The recovery method of many components waste liquid in a kind of high-performance aramid fiber production process
Technical field
The present invention relates to the recovery method of many components waste liquid in a kind of high-performance aramid fiber production process, be specifically related to the recovery method of the many components waste liquid in a kind of high-performance poly mpd-i fiber production process.
Background technology
In prior art, poly(isophthaloyl metaphenylene diamine) polymkeric substance is processed through neutralization, filtration and deaeration, by shower nozzle coagulation forming inside solidification liquid, again by drawing-off, washing, oven dry and sizing, the high-performance polyisophthaloyl metaphenylene diamide fibre finally obtaining, the intensity of high-performance polyisophthaloyl metaphenylene diamide fibre is very high, and its cross section is not regular circular or oval, but irregular broadband shape or waist beans shape.In the production process of high-performance polyisophthaloyl metaphenylene diamide fibre, can produce waste liquid, the moiety of waste liquid has: amide solvent, salt and dispersion agent etc., the component of the waste water that polyisophthaloyl metaphenylene diamide fibre production process produces is various, the component more complicated of waste water, to the recycling of its waste water and at present domestic and international rare its technology of introducing of recycle utilization.With general distillation technology, be difficult to each component separation totally, the needed energy consumption of sepn process is very high, and power consumption is serious, and very high to the processing cost of waste liquid, economic benefit is very low.Therefore, be necessary to improve.
Summary of the invention
The deficiency existing for prior art; the recovery method that the object of this invention is to provide many components waste liquid in a kind of high-performance aramid fiber production process, it reaches the object that can recycle, reduce production costs, protect production environment more to save the method for energy consumption.
To achieve these goals, the technical solution adopted in the present invention is.
A recovery method for many components waste liquid in high-performance aramid fiber production process, comprises the following steps:
Waste collection step, arrives waste liquor storage tank the many components waste collection in high-performance poly mpd-i fiber production process;
Neutralization procedure, in by pump, the waste liquid in waste liquor storage tank being passed to and basin, waste liquid and in and the neutralization of the neutralizing agent in basin, the pH value of waste liquid is transferred to 6.8~7.2;
Compression filtration step, in and waste liquid in basin through Filter Press, suspended substance filtration wherein totally, by pump delivery, arrive middle vessel;
Extraction step, waste liquid in middle vessel enters the bottom of the first tower by pump delivery, from the top of the first tower, according to the ratio of setting, carry extraction agent simultaneously, the filler with high mixed effect is filled in the first tower the inside, waste liquid and extraction agent mix fully in the first tower the inside, from extraction phase out at the bottom of tower, leave in the 4th basin
Concentration step, from the tower top of the first tower liquid out, is transported to vaporizer and carries out concentration, and what output reached that fiber production recycles requires the first finished product containing the calcium chloride of a small amount of glycerol;
Extraction agent is deviate from step, the mixed solution of the 4th basin enters the top of the second tower by pump delivery, in the second tower, carry out the processing of deviating from of extraction agent, from the top output of the second tower, reach the second finished product extraction agent that recycles requirement, extraction agent enters the 5th basin after by condenser condenses, the extraction agent of the 5th basin is the top to the first tower by pump delivery, recycles extraction agent;
Dehydrating step, the still bed material of the second tower, by the top of pump delivery to the three towers, carries out processed;
Rectification step, the kettle base solution of the 3rd tower, by the top of pump delivery to the four towers, carries out rectification process;
Finished product, amide solvent pure, polymerization-grade is from the top output of the 4th tower, amide solvent is by after the condenser condenses of tower top, and collection obtains the amide solvent finished product that can again put into production and recycle, and at the bottom of the still of the 4th tower, heavy component arrives waste water basin or burning disposal by pump delivery.
Further, in technical scheme, in described waste collection step, waste liquid includes 10~40% N,N-DIMETHYLACETAMIDEs, 5~20% calcium chloride or magnesium chloride, 0~10% glycerol or ethylene glycol, surplus is water.
Further, in technical scheme, in described neutralization procedure, neutralizing agent is selected calcium hydroxide or sodium hydroxide.
Further, in technical scheme, in described extraction step, extraction agent is selected chloroform, and from the top of the first tower, carrying the ratio of extraction agent is extraction agent: N,N-DIMETHYLACETAMIDE effective content=5~10:1 waste water.
Further, in technical scheme, in described extraction step, extraction agent is selected chloroform, and from the top of the first tower, carrying the ratio of extraction agent is extraction agent: N,N-DIMETHYLACETAMIDE effective content=6~8:1 waste water.
Further, in technical scheme, described extraction agent is deviate from step, and the second tower is selected the atmospheric distillation tower of mono-disperse, and the temperature of tower reactor is controlled at 105~120 degree, and the temperature of tower top is controlled at 60~80 degree by backflow.
Further, in technical scheme, described the 3rd tower is selected the vacuum still of mono-disperse, and the temperature of tower reactor is controlled at 115~130 degree, and the temperature of tower top is controlled at 60~80 degree, and vacuum degree control is at-0.07Mpa~-0.09Mpa.
Further, in technical scheme, described the 4th tower is selected the vacuum still of mono-disperse, and the temperature of tower reactor is controlled at 120~130 degree, and the temperature of tower top is controlled at 110~120 degree, and vacuum degree control is at-0.07Mpa~-0.09Mpa.
Adopt after said structure, the advantage that compared to the prior art the present invention had is: the present invention adopts and first extracts the way of distilling afterwards, by vaporizer, the tower top of the first tower liquid is out carried out to concentration simultaneously, can reach the requirement that fiber production recycles, solve common distillation and processed the high problem of energy consumption, reach the economic aim recycling, increase economic efficiency, reduce production costs, do not pollute the environment simultaneously, environmental protection and energy saving.
Accompanying drawing explanation
Below in conjunction with drawings and Examples, the present invention is further described.
Fig. 1 is schematic flow sheet of the present invention.
Embodiment
The following stated is only preferred embodiment of the present invention, does not therefore limit protection scope of the present invention.
Embodiment
A recovery method for many components waste liquid in high-performance aramid fiber production process, comprises the following steps:
Waste collection step, the many components waste collection in high-performance poly mpd-i fiber production process, to waste liquor storage tank, waste liquid includes 10~40% N,N-DIMETHYLACETAMIDEs, 5~20% calcium chloride or magnesium chloride, 0~10% glycerol or ethylene glycol, surplus is water;
Neutralization procedure, in by pump, the waste liquid in waste liquor storage tank being passed to and basin, waste liquid and in and the neutralization of the neutralizing agent in basin, neutralizing agent is selected calcium hydroxide or sodium hydroxide, the pH value of waste liquid is transferred to 6.8~7.2;
Compression filtration step, in and waste liquid in basin through Filter Press, suspended substance filtration wherein totally, by pump delivery, arrive middle vessel;
Extraction step, the waste liquid in middle vessel enters the bottom of the first tower by pump delivery, carry extraction agent from the top of the first tower according to the ratio of setting simultaneously; Extraction agent is selected chloroform, from the top of the first tower, carrying the ratio of extraction agent is extraction agent: N,N-DIMETHYLACETAMIDE effective content=5~10:1 waste water, wherein, carrying the preferred proportion scope of extraction agent is extraction agent: N,N-DIMETHYLACETAMIDE effective content=6~8:1 in waste water.The filler with high mixed effect is filled in the first tower the inside, and waste liquid and extraction agent mix fully in the first tower the inside, from extraction phase out at the bottom of tower, leaves in the 4th basin;
Concentration step, from the tower top of the first tower liquid out, is transported to vaporizer and carries out concentration, and what output reached that fiber production recycles requires the first finished product containing the calcium chloride of a small amount of glycerol;
Extraction agent is deviate from step, and the second tower is selected the atmospheric distillation tower of mono-disperse, and the temperature of tower reactor is controlled at 105~120 degree, and the temperature of tower top is controlled at 60~80 degree by backflow; The mixed solution of the 4th basin enters the top of the second tower by pump delivery, in the second tower, carry out the processing of deviating from of extraction agent, from the top output of the second tower, reach the second finished product extraction agent that recycles requirement, extraction agent enters the 5th basin after by condenser condenses, the extraction agent of the 5th basin is the top to the first tower by pump delivery, recycles extraction agent;
Dehydrating step, the 3rd tower is selected the vacuum still of mono-disperse, and the temperature of tower reactor is controlled at 115~130 degree, and the temperature of tower top is controlled at 60~80 degree, and vacuum degree control is at-0.07Mpa~-0.09Mpa; The still bed material of the second tower, by the top of pump delivery to the three towers, carries out processed;
Rectification step, the 4th tower is selected the vacuum still of mono-disperse, and the temperature of tower reactor is controlled at 120~130 degree, and the temperature of tower top is controlled at 110~120 degree, and vacuum degree control is at-0.07Mpa~-0.09Mpa; The kettle base solution of the 3rd tower, by the top of pump delivery to the four towers, carries out rectification process;
Finished product, amide solvent pure, polymerization-grade is from the top output of the 4th tower, amide solvent is by after the condenser condenses of tower top, and collection obtains the amide solvent finished product that can again put into production and recycle, and at the bottom of the still of the 4th tower, heavy component arrives waste water basin or burning disposal by pump delivery.
Below in conjunction with experimental data, further illustrate the present invention.
After waste liquid is processed by the first tower, its experimental data is as shown in table 1~3.
Waste liquid component is: containing N,N-DIMETHYLACETAMIDE 7% and calcium chloride 10%, experimental data is as shown in table 1.
Table 1
Waste liquid component is: containing N,N-DIMETHYLACETAMIDE 10%, calcium chloride 12% and glycerol 2%, experimental data is as shown in table 2.
Table 2
Waste liquid component is: containing N,N-DIMETHYLACETAMIDE 20% and calcium chloride 22%, experimental data is as shown in table 2.
Table 3
From above-mentioned data, can find out, ratio increase along with extraction agent, the direction that the data of extracting phase are become better, but too high ratio is also worthless, because too high ratio regular meeting causes the amount of de-extraction agent below to increase, energy consumption also just increases to some extent, conventionally extraction agent: N,N-DIMETHYLACETAMIDE effective content=5~10:1 in waste water; More preferably extraction agent: N,N-DIMETHYLACETAMIDE effective content=6~8:1 in waste water.
The present invention, for the separating treatment of mixed solution, processes the first tower extraction tower reactor mixed solution out respectively by the second tower, the 3rd tower and the 4th tower, its experimental data is as shown in table 4~6.
The second tower |
Inlet amount |
Tower reactor discharging |
Discharging data |
Tower top temperature |
Tower reactor temperature |
Reflux |
1 |
2500kg/h |
600kg/h |
DMAC:88.65%, |
68 |
117 |
200kg/h |
2 |
4500kg/h |
1000kg/h |
DMAC:85.26%, |
70 |
122 |
400kg/h |
Table 4
The 3rd tower |
Tower reactor discharging |
Discharging data |
Tower top temperature |
Tower reactor temperature |
Reflux |
Tower vacuum |
1 |
520kg/h |
Moisture content 150ppm |
74 |
120 |
50 |
-0.082mpa |
2 |
830kg/h |
Moisture content 260ppm |
86 |
127 |
80 |
-0.085mpa |
Table 5
Table 6
From the data of the 4th tower, can find out, the product water white transparency that the present invention obtains, and moisture is extremely low, the top standard of the quality product of solvent in colleague.Due in meta-aramid synthetic, the impact of moisture is very large, so the Disposal quality of solvent quality is closely related with the quality product of aramid fiber.
Above content is only preferred embodiment of the present invention, for those of ordinary skill in the art, according to thought of the present invention, all will change in specific embodiments and applications, and this description should not be construed as limitation of the present invention.