CN112678912A - Method for removing wax in quenching water for preparing olefin from methanol by extraction method - Google Patents
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Abstract
The invention relates to a method for removing wax in quenching water for preparing olefin from methanol by an extraction method. The method comprises the following steps: wastewater from a quench tower enters the top of an extraction tower after being pretreated, flows through a packing layer from top to bottom in the extraction tower, reaches a tower kettle and is discharged to obtain extracted wastewater; meanwhile, the extractant from the extractant storage tank is conveyed to the extractant heat exchanger through an extractant pump, is heated to be consistent with the temperature of the wastewater, enters the bottom of the extraction tower, is mixed with pulse compressed air, flows through the packing layer from bottom to top and reaches the top of the extraction tower. The extraction efficiency of the organic solvent on the wax can be greatly improved by utilizing the extraction tower, the highest aromatic hydrocarbon removal rate can reach 99%, and the use amount of the organic solvent is reduced; meanwhile, the extraction tower can realize continuous operation, the water production is stable, the process is simple, the cost of stopping and cleaning can be reduced, and the method is suitable for large-scale production processes.
Description
Technical Field
The invention relates to a method for removing wax in quenching water for preparing olefin from methanol by an extraction method, belonging to the fields of coal chemical industry and wastewater treatment.
Background
In recent years, the technology of Methanol To Olefin (MTO) is developed vigorously, and the technology of preparing low-carbon olefins such as ethylene and the like by using methanol as a raw material provides a new way for meeting the increasing demand of short-chain olefins. Most of the used raw material methanol comes from the coal chemical industry process, so the methanol is an important composition and extension of the coal chemical industry, and has important significance for developing the core technology of producing products such as ethylene, propylene and the like from non-petroleum resources and realizing clean utilization of coal. During the MTO reaction, trace amounts of high melting aromatics are produced with the desired product. During the operation of the system, waxy substances are solidified and separated out on components or equipment such as a tray, a heat exchanger and the like. The long-time accumulation of waxy materials can lead to the pressure drop of a water washing tower and a quench tower to rise, the heat exchange efficiency of a heat exchanger is reduced, the energy consumption is increased, and even a series of problems such as blockage of pipelines and heat exchangers cause influence on normal production.
At present, the solutions to the above problems mainly include: parking, dismounting and cleaning, injecting organic solvent for dissolving and cleaning, and modifying the structure of equipment and components. In the aspect of organic solvent dissolving and cleaning, patent CN102659497A discloses a water system of a methanol-to-olefin device and an online washing method thereof, and specifically, in the operation process, a single benzene ring aromatic hydrocarbon, medium-long chain alkane or gasoline is injected into the water system, so that the single benzene ring aromatic hydrocarbon, the medium-long chain alkane or the gasoline, oil sludge and wax form a flow dynamic mixture and are discharged out of the system, and blockage caused by adhesion and accumulation in the water system after condensation is avoided. However, in this method, the solvent is simply mixed and contacted with water, so that the amount of the extractant used is large and the extraction effect is limited. In the aspect of equipment improvement, patent CN104722155A discloses a methanol-to-olefin reaction gas washing system and method, wherein a superheating section is arranged to desuperheat the reaction gas from a methanol-to-olefin reaction device, so that the reaction gas quickly reaches a saturated state, and when entering a quench tower for quenching, solid particles of the catalyst are easily removed with quench water, thereby optimizing the removal effect of the catalyst and reducing the fouling of the tower plates.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a method for removing wax in quenching water for preparing olefin from methanol by an extraction method. The method is characterized in that an extraction tower is additionally arranged between a quenching tower and a separation tower in the process of preparing the olefin from the methanol, the wax in the quenching water of the olefin from the methanol is removed by utilizing an extraction technology, and a proper extracting agent is obtained by screening. The extraction efficiency of the organic solvent on the wax can be greatly improved by utilizing the extraction tower, the highest aromatic hydrocarbon removal rate can reach 99%, and the use amount of the organic solvent is reduced; meanwhile, the extraction tower can realize continuous operation, the water production is stable, the process is simple, the cost of stopping and cleaning can be reduced, and the method is suitable for large-scale production processes.
The invention adopts the following technical scheme:
a method for removing wax in quenching water for preparing olefin from methanol by an extraction method comprises the following steps:
after catalyst particles contained in wastewater from a quenching tower are removed through pretreatment, the temperature is 60-90 ℃, the wastewater enters the top of an extraction tower through a quenching water pump, flows through a packing layer from top to bottom in the extraction tower, reaches a tower kettle and is discharged to obtain extracted wastewater, and the temperature of the wastewater is 60-90 ℃; meanwhile, the extractant from the extractant storage tank is conveyed to an extractant heat exchanger through an extractant pump, is heated to be consistent with the temperature of the wastewater, enters the bottom of the extraction tower, is mixed with compressed air, flows through a packing layer from bottom to top, flows out of the extraction tower from the top of the extraction tower, passes through an extraction phase heat exchanger, and enters a post-treatment working section;
the compressed air is blown into the lower part of the extraction tower by an air compressor, and the pulse frequency is controlled by a gas pulse generator; the pulse period of the gas is 1-10s, the gas is introduced for 1-5 s/period, and the gas pressure is 0.1-0.3 MPa;
the ratio of the volume flow of the extracting agent to the volume flow of the waste water of the quenching tower is 0.5:200-10: 200;
the pretreatment is filtration, a ceramic membrane device is adopted, and the aperture of the ceramic membrane device is 0.1-1 mu m;
the packing layer is in the form of random packing or regular packing;
the extractant is preferably one or more of gasoline, zero diesel oil, n-octane, cyclohexane, xylene, methyl ethyl ketone, tetrachloroethylene, petroleum ether and the like;
the composition of the waste water contains 5-300mg/L of oily substances; the oily substance is aromatic hydrocarbon substance.
The oily substance comprises toluene, pentamethylbenzene, hexamethylbenzene, trimethylbenzene, 1, 2-diethyl-3, 4-dimethylbenzene, 2,3, 6-trimethylnaphthalene and 1, 4-dimethylnaphthalene.
The aromatic compound removal rate of the extracted wastewater is more than 90 percent;
the temperature of the extract phase at the outlet of the extract phase heat exchanger is reduced to normal temperature; or heating to 100-200 ℃, and then entering an extractant recovery tower for rectification separation.
The technological process for removing the wax in the quenching water for preparing the olefin from the methanol by the extraction method comprises an extraction tower, a pretreatment device, an extractant heat exchanger, an air compressor, a pulse controller and an extraction phase heat exchanger; wherein, the outlet of the pretreatment device is connected with the top of the extraction tower; the extractant heat exchanger and the pulse controller are respectively connected with the bottom of the extraction tower; the extraction phase heat exchanger is connected with the top of the extraction tower;
the extraction tower is a packed tower; the height of the filler is 1-10 m.
The invention has the substantive characteristics that:
a traditional methanol-to-olefin production line does not have special equipment for removing wax, and the main solution method is to stop production and clean the production line or inject a large amount of organic solvent into a quenching tower along with water.
The invention removes the wax in the quenching water of the methanol-to-olefin by adding the extraction tower and utilizing the extraction technology. The method directly introduces the quenching water in the quenching tower into a liquid-liquid pulse extraction tower, utilizes an organic extractant to extract and remove the wax in the quenching water, reduces the wax content to relieve or eliminate the wax separation influence, and enters a subsequent separation tower to realize a continuous reaction process.
Compared with the prior art, the invention has the following beneficial effects:
(1) the extraction operation adopted by the method can directly add the process flow into the original process, the inconvenience and loss of the original direct cleaning requiring shutdown are reduced through the extraction process, the extraction tower is easy to modify so as to realize continuous production, the extraction efficiency is high, the contact area is large, the use of organic solvents of the original cleaning method can be reduced, and the waste and loss generated by the shutdown cleaning operation are greatly reduced;
(2) the method adopts extraction tower equipment and has larger liquid-liquid contact area, so that the extraction efficiency can be improved, and the removal rate of aromatic substances in the quenching water can reach 99 percent to the maximum; compared with patent CN102659497A, the amount of solvent used is reduced.
Drawings
FIG. 1 is a block diagram of the process flow of the present invention.
Detailed Description
In order to better illustrate the invention and to facilitate the understanding of the technical solutions thereof, typical but non-limiting examples of the invention are as follows:
the wastewater produced in the process of preparing olefin from methanol contains 5-300mg/L of oily substances (oil components mainly comprise aromatic substances such as toluene, pentamethylbenzene, hexamethylbenzene, trimethylbenzene, 1, 2-diethyl-3, 4-dimethylbenzene, 2,3, 6-trimethylnaphthalene, 1, 4-dimethylnaphthalene and the like); after being cooled by the quenching tower, the temperature is reduced to 60-90 ℃.
The technological process designed by the method of the invention is shown in figure 1, and comprises an extraction tower, a pretreatment device, an extractant heat exchanger, an air compressor, a pulse controller and an extraction phase heat exchanger; wherein, the outlet of the pretreatment device is connected with the top of the extraction tower; the extractant heat exchanger and the pulse controller are respectively connected with the bottom of the extraction tower; the extraction phase heat exchanger is connected with the top of the extraction tower;
the extraction tower is a packed tower; the height of the filler is 1-10 m.
The mechanism of the extraction process is as follows: the extractant rise is mainly caused by the density difference between the extractant and the wastewater. After the water phase enters the tower body from the upper part, the water phase descends under the action of gravity due to high density; the extractant enters the extraction tower from the lower part, and rises due to the lower density of the extractant compared with the waste water phase, so that the extractant and the waste water phase form countercurrent contact in the extraction tower. Also in this process, the compressed gas disturbs the two counter-current phases, breaking up the droplets, causing sufficient contact between the two to promote the transfer of the oily substances from the waste water to the extractant.
Example 1
Quenching water with the temperature of 80 ℃ and the oil content of 174mg/L and the suspended matter content of 200mg/L are pretreated by a ceramic membrane with the aperture of 0.2 mu m, the suspended matter content of 0mg/L and the oil content are kept unchanged, the water enters the top of the extraction tower through a quenching water pump at the flow rate of 2L/h, and flows through a filler layer from top to bottom in the extraction tower; xylene as an extractant is conveyed to an extractant heat exchanger from an extractant storage tank at a flow rate of 10mL/h through an extractant pump, the temperature is raised to 80 ℃, and the xylene flows through a filler layer from bottom to top of the extraction tower. Air passes through an air compressor and is controlled by a pulse controller, the pulse period is 2s, the gas introduction time is 1 s/period, the pressure is 0.1MPa, and the air enters from the lower part of the extraction tower. Wherein the packing is phi 3 theta ring packing, the height of the packing layer is 1.0m, the diameter is 0.04m, and the quenching water is contacted with the dimethylbenzene in the extraction tower to complete the extraction. The extractant and the waste water are respectively discharged from the top of the extraction tower and the bottom of the extraction tower after contacting the extraction tower. The oil content of the first wastewater at the outlet of the tower bottom is measured to be 2.0mg/L, and the oil removal rate is 98.84 percent. Wherein the temperature of the extract phase is reduced to 20 ℃ by an extract phase heat exchanger and then enters a subsequent treatment process, and the extracted wastewater directly enters a subsequent production process for preparing olefin from alcohol.
Example 2
Quenching water with the temperature of 60 ℃, the oil content of 193mg/L and the suspended matter content of 240mg/L are pretreated by a ceramic membrane with the aperture of 0.2 mu m, the suspended matter content of 5mg/L and the oil content are kept unchanged, the water enters the top of the extraction tower through a quenching water pump at the flow rate of 800L/h, and flows through a filler layer from top to bottom in the extraction tower; cyclohexane as an extracting agent is conveyed to an extracting agent heat exchanger from an extracting agent storage tank at the flow rate of 2L/h through an extracting agent pump, the temperature is raised to 60 ℃, and the cyclohexane flows through a filling layer from bottom to top of the extracting tower. Air passes through an air compressor and is controlled by a pulse controller, the pulse period is 5s, the gas introduction time is 1 s/period, the pressure is 0.15MPa, and the air enters from the lower part of the extraction tower. Wherein the filler is a phi 38mm ladder ring filler, the height of the filler layer is 3.0m, the diameter is 0.8m, and the quenching water is contacted with cyclohexane in the extraction tower to complete the extraction. The extractant and the waste water are respectively discharged from the top of the extraction tower and the bottom of the extraction tower after contacting the extraction tower. The oil content of the wastewater at the bottom outlet of the tower was measured to be 10.5mg/L, and the oil removal rate was 94.57%. Wherein the temperature of the extract phase is reduced to 20 ℃ by an extract phase heat exchanger and then enters a subsequent treatment process, and the extracted wastewater directly enters a subsequent production process for preparing olefin from alcohol.
Example 3
Quenching water with the temperature of 70 ℃ and the oil content of 168mg/L and the suspended matter content of 180mg/L are pretreated by a ceramic membrane with the aperture of 0.2 mu m, the suspended matter content of 0mg/L and the oil content are kept unchanged, the water enters the top of the extraction tower through a quenching water pump at the flow rate of 800L/h, and flows through a filler layer from top to bottom in the extraction tower; the n-octane as the extractant is conveyed to the extractant heat exchanger from the extractant storage tank at the flow rate of 8L/h through the extractant pump, the temperature is raised to 70 ℃, and the n-octane flows through the packing layer from bottom to top of the extraction tower. Air passes through an air compressor and is controlled by a pulse controller, the pulse period is 6s, the gas introduction time is 2 s/period, the pressure is 0.2MPa, and the air enters from the lower part of the extraction tower. Wherein the filler is phi 12mm ceramic intalox saddle ring filler, the height of the filler layer is 5.0m, the diameter is 0.8m, and the quenching water and the normal octane are contacted in the extraction tower to complete the extraction. The extractant and the waste water are respectively discharged from the top of the extraction tower and the bottom of the extraction tower after contacting the extraction tower. The oil content of the wastewater at the outlet of the tower bottom is measured to be 1.0mg/L, and the oil removal rate is 99.39 percent. Wherein the temperature of the extract phase is raised to 130 ℃ by an extract phase heat exchanger and then the extract phase enters a subsequent treatment process, and the extracted wastewater directly enters a subsequent production process for preparing olefin by alcohol.
Example 4
Quenching water with the temperature of 90 ℃, the oil content of 173mg/L and the suspended matter content of 220mg/L are pretreated by a ceramic membrane with the aperture of 0.2 mu m, the suspended matter content of 0.1mg/L and the oil content are kept unchanged, the water enters the top of the extraction tower through a quenching water pump at the flow rate of 5000L/h, and flows through a filler layer from top to bottom in the extraction tower; the zero diesel oil as extractant is conveyed to the extractant heat exchanger by the extractant pump at a flow rate of 65L/h from the extractant storage tank, heated to 90 ℃, and flows through the packing layer from bottom to top from the bottom of the extraction tower. Air passes through an air compressor and is controlled by a pulse controller, the pulse period is 7s, the gas introduction time is 2 s/period, the pressure is 0.15MPa, and the air enters from the lower part of the extraction tower. Wherein the filler is phi 38mm ceramic Bell ring filler, the height of the filler layer is 10.0m, the diameter is 2m, and the quenching water is contacted with zero diesel oil in the extraction tower to complete the extraction. The extractant and the waste water are respectively discharged from the top of the extraction tower and the bottom of the extraction tower after contacting the extraction tower. The oil content of the wastewater at the outlet of the tower bottom is measured to be 2.3mg/L, and the oil removal rate is 98.70 percent. Wherein the temperature of the extract phase is reduced to 20 ℃ by an extract phase heat exchanger and then enters a subsequent treatment process, and the extracted wastewater directly enters a subsequent production process for preparing olefin from alcohol.
The invention is not the best known technology.
Claims (10)
1. A method for removing wax in quenching water for preparing olefin from methanol by an extraction method is characterized by comprising the following steps:
after catalyst particles contained in wastewater from a quenching tower are removed through pretreatment, the temperature is 60-90 ℃, the wastewater enters the top of an extraction tower through a quenching water pump, flows through a packing layer from top to bottom in the extraction tower, reaches a tower kettle and is discharged to obtain extracted wastewater, and the temperature of the wastewater is 60-90 ℃; meanwhile, the extractant from the extractant storage tank is conveyed to an extractant heat exchanger through an extractant pump, is heated to be consistent with the temperature of the wastewater, enters the bottom of the extraction tower, is mixed with compressed air, flows through a packing layer from bottom to top, flows out of the extraction tower from the top of the extraction tower, passes through an extraction phase heat exchanger, and enters a post-treatment working section;
the compressed air is blown into the lower part of the extraction tower by an air compressor, and the pulse frequency is controlled by a gas pulse generator; the pulse period of the gas is 1-10s, the gas is introduced for 1-5 s/period, and the gas pressure is 0.1-0.3 MPa;
the ratio of the volume flow of the extracting agent to the volume flow of the waste water of the quenching tower is 0.5:200-10: 200.
2. The method for removing the wax in the quenching water for preparing the olefin from the methanol by the extraction method as claimed in claim 1, wherein the pretreatment is filtration, and a ceramic membrane device is adopted, and the aperture of the ceramic membrane device is 0.1-1 μm.
3. The method for removing wax from quenching water of methanol-to-olefin according to claim 1, wherein the packing layer is in the form of random packing or structured packing.
4. The method for removing the wax in the quenching water for preparing the olefin from the methanol by the extraction method as claimed in claim 1, wherein the extraction tower is a packed tower; the height of the filler is 1-10 m.
5. The method for removing the wax in the quenching water for preparing the olefin from the methanol by the extraction method as claimed in claim 1, wherein the extracting agent is preferably one or more of gasoline, zero-grade diesel oil, n-octane, cyclohexane, xylene, methyl ethyl ketone, tetrachloroethylene, petroleum ether and the like.
6. The method for removing wax in quenching water for preparing olefin from methanol by extraction as claimed in claim 1, wherein the composition of the wastewater contains 5-300mg/L of oily substances; the oily substance is aromatic hydrocarbon substance.
7. The method for removing wax from quenching water of olefin production from methanol by extraction as claimed in claim 6, wherein the oily substances include toluene, pentamethylbenzene, hexamethylbenzene, trimethylbenzene, 1, 2-diethyl-3, 4-dimethylbenzene, 2,3, 6-trimethylnaphthalene and 1, 4-dimethylnaphthalene.
8. The method for removing the wax in the quenching water for preparing the olefin from the methanol by the extraction method as claimed in claim 1, wherein the removal rate of the aromatic hydrocarbon compounds in the extracted wastewater is more than 90 percent.
9. The method for removing the wax in the quenching water for preparing the olefin from the methanol by the extraction method as claimed in claim 1, wherein the temperature of the extract phase at the outlet of the extract phase heat exchanger is reduced to normal temperature; or heating to 100-200 ℃, and then entering an extractant recovery tower for rectification separation.
10. The process flow of the method for removing the wax in the quenching water for preparing the olefin from the methanol by the extraction method as claimed in claim 1, which is characterized by comprising an extraction tower, a pretreatment device, an extractant heat exchanger, an air compressor, a pulse controller and an extraction phase heat exchanger; wherein, the outlet of the pretreatment device is connected with the top of the extraction tower; the extractant heat exchanger and the pulse controller are respectively connected with the bottom of the extraction tower; the extraction phase heat exchanger is connected with the top of the extraction tower.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1117700A1 (en) * | 1998-07-30 | 2001-07-25 | 3M Innovative Properties Company | Process and apparatus for removing impurities from polymers |
| CN110724024A (en) * | 2018-07-16 | 2020-01-24 | 中国石油化工股份有限公司 | Method and device for removing wax from MTO product gas |
| CN210078897U (en) * | 2019-05-07 | 2020-02-18 | 山东莱威新材料有限公司 | A tetrachloroethylene extraction device for production of ultra high molecular weight polyethylene fiber |
-
2020
- 2020-12-28 CN CN202011580436.4A patent/CN112678912A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1117700A1 (en) * | 1998-07-30 | 2001-07-25 | 3M Innovative Properties Company | Process and apparatus for removing impurities from polymers |
| CN110724024A (en) * | 2018-07-16 | 2020-01-24 | 中国石油化工股份有限公司 | Method and device for removing wax from MTO product gas |
| CN210078897U (en) * | 2019-05-07 | 2020-02-18 | 山东莱威新材料有限公司 | A tetrachloroethylene extraction device for production of ultra high molecular weight polyethylene fiber |
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