CN101774721A - Method for treating production solvent-containing waste liquid from production of m-aramid fibers - Google Patents
Method for treating production solvent-containing waste liquid from production of m-aramid fibers Download PDFInfo
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Abstract
The invention discloses a method for treating production solvent-containing waste liquid from m-aramid fiber production, which comprises the following steps: (1), filtering production solvent-containing waste liquid produced in the production of m-aramid fibers; (2), delivering liquid obtained by the step (1) to an extracting device to perform extraction separation in an extraction ratio of (1-3):1 and directly discharging the waste water; (3) delivering an extractive phase in a container used in the step (2) to a distillation tower, and subjecting the extractive phase to reduced pressure distillation separation, wherein the filler accounts for 15 to 25 percent of the volume of the distillation tower, the feeding speed is 8.4 to 16.8 percent of the volume of the distilled tower per hour, the temperature in the tower is 80 to 120 DEG C, the temperature at the bottom of the tower is 130 to 150 DEG C, the refluxing speed is 1.7 to 8.5 percent of the volume of the distillation tower per hour, and the discharge speed is 0.7 to 2.5 percent of the volume of the distillation tower per hour; and (4) rectifying the production solvent obtained by the step (3). The method can save energy and causes little corrosion of rectifying device.
Description
Technical field
The present invention relates to the treatment process of waste liquid, the treatment process that contains production solvent waste liquid that is particularly produced in the meta-aramid fibers production process.
Background technology
Meeting generation water content only is 80% waste liquid in the tradition meta-aramid fibers production process, wherein contains the production solvent and the salt that are produced in the aramid fiber production process, and contained production solvent is a N,N-DIMETHYLACETAMIDE.If directly it is discharged in the environment, not only can serious environment pollution, also cause the huge waste of resource, therefore, must the low levels solvent in the solution be reclaimed.At present, domestic general treatment process is rectifying, yet even adopt rectification under vacuum, its energy consumption also is huge, and traditional recovery technology energy consumption situation sees Table-1.In addition, the partial solvent that contains in the residue can't thoroughly separate, and further caused the waste of resource and product cost to raise, and level of residue is big, and the processing costs of residue is up to nearly 1,000 yuan per ton.Simultaneously, because the salts contg in the solution causes very big corrosion up to 7% to rectifying device, seriously restricted the stability of rectifying operating system.
Table-1 traditional recovery technology energy consumption situation unit: production solvent per ton
| Steam consumption | Current consumption | Level of residue | The rate of recovery |
| 8.5 ton | ??1000kwh | 400 kilograms | ??92％ |
Summary of the invention
It is little that the technical problem to be solved in the present invention provides a kind of energy consumption, little to rectifying device corrosion, and what produced in the few meta-aramid fibers production process of processing costs contains the treatment process of producing the solvent waste liquid.
The treatment process that contains production solvent waste liquid that is produced in a kind of meta-aramid fibers production process, wherein, treating processes may further comprise the steps successively:
(1) filters the waste liquid of producing solvent that contains that is produced in the meta-aramid fibers production process, collect in the holder then;
(2) liquid of step (1) gained is sent into extraction plant and carry out extracting and separating, wherein extraction agent is selected from one or more in trichloromethane, isopropylcarbinol, methylene dichloride and the trieline, extraction is than being (1～3): 1, and waste water is directly discharged, and extraction phase is introduced in the holder;
(3) with the input of the extraction phase in step (2) holder distillation tower, extraction phase is carried out underpressure distillation to be separated, amount of filler accounts for 15～25% of distillation tower capacity, input speed per hour be the distillation tower capacity 8.4～16.8%, 80～120 ℃ of temperature, 130～150 ℃ of column bottom temperatures in the tower, quantity of reflux speed per hour is 1.7～8.5% of distillation tower capacity, and discharging speed per hour is 0.7～2.5% of a distillation tower capacity;
(4) the production solvent with step (3) gained carries out rectifying again, obtains qualified production solvent finished product, step (3) gained extraction agent is dropped into extraction plant recycle.
The treatment process that contains production solvent waste liquid that is produced in the meta-aramid fibers production process of the present invention, wherein, described production solvent is a N,N-DIMETHYLACETAMIDE.
The treatment process that contains production solvent waste liquid that is produced in the meta-aramid fibers production process of the present invention, wherein, described extraction plant is an extraction tower.
The treatment process that contains production solvent waste liquid that is produced in the meta-aramid fibers production process of the present invention, wherein, extraction tower is the rotating disc type packed extraction tower of adjustable speed, rotating speed is 10-50r/min.
The treatment process that contains production solvent waste liquid that is produced in the meta-aramid fibers production process of the present invention, wherein, distillation tower is the material filling type distillation tower.
The treatment process that contains production solvent waste liquid that is produced in the meta-aramid fibers production process of the present invention, wherein, amount of filler accounts for 17～23% of distillation tower capacity, input speed per hour be the distillation tower capacity 10～12.5%, 90～110 ℃ of temperature, 140 ℃ of column bottom temperatures in the tower, quantity of reflux speed per hour is 5% of distillation tower capacity, and discharging speed per hour is 1.4～2.0% of a distillation tower capacity.
The extraction phase of being mentioned in the application documents of the present invention is: the mixed solution of extraction agent and the material that need be extracted, extraction is than being: extraction agent and the volume ratio that contains the waste liquid of producing solvent.
Advantage of the present invention:
1, save energy, the present invention adopts in trichloromethane, isopropylcarbinol, methylene dichloride and the trieline one or more extract to produce solvent as extraction agent, and then the liquid of gained distilled and rectifying successively, water-content accounts for 80% in the waste liquid, be discharged from by extracting the most of water in back, power consumption process after not participating in is so present method can save energy reach more than 30%.
2, the present invention is little to the corrosion of rectifier unit, at first, the waste liquid after extraction treatment, salts contg reduces, so can reduce the corrosion of salt pair rectifying device.Secondly, although the boiling point of solvent and extraction agent differs bigger, but adopt the extraction agent that usually contains in the conventional isolated production solvent of separation method about 1 ‰-1%, thereby cause the subsequent production solvent again in the rectifying, equipment corrosion increases the weight of, problems such as increase of parking wash number and extraction agent consumption increase.The present invention controls in inlet amount, the tower temperature, column bottom temperature, quantity of reflux, load by strictness and makes and do not contain the production solvent in the isolated extraction agent, simultaneously, produces in the solvent and does not also contain extraction agent.
3, save energy of the present invention, and can reduce corrosion to rectifier unit, so can save a large amount of funds that dispose waste liquid.
Embodiment
Embodiment 1
The treatment process that contains production solvent waste liquid that is produced in this example meta-aramid fibers production process, treating processes may further comprise the steps successively:
(1) solvent N,N-DIMETHYLACETAMIDE waste liquid is produced in containing of being produced in the meta-aramid fibers production process, and the waste liquid composition sees Table-2, and waste liquid filters through filter, collects in the storage tank, sends into the rotating disc type packed extraction tower continuously by transferpump.
(2) start the rotating disc type packed extraction tower, adjust rotating speed, waste liquid enters in the tower continuously from the extraction tower below, adjusts flow; The extraction agent trichloromethane enters from the extraction tower top continuously, adjusts flow, and controlling both ratios is 1: 1, and rotating speed is 10r/min.Waste water after rotating disc type packed extraction tower extraction is directly discharged by extraction tower top overflow port, N,N-DIMETHYLACETAMIDE content 0.5% in this moment waste water, and salts contg reaches 9%, sees table-3 for details, and waste water can directly enter Sewage treatment systems, extraction phase introducing storage tank.
(3) with the liquid imported fill formula distillation tower in step (2) storage tank, extraction phase is carried out underpressure distillation separate, the volume of material filling type distillation tower is 60 cubic metres, amount of filler is 9 cubic metres, accounts for 15% of material filling type distillation tower capacity; Input speed is 5.02 cubic metres per hour, accounts for 8.4% of material filling type distillation tower capacity; 80 ℃ of temperature, 130 ℃ of column bottom temperatures in the tower; Quantity of reflux speed is 1.02 cubic metres per hour, accounts for 1.7% of material filling type distillation tower capacity; Discharging speed is 0.42 cubic metre per hour, accounts for 0.7% of material filling type distillation tower capacity; The content of impurity sees Table-4 in the isolated extraction agent trichloromethane.
By detecting proof: do not contain N,N-DIMETHYLACETAMIDE in the isolated extraction agent trichloromethane, simultaneously, also do not contain trichloromethane in the N,N-DIMETHYLACETAMIDE.
(4) the production solvent N,N-DIMETHYLACETAMIDE with step (3) gained carries out rectifying again, obtains qualified solvent N,N-DIMETHYLACETAMIDE, and the content of impurity sees Table-5 in the N,N-DIMETHYLACETAMIDE after the rectifying.The extraction agent trichloromethane input extraction plant of step (3) gained is recycled.
In the present embodiment, fully take into account the recycle of energy, the treatment process of embodiment 1, the situations such as production solvent N,N-DIMETHYLACETAMIDE steam consumption per ton, residue generation, the N,N-DIMETHYLACETAMIDE rate of recovery that obtain see Table-6.
Table-2 waste liquids are formed
| Title | Moisture | Salt | Specific conductivity |
| Waste liquid | ??80％ | ??7％ | ??12000μs/cm |
Table-3 waste water compositions of from extraction tower, discharging
| Title | N,N-DIMETHYLACETAMIDE | Salt | Specific conductivity |
| Waste water | ??0.5％ | ??9％ | ??15000μs/cm |
Solvent 0.5% in the waste water, and salts contg reaches 9%, can directly enter Sewage treatment systems.
The content of impurity in the trichloromethane after table-4 is handled through the material filling type distillation tower
| Title | Moisture | Salt | Specific conductivity |
| The content of impurity in the trichloromethane | ??0.1％ | Do not measure | ??0.1μs/cm |
The content of impurity in the N,N-DIMETHYLACETAMIDE after table-5 rectifying
| Title | Moisture | Salt | Specific conductivity |
| The content of impurity in the N,N-DIMETHYLACETAMIDE | ??0.1％ | Do not measure | Specific conductivity 0.8 μ s/cm |
Table 6 unit: get production solvent N,N-DIMETHYLACETAMIDE per ton
| Steam consumption | Current consumption | The residue generation | The N,N-DIMETHYLACETAMIDE rate of recovery |
| 5.5 ton | ??800kwh | 40 kilograms | ??＞98％ |
Embodiment 2
The treatment process that contains production solvent waste liquid that is produced in this example meta-aramid fibers production process, treating processes may further comprise the steps successively:
(1) solvent N,N-DIMETHYLACETAMIDE waste liquid is produced in containing of being produced in the meta-aramid fibers production process, and the waste liquid composition sees Table-7, and waste liquid filters through filter, collects in the storage tank, sends into the rotating disc type packed extraction tower continuously by transferpump.
(2) start the rotating disc type packed extraction tower, adjust rotating speed, waste liquid enters in the tower continuously from the extraction tower below, adjusts flow; The extraction agent trichloromethane enters from the extraction tower top continuously, adjusts flow, and controlling both ratios is 2: 1, and rotating speed is 30r/min.Waste water after rotating disc type packed extraction tower extraction is directly discharged by extraction tower top overflow port, N,N-DIMETHYLACETAMIDE content 0.5% in this moment waste water, and salts contg reaches 9%, sees table-8 for details, and waste water can directly enter Sewage treatment systems.Extraction phase is introduced storage tank.
(3) with the liquid imported fill formula distillation tower in step (2) storage tank, extraction phase is carried out underpressure distillation separate, the volume of material filling type distillation tower is 60 cubic metres, amount of filler is 12 cubic metres, accounts for 20% of material filling type distillation tower capacity; Input speed is 7.5 cubic metres per hour, accounts for 12% of material filling type distillation tower capacity; 100 ℃ of temperature, 140 ℃ of column bottom temperatures in the tower; Quantity of reflux speed is 3 cubic metres per hour, accounts for 5% of material filling type distillation tower capacity; Discharging speed is 0.96 cubic metre per hour, accounts for 1.6% of material filling type distillation tower capacity; The content of impurity sees Table-9 in the isolated extraction agent trichloromethane.
By detecting proof: do not contain N,N-DIMETHYLACETAMIDE in the isolated extraction agent trichloromethane, simultaneously, also do not contain trichloromethane in the N,N-DIMETHYLACETAMIDE.
(4) the production solvent N,N-DIMETHYLACETAMIDE with step (3) gained carries out rectifying again, obtains qualified solvent N,N-DIMETHYLACETAMIDE, and the content of impurity sees Table-10 in the N,N-DIMETHYLACETAMIDE after the rectifying.The extraction agent trichloromethane input extraction plant of step (3) gained is recycled.
In the present embodiment, fully take into account the recycle of energy, the treatment process of embodiment 1, the situations such as production solvent N,N-DIMETHYLACETAMIDE per ton institute steam consumption, residue generation, the N,N-DIMETHYLACETAMIDE rate of recovery that obtain see Table-11.
Table-7 waste liquids are formed
| Title | Moisture | Salt | Specific conductivity |
| Waste liquid | ??80％ | ??7％ | ??12000μs/cm |
Table-8 waste water compositions of from extraction tower, discharging
| Title | N,N-DIMETHYLACETAMIDE | Salt | Specific conductivity |
| Waste water | ??0.5％ | ??9％ | ??14000μs/cm |
Solvent 0.5% in the waste water, and salts contg reaches 9%, can directly enter Sewage treatment systems.
The content of impurity in the trichloromethane after table-9 is handled through the material filling type distillation tower
| Title | Moisture | Salt | Specific conductivity |
| The content of impurity in the trichloromethane | ??0.1％ | Do not measure | ??0.1μs/cm |
The content of impurity in the N,N-DIMETHYLACETAMIDE after table-10 rectifying
| Title | Moisture | Salt | Specific conductivity |
| The content of impurity in the N,N-DIMETHYLACETAMIDE | ??0.1％ | Do not measure | ??0.8μs/cm |
Table-11 units: get production solvent N,N-DIMETHYLACETAMIDE per ton
| Steam consumption | Current consumption | The residue generation | The N,N-DIMETHYLACETAMIDE rate of recovery |
| 5.5 ton | ??810kwh | 40 kilograms | ??＞98％ |
Embodiment 3
The treatment process that contains production solvent waste liquid that is produced in this example meta-aramid fibers production process, treating processes may further comprise the steps successively:
(1) solvent N,N-DIMETHYLACETAMIDE waste liquid is produced in containing of being produced in the meta-aramid fibers production process, and the waste liquid composition sees Table-12, and waste liquid filters through filter, collects in the storage tank, sends into the rotating disc type packed extraction tower continuously by transferpump.
(2) start the rotating disc type packed extraction tower, adjust rotating speed, waste liquid enters in the tower continuously from the extraction tower below, adjusts flow; The extraction agent trichloromethane enters from the extraction tower top continuously, adjusts flow, and controlling both ratios is 3: 1, and rotating speed is 50r/min.Waste water after rotating disc type packed extraction tower extraction is directly discharged by extraction tower top overflow port, N,N-DIMETHYLACETAMIDE content 0.3% in this moment waste water, and salts contg reaches 9%, sees table-13 for details, and waste water can directly enter Sewage treatment systems.Extraction phase is introduced storage tank.
(3) with the liquid imported fill formula distillation tower in step (2) storage tank, extraction phase is carried out underpressure distillation separate, the volume of material filling type distillation tower is 60 cubic metres, amount of filler is 15 cubic metres, accounts for 25% of material filling type distillation tower capacity; Input speed is 10.08 cubic metres per hour, accounts for 16.8% of material filling type distillation tower capacity; 120 ℃ of temperature, 150 ℃ of column bottom temperatures in the tower; Quantity of reflux speed is 5.1 cubic metres per hour, accounts for 8.5% of material filling type distillation tower capacity; Discharging speed is 1.5 cubic metres per hour, accounts for 2.5% of material filling type distillation tower capacity; The content of impurity sees Table-14 in the isolated extraction agent trichloromethane.
By detecting proof: do not contain N,N-DIMETHYLACETAMIDE in the isolated extraction agent trichloromethane, simultaneously, also do not contain trichloromethane in the N,N-DIMETHYLACETAMIDE.
(4) the production solvent N,N-DIMETHYLACETAMIDE with step (3) gained carries out rectifying again, obtains qualified solvent N,N-DIMETHYLACETAMIDE, and the content of impurity sees Table-15 in the N,N-DIMETHYLACETAMIDE after the rectifying.The extraction agent trichloromethane input extraction plant of step (3) gained is recycled.
In the present embodiment, fully take into account the recycle of energy, the treatment process of embodiment 1, the situations such as production solvent N,N-DIMETHYLACETAMIDE per ton institute steam consumption, residue generation, the N,N-DIMETHYLACETAMIDE rate of recovery that obtain see Table-16.
Table-12 waste liquids are formed
| Title | Moisture | Salt | Specific conductivity |
| Waste liquid | ??80％ | ??7％ | ??12000μs/cm |
Table-13 waste water compositions of from extraction tower, discharging
| Title | N,N-DIMETHYLACETAMIDE | Salt | Specific conductivity |
| Waste water | ??0.3％ | ??9％ | ??13000μs/cm |
Solvent 0.5% in the waste water, and salts contg reaches 9%, can directly enter Sewage treatment systems.
The content of impurity in the trichloromethane after table-14 is handled through the material filling type distillation tower
| Title | Moisture | Salt | Specific conductivity |
| The content of impurity in the trichloromethane | ??0.1％ | Do not measure | ??0.1μs/cm |
The content of impurity in the N,N-DIMETHYLACETAMIDE after table-15 rectifying
| Title | Moisture | Salt | Specific conductivity |
| The content of impurity in the N,N-DIMETHYLACETAMIDE | ??0.1％ | Do not measure | Specific conductivity 0.8 μ s/cm |
Table-16 units: get production solvent N,N-DIMETHYLACETAMIDE per ton
| Steam consumption | Current consumption | The residue generation | The N,N-DIMETHYLACETAMIDE rate of recovery |
| 5.5 ton | ??830kwh | 40 kilograms | ??＞98％ |
Above embodiment is described preferred implementation of the present invention; be not that scope of the present invention is limited; design under the prerequisite of spirit not breaking away from the present invention; various distortion and improvement that those of ordinary skills make technical scheme of the present invention all should fall in the definite protection domain of claims of the present invention.
Claims (6)
1. what produced in the meta-aramid fibers production process contains the treatment process of producing the solvent waste liquid, it is characterized in that treating processes may further comprise the steps successively:
(1) filters the waste liquid of producing solvent that contains that is produced in the meta-aramid fibers production process, collect in the holder then;
(2) liquid of step (1) gained is sent into extraction plant and carry out extracting and separating, wherein extraction agent is selected from one or more in trichloromethane, isopropylcarbinol, methylene dichloride and the trieline, extraction is than being (1～3): 1, and waste water is directly discharged, and extraction phase is introduced in the holder;
(3) with the input of the extraction phase in step (2) holder distillation tower, extraction phase is carried out underpressure distillation to be separated, amount of filler accounts for 15～25% of distillation tower capacity, input speed per hour be the distillation tower capacity 8.4～16.8%, 80～120 ℃ of temperature, 130～150 ℃ of column bottom temperatures in the tower, quantity of reflux speed per hour is 1.7～8.5% of distillation tower capacity, and discharging speed per hour is 0.7～2.5% of a distillation tower capacity;
(4) the production solvent with step (3) gained carries out rectifying again, obtains qualified production solvent finished product, step (3) gained extraction agent is dropped into extraction plant recycle.
2. the treatment process that contains production solvent waste liquid that is produced in the meta-aramid fibers production process as claimed in claim 1 is characterized in that described production solvent is a N,N-DIMETHYLACETAMIDE.
3. the treatment process that contains production solvent waste liquid that is produced in the meta-aramid fibers production process as claimed in claim 2 is characterized in that described extraction plant is an extraction tower.
4. the treatment process that contains production solvent waste liquid that is produced in the meta-aramid fibers production process as claimed in claim 3 is characterized in that described extraction tower is the rotating disc type packed extraction tower of adjustable speed, and rotating speed is 10-50r/min.
5. the treatment process that contains production solvent waste liquid that is produced in the meta-aramid fibers production process as claimed in claim 4 is characterized in that described distillation tower is the material filling type distillation tower.
6. the treatment process that contains production solvent waste liquid that is produced in the meta-aramid fibers production process as claimed in claim 5, it is characterized in that, amount of filler accounts for 17～23% of distillation tower capacity, input speed per hour be the distillation tower capacity 10～12.5%, 90～110 ℃ of temperature, 140 ℃ of column bottom temperatures in the tower, quantity of reflux speed per hour is 5% of distillation tower capacity, and discharging speed per hour is 1.4～2.0% of a distillation tower capacity.
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| CN102557347A (en) * | 2012-01-06 | 2012-07-11 | 江苏蓝星环保科技有限公司 | Method for treating aramid waste water |
| CN102838249A (en) * | 2012-10-05 | 2012-12-26 | 上海会博新材料科技有限公司 | Device for treating filtrate generated in washing process of para-aramid resin |
| CN103980145A (en) * | 2014-05-28 | 2014-08-13 | 深圳市灿森科技有限公司 | Recovery method of waste liquid in production process of salt-free m-aramid fiber |
| CN104003566A (en) * | 2014-05-28 | 2014-08-27 | 东莞市灿森新材料有限公司 | Method for recovering multi-component liquid waste in process of producing high-performance aramid fibrid |
| CN104003565A (en) * | 2014-05-28 | 2014-08-27 | 东莞市灿森新材料有限公司 | Method for recycling liquid waste containing multiple components in production of high performance aramid fiber |
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| FR2176488B1 (en) * | 1972-03-20 | 1975-03-21 | Inst Francais Du Petrole | |
| JP2003080001A (en) * | 2001-09-14 | 2003-03-18 | Kanegafuchi Chem Ind Co Ltd | Method for refining water-containing organic solvent |
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| CN102838249B (en) * | 2012-10-05 | 2014-02-19 | 上海会博新材料科技有限公司 | Device for treating filtrate generated in washing process of para-aramid resin |
| CN103980145B (en) * | 2014-05-28 | 2015-09-02 | 深圳市灿森科技有限公司 | The recovery method of waste liquid in a kind of not saliferous meta-aramid production process |
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| CN103980145A (en) * | 2014-05-28 | 2014-08-13 | 深圳市灿森科技有限公司 | Recovery method of waste liquid in production process of salt-free m-aramid fiber |
| CN105481650A (en) * | 2015-12-11 | 2016-04-13 | 烟台泰和新材料股份有限公司 | Separation and recovery method of aramid fibrid multicomponent solvent |
| CN105481650B (en) * | 2015-12-11 | 2017-08-22 | 烟台泰和新材料股份有限公司 | A kind of separation and recovery method of aramid fiber fibrid multicomponent solvent |
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