CN205442665U - Purification recovery of sodium sulfocyanate aqueous solution in production of two step method acrylic fibres - Google Patents

Purification recovery of sodium sulfocyanate aqueous solution in production of two step method acrylic fibres Download PDF

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Publication number
CN205442665U
CN205442665U CN201620231336.3U CN201620231336U CN205442665U CN 205442665 U CN205442665 U CN 205442665U CN 201620231336 U CN201620231336 U CN 201620231336U CN 205442665 U CN205442665 U CN 205442665U
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holding tank
solution
intermediate storage
rolled film
storage tank
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CN201620231336.3U
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Chinese (zh)
Inventor
谭颖士
叶士杰
钱军
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Hubei Liansi New Material Technology Co ltd
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Shanghai Mojing Water Treatment Engineering Co ltd
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Abstract

The utility model discloses a purification recovery of sodium sulfocyanate aqueous solution in production of two step method acrylic fibres, including first holding tank, a bag filter, hollow fiber ultrafiltration device, intermediate storage tanks, the 2nd bag filter, the book formula membrane device that feeds through in proper order, warp dope after the formula of book membrane device is handled is retrieved extremely intermediate storage tanks, scavenging solution send into the second holding tank and treat the evaporation, just be equipped with a plate heat exchanger on the pipeline between book formula membrane device and the second storage jar, evaporated liquor in the second holding tank after the evaporation gets into the third holding tank, sodium sulfocyanate solution flow in the third holding tank is concentrated to the evaporimeter. The utility model discloses simple structure, easy operation utilizes the hollow fiber milipore filter as first impurity removal treatment technique, adopts the stage treatment theory can not only stabilize the effect of edulcoration, also can improve the stability of this technique in the actual motion greatly.

Description

The purification recovery device of sodium thiocyanate water solution in a kind of two step method acrylic fiber production process
Technical field
This utility model relate to a kind of can not sewer process and solvent recycle device, the purification recovery device of sodium thiocyanate water solution in a kind of two step method acrylic fiber production process.
Background technology
Most two step method acrylic fiber production process process is to use sodium thiocyanate solution to cool down solvent as polymerization solvent and molten silk, has the impurity such as sulfate ion, iron ion, P-SPN, P-SPA and enter in sodium thiocyanate solution in production link.Sodium thiocyanate solution is to recycle during acrylic fiber production process, and the accumulation of impurity can cause many harmful effects, therefore has special solution purification remanufacture process to make a return journey the removal of impurity.
Having multiple method at present for purification of sodium thiocyanate solution via, preliminary purifying generally uses sodium hydroxide pellets method to combine kieselguhr filtration or ion exchange to the impurity iron ion removing in solution;Two steps process the method generally using evaporation and concentration and Crystallization Separation;Three step process uses delay ion exchange to remove other some impurity, postpones ion-exchange resins and uses sulphuric acid and sodium hydroxide to regenerate, the most also has the simple membrane process craft using nanofiltration membrane,
The shortcoming of these techniques: operation is many, control is complicated, industrial chemicals consumption greatly outside, also produce a large amount of useless solid and waste water, the consumption such as sulphuric acid used, sodium hydroxide, diisopropyl ether is big, and cost is high, dangerous big, and environmental pollution is serious.And dust removal rate is low, make the quality of NaSCN solvent occur deteriorating, reflect that the jaundice of original liquid coloring, fiber and production stability decline.
The response rate of traditional sodium thiocyanate solution method for purifying and recovering is typically only capable to reach 90%, high energy consumption and the consumption of chemical agent (kieselguhr, sulphuric acid, sodium hydroxide) due to evaporating, concentrating and crystallizing, not only energy and material consumption cost is high, and produce substantial amounts of waste water, useless solid, and occur due to side reaction and the impurity brought into chemical agent also can affect the quality of sodium thiocyanate solution.
Utility model content
The purpose of this utility model is to provide a kind of high-recovery, low cost, high-quality, and can the purification recovery device of sodium thiocyanate water solution in the two step method acrylic fiber production process of more stable operation, to solve the problem that prior art exists.
For achieving the above object, this utility model is achieved by the following technical programs:
The purification recovery device of sodium thiocyanate water solution in a kind of two step method acrylic fiber production process of the present utility model, including the first holding tank being sequentially communicated, first bag filter, hollow-fibre ultrafiltration device, intermediate storage tank, second bag filter, rolled film device, dope after described rolled film device processes is recycled to described intermediate storage tank, it is to be evaporated that scavenging solution sends into the second holding tank, and the pipeline between described rolled film device and the second storage tank is provided with a plate type heat exchanger, in described second holding tank, the evaporation liquid after evaporation enters the 3rd holding tank, sodium thiocyanate solution in described 3rd holding tank flow to vaporizer and concentrates.
The device of method for purifying and recovering described in the utility model, described 3rd holding tank connects with described intermediate storage tank.
The device of method for purifying and recovering described in the utility model, described hollow-fibre ultrafiltration device is provided with electromagnetic flowmeter.
Beneficial effect
This utility model compared with prior art, has the advantage that
This utility model apparatus structure is simple, easily operation, after using device Recovery Purifying of the present utility model, during in waste liquid, the quality of sodium rhodanate accounts for former feedstock solution, the gross mass of sodium rhodanate is less than 1%, reclaim sodium rhodanate and can reach more than 99%, production process need not add the chemical raw materials such as Caustic soda, sulphuric acid, kieselguhr, flush distillation concentration process is reduced than common conventional purge recovery method, desalted water consumption reduces more than 80%, the evaporation and concentration water yield also greatly reduces, and quantity of wastewater effluent also greatly reduces.Simultaneously, compare simple employing NF membrane impurity removing technology, this utility model utilizes hollow fiber ultrafiltration membrane as first remove impurity treatment technology, uses staged care theory can not only stablize the effect of remove impurity, also can be greatly improved this technology stability in actual motion.
Accompanying drawing explanation
Fig. 1 is the structured flowchart of the purification recovery device of sodium thiocyanate water solution in this utility model two step method acrylic fiber production process
Detailed description of the invention
Below in conjunction with detailed description of the invention, this utility model is expanded on further.Should be understood that these embodiments are merely to illustrate this utility model rather than limit scope of the present utility model.In addition, it is to be understood that after having read the content that this utility model is lectured, this utility model can be made various changes or modifications by those skilled in the art, and these equivalent form of values fall within the application appended claims limited range equally.
As shown in Figure 1, the purification recovery device of sodium thiocyanate water solution in two step method acrylic fiber production process of the present utility model, including the first holding tank 1 being sequentially communicated, first bag filter 2, hollow-fibre ultrafiltration device 3, intermediate storage tank 4, second bag filter 5, rolled film device 7, dope after rolled film device 7 processes is recycled to intermediate storage tank 4, it is to be evaporated that scavenging solution sends into the second holding tank 8, and the pipeline between rolled film device 7 and the second storage tank 8 is provided with a plate type heat exchanger 6, in second holding tank 8, the evaporation liquid after evaporation enters the 3rd holding tank 10, sodium thiocyanate solution in 3rd holding tank flow to vaporizer and concentrates.3rd holding tank 10 connects with intermediate storage tank 4.
Embodiment 1
Step one:
The height that the production processes such as spinning produce is containing miscellaneous sodium thiocyanate solution A (control sodium rhodanate concentration and account for solution weight percent concentration 17%), and temperature controls at 15 DEG C, enters buffering the first holding tank 1 afterwards, excludes the oily substance in solution;The impurity such as the insoluble solid suspension during hereafter the first bag filter 2 through precision 100 microns filters interception solution;
Step 2:
Hollow-fibre ultrafiltration device 3 by the modified PVDF material of 50,000 molecular weight, the sodium thiocyanate solution leaching impurity after removing overwhelming majority oligomer is collected to intermediate storage tank 4, hollow-fibre ultrafiltration device uses cross-flow circulation and the full filter type of final cecum (cross flow filter: feed liquid is parallel to face flowing under the promotion of pump, the shearing force that feed liquid unlike filtering from cecum produces when flowing through face takes away the granule being detained on face, so that pollution layer is maintained at a relatively thin level), during cross-flow circulation, dope is back to the first holding tank 1.Hollow-fibre ultrafiltration device 3 filter liquor is measured by electromagnetic flowmeter batch, and when every batch filter liquor reaches setting value, ultrafiltration apparatus is out of service, treats that next batch processes after safeguarding;
Step 3:
Filtering accuracy is to start after 150 molecular weight rolled film devices 7 receive hollow-fibre ultrafiltration device 3 filter liquor to run simultaneously with hollow-fibre ultrafiltration device 3 device, prevent system pipeline and dynamical system from having impurity to enter rolling system, the second bag filter 5 that a precision is 25 microns is set before rolled film device 7.Dope is back to intermediate storage tank 4, by the constant temperature of intermediate storage tank 4 that is back to of plate type heat exchanger 6 at 25 DEG C.It is to be evaporated that scavenging solution after rolled film device 7 process sends into the second holding tank 8.Until the amount of solution that hollow-fibre ultrafiltration device 3 is sent to medial launder 4 reaches the setting value that hollow-fibre ultrafiltration device 3 processes, and when after rolled film device 7 processes, qualified sodium thiocyanate solution reaches enter the first holding tank 1 feed liquid 90%.The desalted water B and the front batch that start surplus solution volume in 5 times of intermediate storage tanks of injection in intermediate storage tank 4 are injected rolled film device 7 after dilution water is dialysed and are collected in the 3rd holding tank 10 permeate of part.Desalted water add rear rolled film device 7 continue to concentrate, now rolled film device 7 purify after solution continue to be fed into the second holding tank 8 to be evaporated until go out liquid amass reach add dilution desalted water 1/2.The liquid that goes out of device 7 sends into the 3rd holding tank 10 afterwards, and the dilution water and the desalted water B that process as rolled film device 7 next batch are used in mixed way.
In intermediate storage tank 4 concentrated solution discharge as waste liquid concentrate separately, burning disposal or collect focuses on to sewage plant C is unified, the sodium rhodanate total amount wherein lost is in feedstock solution B the 0.9% of sodium rhodanate total amount.
Step 4:
Cleaning sodium thiocyanate solution in solution the 3rd holding tank 8, through the concentration of quintuple effect evaporator 9, controls feed flow rate and becomes the sodium thiocyanate solution D of 52% concentration and condense water E, use other production link.After process above processes, reclaim sodium rhodanate and can reach 99.2%.
Embodiment 2
Step one:
The height that the production processes such as spinning produce is containing miscellaneous sodium thiocyanate solution A (control sodium rhodanate concentration and account for solution weight percent concentration 16%), and temperature controls at 45 DEG C, enters buffering the first holding tank 1 afterwards, excludes the oily substance in solution;The impurity such as the insoluble solid suspension during hereafter the first bag filter 2 through precision 100 microns filters interception solution;
Step 2:
Hollow-fibre ultrafiltration device 3 by the modified PVDF material of 100,000 molecular weight, the sodium thiocyanate solution leaching impurity after removing overwhelming majority oligomer is collected to intermediate storage tank 4, hollow-fibre ultrafiltration device uses cross-flow circulation and the blindest section of full filter type (cross flow filter: feed liquid is parallel to face flowing under the promotion of pump, the shearing force produced when feed liquid unlike dead-end filtration flows through face takes away the granule being detained on face, so that pollution layer is maintained at a relatively thin level), during cross-flow circulation, dope is back to the first holding tank 1.Hollow-fibre ultrafiltration device 3 filter liquor is measured by electromagnetic flowmeter batch, and when every batch filter liquor reaches setting value, ultrafiltration apparatus is out of service, treats that next batch processes after safeguarding;
Step 3:
Filtering accuracy is to start after 500 molecular weight rolled film devices 7 receive hollow-fibre ultrafiltration device 3 filter liquor to run simultaneously with hollow-fibre ultrafiltration device 3 device, prevent system pipeline and dynamical system from having impurity to enter rolling system, the second bag filter 5 that a precision is 25 microns is set before rolled film device 7.Dope is back to intermediate storage tank 4, by the constant temperature of intermediate storage tank 4 that is back to of plate type heat exchanger 6 at 25 DEG C.It is to be evaporated that scavenging solution after rolled film device 7 process sends into the second holding tank 8.Until the amount of solution that hollow-fibre ultrafiltration device 3 is sent to medial launder 4 reaches the setting value that hollow-fibre ultrafiltration device 3 processes, and when after rolled film device 7 processes, qualified sodium thiocyanate solution reaches enter the first holding tank 1 feed liquid 92%.The desalted water B and the front batch that start surplus solution volume in 4 times of intermediate storage tanks 4 of injection in intermediate storage tank 4 are injected rolled film device 7 after dilution water is dialysed and are collected in the 3rd holding tank 10 permeate of part.Desalted water add rear rolled film device 7 continue to concentrate, now rolled film device 7 purify after solution continue to be fed into the second holding tank 8 to be evaporated until go out liquid amass reach add dilution desalted water 1/20.The liquid that goes out of device 7 sends into the 3rd holding tank 10 afterwards, and the dilution water and the desalted water B that process as rolled film device 7 next batch are used in mixed way.
In intermediate storage tank 4 concentrated solution discharge as waste liquid concentrate separately, burning disposal or collect focuses on to sewage plant C is unified, the sodium rhodanate total amount wherein lost is in feedstock solution B the 0.85% of sodium rhodanate total amount.
Step 4:
Cleaning sodium thiocyanate solution in solution the 3rd holding tank 8, through the concentration of quintuple effect evaporator 9, controls feed flow rate and becomes the sodium thiocyanate solution D of 50% concentration and condense water E, use other production link.After process above processes, reclaim sodium rhodanate and can reach 99.6%.
Embodiment 3
Step one:
The height that the production processes such as spinning produce is containing miscellaneous sodium thiocyanate solution A (control sodium rhodanate concentration and account for solution weight percent concentration 15%), and temperature controls at 25 DEG C, enters buffering the first holding tank 1 afterwards, excludes the oily substance in solution;The impurity such as the insoluble solid suspension during hereafter the first bag filter 2 through precision 100 microns filters interception solution;
Step 2:
Hollow-fibre ultrafiltration device 3 by the modified PVDF material of 80,000 molecular weight, the sodium thiocyanate solution leaching impurity after removing overwhelming majority oligomer is collected to intermediate storage tank 4, hollow-fibre ultrafiltration device uses cross-flow circulation and the blindest section of full filter type (cross flow filter: feed liquid is parallel to face flowing under the promotion of pump, the shearing force produced when feed liquid unlike dead-end filtration flows through face takes away the granule being detained on face, so that pollution layer is maintained at a relatively thin level), during cross-flow circulation, dope is back to the first holding tank 1.Hollow-fibre ultrafiltration device 3 filter liquor is measured by electromagnetic flowmeter batch, and when every batch filter liquor reaches setting value, ultrafiltration apparatus is out of service, treats that next batch processes after safeguarding;
Step 3:
Filtering accuracy is to start after 450 molecular weight rolled film devices 7 receive hollow-fibre ultrafiltration device 3 filter liquor to run simultaneously with hollow-fibre ultrafiltration device 3 device, prevent system pipeline and dynamical system from having impurity to enter rolling system, the second bag filter 5 that a precision is 25 microns is set before rolled film device 7.Dope is back to intermediate storage tank 4, by the constant temperature of intermediate storage tank 4 that is back to of plate type heat exchanger 6 at 25 DEG C.It is to be evaporated that scavenging solution after rolled film device 7 process sends into the second holding tank 8.Until the amount of solution that hollow-fibre ultrafiltration device 3 is sent to medial launder 4 reaches the setting value that hollow-fibre ultrafiltration device 3 processes, and when after rolled film device 7 processes, qualified sodium thiocyanate solution reaches enter the first holding tank 1 feed liquid 95%.The desalted water B and the front batch that start surplus solution volume in 4 times of intermediate storage tanks of injection in intermediate storage tank 4 are injected rolled film device 7 after dilution water is dialysed and are collected in the 3rd holding tank 10 permeate of part.Desalted water add rear rolled film device 7 continue to concentrate, now rolled film device 7 purify after solution continue to be fed into the second holding tank 8 to be evaporated until go out liquid amass reach add dilution desalted water 1/18.The liquid that goes out of device 7 sends into the 3rd holding tank 10 afterwards, and the dilution water and the desalted water B that process as rolled film device 7 next batch are used in mixed way.
In intermediate storage tank 4 concentrated solution discharge as waste liquid concentrate separately, burning disposal or collect focuses on to sewage plant C is unified, the sodium rhodanate total amount wherein lost is in feedstock solution B the 0.8% of sodium rhodanate total amount.
Step 4:
Cleaning sodium thiocyanate solution in solution the 3rd holding tank 8, through the concentration of quintuple effect evaporator 9, controls feed flow rate and becomes the sodium thiocyanate solution D of 51% concentration and condense water E, use other production link.After process above processes, reclaim sodium rhodanate and can reach 99.5%.
Embodiment 4
Step one:
The height that the production processes such as spinning produce is containing miscellaneous sodium thiocyanate solution A (control sodium rhodanate concentration and account for solution weight percent concentration 14%), and temperature controls at 35 DEG C, enters buffering the first holding tank 1 afterwards, excludes the oily substance in solution;The impurity such as the insoluble solid suspension during hereafter the first bag filter 2 through precision 100 microns filters interception solution;
Step 2:
Hollow-fibre ultrafiltration device 3 by the modified PVDF material of 60,000 molecular weight, the sodium thiocyanate solution leaching impurity after removing overwhelming majority oligomer is collected to intermediate storage tank 4, hollow-fibre ultrafiltration device uses cross-flow circulation and the blindest section of full filter type (cross flow filter: feed liquid is parallel to face flowing under the promotion of pump, the shearing force produced when feed liquid unlike dead-end filtration flows through face takes away the granule being detained on face, so that pollution layer is maintained at a relatively thin level), during cross-flow circulation, dope is back to the first holding tank 1.Hollow-fibre ultrafiltration device 3 filter liquor is measured by electromagnetic flowmeter batch, and when every batch filter liquor reaches setting value, ultrafiltration apparatus is out of service, treats that next batch processes after safeguarding;
Step 3:
Filtering accuracy is to start after 250 molecular weight rolled film devices 7 receive hollow-fibre ultrafiltration device 3 filter liquor to run simultaneously with hollow-fibre ultrafiltration device 3 device, prevent system pipeline and dynamical system from having impurity to enter rolling system, the second bag filter 5 that a precision is 25 microns is set before rolled film device 7.Dope is back to intermediate storage tank 4, by the constant temperature of intermediate storage tank 4 that is back to of plate type heat exchanger 6 at 25 DEG C.It is to be evaporated that scavenging solution after rolled film device 7 process sends into the second holding tank 8.Until the amount of solution that hollow-fibre ultrafiltration device 3 is sent to medial launder 4 reaches the setting value that hollow-fibre ultrafiltration device 3 processes, and when after rolled film device 7 processes, qualified sodium thiocyanate solution reaches enter the first holding tank 1 feed liquid 95%.The desalted water B and the front batch that start surplus solution volume in 5 times of intermediate storage tanks of injection in intermediate storage tank 4 are injected rolled film device 7 after dilution water is dialysed and are collected in the 3rd holding tank 10 permeate of part.Desalted water add rear rolled film device 7 continue to concentrate, now rolled film device 7 purify after solution continue to be fed into the second holding tank 8 to be evaporated until go out liquid amass reach add dilution desalted water 1/15.The liquid that goes out of device 7 sends into the 3rd holding tank 10 afterwards, and the dilution water and the desalted water B that process as rolled film device 7 next batch are used in mixed way.
In intermediate storage tank 4 concentrated solution discharge as waste liquid concentrate separately, burning disposal or collect focuses on to sewage plant C is unified, the sodium rhodanate total amount wherein lost is in feedstock solution B the 0.8% of sodium rhodanate total amount.
Step 4:
Cleaning sodium thiocyanate solution in solution the 3rd holding tank 8, through the concentration of quintuple effect evaporator 9, controls feed flow rate and becomes the sodium thiocyanate solution D of 52% concentration and condense water E, use other production link.After process above processes, reclaim sodium rhodanate and can reach 99.5%.

Claims (3)

1. the purification recovery device of sodium thiocyanate water solution in a two step method acrylic fiber production process, it is characterized in that, including the first holding tank being sequentially communicated, first bag filter, hollow-fibre ultrafiltration device, intermediate storage tank, second bag filter, rolled film device, dope after described rolled film device processes is recycled to described intermediate storage tank, it is to be evaporated that scavenging solution sends into the second holding tank, and the pipeline between described rolled film device and the second storage tank is provided with a plate type heat exchanger, in described second holding tank, the evaporation liquid after evaporation enters the 3rd holding tank, sodium thiocyanate solution in described 3rd holding tank flow to vaporizer and concentrates.
Purification recovery device the most according to claim 1, it is characterised in that described 3rd holding tank connects with described intermediate storage tank.
Purification recovery device the most according to claim 1, it is characterised in that described hollow-fibre ultrafiltration device is provided with electromagnetic flowmeter.
CN201620231336.3U 2016-03-24 2016-03-24 Purification recovery of sodium sulfocyanate aqueous solution in production of two step method acrylic fibres Expired - Fee Related CN205442665U (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105621456A (en) * 2016-03-24 2016-06-01 上海膜净水处理工程有限公司 Purification recycling method and device for sodium thiocyanate solution in two-step method acrylic fiber production

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105621456A (en) * 2016-03-24 2016-06-01 上海膜净水处理工程有限公司 Purification recycling method and device for sodium thiocyanate solution in two-step method acrylic fiber production

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