CN106943775B - Device and method for continuously separating solid phase from liquid phase in caprolactam distillation heavy residual liquid - Google Patents
Device and method for continuously separating solid phase from liquid phase in caprolactam distillation heavy residual liquid Download PDFInfo
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- CN106943775B CN106943775B CN201710288480.XA CN201710288480A CN106943775B CN 106943775 B CN106943775 B CN 106943775B CN 201710288480 A CN201710288480 A CN 201710288480A CN 106943775 B CN106943775 B CN 106943775B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D21/00—Separation of suspended solid particles from liquids by sedimentation
- B01D21/02—Settling tanks with single outlets for the separated liquid
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D21/00—Separation of suspended solid particles from liquids by sedimentation
- B01D21/003—Sedimentation tanks provided with a plurality of compartments separated by a partition wall
- B01D21/0033—Vertical, perforated partition walls
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D21/00—Separation of suspended solid particles from liquids by sedimentation
- B01D21/0039—Settling tanks provided with contact surfaces, e.g. baffles, particles
- B01D21/0045—Plurality of essentially parallel plates
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D21/00—Separation of suspended solid particles from liquids by sedimentation
- B01D21/009—Heating or cooling mechanisms specially adapted for settling tanks
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Abstract
The invention discloses a device and a method for continuously separating solid and liquid phases in caprolactam distillation heavy residual liquid, wherein the device comprises a settler, one side of the settler is provided with a feed inlet, the other side of the settler is provided with an overflow port, and the bottom of the settler is provided with a slag discharge port; the overflow port is connected with the clarifying liquid intermediate tank, and the slag discharge port is connected with the residue clarifying tank; the clarifying solution intermediate tank is connected to the caprolactam working procedure through a pipeline and a pump, and the clarifying solution intermediate tank is also connected with a caprolactam process water pipeline. The caprolactam process water is used for cleaning and diluting the clarified liquid and the residues, so that the continuous separation of caprolactam and oligomers in the caprolactam distillation heavy residual liquid and the cyclic utilization of the caprolactam process water are realized.
Description
Technical Field
The invention belongs to the technical field of chemical industry, relates to production of caprolactam, and particularly relates to a device and a method for continuously separating a solid phase from a liquid phase in heavy residual liquid of caprolactam distillation.
Background
The caprolactam distillation process is the last step in the refining of caprolactam. In the distillation process, high vacuum operation is adopted to reduce the boiling point of caprolactam, so that high-temperature polycondensation of caprolactam can be avoided, and simultaneously alkali is added into the distillation feed liquid to neutralize a small amount of organic acid possibly existing to form stable salts so as to be separated from caprolactam in distillation and reduce the content of volatile alkali in the product. However, the steam-heated heater tube inevitably has local overheating, and has caustic soda and moisture which are beneficial to caprolactam polymerization, so that the caprolactam polymerization is caused, solid particles are formed, in order to ensure that particles formed by the polymers and heavy components such as caustic soda added in the early stage can be smoothly discharged from the distillation tower, the evaporation capacity of the distillation tower is strictly controlled, and the volume flow of the distillation residual liquid is ensured to be 1.5-2.0 m3And h, analyzing that the solid content of the residual liquid is between 0.8 and 3.0 percent by weight, and the change of the concentration of the residual liquid is related to the control of the evaporation capacity of the distillation tower.
The conventional method is that the residual liquid is mixed with condensed water of a steam vacuum pump in a distillation process and a flash evaporation process and then directly pumped back to an ammonium sulfate process for use, so that crude oil which is an extraction phase of an extraction tower is obtained. The method has no treatment, only circulates for one circle in the ammonium sulfate crystallizer, part of polymer is discharged along with ammonium sulfate crystals, and the other part of polymer enters the stripping tower along with crude oil. The extraction tower has no problem in a short time, the production is normal, but the working condition of the extraction tower fluctuates greatly along with the long-time accumulation of polymers: firstly, the extract phase carries with the water phase; and secondly, the amount of the extracted water phase is small, the boundary level of the extracted tower cannot be ensured, and the extracted water phase is often accompanied by a large amount of particles, so that the turntable and the fixed disk are blocked. The fluctuation of the working condition of the extraction tower causes great fluctuation to the yield and the quality of the final product.
The same industry has more treatment methods for caprolactam distillation raffinate, and each method has the characteristics that:
1) and (3) carrying out batch distillation on the distillation residual liquid: namely, a plurality of stills are used, a certain amount of distillation residual liquid is put in, caprolactam is evaporated under high vacuum and then condensed and recovered, after a period of time, the stills are stopped after more impurities are left in the stills for cleaning, and the distillation residual liquid is treated by using another stills in the cleaning process. The method causes high labor intensity of workers, and intermittent operation is not favorable for stable production;
2) directly selling the distillation raffinate: under the condition of proper working conditions, the evaporation capacity of the distillation tower is increased as much as possible, the flow of the distillation raffinate is reduced, and then a little water is added to the distillation raffinate, and the distillation raffinate is sold to other manufacturers for purification. The method has low yield, the residual liquid pipeline is easy to block due to the small amount of the distilled residual liquid, and the distillation working condition is poor due to the frequent use;
3) intercepting by using a filter: mixing the distillation residual liquid with water, sending to an ammonium sulfate process, and filtering out water insoluble substances by using a filter, an active carbon bed layer, a filter cloth centrifuge and the like. By using different sizes of sand core funnel G4: 5-15 μm, G5: 2-5 μm, G6: <2 μm poor weight after filtration and drying of the heavy residue, it was found that G4 was significantly smaller in weight than G5 and G6, so that the diameter of water-insoluble particles was mostly below 5 μm, and thus ordinary mechanical filtration had little effect, and the filtration efficiency of a high-precision filter cloth centrifuge was too low;
4) physical sedimentation: the heavy distillation residue is stored in a storage tank, and after standing for a period of time, granular water insoluble substances are deposited at the bottom of the storage tank, clear liquid caprolactam on the upper layer is extracted for recycling, the settled particles in the storage tank increase, the storage tank is isolated after the clarification effect is reduced, and the heavy distillation residue is cleaned and replaced and then put into use after the particles are removed.
The caprolactam manufacturer has its own treatment of the caprolactam distillation residue, and whatever its effectiveness, at least the polymer in the caprolactam distillation residue is considered to be bad.
Disclosure of Invention
The invention aims to provide a device and a method for continuously separating a solid phase from a liquid phase in caprolactam distillation heavy residual liquid, which can realize the continuous separation of caprolactam and oligomers in the caprolactam distillation heavy residual liquid and the cyclic utilization of caprolactam process water.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows: a device for continuously separating solid and liquid phases in caprolactam distillation heavy residual liquid comprises a settler, wherein one side of the settler is provided with a feed inlet, the other side of the settler is provided with an overflow port, and the bottom of the settler is provided with a slag discharge port; the overflow port is connected with the clarifying liquid intermediate tank, and the slag discharge port is connected with the residue clarifying tank; the clarifying solution intermediate tank is connected to the caprolactam working procedure through a pipeline and a pump, and the clarifying solution intermediate tank is also connected with a caprolactam process water pipeline.
Furthermore, the feed inlet is connected with a caprolactam distillation heavy residual liquid pipeline, a valve is arranged at the position close to the feed inlet, and a branch pipe is arranged between the caprolactam distillation heavy residual liquid pipeline and the valve and is connected to a residue clarifying tank.
Furthermore, the settler is a high-efficiency settler, the interior of the settler is provided with an internal part, the top of the settler is provided with an explosion-proof membrane and a single exhalation valve, the bottom of the settler is of a conical structure, and the outside of the settler is provided with heat tracing equipment; the settler is also connected with a nitrogen pipeline.
In a preferred scheme, the internal member is an inclined plate, an orifice plate corrugated packing or a wire mesh packing, and a metal inclined plate is preferred.
Furthermore, a plurality of settlers are connected in series, the lower parts of two adjacent settlers are divided by a partition plate, and the tops of the partition plates are not in contact with the tops of the settlers.
Furthermore, the caprolactam process water pipeline is also connected with a flushing pipeline which is positioned between the slag discharging port and the residue clarifying tank and is close to the slag discharging port; the residue clarifying tank is connected to the caprolactam working procedure through a pipeline and a pump.
Furthermore, a slag discharge pipeline is arranged at the bottom of the clear liquid intermediate tank and connected to the residue clarifying tank, and a drain pipe is arranged at the top of the clear liquid intermediate tank.
The invention also relates to a method for continuously separating solid and liquid phases in caprolactam distillation heavy residual liquid by adopting the device, which comprises the following steps:
introducing the caprolactam distillation heavy residual liquid into a settler for sedimentation, controlling the temperature in the settler at 70-90 ℃, allowing settled clear liquid to enter a clear liquid intermediate tank through an overflow port for further sedimentation, introducing process water in a caprolactam process water pipeline into the clear liquid intermediate tank for diluting the clear liquid therein, and conveying the liquid in the clear liquid intermediate tank to a caprolactam working procedure.
Further, the volume ratio of the process water to the clear liquid in the clear liquid intermediate tank is 1-5: 1; the liquid level in the clear liquid intermediate tank is controlled to be 40-70% of the total volume of the clear liquid intermediate tank.
Furthermore, when the slag discharging port in the settler discharges slag, process water in a caprolactam process water pipeline is adopted to wash a pipeline between the slag discharging port and the residue clarifying tank, clarification is carried out after washing, and clarified liquid is also conveyed to a caprolactam working procedure.
The solid content of the caprolactam distillation heavy residual liquid is 0.8-1.5 wt%, the solid content of clear liquid obtained after sedimentation and clarification by the device and the process provided by the invention is reduced to be below 0.1%, the clear liquid is diluted by caprolactam process water, the solidification of high-concentration caprolactam or the heat loss of a jacket pipeline, a jacket pump and a heat tracing pipeline is avoided, and the diluted caprolactam water solution is directly sent back to a caprolactam working procedure for recycling.
And after solid phase at the bottom of the settler is collected, discharging the solid phase into a residue clarifying tank through a residue discharge port, flushing a pipeline and diluting caprolactam in the residue by using caprolactam process water, wherein clear liquid after the residue clarifying tank is subjected to standing clarification for a period of time can be sent back to a caprolactam working procedure for utilization, and when more solid phase exists in the residue clarifying tank, the solid phase is cleaned.
The separation of the solid phase in the distillation heavy raffinate is not the final object of the invention. The inventors have experimentally found that a significant intermediate layer was found after mixing the heavy distillate with water and benzene, which is very similar to the intermediate layer in the extracted column of a caprolactam plant. The solid phase in the separated distillation heavy residual liquid is mixed with water and benzene in different proportions and then is subjected to static culture, the middle layer is found to grow up to be white particles, the diameter of the white particles can be increased along with the lapse of time, the larger the solid phase proportion is, the larger the particle diameter is, the same as the beige particles discharged by the extraction tower, only the colors of the particles are different, namely, the polymer heavy in the distillation heavy residual liquid is the culprit of generation of the middle phase and crystals in the extraction tower, and the operation condition of the extraction tower is directly influenced.
According to the invention, after the distillation heavy residual liquid is subjected to primary separation, although the middle layer of the extraction tower is in intermittent existence, the granular crystal basically disappears and does not appear, so that the entrainment phenomenon in the benzene extraction phase of the extraction tower is obviously reduced, the removal of impurities in the extraction tower is promoted, and the method has a very important significance for improving the quality of the caprolactam product.
The caprolactam distillation tower has obvious change after the working condition of the extraction tower is changed, and the operation period of the most main distillation tower is prolonged. The previous caprolactam distillation tower is stopped and cleaned for 2-4 times every month, but after the working condition of the extraction tower is improved, the operation cycle of the caprolactam distillation tower is cleaned once every 52 days on average, and the longest operation cycle can reach 90 days. The extension of the operation period of the caprolactam distillation tower has a more obvious change that the solid content in the distillation heavy residual liquid is reduced to 0.8-1.5% by weight from the original 1.8-2.2% by weight.
Therefore, the removal of the solid phase in the caprolactam distillation heavy residual liquid is a virtuous cycle, which is not only beneficial to the continuous and stable operation of a caprolactam device, but also beneficial to the improvement of the quality of caprolactam products.
Drawings
FIG. 1 is a schematic view of the structure of the apparatus of the present invention
Detailed Description
The invention is further illustrated by the following examples, but the scope of the invention as claimed is not limited to the scope of the examples.
Example 1:
as shown in figure 1, the invention relates to a device for continuously separating solid and liquid phases in heavy residual liquid from caprolactam distillation, which comprises a settler 1, wherein one side of the settler is provided with a feed inlet 11, the other side of the settler is provided with an overflow port 12, and the bottom of the settler is provided with a slag discharge port 13; the overflow port is connected with the clarifying solution intermediate tank 2, and the slag discharge port 13 is connected with the residue clarifying tank 3; the clear liquid intermediate tank 2 is connected to the caprolactam working procedure 4 through a pipeline and a pump, and the clear liquid intermediate tank 2 is also connected with a caprolactam process water pipeline 5.
Furthermore, the feed inlet 11 is connected with a caprolactam distillation heavy residual liquid pipeline 6, a valve is arranged at the position close to the feed inlet, and a branch pipe 7 is arranged between the caprolactam distillation heavy residual liquid pipeline 6 and the valve and is connected to the residue clarifying tank 3. The process water contains solid phase, and is discharged into a residue clarifying tank for clarification through a branch pipe, and meanwhile, the process water is prevented from entering a settler to cause polymerization of caprolactam, so that more solid particles are formed. In addition, the added process water can dilute caprolactam in the residue clarifying tank, so that the caprolactam can be conveniently recycled in the caprolactam working procedure in the later period.
Further, the settler 1 is a high efficiency settler. The inner part is arranged inside the inner part. The top is provided with an explosion-proof membrane and a single exhalation valve to ensure the safety of the equipment. The bottom is a conical structure, which is convenient for solid phase sedimentation and collection. The heat tracing equipment is arranged outside the settler, so that the temperature of caprolactam can be controlled at 70-90 ℃, and crystallization of high-concentration caprolactam is avoided. The settler is also connected with a nitrogen pipeline 8, caprolactam in the settler is prevented from deteriorating by contacting with air through nitrogen sealing, and the nitrogen pipeline is also provided with a regulating valve which is a self-operated regulating valve.
Furthermore, the internal parts are inclined plates, orifice plate corrugated packing or wire mesh packing, preferably metal inclined plates, so that blockage is avoided, and cleaning is convenient.
Further, the settler 1 is formed by connecting a plurality of settlers in series, the lower part of each two adjacent settlers is divided by a partition plate, and the top of each partition plate is not in contact with the top of the settler 1. The clarification effect is improved by connecting a plurality of settlers in series.
Furthermore, the caprolactam process water pipeline 5 is also connected with a flushing pipeline 9 which is positioned between the slag discharging port 13 and the residue clarifying tank 3 and is close to the slag discharging port 13; the residue clarifying tank 3 is connected to the caprolactam step 4 by a pipe and a pump. The arrangement can prevent the pipeline from being blocked after deslagging; and the caprolactam in the residue can be diluted by process water.
Furthermore, a slag discharge pipeline is arranged at the bottom of the clarified liquid intermediate tank 2 and is connected to the residue clarifying tank 3, and settled residues enter the residue clarifying tank; the top of the clarifying solution intermediate tank is provided with an emptying pipe which is an atmospheric pressure tank.
Intermittently conveying the clear liquid in the residue clarifying tank to a caprolactam working procedure, conveying by a pump, and cleaning the solid phase in the residue clarifying tank when the solid phase concentration at the inlet of the pump reaches 1% by weight or the running time reaches 72 hours; the residue clarifying tank is a topless underground tank, so that solid residues are conveniently cleaned.
Example 2: the solid-liquid separation is carried out on the caprolactam distillation heavy residual liquid by adopting the device, and the evaporation capacity of a caprolactam distillation tower is controlled to ensure that the flow capacity of the caprolactam distillation heavy residual liquid reaches 1.5m3And h, analyzing the solid content of 0.8-1.2 wt%, introducing the heavy residual liquid into a settler for settlement, controlling the temperature in the settler to be 70-75 ℃, introducing settled clear liquid into a clear liquid intermediate tank through an overflow port for further settlement, introducing process water in a caprolactam process water pipeline into the clear liquid intermediate tank for diluting the clear liquid, and conveying the liquid in the clear liquid intermediate tank to a caprolactam process.
In the operation process, the volume ratio of process water to clear liquid in the clear liquid intermediate tank is 1-5: 1, so that the concentration of the mixed caprolactam water solution is controlled to be 20-50 wt%, and the caprolactam crystallization after the concentration is too high or the fresh desalted water is supplemented after the concentration is too low is avoided; the liquid level in the clear liquid intermediate tank is controlled to be 40-70% of the total capacity of the clear liquid intermediate tank, so that the overflow of slag when the liquid level is too low or the distillation weight of residual liquid is large is avoided.
In the operation process, when the slag discharging port in the settler discharges slag, process water in a caprolactam process water pipeline is adopted to wash a pipeline between the slag discharging port and a residue clarifying tank, clarification is carried out after washing, and clarified liquid is also conveyed to a caprolactam working procedure.
After stable operation for nearly two months, the average value of the solid content in clear liquid overflowing from the settling tank is 0.09 percent by weight, the entrainment condition does not occur under the working condition of the extraction tower, and the caprolactam distillation tower is not stopped and cleaned.
Comparative example 1:
in a certain 100 kt/year caprolactam device, heavy caprolactam distillation raffinate and part of process water are mixed and then directly conveyed back to the caprolactam device to recover caprolactam, but after a caprolactam extraction tower runs for a period of time, the working condition always easily fluctuates, an extract phase is entrained, a raffinate phase contains a large amount of particles, the rotating disc tower and a pipeline are very easily blocked, and the caprolactam extraction tower needs to be stopped for cleaning about 4 months. In addition, the operation period of the caprolactam distillation tower is obviously shortened during the fluctuation of the working condition of the extraction tower, the temperature difference between the upper part and the lower part of a silk screen demister of the caprolactam distillation tower is increased, the yield requirement cannot be met, the silk screen demister is stopped to check that a large amount of white powdery substances are attached to the silk screen demister, so that the pressure difference of the silk screen demister is increased, and the distillation tower is stopped for cleaning the primary silk screen demister about 7 days under the condition of ensuring the yield. In order to solve the problem of the operation period of the caprolactam distillation tower, a part of caprolactam distillation heavy raffinate is directly sold at the moment, the operation period of the caprolactam distillation tower is obviously increased, and the working condition of the extraction tower is also improved.
Comparative example 2:
the same 100 kt/year caprolactam plant as in comparative example 1 was supplemented with a 200m addition3The storage tank is used as a settling tank to recover clarified caprolactam after settling particulate matters in caprolactam heavy residual liquid, the solid content of the clarified caprolactam is reduced to about 0.3 percent, but the solid content of clarified caprolactam in clarified liquid is gradually increased after a period of settling, so that the operation period of a caprolactam distillation tower and the working condition of an extraction tower are influenced, the storage tank needs to be regularly cleaned, and the labor intensity is too high.
Compared with comparative examples 1 and 2, the residual liquid in distillation produced by the same caprolactam device of 100 kt/year is adopted in example 2, after the device and the method are implemented according to the invention, the solid content of the clarified caprolactam is stabilized below 0.1 percent by continuously clarifying the caprolactam residual liquid and discontinuously discharging slag, the operation period of a caprolactam distillation tower reaches about 60 days, and the continuous operation of an extraction tower also reaches more than 480 days, so that the operation period of the caprolactam distillation tower and the working condition of the extraction tower are not influenced basically.
Claims (8)
1. The device for continuously separating the solid phase from the liquid phase in the caprolactam distillation heavy residual liquid is characterized in that: comprises a settler (1), one side of the settler is provided with a feed inlet (11), the other side of the settler is provided with an overflow port (12), and the bottom of the settler is provided with a slag discharge port (13); the overflow port is connected with the clear liquid intermediate tank (2), and the slag discharge port (13) is connected with the residue clarifying tank (3); the clear liquid intermediate tank (2) is connected to the caprolactam working procedure (4) through a pipeline and a pump, and the clear liquid intermediate tank (2) is also connected with a caprolactam process water pipeline (5); the feed inlet (11) is connected with a caprolactam distillation heavy residual liquid pipeline (6), a valve is arranged at the position close to the feed inlet, and a branch pipe (7) is arranged between the caprolactam distillation heavy residual liquid pipeline (6) and the valve and is connected to the residue clarifying tank (3);
during the specific operation, introducing the caprolactam distillation heavy residual liquid into a settler for settlement, controlling the temperature in the settler to be 70-90 ℃, allowing settled clear liquid to enter a clear liquid intermediate tank through an overflow port for further settlement, introducing process water in a caprolactam process water pipeline into the clear liquid intermediate tank for diluting the clear liquid therein, and conveying the liquid in the clear liquid intermediate tank to a caprolactam process.
2. The apparatus of claim 1, wherein: the settler (1) is a high-efficiency settler, an internal part is arranged in the settler, an explosion-proof membrane and a single-breath valve are arranged at the top of the settler, the bottom of the settler is of a conical structure, and heat tracing equipment is arranged outside the settler; the settler is also connected with a nitrogen pipeline (8).
3. The apparatus of claim 2, wherein: the internal member is inclined plate, orifice plate corrugated filler or wire mesh filler.
4. The apparatus of claim 1, wherein: the settlers (1) are connected in series, the lower parts of every two adjacent settlers are divided by a partition plate, and the tops of the partition plates are not in contact with the tops of the settlers (1).
5. The apparatus of claim 1, wherein: the caprolactam process water pipeline (5) is also connected with a flushing pipeline (9) which is positioned between the slag discharging port (13) and the residue clarifying tank (3) and is close to the slag discharging port (13); the residue clarifying tank (3) is connected to the caprolactam working procedure (4) through a pipeline and a pump.
6. The apparatus of claim 1, wherein: the bottom of the clear liquid intermediate tank (2) is provided with a slag discharge pipeline which is connected to the residue clarifying tank (3), and the top of the clear liquid intermediate tank is provided with an emptying pipe.
7. The apparatus of claim 1, wherein: the volume ratio of the process water to the clear liquid in the clear liquid intermediate tank is 1-5: 1; the liquid level in the clear liquid intermediate tank is controlled to be 40-70% of the total volume of the clear liquid intermediate tank.
8. The apparatus of claim 1, wherein: when the slag discharging port in the settler discharges slag, process water in a caprolactam process water pipeline is adopted to wash a pipeline between the slag discharging port and a residue clarifying tank, clarification is carried out after washing, and clarified liquid is also conveyed to a caprolactam working procedure.
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| CN109173673A (en) * | 2018-10-25 | 2019-01-11 | 山东环达环保科技有限公司 | Tar slag-drip opening slag-draining device and exhaust gas treating method and device |
| CN110508038B (en) * | 2019-08-09 | 2024-03-12 | 浙江省天正设计工程有限公司 | Method and device for continuous liquid-solid separation of sulfuric acid solution containing imine series products |
| CN113716773A (en) * | 2021-08-10 | 2021-11-30 | 湖北三宁化工股份有限公司 | System and method for separating and crystallizing caprolactam residual liquid |
| CN115738477A (en) * | 2022-11-17 | 2023-03-07 | 科城精铜(广州)有限公司 | Copper rod rolling emulsion circulating system and method |
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| CN101069794A (en) * | 2007-03-22 | 2007-11-14 | 吉林市恒昌过滤机械有限公司 | Boron-ore-slurry solid-liquid separation method |
| CN102351380A (en) * | 2011-08-15 | 2012-02-15 | 浙江华建尼龙有限公司 | Method and device for treating caprolactam-containing waste water |
| CN105541044A (en) * | 2016-01-28 | 2016-05-04 | 中国天辰工程有限公司 | Method for treating caprolactam production wastewater |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101069794A (en) * | 2007-03-22 | 2007-11-14 | 吉林市恒昌过滤机械有限公司 | Boron-ore-slurry solid-liquid separation method |
| CN102351380A (en) * | 2011-08-15 | 2012-02-15 | 浙江华建尼龙有限公司 | Method and device for treating caprolactam-containing waste water |
| CN105541044A (en) * | 2016-01-28 | 2016-05-04 | 中国天辰工程有限公司 | Method for treating caprolactam production wastewater |
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