CN105731568A - Method for recycling polyacrylonitrile carbon fiber precursor production wastewater through multi-effect distillation - Google Patents
Method for recycling polyacrylonitrile carbon fiber precursor production wastewater through multi-effect distillation Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/02—Treatment of water, waste water, or sewage by heating
- C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/02—Treatment of water, waste water, or sewage by heating
- C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
- C02F1/048—Purification of waste water by evaporation
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- C—CHEMISTRY; METALLURGY
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- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C315/00—Preparation of sulfones; Preparation of sulfoxides
- C07C315/06—Separation; Purification; Stabilisation; Use of additives
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/34—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32
- C02F2103/36—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32 from the manufacture of organic compounds
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Abstract
The invention provides a method for recycling polyacrylonitrile carbon fiber precursor production wastewater through multi-effect distillation. The defect that the recycling cost of polyacrylonitrile carbon fiber precursor production wastewater is too high is overcome. The recycling method is low in cost. The energy consumption of a whole device is lowered by 60-80% compared with existing distillation equipment. The method for recycling polyacrylonitrile carbon fiber precursor production wastewater through multi-effect distillation has the advantages that a fourth-effect distillation tower is combined with a fifth-effect distillation tower, the steam utilization rate is improved, the load of the distillation towers is reduced, and the production cost is greatly reduced; the purity of a solvent obtained through the technology and device can reach the AA-grade standard in America.
Description
Technical field
The invention belongs to technical field of rectification, be specifically related to a kind of multi-effect distillation recovery polyacrylonitrile carbon fiber former
Silk produces the method for waste water.
Background technology
In polyacrylonitrile carbon fiber production process, inevitably having the generation of lean solution, these give up molten
Liquid concentration is relatively low, and is dissolved with oligomer in solution, if arbitrarily discharging, inherently causes the pollution of environment.
Therefore, how to recycle these solvents, and ensure that the purity of recovery and the economy of energy consumption are to be related to often
Individual enterprise seeks development, drops the major issue of energy consumption, high benefit.
At present, many enterprises use the mode of direct rectification to reclaim useless dilute solvent, this single essence
Evaporating mode, the capacity of returns of needs is relatively big, higher to the load of overhead condenser, tower bottom reboiler and oligomeric
The existence of thing, considerably increases heat transmission resistance and cleaning difficulty, the overall manufacturing high cost of reboiler, is
Worthless.Multi-effect distillation device has the advantage that single rectification method is incomparable, and multi-effect distillation fully improves
The utilization rate of indirect steam, is successfully realized the concentration to useless dilute solvent.But the material gone out at the bottom of quadruple effect tower,
Do not reach the high-purity of more than 99.99%, therefore a rectifying column need to be increased after quadruple effect tower, to realize material
High-purity reclaim and the collection discharge of oligomer, therefore invention uses rectification based on quadruple effect rectification to reclaim
Technique.
Summary of the invention
The present invention mainly overcomes the deficiency reclaiming polyacrylonitrile carbon fiber precursor production waste water high cost, it is provided that
A kind of lower-cost recovery method, makes energy consumption fall for the more existing rectifying device of energy consumption of whole device
Low 60-80%.
It is an object of the invention to provide a kind of multi-effect distillation and reclaim polyacrylonitrile carbon fiber precursor production waste water
Method, it is characterised in that comprise the following steps:
(1) the low concentration wastewater solution (polyacrylonitrile carbon fiber precursor waste water) of 3-25% is sequentially passed through useless
After steam heater preheats, enter the first effect rectifier bottoms, by steam, reboiler is heated, first
At the bottom of weak solution input the second effect rectifying tower at the bottom of effect rectifying tower, the first effect rectifying column tower top steam is as the
The thermal source of the reboiler of two effect rectifying columns, the thermal source of wherein said exhaust steam heater is that steam at different levels is to boiling again
Gained low-pressure steam after device heating.
Solution at the bottom of (2) second effect rectifying towers sequentially inputs three-effect rectification tower, quadruple effect rectification after concentrating
At the bottom of tower tower concentrate, second effect rectifying column, three-effect rectification column overhead steam successively as rear one effect reboiler,
Thermal source, carry out atmospheric distillation.
(3) quadruple effect rectifying column materials at bottom of tower input the 5th effect rectifying columns, the 5th effect rectifying column uses decompression
Rectification, top vacuum degree is-90KPa to-101KPa, is heated reboiler by steam, overhead condenser
Condensing material, reflux ratio is 3.5, and along with the rising of temperature, tower top first goes out material B, i.e. waste water,
When tower top temperature reaches 120-145 DEG C, go out more than 99.99% neat solvent C during column bottom temperature 130-155 DEG C, i.e.
Pure sulfoxide, remains D, is high-boiling components at the bottom of tower.
Wherein, the low concentration wastewater solution of described 3-25% is that dimethyl sulphoxide solution, dimethylformamide are molten
Liquid or dimethylacetamide solution, and wherein contain the polyacrylonitrile oligomer of 0.1%-3% mass concentration,
Its degree of polymerization is at 500-2000.
Preferably, at the bottom of described second effect rectifying tower, go out the weak solution of 50-65%, column bottom temperature 125-140 DEG C,
Overhead reflux ratio is 2.0, goes out the weak solution of 70-83% at the bottom of three-effect rectification tower tower, column bottom temperature 110-130 DEG C,
Overhead reflux ratio 2.0；The weak solution of 87-94%, tower top temperature 30-65 DEG C, tower is gone out at the bottom of quadruple effect rectifying tower
End temperature 80-98 DEG C, top vacuum degree is-90Kpa to-98KPa, and overhead reflux ratio is 1.2.
Preferably, the first effect rectifying column column bottom temperature 130-155 DEG C, overhead reflux ratio described in step (1)
It is 2.0, carries out atmospheric distillation, go out at the bottom of tower at the bottom of the described second effect rectifying tower of 30-45% weak solution input.
Using above-mentioned multi-effect distillation to reclaim the method that polyacrylonitrile carbon fiber precursor produces waste water, the present invention has
Advantages below:
(1) this device utilizes quadruple effect rectifying column and the 5th effect rectifying column combination, improves the utilization rate of steam,
Decrease the load of rectifying column, greatly reduce the cost of production；
(2) utilizing this technique and the solvent of device gained, purity is up to U.S.'s AA grade standard.
Detailed description of the invention
The present invention is expanded on further below by way of specific embodiment, but is not limited to following embodiment.
A kind of multi-effect distillation reclaims the method that polyacrylonitrile carbon fiber precursor produces waste water, comprises the following steps:
(1) the low concentration wastewater solution (polyacrylonitrile carbon fiber precursor waste water) of 3-25% is sequentially passed through useless
After steam heater 1-1,1-2,1-3,1-4 preheat, enter bottom the first effect rectifying column 3-1, by steaming
Reboiler 4-1 is heated by vapour, the first effect rectifying column 3-1 column bottom temperature 130-155 DEG C, and overhead reflux ratio is 2.0,
Carry out atmospheric distillation, go out at the bottom of 30-45% weak solution input the second effect rectifying column 3-2 tower at the bottom of tower, the first effect rectification
Tower 3-1 overhead water steam is as the thermal source of the reboiler 4-2 of the second effect rectifying column 3-2, wherein said exhaust steam
The thermal source of heater is gained low-pressure steam after reboiler is heated by steam at different levels.
(2) second effect rectifying column 3-2 towers at the bottom of solution concentrate after sequentially input three-effect rectification tower 3-3, the 4th
Concentrating at the bottom of effect rectifying column 3-4 tower, the second effect rectifying column 3-2, three-effect rectification tower 3-3 overhead vapours are made successively
For the thermal source of rear effect reboiler 4-3,4-4, carry out atmospheric distillation, wherein at the bottom of the second effect rectifying column 3-2 tower
Going out the weak solution of 50-65%, column bottom temperature 125-140 DEG C, overhead reflux ratio is 2.0, three-effect rectification tower 3-3
The weak solution of 70-83%, column bottom temperature 110-130 DEG C, overhead reflux ratio 2.0 is gone out at the bottom of tower；Quadruple effect rectifying column
The weak solution of 87-94%, tower top temperature 30-65 DEG C, column bottom temperature 80-98 DEG C, top vacuum is gone out at the bottom of 3-4 tower
Degree is-90Kpa to-98KPa, and overhead reflux ratio is 1.2.
(3) quadruple effect rectifying column 3-4 materials at bottom of tower input the 5th effect rectifying columns 5, the 5th effect rectifying column 5 is adopted
With rectification under vacuum, top vacuum degree is-90KPa to-101KPa, is heated reboiler 6 by steam, tower
Material is condensed by top condenser 7, and reflux ratio is 3.5, and along with the rising of temperature, tower top first goes out material B,
I.e. waste water, when tower top temperature reaches 120-145 DEG C, goes out more than 99.99% pure molten during column bottom temperature 130-155 DEG C
Agent C, the purest sulfoxide, remain D at the bottom of tower, be high-boiling components.
Wherein, the low concentration wastewater solution of described 3-25% is that dimethyl sulphoxide solution, dimethylformamide are molten
Liquid or dimethylacetamide solution, and wherein contain the polyacrylonitrile oligomer of 0.1%-3% mass concentration,
Its degree of polymerization is at 500-2000.
Specific embodiment
Embodiment 1
(1) the low concentration wastewater solution (polyacrylonitrile carbon fiber precursor waste water) of 3% is sequentially passed through useless steaming
After vapour heater 1-1,1-2,1-3,1-4 preheat, enter bottom the first effect rectifying column 3-1, pass through steam
Heating reboiler 4-1, the first effect rectifying column 3-1 column bottom temperature 130 DEG C, overhead reflux ratio is 2.0, carries out
Atmospheric distillation, goes out at the bottom of 45% weak solution input the second effect rectifying column 3-2 tower, the first effect rectifying column 3-1 tower at the bottom of tower
Push up the steam thermal source as the reboiler 4-2 of the second effect rectifying column 3-2, wherein said exhaust steam heater
Thermal source is gained low-pressure steam after reboiler is heated by steam at different levels.
(2) second effect rectifying column 3-2 towers at the bottom of solution concentrate after sequentially input three-effect rectification tower 3-3, the 4th
Concentrating at the bottom of effect rectifying column 3-4 tower, the second effect rectifying column 3-2, three-effect rectification tower 3-3 overhead vapours are made successively
For the thermal source of rear effect reboiler 4-3,4-4, carry out atmospheric distillation, wherein at the bottom of the second effect rectifying column 3-2 tower
Going out the weak solution of 50%, column bottom temperature 125 DEG C, overhead reflux ratio is 2.0, at the bottom of three-effect rectification tower 3-3 tower
Go out the weak solution of 83%, column bottom temperature 110 DEG C, overhead reflux ratio 2.0；Go out at the bottom of quadruple effect rectifying column 3-4 tower
The weak solution of 94%, tower top temperature 30 DEG C, column bottom temperature 98 DEG C, top vacuum degree is-90KPa, and tower top returns
Flow ratio is 1.2.
(3) quadruple effect rectifying column 3-4 materials at bottom of tower input the 5th effect rectifying columns 5, the 5th effect rectifying column 5 is adopted
With rectification under vacuum, top vacuum degree is-101KPa, is heated reboiler 6 by steam, overhead condenser 7
Condensing material, reflux ratio is 3.5, and along with the rising of temperature, tower top first goes out material B, i.e. waste water,
When tower top temperature reaches 145 DEG C, during column bottom temperature 155 DEG C, go out more than 99.99% neat solvent C, the purest sulfoxide,
Remain D at the bottom of tower, be high-boiling components.
Wherein, the low concentration wastewater solution of described 3% is dimethyl sulphoxide solution, dimethyl formamide solution
Or dimethylacetamide solution, and wherein contain the polyacrylonitrile oligomer of 0.1% mass concentration, its polymerization
Degree is 2000.
Embodiment 2
(1) the low concentration wastewater solution (polyacrylonitrile carbon fiber precursor waste water) of 10% is sequentially passed through useless steaming
After vapour heater 1-1,1-2,1-3,1-4 preheat, enter bottom the first effect rectifying column 3-1, pass through steam
Heating reboiler 4-1, the first effect rectifying column 3-1 column bottom temperature 140 DEG C, overhead reflux ratio is 2.0, carries out
Atmospheric distillation, goes out at the bottom of 40% weak solution input the second effect rectifying column 3-2 tower, the first effect rectifying column 3-1 tower at the bottom of tower
Push up the steam thermal source as the reboiler 4-2 of the second effect rectifying column 3-2, wherein said exhaust steam heater
Thermal source is gained low-pressure steam after reboiler is heated by steam at different levels.
(2) second effect rectifying column 3-2 towers at the bottom of solution concentrate after sequentially input three-effect rectification tower 3-3, the 4th
Concentrating at the bottom of effect rectifying column 3-4 tower, the second effect rectifying column 3-2, three-effect rectification tower 3-3 overhead vapours are made successively
For the thermal source of rear effect reboiler 4-3,4-4, carry out atmospheric distillation, wherein at the bottom of the second effect rectifying column 3-2 tower
Going out the weak solution of 60%, column bottom temperature 130 DEG C, overhead reflux ratio is 2.0, at the bottom of three-effect rectification tower 3-3 tower
Go out the weak solution of 75%, column bottom temperature 115 DEG C, overhead reflux ratio 2.0；Go out at the bottom of quadruple effect rectifying column 3-4 tower
The weak solution of 89%, tower top temperature 50 DEG C, column bottom temperature 95 DEG C, top vacuum degree is-93Kpa, and tower top returns
Flow ratio is 1.2.
(3) quadruple effect rectifying column 3-4 materials at bottom of tower input the 5th effect rectifying columns 5, the 5th effect rectifying column 5 is adopted
With rectification under vacuum, top vacuum degree is-95KPa, is heated reboiler 6 by steam, overhead condenser 7
Condensing material, reflux ratio is 3.5, and along with the rising of temperature, tower top first goes out material B, i.e. waste water,
When tower top temperature reaches 120 DEG C, during column bottom temperature 145 DEG C, go out more than 99.99% neat solvent C, the purest sulfoxide,
Remain D at the bottom of tower, be high-boiling components.
Wherein, the low concentration wastewater solution of described 10% is that dimethyl sulphoxide solution, dimethylformamide are molten
Liquid or dimethylacetamide solution, and wherein contain the polyacrylonitrile oligomer of 1% mass concentration, its polymerization
Degree is 500.
Embodiment 3
(1) the low concentration wastewater solution (polyacrylonitrile carbon fiber precursor waste water) of 20% is sequentially passed through useless
After steam heater 1-1,1-2,1-3,1-4 preheat, enter bottom the first effect rectifying column 3-1, by steaming
Reboiler 4-1 is heated by vapour, and the first effect rectifying column 3-1 column bottom temperature 150 DEG C, overhead reflux ratio is 2.0, enters
Row atmospheric distillation, goes out at the bottom of 30% weak solution input the second effect rectifying column 3-2 tower, the first effect rectifying column 3-1 at the bottom of tower
Overhead water steam is as the thermal source of the reboiler 4-2 of the second effect rectifying column 3-2, wherein said exhaust steam heater
Thermal source gained low-pressure steam after to be steam at different levels heat reboiler.
(2) second effect rectifying column 3-2 towers at the bottom of solution concentrate after sequentially input three-effect rectification tower 3-3, the 4th
Concentrating at the bottom of effect rectifying column 3-4 tower, the second effect rectifying column 3-2, three-effect rectification tower 3-3 overhead vapours are made successively
For the thermal source of rear effect reboiler 4-3,4-4, carry out atmospheric distillation, wherein at the bottom of the second effect rectifying column 3-2 tower
Going out the weak solution of 65%, column bottom temperature 140 DEG C, overhead reflux ratio is 2.0, at the bottom of three-effect rectification tower 3-3 tower
Go out the weak solution of 70%, column bottom temperature 130 DEG C, overhead reflux ratio 2.0；Go out at the bottom of quadruple effect rectifying column 3-4 tower
The weak solution of 87%, tower top temperature 65 DEG C, column bottom temperature 80 DEG C, top vacuum degree is-95Kpa, and tower top returns
Flow ratio is 1.2.
(3) quadruple effect rectifying column 3-4 materials at bottom of tower input the 5th effect rectifying columns 5, the 5th effect rectifying column 5 is adopted
With rectification under vacuum, top vacuum degree is-98KPa, is heated reboiler 6 by steam, overhead condenser 7
Condensing material, reflux ratio is 3.5, and along with the rising of temperature, tower top first goes out material B, i.e. waste water,
When tower top temperature reaches 130 DEG C, during column bottom temperature 130 DEG C, go out more than 99.99% neat solvent C, the purest sulfoxide,
Remain D at the bottom of tower, be high-boiling components.
Wherein, the low concentration wastewater solution of described 20% is that dimethyl sulphoxide solution, dimethylformamide are molten
Liquid or dimethylacetamide solution, and wherein contain the polyacrylonitrile oligomer of 2% mass concentration, its polymerization
Degree is 1500.
Embodiment 4
(1) the low concentration wastewater solution (polyacrylonitrile carbon fiber precursor waste water) of 25% is sequentially passed through useless steaming
After vapour heater 1-1,1-2,1-3,1-4 preheat, enter bottom the first effect rectifying column 3-1, pass through steam
Heating reboiler 4-1, the first effect rectifying column 3-1 column bottom temperature 138 DEG C, overhead reflux ratio is 2.0, carries out
Atmospheric distillation, goes out at the bottom of 38% weak solution input the second effect rectifying column 3-2 tower, the first effect rectifying column 3-1 tower at the bottom of tower
Push up the steam thermal source as the reboiler 4-2 of the second effect rectifying column 3-2, wherein said exhaust steam heater
Thermal source is gained low-pressure steam after reboiler is heated by steam at different levels.
(2) second effect rectifying column 3-2 towers at the bottom of solution concentrate after sequentially input three-effect rectification tower 3-3, the 4th
Concentrating at the bottom of effect rectifying column 3-4 tower, the second effect rectifying column 3-2, three-effect rectification tower 3-3 overhead vapours are made successively
For the thermal source of rear effect reboiler 4-3,4-4, carry out atmospheric distillation, wherein at the bottom of the second effect rectifying column 3-2 tower
Going out the weak solution of 58%, column bottom temperature 138 DEG C, overhead reflux ratio is 2.0, at the bottom of three-effect rectification tower 3-3 tower
Go out the weak solution of 78%, column bottom temperature 120 DEG C, overhead reflux ratio 2.0；Go out at the bottom of quadruple effect rectifying column 3-4 tower
The weak solution of 92%, tower top temperature 55 DEG C, column bottom temperature 87 DEG C, top vacuum degree is-98KPa, and tower top returns
Flow ratio is 1.2.
(3) quadruple effect rectifying column 3-4 materials at bottom of tower input the 5th effect rectifying columns 5, the 5th effect rectifying column 5 is adopted
With rectification under vacuum, top vacuum degree is-90KPa, is heated reboiler 6 by steam, overhead condenser 7
Condensing material, reflux ratio is 3.5, and along with the rising of temperature, tower top first goes out material B, i.e. waste water,
When tower top temperature reaches 128 DEG C, during column bottom temperature 155 DEG C, go out more than 99.99% neat solvent C, the purest sulfoxide,
Remain D at the bottom of tower, be high-boiling components.
Wherein, the low concentration wastewater solution of described 25% is that dimethyl sulphoxide solution, dimethylformamide are molten
Liquid or dimethylacetamide solution, and wherein contain the polyacrylonitrile oligomer of 3% mass concentration, its polymerization
Degree is 800.
It will be apparent to those skilled in the art that can technical scheme as described above and design, make it
Its various corresponding changes and deformation, and all these changes and deformation all should belong to present invention power
Within the protection domain that profit requires.
Claims (3)
1. a multi-effect distillation reclaims the method that polyacrylonitrile carbon fiber precursor produces waste water, it is characterised in that bag
Include following steps:
(1) the low concentration wastewater solution (polyacrylonitrile carbon fiber precursor waste water) of 3-25% is sequentially passed through useless
After steam heater preheats, enter the first effect rectifier bottoms, by steam, reboiler is heated, first
At the bottom of weak solution input the second effect rectifying tower at the bottom of effect rectifying tower, the first effect rectifying column tower top steam is as the
The thermal source of the reboiler of two effect rectifying columns, the thermal source of wherein said exhaust steam heater is that steam at different levels is to boiling again
Gained low-pressure steam after device heating.
Solution at the bottom of (2) second effect rectifying towers sequentially inputs three-effect rectification tower, quadruple effect rectification after concentrating
At the bottom of tower tower concentrate, second effect rectifying column, three-effect rectification column overhead steam successively as rear one effect reboiler,
Thermal source, carry out atmospheric distillation.
(3) quadruple effect rectifying column materials at bottom of tower input the 5th effect rectifying columns, the 5th effect rectifying column uses decompression
Rectification, top vacuum degree is-90KPa to-101KPa, is heated reboiler by steam, overhead condenser
Condensing material, reflux ratio is 3.5, and along with the rising of temperature, tower top first goes out material B, i.e. waste water,
When tower top temperature reaches 120-145 DEG C, go out more than 99.99% neat solvent C during column bottom temperature 130-155 DEG C, i.e.
Pure sulfoxide, remains D, is high-boiling components at the bottom of tower.
Wherein, the low concentration wastewater solution of described 3-25% is that dimethyl sulphoxide solution, dimethylformamide are molten
Liquid or dimethylacetamide solution, and wherein contain the polyacrylonitrile oligomer of 0.1%-3% mass concentration,
Its degree of polymerization is at 500-2000.
2. multi-effect distillation reclaims the method that polyacrylonitrile carbon fiber precursor produces waste water as claimed in claim 1,
It is characterized in that: at the bottom of described second effect rectifying tower, go out the weak solution of 50-65%, column bottom temperature 125-140 DEG C,
Overhead reflux ratio is 2.0, goes out the weak solution of 70-83% at the bottom of three-effect rectification tower tower, column bottom temperature 110-130 DEG C,
Overhead reflux ratio 2.0；The weak solution of 87-94%, tower top temperature 30-65 DEG C, tower is gone out at the bottom of quadruple effect rectifying tower
End temperature 80-98 DEG C, top vacuum degree is-90Kpa to-98KPa, and overhead reflux ratio is 1.2.
3. multi-effect distillation reclaims the method that polyacrylonitrile carbon fiber precursor produces waste water as claimed in claim 1,
It is characterized in that: the first effect rectifying column column bottom temperature 130-155 DEG C, overhead reflux ratio described in step (1)
It is 2.0, carries out atmospheric distillation, go out at the bottom of tower at the bottom of the described second effect rectifying tower of 30-45% weak solution input.
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| CN113583292A (en) * | 2021-07-30 | 2021-11-02 | 中复神鹰碳纤维股份有限公司 | Method for recycling DMSO (dimethyl sulfoxide) aqueous solution rectification residues in production of polyacrylonitrile carbon fibers |
| CN113583292B (en) * | 2021-07-30 | 2023-10-13 | 中复神鹰碳纤维股份有限公司 | Recycling method of DMSO (dimethyl sulfoxide) aqueous solution rectification residues for producing polyacrylonitrile carbon fibers |
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