
Open ultrasonic cleaner, clean 60min ± 2min;
Close ultrasonic cleaner, and the water in ultrasonic cleaner is put only;
The desalted water that is enough to submergence spinneret is added in ultrasonic cleaner;
Open ultrasonic cleaner, clean 60min ± 2min;
Close ultrasonic cleaner, and water is put only;
(7) spinneret of Ultrasonic Cleaning being crossed is kept in box after drying up with compressed air after filtering;
(8) detect: spinneret is placed on optical projector, according to the imaging of spinneret orifice, observe spinneret orifice diameter and inThe fineness in hole; For underproof spinneret, again process by above-mentioned steps (1)-(6), until qualified.
The polyacrylonitrile fibril of preparing provided by the present invention is for squirting purging system and the method and existing of spinning spinneretTechnology is compared has obvious good effect, and it is high for dry-jet wet-spinning spinning fluid viscosity and molecular weight, and filter effect is bad,The plug-hole that the factor such as the poor and spinneret of spinning solution homogeneity is thicker causes, not easy-clear of the polymer in spinneret orifice, in order to ensureSpinneret surface and spinneret orifice are indeformable, do not corrode, according to the similar principle mixing of chemical substance structure composition, with DMSO solventMake cleaning agent, cleaning in presoaking tank, circulation cleaning washing trough and being heated to 60 DEG C, complete spray silk through prerinse, wash cyclesThe preliminary cleaning of plate, then, through process and steps such as steam treatment, Ultrasonic Cleaning, compressed air dry up, finally completes sprayThe cleaning of filament plate. This cleaning method technological process is short, and use equipment is few, device structure simple, cleaning performance is very good, spinneretThe cleaning rate of attachment reaches 99.99%, can ensure that spinneret orifice is indeformable simultaneously, corrosion-free phenomenon, and spinneret any surface finish, is tenThe cleaning method that divides desirable preparation PAN precursor used for high-performance carbon fibre dry-jet wet-spinning spinneret, also can clean by the method attachedOther spinning parts of DMSO+PAN.
Brief description of the drawings
The structural representation of the spinneret pre-soaking device that Fig. 1 provides for embodiment 1;
The structural representation of the circulation cleaning device that Fig. 2 provides for embodiment 1;
The structural representation of the equipment for steam treatment that Fig. 3 provides for embodiment 1.
Main drawing reference numeral explanation:
Spinneret presoaking tank 1 nozzle 2 dividing plate 3 compressed air inlet 4DMSO entrance 5 desalted water entrances 6Steam inlet 7 steam (vapor) outlet 8 control valve group 9 drain valve group 10 temperature controller 11DMSO solvent circulating slots 12DMSO circulating pump 13 filter 14 spinneret fixing seal chamber 15 temperature controller 16 liquid level gauge 17 drain valve groups18 control valve group 19DMSO entrance 20 desalted water entrance 21 clean cycle pipeline drain 22 steam inlets 23Steam (vapor) outlet 24DMSO self loop head 25 wash cycles pipeline DMSO outlet 26 spinneret steam treatment grooves 27Spinneret fixing seal chamber 28 desalted water circulating pump 29 plate type heat exchanger 30 cylinder valve 31 control valve group 32 temperatureController 33 steam inlet 34 compressed air inlet 35 chilled water inlet 36 chilled water outlet 37 overfalls 38Steam treatment groove desalted water exports 39 steam treatment groove desalted water entrance 40 desalted water water supplement port 41 steam (vapor) outlets 42 and arrangesPut a mouthful 43DMSO and export 44 exhaust outlets 45
Detailed description of the invention
Understand for technical characterictic of the present invention, object and beneficial effect being had more clearly, existing to skill of the present inventionArt scheme is carried out following detailed description, but can not be interpreted as restriction that can practical range of the present invention.
Embodiment 1
The present embodiment provides a kind of purging system of preparing polyacrylonitrile fibril dry-jet wet-spinning spinneret, and it comprises in advanceInfuser device, circulation cleaning device, equipment for steam treatment, its structure respectively as shown in Figure 1, Figure 2, Figure 3 shows.
As shown in Figure 1, pre-soaking device comprises spinneret presoaking tank 1, a side of this spinneret presoaking tank 1 by height toLow desalted water entrance 6, DMSO entrance 5, the compressed air inlet 4 of being provided with successively, spinneret presoaking tank 1 inside be provided with level everyPlate 3, the height of dividing plate 3 between desalted water entrance 6 and DMSO entrance 5, compressed air inlet 4 be positioned at spinneret pre-soakingThe nozzle 2 of groove 1 inside connects, for input compressed-air;
Spinneret presoaking tank 1 be internally connected with steam-heating apparatus, this steam-heating apparatus is a steam-heating pipeLine, this Steam Heating pipeline is provided with steam inlet 7, control valve group 9, drain valve group 10, steam (vapor) outlet 8 and temperature controller11, a part for this Steam Heating pipeline is positioned at the inside of spinneret presoaking tank 1, and control valve group 9 is positioned at steam inlet 7 and positionBetween the pipeline of spinneret presoaking tank 1 inside, (be provided with the bypass of control valve group 9 in a side of control valve group 9, at control valveWhile organizing 9 self-regulateds inefficacy, can open this bypass), drain valve group 10 is positioned at steam (vapor) outlet 8 and is positioned at spinneret presoaking tank 1Between the pipeline of portion, (be provided with the bypass of drain valve group 10 in a side of drain valve group 10, in the time that drain valve group 10 lost efficacy, can beatOpen this bypass to unnecessary condensed water is discharged), temperature controller 11 is connected with control valve group 9, and it is fixed to by flangeOn the sidewall of spinneret presoaking tank 1, for measuring the temperature of the liquid in spinneret presoaking tank 1; Spinneret pre-soakingThe top of groove 1 is provided with exhaust outlet, and bottom is provided with the drain of cell body;
As shown in Figure 2, circulation cleaning device comprises DMSO solvent circulating slot 12, and a side of this DMSO solvent circulating slot 12 is establishedHave DMSO entrance 20 and desalted water entrance 21, opposite side is provided with DMSO outlet 44 and is connected with a liquid level gauge 17, this DMSO solventThe top of circulating slot 12 is provided with multiple spinneret fixing seals chamber 15; DMSO outlet 44 connects by pipeline and DMSO circulating pump 13Connect, DMSO circulating pump 13 is connected with spinneret fixing seal chamber 15 by filter 14 and its connecting pipe is provided with circulation cleaningWash pipeline drain 22; DMSO circulating pump 13 is also connected to by pipeline the DMSO self that is positioned at DMSO solvent circulating slot 12 insideLoop head 25; Spinneret fixing seal chamber 17 respectively with the wash cycles pipeline DMSO that is positioned at DMSO solvent circulating slot 12 insideOutlet 26 connects; The horizontal pipeline that the outlet in spinneret fixing seal chamber 15 connects (is positioned at the transverse pipe at top in Fig. 2Road) two ends seal;
Circulation cleaning device be internally connected with steam-heating apparatus, this steam-heating apparatus is a Steam Heating pipeline,It is provided with steam inlet 23, control valve group 19, drain valve group 18, steam (vapor) outlet 24 and temperature controller 16, this Steam HeatingA part for pipeline is positioned at the inside of DMSO solvent circulating slot 12, and control valve group 19 is positioned at steam inlet 23 and is positioned at DMSO solventBetween the pipeline of circulating slot 12 inside, (be provided with the bypass of control valve group 19 in a side of control valve group 19, in control valve group 19 certainlyAdjust while inefficacy, can open this bypass), drain valve group 18 is positioned at steam (vapor) outlet 24 and is positioned at DMSO solvent circulating slot 12 insideBetween pipeline, (be provided with the bypass of drain valve group 18 in a side of drain valve group 18, in the time that drain valve group 18 lost efficacy, can open thisBypass is to discharge unnecessary condensed water), temperature controller (ITC) 16 is connected with control valve group 19, and it is fixed by flangeOn the cell body of DMSO solvent circulating slot 12, for measuring the temperature of liquid in cell body; DMSO solvent circulating slot 12 bottoms are provided withThermometer, to detect the temperature of the DMSO solvent in DMSO solvent circulating slot 12; DMSO solvent circulating slot 12 is provided with an exhaust outlet45；
As shown in Figure 3, equipment for steam treatment comprises spinneret steam treatment groove 27 and desalted water recycle unit, this spinneretThe top of steam treatment groove 27 is provided with a spinneret fixing seal chamber 28, and this spinneret fixing seal chamber 28 is provided with steam (vapor) outlet42, and this spinneret fixing seal chamber 28 is connected with steam input pipe line, and this steam input pipe line is provided with steam inlet 34With compressed air inlet 35, steam inlet 34 and compressed air inlet 35 connect by cylinder valve 31 and spinneret fixing seal chamber 28Connect; One side of spinneret steam treatment groove 27 is provided with overfall 38, steam treatment groove desalted water outlet 39, de-from high to low successivelySalt solution water supplement port 41; The bottom of spinneret steam treatment groove 27 is provided with steam treatment groove desalted water entrance 40; Spinneret steam placeThe bottom of reason groove 27 can also arrange a liquid outlet (clean for putting of liquid in spinneret steam treatment groove 27 cell bodies), and it canTo be connected to a common floss hole 43 with overfall 38;
Desalted water recycle unit comprises plate type heat exchanger 30 and temperature controller 33, and wherein, plate type heat exchanger 30 is provided with coldFreeze water inlet 36 and chilled water outlet 37, and chilled water inlet place is provided with control valve group 32, plate type heat exchanger 30 also respectively withSteam treatment groove desalted water entrance 40, steam treatment groove desalted water outlet 39 connect, and plate type heat exchanger 30 is de-with steam treatment grooveConnecting pipe between brine outlet 39 is provided with desalted water circulating pump 29, and temperature controller 33 is connected with control valve group 32, itsBe fixed to by flange on the pipeline on temperature controller 33 right sides, pass through steam treatment for measuring 29 outlets of desalted water circulating pumpGroove desalted water entrance 40 is got back to the temperature of the desalted water in spinneret steam treatment groove 27.
Embodiment 2
The present embodiment provides a kind of cleaning method of preparing polyacrylonitrile fibril dry-jet wet-spinning spinneret, and it is to adoptThe purging system that embodiment 1 provides cleans spinneret according to following steps:
(1) with the prerinse of DMSO solvent
A, be enough to the DMSO solvent of submergence spinneret to the interior injection of spinneret presoaking tank 1 by DMSO entrance 5, make in grooveThe liquid level that keeps 60-70% passes into compressed air by compressed air inlet 4 simultaneously, and is sprayed by nozzle 2, to protect in grooveCard cleaning fluid floods spinneret, and in flow regime;
B, spinneret is placed on the dividing plate 3 in spinneret presoaking tank 1, steam enters spray silk by steam inlet 7DMSO solvent in plate presoaking tank 1 heats, by regulating control valve group 9 and temperature controller 11 to make the temperature control of DMSO solventBuilt in 60 ± 1 DEG C, and make to soak 12 hours in the DMSO solvent of spinneret in 60 ± 1 DEG C;
C, by clear spinneret presoaking tank 1 containing the DMSO of polymer put clean after, inject fresh DMSO solvent;
D, spinneret is soaked 12 hours in the fresh DMSO solvent of 60 DEG C again;
(2) rinse with desalted water
Spinneret, from the interior taking-up of spinneret presoaking tank 1, is put into flushed channel, rinse 5min with desalted water, make it cleanOnly;
(3) by DMSO solvent wash cycles
A, spinneret is placed in the spinneret sealing lock chamber 15 of DMSO solvent circulating slot 12 tops;
B. spinneret is sealed to the import and export of lock chamber 15 and the import and export of DMSO solvent circulation connect, spinneretThe import of sealing lock chamber 15 be connected from the pipeline of filter 24, spinneret seals the outlet of lock chamber 15 and is connected to circulationClean pipeline DMSO outlet 26;
C, be enough to the DMSO solvent of submergence spinneret to the 12 interior injections of DMSO solvent circulating slot by DMSO entrance 20, pass throughLiquid level gauge 17 is controlled at liquid level the 60-70% of DMSO solvent circulating slot volume;
D, steam input by steam inlet 23 that DMSO solvent circulating slot 12 is interior to be heated solvent, by control valve group19 control temperature with temperature controller 16, make the DMSO solvent temperature in DMSO solvent circulating slot 12 be controlled at 60 ± 1 DEG C;
E, startup DMSO solvent circulating pump 13, make DMSO solvent circulating pump 13 outlet pressures reach 0.3-0.4MPa;
F, open the terminal valve of spinneret sealing lock chamber 15;
G, pass into the DMSO solvent wash cycles at least 10 hours of 60 DEG C;
H, steam off control valve 19;
I, close DMSO solvent circulating pump 13;
J, spinneret is cooled to room temperature, and takes out from spinneret sealing lock chamber 15;
(4) desalted water rinses
Spinneret after wash cycles is put into flushed channel, rinse 5min with desalted water, make its cleaning;
(5) use steam treatment
A, spinneret is placed in the spinneret sealing lock chamber 28 on spinneret steam treatment groove 27 tops, and good seal;
The steam that b, the pressure that process is filtered are 0.3MPa is sent into spinneret sealing lock chamber 28 by steam inlet 34Before the cylinder valve 31 of entrance;
C, by desalted water water supplement port 41 to the interior injection desalted water of spinneret steam treatment groove 27 to overfall 38 places;
D, open the inlet valve of desalted water circulating pump 29, start desalted water circulating pump 29;
E, progressively open the outlet valve of desalted water circulating pump 29, make pump discharge pressure reach 0.2MPa, and open plate simultaneouslyDesalted water inlet valve and the outlet valve of formula heat exchanger 30;
F, chilled water enter plate type heat exchanger 30 by chilled water inlet 36, by control valve group 32 and temperature controller 33Control temperature, the desalted water temperature of circulation is controlled to 40 ± 1 DEG C;
The steam cylinder valve 31 of g, startup spinneret sealing lock chamber 28 entrances, steam enters spray silk by steam inlet 34Plate sealing lock chamber 28 is processed spinneret, and the steam of discharge enters spinneret steam treatment groove 27 by steam (vapor) outlet 42Inside be desalted water and absorb, the processing time is 3 hours;
H, the cylinder valve 31 of closing spinneret sealing lock chamber 28 steam inlets;
I, close desalted water circulating pump 29;
J, spinneret is cooled to after room temperature and is taken out from spinneret sealing lock chamber 28;
(6) use Ultrasonic Cleaning spinneret
A, the spinneret face after steam treatment is placed in ultrasonic cleaner upward;
B, the Living Water that is enough to submergence spinneret is added in ultrasonic cleaner;
C, unlatching ultrasonic cleaner, clean 60min ± 2min;
D, close ultrasonic wave, and the water in ultrasonic cleaner is put only;
E, the desalted water that is enough to submergence spinneret is added in ultrasonic cleaner;
F, unlatching ultrasonic cleaner, clean 60min ± 2min;
G, close ultrasonic cleaner, and water is put only;
(7) spinning head of Ultrasonic Cleaning being crossed is kept in box after drying up with compressed air after filtering;
(8) detect
Spinneret is placed on optical projector, according to the imaging of spinneret orifice, observes the bright and clean of spinneret orifice diameter and endoporusDegree; For underproof spinneret, again process by above-mentioned steps (1)-(6), until qualified.
The optical projection detector special by spinneret detects by hole, by the preparation that adopts the present embodiment to provideAfter polyacrylonitrile fibril is processed with the cleaning method of dry-jet wet-spinning spinneret, the percentage of plugged hole of spinneret is less than ten thousand/.
Claims (5)
1. a purging system of preparing polyacrylonitrile fibril dry-jet wet-spinning spinneret, is characterized in that: described purging systemComprise pre-soaking device, circulation cleaning device, equipment for steam treatment, wherein:
Described pre-soaking device comprises spinneret presoaking tank, and a side of this spinneret presoaking tank is provided with de-from high to low successivelySalt water inlet, DMSO entrance, compressed air inlet, this spinneret presoaking tank inside is provided with the dividing plate of level, and, described pressureContracting air intake is connected with the nozzle that is positioned at described spinneret presoaking tank inside;
Described circulation cleaning device comprises DMSO solvent circulating slot, and a side of this DMSO solvent circulating slot is provided with DMSO entrance and de-Salt water inlet, opposite side is provided with DMSO and exports and be connected with a liquid level gauge, and the top of this DMSO solvent circulating slot is provided with multiple spraysFilament plate fixing seal chamber; Described DMSO outlet is connected with DMSO circulating pump by pipeline, and described DMSO circulating pump passes through filterBe connected with described spinneret fixing seal chamber and its connecting pipe is provided with wash cycles pipeline drain; Described DMSO circulationPump is also connected to by pipeline DMSO self loop head that is positioned at described DMSO solvent circulating slot inside; Described spinneret is fixedAnnular seal space is connected with the wash cycles pipeline DMSO outlet that is positioned at described DMSO solvent circulating slot inside respectively;
Described equipment for steam treatment comprises spinneret steam treatment groove and desalted water recycle unit, this spinneret steam treatment grooveTop is provided with a spinneret fixing seal chamber, and this spinneret fixing seal chamber is provided with steam (vapor) outlet, and this spinneret is fixing closeEnvelope chamber is connected with steam input pipe line, and this steam input pipe line is provided with steam inlet and compressed air inlet, and described steam entersMouth is connected with described spinneret fixing seal chamber by cylinder valve with compressed air inlet; One of described spinneret steam treatment grooveSide is provided with overfall, the outlet of steam treatment groove desalted water, desalted water water supplement port from high to low successively; Described spinneret steam treatmentThe bottom of groove is provided with steam treatment groove desalted water entrance;
Described desalted water recycle unit comprises plate type heat exchanger and temperature controller, and wherein, described plate type heat exchanger is provided with freezingWater inlet and chilled water outlet, and described chilled water inlet place is provided with control valve group, described plate type heat exchanger also respectively with instituteState steam treatment groove desalted water entrance, described steam treatment groove desalted water outlet connection, described plate type heat exchanger and described steamConnecting pipe between the outlet for the treatment of trough desalted water is provided with desalted water circulating pump, described temperature controller and described control valve groupConnect.
2. the purging system of preparing polyacrylonitrile fibril dry-jet wet-spinning spinneret according to claim 1, wherein, described inSpinneret presoaking tank be internally connected with steam-heating apparatus, this steam-heating apparatus is a Steam Heating pipeline, this steamHeating pipeline is provided with steam inlet, control valve group, drain valve group, steam (vapor) outlet and temperature controller, this Steam Heating pipelineA part be positioned at the inside of described spinneret presoaking tank, described control valve group is positioned at described steam inlet and is positioned at described sprayBetween the pipeline of filament plate presoaking tank inside, described drain valve group is positioned at described steam (vapor) outlet and is positioned at described spinneret pre-soakingBetween the pipeline of groove inside, described temperature controller is connected with described control valve group.
3. the purging system of preparing polyacrylonitrile fibril dry-jet wet-spinning spinneret according to claim 1, wherein, described inCirculation cleaning device be internally connected with steam-heating apparatus, this steam-heating apparatus is a Steam Heating pipeline, it is provided with steamingVapour entrance, control valve group, drain valve group, steam (vapor) outlet and temperature controller, a part for this Steam Heating pipeline is positioned at instituteState the inside of DMSO solvent circulating slot, described control valve group is positioned at described steam inlet and is positioned at described DMSO solvent circulating slotBetween the pipeline of portion, described drain valve group be positioned at described steam (vapor) outlet be positioned at described DMSO solvent circulating slot inside pipeline itBetween, described temperature controller is connected with described control valve group.
4. the purging system of preparing polyacrylonitrile fibril dry-jet wet-spinning spinneret according to claim 1, wherein, described inThe height of dividing plate is between described desalted water entrance and described DMSO entrance.
5. prepare a cleaning method for polyacrylonitrile fibril dry-jet wet-spinning spinneret, the method is to adopt claim 1-4The cleaning device of preparing polyacrylonitrile fibril dry-jet wet-spinning spinneret described in any one carries out, and it comprises the following steps:
(1) with the prerinse of DMSO solvent
To injecting the DMSO solvent that is enough to submergence spinneret in spinneret presoaking tank, and in spinneret presoaking tank with 0.5-1.0m3The flow of/h passes into compressed air, makes in groove DMSO solvent in dynamically;
Spinneret is placed in spinneret presoaking tank, in the DMSO solvent of 60 DEG C, soaks 12 hours;
The DMSO solvent that spinneret presoaking tank is included to polymer put clean after, the DMSO solvent that reinjects new;
Spinneret is soaked 12 hours in the new DMSO of 60 DEG C again;
(2) rinse with desalted water
Spinneret is taken out in spinneret presoaking tank, rinse 5min with desalted water, make its cleaning;
(3) by DMSO solvent wash cycles
Spinneret is placed in the spinneret sealing lock chamber of spinneret circulation cleaning washing trough top;
The import, the outlet that spinneret are sealed to import, outlet and the DMSO solvent circulation of lock chamber connect;
In DMSO solvent circulating slot, inject the DMSO solvent that is enough to submergence spinneret, liquid level is controlled at DMSO solvent circulating slot and holdsLong-pending 60-70%;
The temperature of the DMSO solvent in DMSO solvent circulating slot is controlled to 60 ± 1 DEG C;
Start DMSO solvent circulating pump, make DMSO solvent circulating pump outlet pressure reach 0.3-0.4MPa;
Inlet valve and the outlet valve of opening spinneret sealing lock chamber, the DMSO solvent that passes into 60 DEG C carries out circulation cleaning to spinneretBe washed till few 10 hours;
Then, steam off control valve, cuts out DMSO solvent circulating pump, and spinneret is cooled to room temperature, and from sealing lock chamberMiddle taking-up;
(4) desalted water rinses
Spinneret after wash cycles is put into flushed channel, rinse 5min with desalted water, make its cleaning;
(5) use steam treatment
Spinneret is placed in the spinneret sealing lock chamber on spinneret equipment for steam treatment top, and good seal;
To deliver to through the steam filtering, pressure is 0.3MPa before the cylinder valve of spinneret sealing lock chamber entrance;
In vapor absorption circulating slot, inject desalted water to overfall place;
The temperature that starts the desalted water of circulating pump controlled circulation is 40 ± 1 DEG C;
Start the steam cylinder valve of spinneret sealing lock chamber entrance, steam enters spinneret sealing lock chamber to spinneret processing3 hours;
Close the cylinder valve of spinneret sealing lock chamber steam inlet, close circulating pump, spinneret is cooled to after room temperature from sprayIn filament plate sealing lock chamber, take out;
(6) use Ultrasonic Cleaning spinneret
Spinneret face after steam treatment is placed in ultrasonic cleaner upward;
The water that is enough to submergence spinneret is added in ultrasonic cleaner;
Open ultrasonic cleaner, clean 60min ± 2min;
Close ultrasonic cleaner, and the water in ultrasonic cleaner is put only;
The desalted water that is enough to submergence spinneret is added in ultrasonic cleaner;
Open ultrasonic cleaner, clean 60min ± 2min;
Close ultrasonic cleaner, and water is put only;
(7) spinneret of Ultrasonic Cleaning being crossed is kept in box after drying up with compressed air after filtering;
(8) detect: spinneret is placed on optical projector, according to the imaging of spinneret orifice, observation spinneret orifice diameter and endoporusFineness; For underproof spinneret, again process by above-mentioned steps (1)-(6), until qualified.
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| CN104775167A (en) * | 2015-03-23 | 2015-07-15 | 中复神鹰碳纤维有限责任公司 | Cleaning method and equipment of spinneret plate for polyacrylonitrile fiber |
| CN105483840B (en) * | 2015-11-24 | 2018-06-26 | 宜宾丝丽雅股份有限公司 | A kind of novel spinning head washing process |
| WO2018234009A1 (en) * | 2017-06-23 | 2018-12-27 | Oerlikon Textile Gmbh & Co. Kg | Method and device for melt-spinning synthetic threads |
| CN111321473A (en) * | 2018-12-13 | 2020-06-23 | 中国石油化工股份有限公司 | Cleaning method of spinneret plate for polyacrylonitrile precursor |
| CN110026141B (en) * | 2019-05-07 | 2020-11-20 | 上海友尹化工装备有限公司 | Chemical reaction temperature control system of alcohol-water system |
| CN110820054B (en) * | 2019-11-22 | 2021-04-27 | 蓝星（成都）新材料有限公司 | Cleaning method for aramid fiber 1414 spinneret plate |
| CN111636152B (en) * | 2020-06-24 | 2021-02-19 | 天津市楚留香新材料有限公司 | Melt and spout melting device of non-woven equipment |
| CN112323149A (en) * | 2020-09-24 | 2021-02-05 | 烟台泰和新材料股份有限公司 | Spinneret plate cleaning process |
| CN112877799B (en) * | 2020-12-31 | 2022-03-11 | 荣成碳纤维科技有限公司 | Method and system for producing carbon fiber dry-jet wet-spun precursor |
| CN114054423B (en) * | 2021-09-08 | 2023-04-28 | 中复神鹰碳纤维股份有限公司 | Automatic cleaning method and device for spinneret plate |
| CN114293271B (en) * | 2021-12-30 | 2023-02-10 | 常州优创机械科技有限公司 | Airflow drafting device for spun-bonded equipment |
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| JPS5721507A (en) * | 1980-07-14 | 1982-02-04 | Nippon Ester Co Ltd | Cleaning method of spinneret apparatus |
| JPS62243697A (en) * | 1986-04-16 | 1987-10-24 | 旭化成株式会社 | Method for washing spinner |
| PL161698B1 (en) * | 1989-12-08 | 1993-07-30 | Zaklady Przemyslu Ponczosznicz | Device for nozzle cleaning in yarn texturing process |
| JPH04185705A (en) * | 1990-11-16 | 1992-07-02 | Mitsui Petrochem Ind Ltd | Method for cleaning nozzle |
| JP2004176194A (en) * | 2002-11-25 | 2004-06-24 | Mitsubishi Rayon Co Ltd | Spinneret cleaning method |
| DE50310828D1 (en) * | 2003-03-14 | 2009-01-08 | Reifenhaeuser Masch | Process for cleaning spinning devices |
| CN101805930B (en) * | 2010-04-28 | 2011-05-11 | 太原理工大学 | Method for cleaning polyphenylene sulfide melt spinning spinneret |
| CN202643935U (en) * | 2012-05-08 | 2013-01-02 | 长乐恒申合纤科技有限公司 | Cleaning system for spinning equipment |
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