CN217869236U - Horizontal multistage water washing device for preparing polyacrylonitrile-based carbon fiber precursor - Google Patents
Horizontal multistage water washing device for preparing polyacrylonitrile-based carbon fiber precursor Download PDFInfo
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- CN217869236U CN217869236U CN202222120786.3U CN202222120786U CN217869236U CN 217869236 U CN217869236 U CN 217869236U CN 202222120786 U CN202222120786 U CN 202222120786U CN 217869236 U CN217869236 U CN 217869236U
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Abstract
The utility model discloses a horizontal multistage washing device for preparing polyacrylonitrile base carbon fiber precursor, the structure is: the hot rolling device comprises a box body, and a primary stretching module, a secondary stretching module and a tertiary stretching module which are sequentially arranged in parallel in the box body, wherein hot rollers which are arranged in parallel are arranged in each stage of stretching module; a movably detachable baffle plate is arranged between the stretching modules, and a wire feeding through hole is arranged on the baffle plate; each stage of stretching module is provided with a solidification liquid circulating box, a solidification liquid inlet and a solidification liquid outlet are arranged on two opposite side walls, and a concentration detection device is arranged in the solidification liquid circulating box. The utility model discloses horizontal multistage washing device is in the same place three solitary drawing module group, compares with the precursor production line that has a plurality of coagulation baths to establish ties, can obviously reduce the silk way auxiliary assembly between the coagulation bath, reduces the cost and drops into, shortens the distance of walking simultaneously, has avoided the unnecessary wearing and tearing of fibre.
Description
Technical Field
The utility model relates to a preparation of polyacrylonitrile base carbon fiber precursor especially relates to a horizontal multistage washing device for preparing polyacrylonitrile base carbon fiber precursor.
Background
Carbon Fiber (CF) is a high-strength, high-modulus fiber material containing over 95% of carbon, and has wide application in national defense, military industry and civil use. It not only has the intrinsic characteristics of carbon material, but also has the soft workability of textile fibre. According to the source of the raw material of the carbon fiber, the carbon fiber can be subdivided into polyacrylonitrile-based carbon fiber, viscose-based carbon fiber and pitch-based carbon fiber, wherein the comprehensive performance of the viscose-based carbon fiber and the pitch-based carbon fiber is lower than that of the polyacrylonitrile-based carbon fiber, and most of the high-performance carbon fiber is prepared from polyacrylonitrile.
The preparation of carbon fiber has extremely strict requirements on various links, and the requirements on carbon fiber precursors are the same. The low-quality polyacrylonitrile protofilament has serious defects and can be broken in the process of preoxidation or carbonization, so that the preoxidized fiber or the carbon fiber with stable performance can not be prepared. The carbon fiber precursor prepared from the polyacrylonitrile nascent fiber is subjected to washing and drafting for many times, and is stretched for many times in coagulating baths with different concentrations and components, a solvent in the fiber is gradually diffused into a coagulating liquid from the fiber, the fiber is gradually solidified, and the carbon fiber precursor with excellent performance is obtained through treatment such as washing, oiling, densification and the like.
The multistage coagulation baths not only can use a large amount of solvents, but also can increase the running distance of fibers due to excessively complicated equipment layout, and each stage of coagulation baths can be used for debugging the process in a targeted manner, so that the failure rate can be increased, and the preparation of high-performance carbon fiber precursors is not facilitated.
Disclosure of Invention
To the too complicated problem of preparation carbon fiber precursor equipment overall arrangement and process control, the utility model provides a horizontal multistage washing device, the device's structure is: the horizontal multistage water washing device comprises a box body, and a primary stretching module, a secondary stretching module and a tertiary stretching module which are arranged in the box body, wherein the primary stretching module, the secondary stretching module and the tertiary stretching module are sequentially arranged in parallel, and hot rollers which are arranged in parallel are arranged in each stage of stretching module; movably detachable baffles are arranged between the primary stretching module and the secondary stretching module and between the secondary stretching module and the tertiary stretching module, and wire feeding through holes are formed in the baffles; each stage of stretching module is provided with a solidification liquid circulating box, a solidification liquid inlet and a solidification liquid outlet are arranged on two opposite side walls, and a concentration detection device is arranged in the solidification liquid circulating box.
The utility model discloses horizontal multistage washing device is in the same place three solitary drawing module group, compares with the precursor production line that has a plurality of coagulation baths to establish ties, can obviously reduce the silk way auxiliary assembly between the coagulation bath, reduces the cost and drops into, shortens the distance of walking simultaneously, has avoided the unnecessary wearing and tearing of fibre.
The utility model discloses horizontal multistage washing device adopts the tensile principle of multistage hot-rolling heating and differential, according to the temperature of solidification liquid and the requirement of predetermineeing the draft rate, sets up 2 ~ 4 hot-rollers in every level of tensile module, is equipped with a temperature sensor between per two hot-rollers to the accurate control temperature avoids self circulation solidification liquid and adjacent tensile module difference in temperature to the disturbance of solidification liquid temperature. In addition, the baffle can be made of heat insulating materials and has enough thickness, and the contact surface of the movable connection is sealed, so that the exchange of solidification liquid at the two sides of the baffle is reduced as much as possible.
Furthermore, a valve is arranged at the inlet of the solidification liquid of each stage of the stretching module, a concentration sensor is arranged at the outlet of the solidification liquid, a circulating pump and a heating coil are arranged in the solidification liquid circulating box of each stage of the stretching module, and the solidification liquid supplementing tank is connected with the concentration sensor. Because there is certain difference in concentration and the temperature of the liquid that congeals among the adjacent tensile module, although the baffle can block the liquid that congeals mixed flow to a certain extent, nevertheless along with the long-time operation of equipment, will inevitably receive the influence of the liquid that congeals among the adjacent tensile module always, therefore tensile module of every grade sets up the liquid circulation case that congeals alone, and the concentration of the liquid that congeals can in time be adjusted when concentration sensor detects unusually.
Furthermore, the solidification liquid circulation box of each stage of stretching module is arranged below the corresponding stretching module, so that the equipment is simpler.
The design of silk road should adapt to specific technology, generally at the 3-5 circles of wire winding of every hot-rolling, goes into the roller position and has direct influence to going out the silk position, and the silk is followed as the principle with reducing the silk road as far as possible to present, therefore need not to consider the influence between different coagulation baths, but in the utility model discloses in, what should avoid most is the mixed flow of adjacent drawing module coagulation liquid, therefore walk the silk through-hole and should set up the upper portion at the baffle. On the premise of reducing silk paths when the silk paths are arranged, the last hot roller of each stage of stretching module winds the silk clockwise, and the fact that fibers leave the rollers along the tangent line of the top of the hot roller and enter the silk running through holes is guaranteed.
Adopt the utility model discloses horizontal multistage washing unit can carry out desolventizing and draft with polyacrylonitrile nascent fibre for preparation polyacrylonitrile base carbon fiber precursor, whole operating procedure as follows:
1) Closing the valve, filling the prepared solidification liquid into a corresponding solidification liquid circulating box, starting the heating plate to heat the solidification liquid to the required temperature, and preserving heat;
2) Starting the hot rollers, keeping the rotating speed and the rotating direction of all the hot rollers consistent, installing a baffle plate, guiding the polyacrylonitrile nascent fiber into a horizontal multistage water washing device through a yarn guide, sequentially running the polyacrylonitrile nascent fiber on the hot rollers according to a preset yarn path, and temporarily collecting the polyacrylonitrile nascent fiber by using a yarn collector after the polyacrylonitrile nascent fiber is discharged from the horizontal multistage water washing device;
3) Opening a valve, simultaneously starting three circulating pumps to pump the solidification liquid into each stretching module, starting hot rollers to heat, heating the solidification liquid to a preset value, adjusting the rotating speed of each hot roller, and drafting the polyacrylonitrile nascent fiber;
4) Taking down the drafted polyacrylonitrile nascent fiber from the fiber collecting device in the step 2), introducing the drafted polyacrylonitrile nascent fiber into water washing equipment for water washing, performing heat setting, oiling and densification after water washing, and finally collecting the fiber to obtain the polyacrylonitrile-based carbon fiber precursor.
The process in the method is selected as follows:
1. the solidification liquid used by each stage of stretching module is an aqueous solution of the same organic solution, the organic solution is selected from one of DMSO, DMAc, DMF, propylene carbonate and N-methylpyrrolidone, the concentration of the solidification liquid in the first stage of stretching module is 25% -40%, the concentration of the solidification liquid in the second stage of stretching module is 15% -30%, and the concentration of the solidification liquid in the third stage of stretching module is 3% -10%;
2. the temperature of the solidification liquid of the primary stretching module is 10-30 ℃, the temperature of the secondary stretching module is 30-50 ℃, and the temperature of the tertiary stretching module is 40-60 ℃;
3. the extra draft multiple of the solidified liquid of the primary stretching module is 150-400%, the extra draft multiple of the secondary stretching module is 100-200%, and the extra draft multiple of the tertiary stretching module is 50-150%.
Drawings
FIG. 1 is a side view of the horizontal multi-stage water washing apparatus of the present invention;
FIG. 2 is a top view of the horizontal multi-stage water washing apparatus of the present invention;
wherein: 1. the device comprises a primary stretching module, a secondary stretching module, a 3 tertiary stretching module, a 4 hot roller, a 5 baffle, a 6 solidification liquid circulating box, a 7 temperature sensor, a 8 wire feeding through hole, a 9 solidification liquid inlet, a 10 solidification liquid outlet, a 11 valve, a 12 solidification liquid replenishing tank.
Detailed Description
The present invention is described below with reference to examples, which are only used to explain the present invention and are not used to limit the scope of the present invention.
As shown in fig. 1 and 2, a horizontal multistage water washing device comprises a box body, a primary stretching module 1, a secondary stretching module 2 and a tertiary stretching module 3 which are arranged in the box body, wherein the primary stretching module 1, the secondary stretching module 2 and the tertiary stretching module 3 are sequentially arranged in parallel, and hot rollers 4 which are arranged in parallel are arranged in each stage of stretching module; movably detachable baffles 5 are arranged between the primary stretching module 1 and the secondary stretching module 2 and between the secondary stretching module 2 and the tertiary stretching module 3, and wire feeding through holes 8 are formed in the baffles 5; each stage of stretching module is provided with a solidification liquid circulating box 6, a solidification liquid inlet 9 and a solidification liquid outlet 10 are arranged on two opposite side walls of the solidification liquid circulating box 6, and a concentration detection device is arranged in the solidification liquid circulating box 6.
The utility model discloses horizontal multistage washing device's one-level drawing module 1, the solidification liquid in second grade drawing module 2 and the tertiary drawing module 3 is the aqueous solution of the organic solvent that concentration reduces in proper order, according to the fibrous index of polyacrylonitrile primary, the preferred DMSO of organic solvent, DMAc, DMF, the concentration of solidification liquid and the rotational speed of temperature and hot-roll turn to in the drawing modules at different levels of control, solvent in the polyacrylonitrile primary is appeared, make polyacrylonitrile primary taper and solidification, carry out conventional washing after primary goes out multistage washing device, heat setting, oil, densifying, receive the silk and obtain polyacrylonitrile base carbon fiber precursor.
In order to facilitate the control of the parameters, the following preferred improvements can be selected on the basis of the device: 1. 2-4 hot rollers 4 in each stage of stretching module are arranged, and a temperature sensor 7 is arranged between every two hot rollers 4, so that the temperature of the hot rollers can be accurately mastered; 2. each solidification liquid inlet 9 is provided with a valve 11, each solidification liquid outlet 10 is provided with a concentration sensor, each solidification liquid circulation box 6 is arranged below the corresponding stretching module, a circulation pump and a heating coil are arranged in each solidification liquid circulation box, each solidification liquid circulation box 6 is provided with a solidification liquid supplement tank 12, and the solidification liquid supplement tank 12 is connected with the concentration sensor, so that the temperature and the concentration of the solidification liquid circulating in each stage of stretching module can be ensured; 3. the wire moving through hole 8 is arranged at the upper part of the baffle 5 and is higher than the liquid level of the solidification liquid, so that the condition that the solidification liquids in adjacent stretching modules are mixed with each other is avoided.
The method for preparing the polyacrylonitrile-based carbon fiber precursor by adopting the preferably configured horizontal multistage water washing device comprises the following steps: 1) Closing the valve 11, filling the prepared solidification liquid into a corresponding solidification liquid circulating box, starting the heating plate to heat the solidification liquid to the required temperature, and preserving heat; 2) Starting the hot rollers 4, keeping the rotating speed and the rotating direction of all the hot rollers 4 consistent, installing a baffle 5, guiding the polyacrylonitrile nascent fiber into a horizontal multistage water washing device through a yarn guide, sequentially running the yarn on the hot rollers 4 and the baffle 5 according to a preset yarn path, and temporarily collecting the yarn by a yarn collector after the polyacrylonitrile nascent fiber exits from the horizontal multistage water washing device; 3) Opening a valve 11, simultaneously starting three circulating pumps to pump the solidification liquid into each stretching module, starting heating of a hot roller 4, heating the solidification liquid to a preset value, adjusting the rotating speed of each hot roller 4, and stretching the polyacrylonitrile nascent fiber; 4) Taking down the drafted polyacrylonitrile nascent fiber from the fiber collecting device in the step 2), introducing the drafted polyacrylonitrile nascent fiber into water washing equipment for water washing, performing heat setting, oiling and densification after water washing, and finally collecting the fiber to obtain the polyacrylonitrile-based carbon fiber precursor.
In most cases, the heat roll 4 is completely immersed in the coagulation liquid, and may be partially immersed or not immersed in the coagulation liquid depending on the properties of the polyacrylonitrile-based fibers; step 2) when the filaments are loaded, the rotating speed and the rotating direction of the hot roller 4 are consistent, but the hot rollers can reversely rotate according to the filament paths during drafting, and in the step 3), the hot rollers need to be slowly decelerated and then reversely and slowly accelerated to a preset rotating speed; the center of the wire feeding through hole 8 is horizontal to the upper edge of the hot roller 4, so that the wire path can be ensured to be horizontal, and wire guides can be arranged on two sides of the baffle 5 to meet the requirement that the wire path is horizontal when the hot roller 4 is completely immersed in the solidification liquid; polyacrylonitrile nascent fibre is getting into the utility model discloses best carry out preliminary coagulation earlier before the horizontal multistage washing device, spinning dope is extruded the back from the spinneret and directly gets into the tensile module of one-level and can be because the coagulating liquid concentration is low excessively (25% ~ 40%), the temperature is low excessively (10 ~ 30 ℃) and the fracture, that is to say, the utility model discloses horizontal multistage washing device is applied to current precursor production facility best, as the replacement of multistage independent coagulation bath.
Taking a dry-jet wet spinning mode as an example, a polyacrylonitrile/DMSO spinning solution with the number average molecular weight of 10 ten thousand, the molecular weight distribution of 1.7 and the solid content of 18% is adopted, the number of spinning holes is 6000, a primary coagulation bath is pure DMSO at 10 ℃, a secondary coagulation bath is DMSO solution at 10 ℃ and the concentration of 60%, a third coagulation bath is DMSO solution at 30 ℃ and the concentration of 40%, a fourth coagulation bath is DMSO solution at 50 ℃ and the concentration of 20%, a fifth coagulation bath is DMSO solution at 60 ℃ and the concentration of 5%, the extra draft multiple of the second coagulation bath is 200%, the extra draft multiple of the third coagulation bath is 300%, the extra draft multiple of the fourth coagulation bath is 150%, and the extra draft multiple of the fifth coagulation bath is 120%. And (3) after the fiber is discharged from a five-stage coagulation bath, washing the fiber in a water bath of 80 ℃ deionized water, wherein the washing draft rate is 60%, after washing, carrying out heat setting for 15s at 120 ℃, feeding the fiber into a sizing tank for oiling, wherein the oiling agent is loose grease T600, the oiling rate is 1.2wt%, and finally, the fiber is subjected to steam drafting at 0.5MPa by 200% to prepare the polyacrylonitrile precursor for preparing the carbon fiber.
Will the utility model discloses horizontal multistage washing unit replacement tertiary, level four and five coagulation baths, nascent fibre get out the back from the second grade coagulation bath and get into the tensile module of one-level, go out the water bath behind the tensile module of tertiary, the solidification liquid concentration, the temperature of the tensile module of one-level and tertiary coagulation bath, the tensile module of second grade and level four coagulation bath, the tensile module of tertiary and five coagulation baths to and tensile multiple is all unanimous.
Compare the polyacrylonitrile precursor who prepares in above-mentioned multistage coagulating bath, adopt the utility model discloses the full volume percentage of polyacrylonitrile precursor that horizontal multistage water washing device prepared has promoted 7%, and precursor intensity has promoted 5.94cN/dtex by 5.67cN/dtex, and precursor elongation at break has reduced to 8.62% by 9.15%.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and any modifications, equivalent replacements, improvements, etc. made within the spirit and principle of the present invention should be included within the protection scope of the present invention.
Claims (5)
1. The utility model provides a horizontal multistage washing device for preparing polyacrylonitrile base carbon fiber precursor which characterized in that, its structure as follows: the horizontal multistage water washing device comprises a box body, and a primary stretching module, a secondary stretching module and a tertiary stretching module which are arranged in the box body, wherein the primary stretching module, the secondary stretching module and the tertiary stretching module are sequentially arranged in parallel, and hot rollers which are arranged in parallel are arranged in each stage of stretching module; movably detachable baffles are arranged between the primary stretching module and the secondary stretching module and between the secondary stretching module and the tertiary stretching module, and wire feeding through holes are formed in the baffles; each level of tensile module is furnished with the solidification liquid circulation case, and solidification liquid import and solidification liquid export set up on two relative lateral walls, are equipped with concentration detection device in the solidification liquid circulation case.
2. The horizontal multistage water washing device for preparing the polyacrylonitrile-based carbon fiber precursor as claimed in claim 1, wherein the number of hot rolls in each stage of the drawing module is 2-4, and a temperature sensor is arranged between every two hot rolls.
3. The horizontal multistage water washing device for preparing the polyacrylonitrile-based carbon fiber precursor as claimed in claim 1, wherein a valve is arranged at each coagulating liquid inlet, and a concentration sensor is arranged at each coagulating liquid outlet.
4. The horizontal multistage water washing device for preparing polyacrylonitrile-based carbon fiber precursors of claim 3, wherein each coagulation liquid circulation tank is arranged below the corresponding stretching module, a circulation pump and a heating coil are arranged in each coagulation liquid circulation tank, each coagulation liquid circulation tank is provided with a coagulation liquid supplement tank, and the coagulation liquid supplement tank is connected with the concentration sensor.
5. The horizontal multistage water washing device for preparing the polyacrylonitrile-based carbon fiber precursor as claimed in any one of claims 1 to 4, wherein the filament passing through holes are arranged at the upper part of the baffle.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202222120786.3U CN217869236U (en) | 2022-08-12 | 2022-08-12 | Horizontal multistage water washing device for preparing polyacrylonitrile-based carbon fiber precursor |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202222120786.3U CN217869236U (en) | 2022-08-12 | 2022-08-12 | Horizontal multistage water washing device for preparing polyacrylonitrile-based carbon fiber precursor |
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| CN202222120786.3U Active CN217869236U (en) | 2022-08-12 | 2022-08-12 | Horizontal multistage water washing device for preparing polyacrylonitrile-based carbon fiber precursor |
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