CN212334901U - Methanol synthesis alkene wastewater treatment recycling system - Google Patents
Methanol synthesis alkene wastewater treatment recycling system Download PDFInfo
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- CN212334901U CN212334901U CN202020266532.0U CN202020266532U CN212334901U CN 212334901 U CN212334901 U CN 212334901U CN 202020266532 U CN202020266532 U CN 202020266532U CN 212334901 U CN212334901 U CN 212334901U
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Abstract
The utility model discloses a methanol synthesis olefin wastewater treatment and recycling system, which comprises an oil separation tank, a solid removal device, a coalescence emulsion breaker, an oil-water separation tank and an adsorption column which are connected in sequence; the utility model discloses equipment is simple, and the play water oil content after this system handles is less than 5mg/L, and COD is less than 100mg/L, and entire system constitutes closed cycle, has reduced comprehensive application cost widely, and whole process does not have secondary pollution and produces, and the environmental protection is economy again, has good application prospect.
Description
Technical Field
The utility model belongs to the advanced wastewater treatment field especially relates to a methanol synthesis alkene wastewater treatment recycling system.
Background
With the economic development and the increasing demand of ethylene and propylene, resources such as naphtha and light diesel oil as olefin production raw materials face more and more serious shortage situations. Chemical routes to olefins from non-petroleum resources are beginning to be generally appreciated. The methanol-to-olefin (MTO) process is a chemical technology for producing low-carbon olefins by using coal-based or natural gas-based synthesized methanol as a raw material, and the perfection of the process technology has important significance for ensuring the stable supply of the low-carbon olefins.
The chemical reaction equation and the thermal effect for preparing ethylene and propylene by taking methanol as a raw material are as follows:
2CH3OH→C2H4+2H2O (ΔH=11.72KJ/mol，427℃)
3CH3OH→C3H6+3H2O (ΔH=30.98KJ/mol，427℃)
the main production system of the methanol-to-olefin device consists of a reaction-regeneration unit, a quenching-water washing unit and a stripping unit 3, and the process flow diagram is shown in figure 1. Liquid methanol from outside the device is gasified after heat exchange, gas-phase methanol is converted into mixed gas (reaction gas) taking hydrocarbon as a main product in a reactor under the action of a catalyst, the reaction gas is separated by cyclone to remove most of carried catalyst fine powder, then the mixed gas is sent to a quenching-washing unit for cooling and washing, and the mixed gas is further sent to a downstream device after residual catalyst and partial impurities are removed. The sewage of the quench tower and the water scrubber is discharged out of the device after sedimentation (oil removal, suspended matter removal) and steam stripping (oxygen-containing compound removal).
The discharged wastewater of the methanol-to-olefin device has larger water amount, and the stripping tower of most of the existing methanol-to-olefin devices only considers the stripping of oxygen-containing compounds, so that the contents of aromatic hydrocarbon and heavy hydrocarbon in the stripped and purified water are high, the COD is higher, and the contents of refractory organic matters and petroleum in the water are higher. Due to the limitation of the separation efficiency of the multi-stage cyclone separator, the strength of the catalyst and other problems, the concentration of catalyst dust in the reaction gas is quite high, and most of unseparated catalyst particles enter the quenching-washing unit along with the reaction gas. Most of unseparated catalyst particles are intercepted by quenching water in a quenching tower, participate in the circulation of the quenching water and are accumulated continuously, and part of the quenching water is pumped out and sent out for treatment, so that the solid content in the discharged quenching water is not lower. The superposition of three characteristics of high content of refractory organic matters and petroleum and high solid content determines that the biodegradability of discharged sewage is poor, so that the load of a sewage treatment plant is increased and the quality of discharged water is unstable. In addition, based on the characteristics of the process for preparing olefin from methanol, a large amount of water resources are consumed in the process, but in the actual situation, the problem of uneven distribution of water resources in China exists, so that the development of enterprises is limited to a certain extent. With the continuous development of the process for preparing the olefin from the methanol, the demand on water resources is also larger and the national protection on the water resources is also increased, so that the normal operation of the process for preparing the olefin from the methanol is difficult. Therefore, the method has an important effect on recycling the discharged sewage in the process of preparing the olefin from the methanol.
According to the principle of methanol conversion reaction, in combination with the solubility of organic matters in water, the organic matters in the wastewater are mainly oxygen-containing organic compounds, and meanwhile, some emulsified oils exist. According to chromatographic analysis, organic matters in the wastewater are oxygen-containing organic compounds, mainly water-miscible substances such as methanol, ethanol, acetaldehyde, isopropanol, acetone, butanone and the like, and COD in the wastewater is mainly emulsifying and soluble COD.
When sewage is treated, most of floating oil and catalyst in water are removed by oil removal precipitation and air floatation by enterprises, and then biochemical treatment and filtration are carried out, so that COD (chemical oxygen demand), ammonia nitrogen and phosphorus content and turbidity in the wastewater are effectively removed, the water replenishing requirement of the circulating water of the enterprises is met, and the water replenishing quantity of the circulating water is greatly reduced; in addition, the biochemical effluent can be sent to a synthesis gas production process, and the mode does not need to remove hydrocarbon and oxygen-containing compounds; excess water in the process can also be produced as 2-isopropyl ether by propylene etherification. Because olefin and water are continuously produced in the methanol-to-olefin process, excessive water is produced even if the water circulation in the device reaches a stable state. Therefore, technicians perform various treatments on the stripped wastewater, including precipitation, alkali adjustment, filtration, aeration and the like, so as to effectively remove COD in the wastewater. After pretreatment, under the action of an ultrafiltration membrane filtration system, colloid, particulate matters and suspended matters are removed from the pretreated wastewater. After the reverse osmosis membrane system removes corresponding soluble organic matters and inorganic ions, the treated water can better meet the water quality specifications corresponding to boiler water replenishing and circulating water replenishing, so that the whole reuse of byproduct water is realized, the integral water consumption of a methanol-to-olefin factory is greatly reduced, the olefin water consumption per ton of an enterprise which carries out zero-emission process design on wastewater at the present stage can be reduced to be below 3 tons, the national requirement on water resource protection is met, the production burden of the enterprise is reduced, and the method can also be better used for the methanol-to-olefin process
Chinese patent CN100355708C discloses a method for recovering and reusing water in a process for preparing olefin from oxygen-containing compound, which comprises the following steps: (1) supplying an oxygenate feed stream to a reactor; (2) contacting the oxygenate feed stream with a molecular sieve catalyst in a reactor to form an effluent stream comprising olefins and by-product water; (3) separating by-product water from the effluent stream as the quench bottoms stream; (4) separating the quench tower bottoms stream into a liquid hydrocarbon phase and an aqueous phase, wherein the aqueous phase comprises solid catalyst particles; (5) separating the aqueous phase into an overhead vapor stream and a bottoms fraction comprising solid particles; (6) the residue fraction is sent to a settling device to remove solid particles; (7) process quality water is recovered from the overhead stream.
Through the above steps, process quality water having a catalyst fine particle content of 0.5wt% or less, an alcohol content of 0.1wt% or less, a methanol content of <0.1wt%, an organic acid content of <0.1wt%, and an aromatic compound content of 0.01wt% or less can be obtained. In this patent it is also stated that the above-mentioned process quality water can be used for catalyst preparation, hydration of hydrocarbons, acetylene production or steam cracking. Although this patent provides some means for recovering and utilizing water from an oxygenate to olefins process, it does not mean that the water produced in an oxygenate to olefins process must be able to be recycled in its entirety as described in this patent, in other words, there is no mention of how water produced in an oxygenate to olefins process that is not recycled as described in this patent is treated.
Chinese patent CN101139118A discloses a process for treating wastewater containing methanol and dimethyl ether, which comprises the following steps: pressurizing waste water containing methanol and dimethyl ether, then exchanging heat with purified water at the bottom of a stripping tower, then entering the stripping tower, exchanging heat with a gas mixture such as methanol generated at the top of the stripping tower, entering a reflux tank, returning one part of the gas mixture serving as reflux to the top of the stripping tower, sending the other part of the gas mixture to the outside of the device or serving as a raw material of an MTO device, and sending purified water from the bottom of the stripping tower to the outside of the device after exchanging heat with the waste water containing methanol and dimethyl ether. The patent states that the total content of methanol and dimethyl ether in the obtained purified water can reach below 100ppm after the treatment by the process. This patent does not deal with whether the purified water contains other pollutants and how to further treat the purified water.
Chinese patent CN102050548A discloses a method for treating and recycling methanol-to-olefin process wastewater, which comprises the following steps: 1, after the material flowing out of the MTO reactor recovers heat through a waste heat boiler, cooling the material by using a separation tower and separating high-concentration MTO wastewater; 2. continuously cooling the material flowing out of the MTO reactor, obtaining a water phase at the bottom of the separation tower, and obtaining olefin gas at the top of the separation tower; the olefin gas is further purified by compression and water washing operations; 3. carrying out steam stripping treatment on water phases from the bottoms of the separation tower and the water scrubber, and cooling the water phase obtained from the bottom of the steam stripper by a tower bottom heat exchanger to obtain low-concentration MTO water; 4. homogenizing and adjusting low-concentration MTO water; 5. carrying out coagulating sedimentation treatment on the low-concentration MTO water after homogenization adjustment; 6. carrying out aerobic aeration treatment on the low-concentration MTO water subjected to the coagulating sedimentation treatment; 7. carrying out precipitation treatment on the aerobic aeration treatment effluent; 8. and (4) performing flocculation filtration treatment on the effluent after the precipitation treatment. According to the method for treating and recycling the process wastewater of the methanol-to-olefin, provided by the invention, most of water can be effectively utilized in the MTO production process, the actual discharged water amount only accounts for less than 20% of the water amount generated by the MTO reaction, and the rest water amount can be recycled. The recycling of sewage generated in the MTO production can not be thoroughly realized through a coagulating sedimentation-aerobic aeration-precipitating filtration process, the actual external drainage amount accounts for 20% of the water generated by the MTO reaction, and in addition, whether the water quality of external drainage contains other pollutants or not and how to further treat the external drainage do not exist, and the patent does not relate to the recycling of the sewage generated in the MTO production.
An enterprise treats the methanol-to-olefin oily wastewater by adopting a combined process of pretreatment, biological treatment and advanced treatment, wherein the pretreatment adopts advection oil separation, Cavitation (CAF) air flotation and Dissolved Air (DAF) air flotation, the biological treatment adopts an A/O process, and the advanced treatment adopts a Biological Aerated Filter (BAF). Oil substances in the wastewater of the MTO process mainly exist in the wastewater in the forms of floating oil, emulsified oil or dispersed oil, and the like, and the MBR process is adopted in the subsequent biochemical treatment, so that the requirement on the oil content in the wastewater is high. The process of horizontal flow type oil separating tank, cavitation air floatation and dissolved air floatation is adopted to remove floating oil, emulsified oil, dispersed oil, suspended matters with large specific gravity and impurities in water. After the two-stage air floatation treatment, the petroleum content of the effluent is reduced to be below 20mg/L, polyaluminium chloride (PAC) and Polyacrylamide (PAM) are added in front of the two-stage air floatation tanks, and emulsified oil in the wastewater is demulsified to enhance the air floatation effect. The biochemical part adopts hydrolytic acidification. The water inlet of the hydrolysis acidification tank adopts up-flow water distribution, and is fully contacted with the filler in the process of sewage rising, so that the contact area between the wastewater and microorganisms is increased, and the treatment efficiency is improved. The organic high molecular substance which is difficult to degrade and can inhibit biochemical is converted into a small molecular intermediate which is easy to degrade biochemically, so that the biodegradability of the sewage is improved. The aeration tank adopts plug flow type water distribution, and adopts an activated sludge method to carry out oxidative decomposition on most aerobic pollutants in the sewage. Aeration tank effluent flows automatically and gets into the MBR pond, uses the dull and stereotyped membrane to carry out filtration treatment, because the effect of holding back of membrane makes mud-water separation, and activated sludge flows back to the aeration tank and intakes the end, and MBR produces water and reaches primary reclaimed water quality standard, mainly used circulating water moisturizing technology. The biological method has high treatment investment cost and large occupied area.
SUMMERY OF THE UTILITY MODEL
To the problem that exists among the prior art, the utility model provides a processing recycling system of methyl alcohol synthetic alkene waste water, this system has not only realized getting rid of oil and COD in the waste water effectively, and entire system constitutes closed cycle moreover, has reduced comprehensive running cost widely, goes out water oil content and is less than 5mg/L after this system handles, and COD is less than 100 mg/L.
In order to achieve the purpose, the utility model adopts the following technical proposal:
the utility model relates to a processing recycling system of methyl alcohol synthetic olefin waste water, the system is including the oil removal groove that connects gradually, remove solid ware, coalescence emulsion breaker, oil-water separator jar and adsorption column.
The system comprises a methanol tank and a clean water tank, wherein the methanol tank and the clean water tank are respectively connected with the top end of the adsorption column.
The system comprises a water outlet tank, wherein the water outlet tank is connected with the bottom end of the adsorption column.
As the utility model discloses preferred technical scheme, the system still includes methyl alcohol recovery unit, methyl alcohol recovery unit is connected with the adsorption column bottom.
As the preferable technical proposal of the utility model, the methanol recovery device is provided with at least two sets of rectification recovery devices in parallel.
As the utility model discloses preferred technical scheme, first set of rectification recovery unit includes the desorption fluid reservoir, desorption fluid reservoir entry is connected with the adsorption column bottom, and the export is connected with first rectifying column.
As the preferred technical scheme of the utility model, first set of rectification recovery unit still includes the condenser, the condenser is connected with first rectification top of the tower end.
As the utility model discloses preferred technical scheme, second set rectification recovery unit includes the washing liquid jar, washing liquid jar entry is connected with the adsorption column bottom, and the export is connected with the second rectifying column.
As the preferred technical scheme of the utility model, the second set of rectification recovery unit still includes another condenser, another condenser is connected with second rectification top of the tower end.
As the preferred technical scheme of the utility model, the second rectifying column bottom goes out water and returns the clear water storage tank.
Compared with the prior art, the utility model discloses following beneficial effect has at least:
(1) the utility model provides a new treatment and recycling system for methanol-to-olefin wastewater, which solves the problems in the prior art and has simple equipment, the effluent oil content after the treatment by the system is less than 5mg/L, and the COD is less than 100 mg/L;
(2) the utility model discloses handle recycling system constitutes closed cycle, has reduced comprehensive application cost widely, and whole process does not have secondary pollution and produces, and the environmental protection is economic again.
Drawings
FIG. 1 is a connection diagram of a system for treating and recycling wastewater from olefin synthesis with methanol according to the present invention.
The present invention will be described in further detail below. However, the following examples are only simple examples of the present invention, and do not represent or limit the scope of the present invention, which is defined by the appended claims.
Detailed Description
The technical solution of the present invention is further explained by the following embodiments with reference to the accompanying drawings.
To better illustrate the present invention, facilitating the understanding of the technical solutions of the present invention, typical but not limiting embodiments of the present invention are as follows:
as shown in figure 1, the system for treating and recycling the methanol-to-olefin wastewater comprises an oil separating tank, a solid removing device, a coalescence demulsifying device, an oil-water separating tank and an adsorption column which are sequentially connected.
The methanol-synthesized olefin wastewater enters an oil separation tank to remove floating oil, the oil content of the wastewater after the floating oil removal is reduced to be below 100mg/L, and the COD is reduced to be below 50000 mg/L; the water discharged from the oil separation tank enters a solid removing device for solid removal, and the ss of the solid removing water is less than 5 mg/L; the water from the solid remover enters a coalescent emulsion breaker to break emulsion of emulsified oil, an emulsion breaking resin bed is arranged in the emulsion breaker, the oleophylic hydrophobicity of the high-temperature emulsion breaking resin DEMR is utilized to separate emulsified oil molecules from the water, and the oil molecules in the wastewater are automatically broken, captured and enriched to be collected on the surface of the resin. When oil molecules adsorbed on the resin reach a saturated state, the oil molecules are impacted by the flow of water, the enriched oil is automatically separated in the form of large oil drops, the separated large oil drops are automatically separated in an oil-water separator, and the deoiled resin is automatically subjected to the processes of demulsification, capture and enrichment; the water discharged from the emulsion breaker enters an oil-water separation tank for oil-water separation, the oil content of the water phase discharged water of the oil-water separation tank is 20-50 mg/L, and the COD is reduced to be less than 10000 mg/L; the water phase effluent of the oil-water separation tank enters an adsorption column to deeply remove oil and COD, and finally the oil content of the effluent is less than 5mg/L and the COD is less than 100 mg/L; after the adsorption column penetrates through the adsorption column, methanol is used for desorption and regeneration, the regenerated liquid enters a methanol recovery device, the methanol is recovered by utilizing a rectification recovery device, the recovered methanol returns to a desorption process for recycling, and the residual heavy component organic matters after the methanol is separated are recovered as fuel.
Example 1
The oil content of the methanol-to-olefin wastewater of a certain enterprise is 1000mg/L, and the COD is 454250 mg/L.
Step (1): firstly, the wastewater is subjected to advection separation to remove floating oil, the oil content of the wastewater after the floating oil is removed is reduced to 82mg/L, and the COD is reduced to about 48000 mg/L;
step (2): removing solids from the effluent obtained in the step (1), wherein SS (suspended solid) of the effluent after solid removal is less than 5 mg/L;
and (3): the effluent obtained in the step (2) enters a demulsifying device to perform demulsification on emulsified oil, the retention time of the wastewater in the demulsifying device is 40min, and the height-diameter ratio of a resin bed is 1.5;
and (4): and (4) allowing the water discharged from the emulsion breaker in the step (3) to enter a high-efficiency oil-water separator, wherein the retention time of the wastewater in the oil-water separator is 120min, and the height-diameter ratio of the oil-water separator is 0.5. The oil content of the water phase effluent of the oil-water separator is 50mg/L, and the COD is reduced to about 8000 mg/L;
and (5): deeply removing oil and COD (chemical oxygen demand) of the water phase effluent in the step (4) in an adsorption column, wherein the retention time of the wastewater in the adsorption column is 40min, the packing height-diameter ratio of an adsorption column material is 0.6, the oil content of the effluent of the adsorption column is less than 5mg/L, and the COD is less than 100 mg/L;
and (6): after the adsorption penetration, the adsorption column is desorbed and regenerated by methanol, the regenerated liquid is used for recovering the methanol by a rectification recovery device, the recovered methanol is returned to the desorption process for recycling, and the residual heavy component organic matters after the methanol separation are recovered as fuel.
Example 2
The oil content of the methanol-to-olefin wastewater of a certain enterprise is 490mg/L, and the COD is 327800 mg/L.
Step (1): firstly, the wastewater is subjected to advection separation to remove floating oil, the oil content of the wastewater after the floating oil is removed is reduced to 50mg/L, and the COD is reduced to about 48000 mg/L;
step (2): removing solids from the effluent obtained in the step (1), wherein SS (suspended solid) of the effluent after solid removal is less than 5 mg/L;
and (3): the effluent obtained in the step (2) enters a demulsifying device to perform demulsification on emulsified oil, the retention time of the wastewater in the demulsifying device is 30min, and the height-diameter ratio of a resin bed is 1.0;
and (4): and (4) allowing the water discharged from the emulsion breaker in the step (3) to enter a high-efficiency oil-water separator, wherein the retention time of the wastewater in the oil-water separator is 60min, and the height-diameter ratio of the oil-water separator is 0.8. The oil content of the water phase outlet water of the oil-water separator is 20mg/L, and the COD is reduced to about 5000 mg/L;
and (5): deeply removing oil and COD (chemical oxygen demand) of the water phase effluent in the step (4) in an adsorption column, wherein the retention time of the wastewater in the adsorption column is 60min, the packing height-diameter ratio of an adsorption column material is 2, the oil content of the effluent of the adsorption column is less than 5mg/L, and the COD is less than 100 mg/L;
and (6) after the adsorption penetration, desorbing and regenerating the adsorption column by using methanol, recovering the methanol from the regenerated liquid by using a rectification recovery device, returning the recovered methanol to the desorption process for recycling, and recovering the residual heavy component organic matters as fuel after the methanol is separated.
Example 3
The oil content of the methanol-to-olefin wastewater of a certain enterprise is 50mg/L, and the COD is 12500 mg/L.
Step (1): firstly, the wastewater is subjected to advection separation to remove floating oil, the oil content of the wastewater after the floating oil is removed is reduced to 30mg/L, and the COD is reduced to about 7500 mg/L;
step (2): removing solids from the effluent obtained in the step (1), wherein SS (suspended solid) of the effluent after solid removal is less than 5 mg/L;
and (3): the effluent obtained in the step (2) enters a demulsifying device to perform demulsification on emulsified oil, the retention time of the wastewater in the demulsifying device is 45min, and the height-diameter ratio of a resin bed is 1.2;
and (4): and (4) allowing the water discharged from the emulsion breaker in the step (3) to enter a high-efficiency oil-water separator, wherein the retention time of the wastewater in the oil-water separator is 90min, and the height-diameter ratio of the oil-water separator is 0.7. The oil-water separator has water phase effluent oil content of 20mg/L and COD lowered to about 2200 mgL;
and (5): deeply removing oil and COD (chemical oxygen demand) of the water phase effluent in the step (4) in an adsorption column, wherein the retention time of the wastewater in the adsorption column is 45min, the packing height-diameter ratio of an adsorption column material is 1, the oil content of the effluent of the adsorption column is less than 5mg/L, and the COD is less than 100 mg/L;
and (6): after the adsorption penetration, the adsorption column is desorbed and regenerated by methanol, the regenerated liquid is used for recovering the methanol by a rectification recovery device, the recovered methanol is returned to the desorption process for recycling, and the residual heavy component organic matters after the methanol separation are recovered as fuel.
The applicant states that the present invention is illustrated by the above embodiments, but the present invention is not limited to the above detailed process equipment and process flow, i.e. the present invention is not meant to be implemented by relying on the above detailed process equipment and process flow. It should be clear to those skilled in the art that any improvement of the present invention, to the equivalent replacement of each raw material of the present invention, the addition of auxiliary components, the selection of specific modes, etc., all fall within the protection scope and disclosure scope of the present invention.
Claims (10)
1. The system for treating and recycling the methanol synthesis olefin wastewater is characterized by comprising an oil separating tank, a solid removing device, a coalescence demulsifying device, an oil-water separation tank and an adsorption column which are sequentially connected.
2. The system of claim 1, wherein the system comprises a methanol tank and a clean water tank, each of which is connected to the top end of the adsorption column.
3. The system of claim 2, comprising a water outlet tank connected to the bottom end of the adsorption column.
4. The system of any one of claims 1-3, further comprising a methanol recovery unit coupled to the bottom end of the adsorption column.
5. The system of claim 4, wherein the methanol recovery unit is provided in parallel with at least two rectification recovery units.
6. The system as claimed in claim 5, wherein the first rectification recovery device comprises a desorption solution tank, an inlet of the desorption solution tank is connected with the bottom end of the adsorption column, and an outlet of the desorption solution tank is connected with the first rectification column.
7. The system of claim 6, wherein the first rectification recovery unit further comprises a condenser connected to an upper end of the first rectification column.
8. The system of claim 7, wherein the second rectification recovery unit comprises a water wash tank, an inlet of the water wash tank is connected with the bottom end of the adsorption column, and an outlet of the water wash tank is connected with the second rectification column.
9. The system of claim 8 wherein the second rectification recovery unit further comprises another condenser connected to the top end of the second rectification column.
10. The system of claim 9, wherein the bottom water from the second rectification column is returned to a clean water storage tank.
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| CN114380435A (en) * | 2021-12-24 | 2022-04-22 | 陕西聚泰新材料科技有限公司 | Online recovery process for lost organic phase of hydrometallurgy extraction separation system |
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| CN114380435A (en) * | 2021-12-24 | 2022-04-22 | 陕西聚泰新材料科技有限公司 | Online recovery process for lost organic phase of hydrometallurgy extraction separation system |
| CN114380435B (en) * | 2021-12-24 | 2023-06-27 | 陕西聚泰新材料科技有限公司 | Online recovery process for lost organic phase of hydrometallurgical extraction separation system |
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