CN104178848A - Recovering device and method for waste spinning solution produced in carbon fiber precursor preparation processes - Google Patents
Recovering device and method for waste spinning solution produced in carbon fiber precursor preparation processes Download PDFInfo
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- CN104178848A CN104178848A CN201310194960.1A CN201310194960A CN104178848A CN 104178848 A CN104178848 A CN 104178848A CN 201310194960 A CN201310194960 A CN 201310194960A CN 104178848 A CN104178848 A CN 104178848A
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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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
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- Y02P70/62—Manufacturing or production processes characterised by the final manufactured product related technologies for production or treatment of textile or flexible materials or products thereof, including footwear
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Abstract
The invention provides a recovering device and a method for a waste spinning solution produced in carbon fiber precursor preparation processes. The device at least comprises a waste spinning solution collecting tank, a polymerization liquid defoaming kettle, a precision filter and a cyclic shearing pump. The waste spinning solution collecting tank comprises a tank body, a heat exchanger, a hot-water feeding pipe, a hot-water discharging pipe, a temperature controller, nozzles, a solvent feeding pipe, a nitrogen feeding pipe, a waste spinning solution inlet, a waste spinning solution outlet, a cyclic mixed solution inlet and a cyclic mixed solution outlet. The method includes: collecting the waste spinning solution into the waste spinning solution collecting tank, injecting a solvent into the waste spinning solution collecting tank through the nozzles, homogenizing through the cyclic shearing pump, feeding nitrogen for protection, filtering by the precision filter, and defoaming by the polymerization liquid defoaming kettle to obtain a spinning solution used for normal spinning. The recovering device and the method are advantaged by short technical processes, few used equipment, simple equipment structure, high recovering rate, and the like.
Description
Technical field
The retracting device and the method that the present invention relates to the useless spinning solution that produces in a kind of carbon fibre precursor preparation technology, belong to carbon fiber spinning solution technical field.
Background technology
In the process of carbon fibre precursor suitability for industrialized production, driving initial stage or while changing spinning machine filter, the useless spinning solution of impure, gel, bubble in a large number need to be drained.This is to should be evenly suitable spinning solution of free from foreign meter, gel, bubble and viscosity owing to preparing the spinning solution of high-performance carbon fibre precursor.And in useless spinning solution due to impure, microgel, bubble etc., when carrying out spinning, can cause that difficulty in spinning, fracture of wire are many, phenomenon that even cannot spinning, can not meet the requirement of normal suitability for industrialized production.
For the useless spinning solution of discharging, general processing method comprises the following steps: first with large water gaging, the spinning solution that gives up is solidified to processing, then to obtain solidify after waste material carry out landfill disposal.But so useless spinning solution processing mode has caused great waste.
Therefore, develop retracting device and the method for the useless spinning solution producing in a kind of carbon fibre precursor preparation technology, be still one of this area problem demanding prompt solution.
Summary of the invention
For solving the problems of the technologies described above, object of the present invention provides retracting device and the method for the useless spinning solution producing in a kind of carbon fibre precursor preparation technology.The retracting device of useless spinning solution of the present invention and method have that technological process is short, use equipment is few, device structure is simple, organic efficiency advantages of higher.
For reaching above-mentioned purpose, the invention provides the retracting device of the useless spinning solution producing in a kind of carbon fibre precursor preparation technology, it at least comprises:
Useless spinning solution feeder, polymer fluid deaeration still, accurate filter, circulation shear pump;
Described useless spinning solution feeder at least comprises: cell body, be positioned at the heat exchanger of described cell body bottom, be connected in hot water inflow pipe and the hot water effuser of described heat exchanger, be connected in the temperature controller of described cell body, be positioned at the nozzle at described cell body top, the solvent that is connected in described nozzle enters pipe, the nitrogen that is connected in described cell body enters pipe, and useless spinning solution entrance, useless spinning solution outlet, circulation entry to mixed solution and circulation mixture export;
Described useless spinning solution entrance is connected with the useless spinning solution outlet of spinning machine by pipeline;
Described circulation entry to mixed solution, circulation mixture export are connected with described circulation shear pump by pipeline respectively;
Described useless spinning solution outlet is connected in the charging aperture of described accurate filter by pipeline, the discharging opening of described accurate filter is connected in the charging aperture of described polymer fluid deaeration still by pipeline, the discharging opening of described polymer fluid deaeration still is connected in the charging aperture of described spinning machine by pipeline.
According to the specific embodiment of the present invention, preferably, above-mentioned retracting device also comprises gear wheel metering pump, and described gear wheel metering pump is arranged at described useless spinning solution and exports on the pipeline being connected with the charging aperture of described accurate filter.The effect of this gear wheel metering pump is the useless spinning solution after homogeneous to send in accurate filter.
According to the specific embodiment of the present invention, preferably, above-mentioned retracting device also comprises feeding gear pump, and described feeding gear pump is arranged on the pipeline that the discharging opening of described polymer fluid deaeration still is connected with the charging aperture of described spinning machine.The effect of this feeding gear pump is spinning solution to send in spinning machine.
According to the specific embodiment of the present invention, above-mentioned retracting device also comprises valve, and those skilled in the art can select the position of valve according to actual conditions.Preferably, described valve is at least positioned on the pipeline that described useless spinning solution entrance is connected with the useless spinning solution outlet of described spinning machine, on the pipeline that described circulation entry to mixed solution is connected with described circulation shear pump, described nitrogen enters on pipe, on described hot water inflow pipe and described hot water effuser, described solvent enters on pipe.In addition, on the pipeline of the discharging opening of described accurate filter, and on the pipeline of the discharging opening of polymer fluid deaeration still, also valve can be set, in order to control the process of reaction and removal process.
According to the specific embodiment of the present invention, preferably, above-mentioned retracting device also comprises flowmeter and Pressure gauge.Described flowmeter is at least positioned at described solvent and enters on pipe.Described Pressure gauge can be positioned on the pipeline that the circulation entry to mixed solution of described useless spinning solution feeder is connected with described circulation shear pump, its role is to monitor the pressure of circulation homogenizing process.Pressure gauge can also be positioned on the pipeline that described gear wheel metering pump is connected with the charging aperture of described accurate filter, its role is to monitor the pressure that feed liquid enters accurate filter.Pressure gauge can also be positioned on the pipeline that the discharging opening of described accurate filter and the charging aperture of described polymer fluid deaeration still be connected, and its role is to monitor the pressure that feed liquid enters polymer fluid deaeration still.
In above-mentioned retracting device, preferably, being positioned at the valve that described solvent enters on pipe is control valve group, and it can enter the flowmeter coupling on pipe with being positioned at described solvent, and the flow of solvent is controlled.
According to the specific embodiment of the present invention, preferably, above-mentioned retracting device also comprises blow-down pipe, and it is connected in described cell body, and can on this blow-down pipe, valve be set.This blow-down pipe plays cell body internal pressure and the basically identical effect of external atmosphere pressure of making.
In above-mentioned retracting device, preferably, described nozzle is atomizer.
In above-mentioned retracting device, preferably, described accurate filter is that pore size filter is the accurate filter of 0.5-3 μ m.
The present invention also provides the recovery method of the useless spinning solution producing in a kind of carbon fibre precursor preparation technology, it is for adopting the give up method of spinning solution recovery of the retracting device of the useless spinning solution producing in above-mentioned carbon fibre precursor preparation technology, and this recovery method comprises the following steps:
(1) the useless spinning solution of spinning machine being discharged is collected in the cell body of useless spinning solution feeder, by hot water inflow pipe and hot water effuser, to the heat exchanger bottom cell body, continue to pass into hot water, and by temperature controller, the useless spinning solution in cell body is carried out to thermostatic control;
(2) the waste spinning silk liquid temp in cell body rises to when identical with the hot water temperature who passes into, start circulation shear pump, simultaneously by solvent enter pipe and nozzle to the useless spinning solution in cell body, spray into solvent, after the abundant homogeneous of mixed liquor of the useless spinning solution in cell body and solvent, stop circulation shear pump, by nitrogen, enter pipe simultaneously and pass into nitrogen protection in cell body, obtain the useless spinning solution after homogeneous;
(3) after making useless spinning solution after described homogeneous enter accurate filter to filter, the useless spinning solution after being filtered;
(4) making useless spinning solution after described filtration enter polymer fluid deaeration still carries out, after deaeration, obtaining spinning solution;
(5) make described spinning solution enter spinning machine.
In the step (2) of above-mentioned recovery method, circulation shear carries out under constant temperature, and this temperature is identical with the hot water temperature who passes into; The pressure of circulation shear can be 0.1-0.2MPa.The method of the abundant homogeneous of mixed liquor of the useless spinning solution of judgement and solvent can comprise the following steps: the mixed liquor that takes out a small amount of useless spinning solution and solvent, whether observe in mixed liquor has solvent to separate out, if there is no solvent separates out, think and the mixed liquor abundant homogeneous of useless spinning solution and solvent can stop circulation shear pump.In addition, when stopping circulation shear pump, in cell body, pass into nitrogen, can play the long-time stay-in-grade effect of spinning solution that makes.
In above-mentioned recovery method, preferably, described solvent is dimethyl sulfoxide (DMSO) (DMSO).More preferably, described solvent is that mass concentration is the dimethyl sulphoxide aqueous solution of 98-99.5%.
In above-mentioned recovery method, preferably, the total amount that sprays into of described solvent is the long-pending 3-5% of waste spinning silk liquid in described cell body.
In above-mentioned recovery method, preferably, the temperature of described hot water is 50-60 ℃.
In above-mentioned recovery method, preferably, the pressure of described nitrogen in cell body is 0.05-0.1MPa.
In above-mentioned recovery method, preferably, described accurate filter is that pore size filter is the accurate filter of 0.5-3 μ m.Through accurate filter, filter, can remove impurity and microgel in useless spinning solution.
In above-mentioned recovery method, preferably, the temperature in described polymer fluid deaeration still is 40-45 ℃, the vacuum on still top be-0.092MPa extremely-0.097MPa.Through polymer fluid deaeration still, carry out after deaeration, can access the spinning solution of free from foreign meter, microgel, bubble.
In above-mentioned recovery method, preferably, the gross weight of the resulting spinning solution of recovery method of the present invention of take is benchmark, and its solid content is 18-22%.
In above-mentioned recovery method, preferably, in step (3), by gear wheel metering pump, make useless spinning solution after described homogeneous enter accurate filter and filter.Adopt the useless spinning solution by after homogeneous that gear wheel metering pump can be more efficient, quantitative to send in accurate filter.
In above-mentioned recovery method, preferably, in step (5), by feeding gear pump, make described spinning solution enter spinning machine.Adopt feeding gear pump more fast and efficiently spinning solution to be sent in spinning machine.
The technological operation of recovery method of the present invention can be step; in recovery method of the present invention; first useless spinning solution is collected in the useless spinning solution feeder with hot water constant temperature function; then by nozzle, in useless spinning solution feeder, spray into solvent; the homogeneous that carries out self-loopa by circulation shear pump is again processed; then pass into nitrogen protection; make useless spinning solution place barotropic state; again through the filtration of accurate filter, after the deaeration of polymer fluid deaeration still processes; can obtain the spinning solution that normal spinning is used, supply with spinning machine and continue spinning.
The retracting device of useless spinning solution of the present invention and method, in the production technology for carbon fibre precursor, at the driving initial stage or change in the processes such as spinning machine filter, spinning head, from spinning machine, discharge in a large number cannot spinning useless spinning solution, and apparatus and method of again recycling.The advantages such as it is short that the retracting device of useless spinning solution of the present invention and method have technological process, and use equipment is few, and device structure is simple; And more than can recycling useless spinning solution 90% gross weight of the useless spinning solution processed (take be benchmark), have the advantages that efficiency is high; The wasting of resources that while can also avoid the direct discharge of useless spinning solution to cause, realizes the cycle development that resource recycling is turned waste into wealth, and avoids contaminated environment, foundation and environment and association's friendly relation.
Accompanying drawing explanation
Fig. 1 is the structural representation of retracting device of the useless spinning solution of embodiment 1.
Primary clustering symbol description:
Cell body 1 polymer fluid deaeration still 2 accurate filter 3 circulation shear pump 4 gear wheel metering pumps 5
Feeding gear pump 6 spinning machine 7 atomizer 8 control valve group 9 flowmeters 10
Temperature controller 11 first Pressure gauge 12 second Pressure gauge 13 the 3rd Pressure gauges 14
Solvent enters pipe 15 nitrogen and enters pipe 16 hot water inflow pipe 17 hot water effusers 18
The specific embodiment
For technical characterictic of the present invention, object and beneficial effect being had more clearly, understand, existing technical scheme of the present invention is carried out to following detailed description, but can not be interpreted as restriction that can practical range of the present invention.
Embodiment 1
The present embodiment provides the retracting device of the useless spinning solution producing in a kind of carbon fibre precursor preparation technology, and as shown in Figure 1, it comprises:
Useless spinning solution feeder, polymer fluid deaeration still 2, pore size filter are accurate filter 3, circulation shear pump 4, gear wheel metering pump 5, the feeding gear pump 6 of 2 μ m;
Described useless spinning solution feeder comprises: cell body 1, be positioned at the heat exchanger of described cell body 1 bottom, be connected in hot water inflow pipe 17 and the hot water effuser 18 of described heat exchanger, be connected in the temperature controller 11 of described cell body 1, be positioned at the atomizer 8 at described cell body 1 top, the solvent that is connected in described atomizer 8 enters pipe 15, the nitrogen that is connected in described cell body 1 enters pipe 16, be connected in the blow-down pipe of described cell body, and useless spinning solution entrance, useless spinning solution outlet, circulation entry to mixed solution and circulation mixture export, wherein, described solvent enters pipe 15 and is provided with control valve group 9 and flowmeter 10, described nitrogen enters pipe, hot water inflow pipe, on hot water effuser and blow-down pipe, be equipped with valve,
Described useless spinning solution entrance is connected with the useless spinning solution outlet of spinning machine 7 by pipeline, and is provided with valve in this pipeline;
Described circulation entry to mixed solution, circulation mixture export are connected with described circulation shear pump 4 by pipeline respectively, and be provided with valve in described circulation entry to mixed solution with the pipeline that described circulation shear pump 4 is connected, and the 3rd Pressure gauge 14 is arranged on the pipeline that described circulation entry to mixed solution is connected with described circulation shear pump 4;
Described useless spinning solution outlet is connected in the charging aperture of described accurate filter 3 by pipeline, and described gear wheel metering pump 5 and the second Pressure gauge 13 are arranged on this pipeline; The discharging opening of described accurate filter 3 is connected in the charging aperture (and on the pipeline of the discharging opening of described accurate filter 3, valve being set) of described polymer fluid deaeration still 2 by pipeline, and the first Pressure gauge 12 is arranged on this pipeline; The discharging opening of described polymer fluid deaeration still 2 is connected in the charging aperture (and on the pipeline of the discharging opening of described polymer fluid deaeration still 2, valve being set) of described spinning machine 7 by pipeline, and described feeding gear pump 6 is arranged on this pipeline.
Embodiment 2
The present embodiment provides the recovery method of the useless spinning solution producing in a kind of carbon fibre precursor preparation technology, its method for adopting the device of embodiment 1 to carry out, and the method comprises the following steps:
(1) impure, the microgel of the initial stage spinning machine 7 of driving being discharged, the useless spinning solution of bubble are collected in the cell body 1 of useless spinning solution feeder, by hot water inflow pipe 17 and hot water effuser 18, to the heat exchanger of cell body 1 bottom, continue to pass into the hot water of 50-60 ℃, and by temperature controller 11 by the useless spinning solution thermostatic control in cell body 1 at 50-60 ℃;
(2) when the waste spinning silk liquid temp in cell body rises to 50-60 ℃, start circulation shear pump 4, open solvent simultaneously and enter the control valve group 9 on pipe 15, by solvent, entering pipe 15 and atomizer 8, to the useless spinning solution in cell body 1, to spray into mass concentration be 99.5% dimethyl sulphoxide aqueous solution, by control valve group 9 and flowmeter 10, control the straying quatity of this dimethyl sulphoxide aqueous solution, make its spray into total amount be waste spinning silk liquid in described cell body 1 long-pending 5%, make the mixed liquor of useless spinning solution in cell body 1 and this dimethyl sulphoxide aqueous solution at 50-60 ℃, homogeneous circulates under 0.1-0.2MPa, and by the pressure of the 3rd Pressure gauge 14 monitoring circulation homogenizing processes, fully after homogeneous, stop circulation shear pump 4, by nitrogen, enter pipe 16 simultaneously and pass into nitrogen protection in cell body 1, and to make the pressure of nitrogen in cell body 1 be 0.05MPa, obtain the useless spinning solution after homogeneous,
(3) by gear wheel metering pump 5, making useless spinning solution after described homogeneous enter pore size filter is that the accurate filter 3 of 2 μ m filters, by 13 pairs, the second Pressure gauge, enter pressure monitors simultaneously, after filtration, remove impurity and microgel in the useless spinning solution after described homogeneous, the useless spinning solution after being filtered;
(4) make the useless spinning solution after described filtration enter polymer fluid deaeration still 2, by 12 pairs, the first Pressure gauge, enter pressure monitors simultaneously, to be 40-45 ℃, the vacuum on still top carry out deaeration for-0.092MPa to temperature in polymer fluid deaeration still to the condition of-0.097MPa, obtain spinning solution, the gross weight of this spinning solution of take is benchmark, and its solid content is 20%;
(5) by feeding gear pump 6, make described spinning solution enter spinning machine.
In the present embodiment, at spinning solution, enter after spinning machine, from the gooseneck discharge of spinning machine can find that this spinning solution is free from foreign meter, microgel, bubble, can be used as normal spinning and use.Therefore, really can the effective recycling useless spinning solution of the retracting device of of the present invention useless spinning solution and method, and have that technological process is short, use equipment is few, device structure simple, organic efficiency advantages of higher.
Claims (10)
1. a retracting device for the useless spinning solution producing in carbon fibre precursor preparation technology, it at least comprises:
Useless spinning solution feeder, polymer fluid deaeration still, accurate filter, circulation shear pump;
Described useless spinning solution feeder at least comprises: cell body, be positioned at the heat exchanger of described cell body bottom, be connected in hot water inflow pipe and the hot water effuser of described heat exchanger, be connected in the temperature controller of described cell body, be positioned at the nozzle at described cell body top, the solvent that is connected in described nozzle enters pipe, the nitrogen that is connected in described cell body enters pipe, and useless spinning solution entrance, useless spinning solution outlet, circulation entry to mixed solution and circulation mixture export;
Described useless spinning solution entrance is connected with the useless spinning solution outlet of spinning machine by pipeline;
Described circulation entry to mixed solution, circulation mixture export are connected with described circulation shear pump by pipeline respectively;
Described useless spinning solution outlet is connected in the charging aperture of described accurate filter by pipeline, the discharging opening of described accurate filter is connected in the charging aperture of described polymer fluid deaeration still by pipeline, the discharging opening of described polymer fluid deaeration still is connected in the charging aperture of described spinning machine by pipeline.
2. retracting device as claimed in claim 1, it also comprises gear wheel metering pump, described gear wheel metering pump is arranged on the pipeline that described useless spinning solution outlet is connected with the charging aperture of described accurate filter.
3. retracting device as claimed in claim 1 or 2, it also comprises feeding gear pump, described feeding gear pump is arranged on the pipeline that the discharging opening of described polymer fluid deaeration still is connected with the charging aperture of described spinning machine.
4. the retracting device as described in claim 1-3 any one, it also comprises valve, described valve is at least positioned on the pipeline that described useless spinning solution entrance is connected with the useless spinning solution outlet of described spinning machine, on the pipeline that described circulation entry to mixed solution is connected with described circulation shear pump, described nitrogen enters on pipe, on described hot water inflow pipe and described hot water effuser, described solvent enters on pipe.
5. the recovery method of the useless spinning solution producing in a carbon fibre precursor preparation technology, it is for adopting the give up method of spinning solution recovery of the retracting device of the useless spinning solution producing in the carbon fibre precursor preparation technology described in claim 1-4 any one, and the method comprises the following steps:
(1) the useless spinning solution of spinning machine being discharged is collected in the cell body of useless spinning solution feeder, by hot water inflow pipe and hot water effuser, to the heat exchanger bottom cell body, continue to pass into hot water, and by temperature controller, the useless spinning solution in cell body is carried out to thermostatic control;
(2) the waste spinning silk liquid temp in cell body rises to when identical with the hot water temperature who passes into; start circulation shear pump; simultaneously by solvent enter pipe and nozzle to the useless spinning solution in cell body, spray into solvent; after the abundant homogeneous of mixed liquor of the useless spinning solution in cell body and solvent; stop circulation shear pump; by nitrogen, enter pipe simultaneously and pass into nitrogen protection in cell body, obtain the useless spinning solution after homogeneous.
(3) after making useless spinning solution after described homogeneous enter accurate filter to filter, the useless spinning solution after being filtered;
(4) making useless spinning solution after described filtration enter polymer fluid deaeration still carries out, after deaeration, obtaining spinning solution;
(5) make described spinning solution enter spinning machine.
6. recovery method as claimed in claim 5, wherein, described solvent is dimethyl sulfoxide (DMSO); Preferably, described solvent is that mass concentration is the dimethyl sulphoxide aqueous solution of 98-99.5%.
7. the recovery method as described in claim 5 or 6, wherein, the total amount that sprays into of described solvent is the long-pending 3-5% of waste spinning silk liquid in described cell body.
8. recovery method as claimed in claim 5, wherein, the temperature of described hot water is 50-60 ℃; The pressure of described nitrogen in cell body is 0.05-0.1MPa; Described accurate filter is that pore size filter is the accurate filter of 0.5-3 μ m.
9. recovery method as claimed in claim 5, wherein, the temperature in described polymer fluid deaeration still is 40-45 ℃, the vacuum on still top be-0.092MPa extremely-0.097MPa.
10. the recovery method as described in claim 5-9 any one, wherein, the gross weight of described spinning solution of take is benchmark, its solid content is 18-22%.
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| CN106012066A (en) * | 2016-07-29 | 2016-10-12 | 广东新会美达锦纶股份有限公司 | Spinning machine with function of automatically cleaning and recovering wastewater |
| CN106012064A (en) * | 2016-07-29 | 2016-10-12 | 广东新会美达锦纶股份有限公司 | Spinning machine with function of automatically cleaning wastewater |
| CN113373540A (en) * | 2021-07-07 | 2021-09-10 | 山西钢科碳材料有限公司 | Polyacrylonitrile fiber and preparation method thereof |
| CN115559024A (en) * | 2022-10-12 | 2023-01-03 | 山西钢科碳材料有限公司 | Method for recycling waste polyacrylonitrile solution |
| CN117512821A (en) * | 2023-09-28 | 2024-02-06 | 山东国泰大成科技有限公司 | Device and method for separating and recovering solvent from spinning solution |
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| CN115559024B (en) * | 2022-10-12 | 2023-11-10 | 山西钢科碳材料有限公司 | Recycling method of waste polyacrylonitrile solution |
| CN117512821A (en) * | 2023-09-28 | 2024-02-06 | 山东国泰大成科技有限公司 | Device and method for separating and recovering solvent from spinning solution |
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| CN104178848B (en) | 2016-06-08 |
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