CN101633600A - Method and device for enriching and recovering methyl chloride by membrane separation method - Google Patents
Method and device for enriching and recovering methyl chloride by membrane separation method Download PDFInfo
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Abstract
The invention relates to a method and a device for enriching and recovering methyl chloride by a membrane separation method, belonging to the technical field of tail gas treatment. In the process, mixed gas enters a compression condensing system at certain pressure and temperature, partial methyl chloride is recovered after the mixed gas is compressed and condensed, aerial fog droplets in the residual tail gas are removed through a multi-level precision filter at 1.0 to 1.3Mpa, the mixed gas is heated to about 5 DEG C to 20 DEG C in a heater, the pretreated mixed gas keeps away from dew points and enters a membrane separator, enriched methyl chloride obtained at the infiltration side of the membrane separator returns to the compression system for pressurized circulation, and components of gas at the infiltration side mainly comprise intercepted nitrogen, methane, and the like and enter other tail gas treating devices. The recovery method has wide adaptability for the content of methyl chloride in industrial waste gas, small lumpy investment, high recovery rate of more than 95 percent and safety, thereby being especially suitable for middle and small enterprises.
Description
Technical field
The present invention relates to a kind of method and device, more specifically say it is that a kind of the coupling with membrane separation unit and compression system, shallow cooling system, strainer and well heater reclaimed the method for methyl chloride by enriching and recovering methyl chloride in the mixed gas that contains methyl chloride.Can relate to the recovery of condensable gases molecule such as many carbon hydrocarbon etc.
Background technology
Methyl chloride and the numerous many carbon hydrocarbon similar to it are important organic synthesis intermediates, are widely used in aspects such as agricultural chemicals, synthetic rubber, resin, industrial auxiliary agent, and they are mainly used to the very high fine chemical product of production economic worth.In addition can also be as the organic solvent in the industrial production, quite a few finally is drained in the atmosphere with the form of organic exhaust gas in these solvents, and the volatile organic matter in the waste gas has toxicity mostly.Organic exhaust gas, particulate (dust), SO
2, NO
XBe listed as four big air pollutant, wherein organic exhaust gas quantity discharged portion in several air pollutant is bigger, and this had both greatly wasted resource, had polluted environment again.Along with the progressively raising of people's living standard and the enhancing gradually of environmental protection consciousness, the recycling paid more and more attention of organic exhaust gas.From the organic exhaust gas of industrial discharge, reclaim organic solvent, both can reduce pollution, reclaimed resource again, created economic benefit environment.The industry that organic solvent is used is very wide, and kind is a lot, is very important so select suitable recovery method.By correct selection with make up existing recovery technology, can reclaim organic solvent more effective, more economically.
In recent ten years, develop condensation method, absorption method and absorption process both at home and abroad and reclaimed the methyl chloride technology.Wherein condensation method generally is the temperature that reduces volatile gases by the method for multistage continuous cooling emission gases, make it cohesion and reclaimed for liquid, its step is generally precooling, mechanical refrigeration, liquid nitrogen refrigerating and waits and realize, but shortcoming is the flow process complexity, energy consumption is bigger, and running cost is higher.The principle comparative maturity of absorption method Separation and Recovery organic gas, adsorption separation process is to utilize in the mixture difference of bonding force power between each component and sorbent material, and promptly each component distributes different character to make the isolating technology of difficult absorbed component in the mixture between sorbent material and fluid.It will select suitable sorbent material, make it have very high adsorption selectivity to organic gas, absorption method rate of recovery high exhaust gas emission concentration is low, but equipment is huger, and output investment ratio is higher, complex process, and device needs frequent the switching, complicated operation, turndown ratio is little, needs the periodic replacement sorbent material.Absorption process is to utilize the difference of mixed gas solubleness in solvent, absorb the technology that organic gas is realized recovery by dissolving, obviously the quality of absorbent properties often becomes the key that absorbs the operating effect quality, because very high to the performance requriements of absorption agent, thus also to a certain degree restriction absorb the application of recovery technology.
The mixed tail gas that contains methyl chloride, methyl alcohol and methylal to producing in the glyphosphonic acid production process is disclosed in the patent documentation of publication number CN1446782A, CN1629111A and CN1639112A, respectively by the pressurization condensation method, with organic solvent absorb methyl chloride method, with solid-state water absorbent reduce water-content method, impurity and hydrogenchloride are shown and the method for transformation etc. that partly or entirely changes into methyl chloride carries out the treatment process of Separation and Recovery, all have above-mentioned similar problem.
Summary of the invention
At the above-mentioned deficiency of prior art, provided by the present inventionly be that technology is simple, facility compact, energy consumption is less, running cost is low, process cost is low, the payback period is short, floor space is little, non-secondary pollution reclaims beneficial good methyl chloride recovery method.
Membrane separation process of the present invention reclaims the methyl chloride processing method and device comprises following system: compression system, shallow cooling system, multistage accurate filtering system, heating system and film separating system.Mixed gas has not only been removed drop and the aerosol that membrane module is polluted after overdraft, condensation, filtration and heating like this, also will reach the temperature and pressure scope that makes membrane separation apparatus performance maximum utility.
Removal process of the present invention can have following step to finish: 1. mixed gas enters compression system under certain pressure and temp, and gas is compressed into the certain pressure scope; 2. the mixed gas that comes out from compression system enters in the shallow cooling system and is condensed, and most methyl chloride and aqueous vapor are condensed recycling; 3. all the other condensation tail gas are introduced in the multistage accurate filter, have removed part drop and the aerosol that membrane module is polluted at this; 4. condensation tail gas enters heater heats to certain temperature range subsequently, removes remainder drop and aerosol; 5. the tail gas after being heated is incorporated in the membrane separation apparatus, obtains the enrichment methyl chloride gas in per-meate side and returns the compression system recovery that circulates, and removes other exhaust gas processing devices and be mainly components such as the nitrogen that is trapped, methane at retentate side gas.
With enriching and recovering methyl chloride in the refining cat head tail gas of organosilane monomer synthesis unit methyl chloride is example, and the technical solution used in the present invention is: the tail gas that the refining cat head of organosilane monomer synthesis unit methyl chloride gives off enters compression system and boosts to about 1.0～1.30MPa under certain pressure and temp; Mixed gas enters shallow cooling system under this pressure range, most of methyl chloride and aqueous vapor condensation are reclaimed; All the other tail gas are removed mist drop in the gas through multistage accurate filter, enter subsequently to be heated in the well heater about 5～20 ℃, and pretreated tail gas enters membrane separation apparatus away from dew point; At per-meate side acquisition enrichment methyl chloride, pressure is about 0.2MPa to gas at this moment by dissolving-diffusion-steps such as parsing, returns the compression system recovery that circulates; Retentate side gas is mainly components such as the nitrogen that is trapped, methane and removes other exhaust gas processing devices.
As the preferred technical solution of the present invention, the preferred organic vapor film separator of above-mentioned membrane separation apparatus.Mixed gas is compressed into the certain pressure scope in compression system, the preferred 1.0～1.3MPa of this pressure range.Condensation tail gas enters heater heats to certain temperature range, preferred 5～20 ℃ of this temperature range.
Characteristics of the present invention are: use pretreatment units such as compression, condensation, heating to make membrane module performance maximum utility; Utilize the selection perviousness difference of membrane separation apparatus to all gases, by dissolving-diffusion-steps such as parsing, to the polycomponent mixed gas separate, purification and enrichment, thereby reach isolating purpose.This apparatus structure is simple, the level of automation height, and running cost is cheap; And the treatment capacity that has added behind this device is increased to present 945.8Nm3/h by original 337.9Nm3/h; Separating effect is remarkable, and the rate of recovery of methyl chloride has reached more than 95%.
Description of drawings
Fig. 1 is the process flow sheet of enriching and recovering methyl chloride by membrane separation method
Explanation among Fig. 1:
1-compression system A-contains methyl chloride tail gas
The shallow cooling system B-of 2-condensation methyl chloride
3-strainer C-enrichment methyl chloride
The 4-well heater
The 5-membrane separation apparatus
Embodiment
Below in conjunction with drawings and Examples technology of the present invention is further elaborated.
As shown in Figure 1, the concrete technology of the present invention is provided with the compression decorum (1), shallow cooling system (2), strainer (3), well heater (4), membrane separation apparatus (5) from left to right successively.
The connection situation of each several part is as follows among the figure: the inlet end of compression system (1) is connected with the refining cat head tail gas discharging pipe of organosilicon synthesis unit methyl chloride, compression system (1) outlet side is connected with the inlet end of shallow cooling system (2), the outlet side of shallow cooling system (2) is connected with the inlet end of strainer (3), the outlet end of shallow cooling system (2) is connected with the methyl chloride withdrawing can, the outlet side of strainer (3) is connected with the inlet end of well heater (4), the outlet side of well heater (4) is connected with the inlet end of membrane separation apparatus (5), the per-meate side outlet of membrane separation apparatus (5) is connected with the inlet end of compression system (1), and the retentate side outlet of membrane separation apparatus (5) is connected with other exhaust gas processing devices.
The operating mode table of the refining cat head tail gas of table 1. organosilicon synthesis unit methyl chloride
Form the mixed gas by the refining tower top discharge of organosilicon synthesis unit methyl chloride as shown in table 1, adopt following scheme to test respectively, with methyl chloride and other components contents in the gas chromatograph analytical gas.
As shown in Figure 1, first embodiment of the invention: methyl chloride content is the refining cat head tail gas A of 13.290% organosilicon synthesis unit methyl chloride after entering compression system (1) under the 0.861MPa pressure and being compressed to 1.03MPa, gas B after the compression enters shallow cooling system (2) condensation and reclaims most of methyl chloride liquid and enter the methyl chloride withdrawing can, remaining gas enters multistage accurate filter (3) and removes wherein aerosol droplets, enter subsequently to be heated in the well heater (4) and remove the residue aerosol droplets about 12 ℃, pretreated gas C enters membrane separation apparatus (5) away from cloud point; Gas goes circulation recovery in the compression system (1) by dissolving-diffusion-steps such as parsing at the per-meate side enriching and recovering methyl chloride E of membrane separation apparatus (5), and entering other exhaust gas processing devices at the retentate side gas D of membrane separation apparatus (5), its main component is for being trapped components such as nitrogen, methane.The rate of recovery of methyl chloride is 96.7% after testing.Its material balance table is as follows:
Material balance table (mol%)
| Item | ??A | ??B | ??C | ??D | ??E |
| ??CH3Cl | ??13.29 | ??12.097 | ??12.097 | ??3.679 | ??16.034 |
| ??N2 | ??55.13 | ??40.421 | ??40.421 | ??61.33 | ??30.538 |
| ??CH4 | ??7.17 | ??6.649 | ??6.649 | ??7.976 | ??6.022 |
| ??C2H4 | ??2.63 | ??4.714 | ??4.714 | ??3.084 | ??5.485 |
| ??C2H6 | ??14.51 | ??26.000 | ??26.000 | ??17.011 | ??30.249 |
| ??C3H6 | ??2.13 | ??1.906 | ??1.906 | ??0.843 | ??2.408 |
| ??HCl | ??5.15 | ??8.212 | ??8.212 | ??5.987 | ??9.264 |
| ??MClSilane | ??0.00 | ??0.00 | ??0.00 | ??0.00 | ??0.00 |
| Temperature ℃ | ??-22.0 | ??-22.0 | ??5~20.0 | ??5~18.0 | ??5~14.8 |
| Pressure Mpag | ??0.87 | ??0.87 | ??0.85 | ??0.78 | ??0.20 |
| Molar flow kmol/h | ??14.29 | ??40.00 | ??40.00 | ??12.84 | ??27.16 |
| Mass rate kg/h | ??446.12 | ??1258.9 | ??1258.9 | ??371.0 | ??887.9 |
| Volumetric flow rate Nm3/h | ??337.87 | ??945.8 | ??945.8 | ??303.6 | ??642.2 |
The second embodiment of the present invention, mode according to embodiment 1, methyl chloride content is that the refining cat head tail gas A of 21.500% organosilicon synthesis unit methyl chloride is compressed into 1.11MPa in compression system (1), compression back gas B enters shallow cooling system (2) condensation and reclaims most of methyl chloride liquid and enter the methyl chloride withdrawing can, remaining gas is removed wherein aerosol droplets entering multistage accurate filter (3), enter subsequently to be heated in the well heater (4) and remove the residue aerosol droplets about 16 ℃, pretreated gas C enters membrane separation apparatus (5) away from cloud point and carries out separating treatment.The rate of recovery of the methyl chloride of this embodiment reaches 98%.Its material balance table is as follows:
Material balance table (wt%)
| Item | ??A | ??B | ??C | ??D | ??E |
| ??CH3Cl | ??21.500 | ??19.406 | ??19.406 | ??6.585 | ??24.764 |
| ??N2 | ??49.464 | ??35.978 | ??35.978 | ??59.452 | ??26.169 |
| ??CH4 | ??3.682 | ??3.389 | ??3.389 | ??4.428 | ??2.956 |
| ??C2H4 | ??2.365 | ??4.202 | ??4.202 | ??2.994 | ??4.707 |
| ??C2H6 | ??13.973 | ??24.841 | ??24.841 | ??17.701 | ??27.825 |
| ??C3H6 | ??3.006 | ??2.670 | ??2.670 | ??1.286 | ??3.248 |
| ??HCl | ??6.010 | ??9.513 | ??9.513 | ??7.554 | ??10.332 |
| ??MClSilane | ??0.000 | ??0.000 | ??0.000 | ??0.000 | ??0.000 |
| Temperature ℃ | ??-22.0 | ??-22.0 | ??5~22.0 | ??5~18.0 | ??5~14.8 |
| Pressure Mpag | ??0.87 | ??0.87 | ??0.87 | ??0.78 | ??0.20 |
| Molar flow kmol/h | ??14.29 | ??40.00 | ??40.00 | ??12.84 | ??27.16 |
| Mass rate kg/h | ??446.12 | ??1258.9 | ??1258.9 | ??371.0 | ??887.9 |
| Volumetric flow rate Nm3/h | ??337.87 | ??945.8 | ??945.8 | ??303.6 | ??642.2 |
The third embodiment of the present invention, mode according to embodiment 1, methyl chloride content is that the refining cat head tail gas A of 13.29% organosilicon synthesis unit methyl chloride is compressed into 1.19MPa in compression system (1), compression back gas B enters shallow cooling system (2) condensation and reclaims most of methyl chloride liquid and enter the methyl chloride withdrawing can, remaining gas is removed wherein aerosol droplets entering multistage accurate filter (3), enter subsequently to be heated in the well heater (4) and remove the residue aerosol droplets about 17 ℃, pretreated gas C enters membrane separation apparatus (5) away from cloud point and carries out separating treatment.The rate of recovery of the methyl chloride of this embodiment is 97%.Its material balance table is as follows:
Material balance table (mol%)
| Item | ??A | ??B | ??C | ??D | ??E |
| ??CH3Cl | ??13.29 | ??11.99 | ??11.99 | ??4.46 | ??16.94 |
| ??N2 | ??55.13 | ??43.28 | ??43.28 | ??61.13 | ??31.56 |
| ??CH4 | ??7.17 | ??6.90 | ??6.90 | ??7.97 | ??6.20 |
| ??C2H4 | ??2.63 | ??4.35 | ??4.35 | ??3.03 | ??5.22 |
| ??C2H6 | ??14.51 | ??23.74 | ??23.74 | ??16.56 | ??28.46 |
| ??C3H6 | ??2.13 | ??2.01 | ??2.01 | ??1.01 | ??2.68 |
| ??HCl | ??5.15 | ??7.72 | ??7.72 | ??5.84 | ??8.95 |
| ??MClSilane | ??0.00 | ??0.00 | ??0.00 | ??0.00 | ??0.00 |
| Temperature ℃ | ??-22.0 | ??-22.0 | ??5~20.0 | ??5~18.0 | ??5~14.8 |
| Pressure Mpag | ??0.87 | ??0.87 | ??0.85 | ??0.78 | ??0.20 |
| Molar flow kmol/h | ??14.29 | ??32.50 | ??32.50 | ??12.89 | ??19.61 |
| Mass rate kg/h | ??446.12 | ??1018.78 | ??1018.78 | ??374.43 | ??644.34 |
| Volumetric flow rate Nm3/h | ??337.87 | ??768.41 | ??768.41 | ??304.67 | ??463.74 |
The fourth embodiment of the present invention, mode according to embodiment 1, methyl chloride content is that the refining cat head tail gas A of 21.500% organosilicon synthesis unit methyl chloride is compressed into 1.19MPa in compression system (1), compression back gas B enters shallow cooling system (2) condensation and reclaims most of methyl chloride liquid and enter the methyl chloride withdrawing can, remaining gas is removed wherein aerosol droplets entering multistage accurate filter (3), enter subsequently to be heated in the well heater (4) and remove the residue aerosol droplets about 15 ℃, pretreated gas C enters membrane separation apparatus (5) away from cloud point and carries out separating treatment.The rate of recovery of the methyl chloride of this embodiment is 95.6%.Its material balance table is as follows:
Material balance table (wt%)
| Item | ??A | ??B | ??C | ??D | ??E |
| ??CH3Cl | ??21.500 | ??19.316 | ??19.316 | ??7.752 | ??26.036 |
| ??N2 | ??49.464 | ??38.679 | ??38.679 | ??58.934 | ??26.909 |
| ??CH4 | ??3.682 | ??3.532 | ??3.532 | ??4.401 | ??3.027 |
| ??C2H4 | ??2.365 | ??3.894 | ??3.894 | ??2.930 | ??4.455 |
| ??C2H6 | ??13.973 | ??22.772 | ??22.772 | ??17.132 | ??26.050 |
| ??C3H6 | ??3.006 | ??2.832 | ??2.832 | ??1.526 | ??3.591 |
| ??HCl | ??6.010 | ??8.974 | ??8.974 | ??7.325 | ??9.932 |
| ??MClSilane | ??0.000 | ??0.000 | ??0.000 | ??0.000 | ??0.000 |
| Temperature ℃ | ??-22.0 | ??-22.0 | ??5~20.0 | ??5~18.0 | ??5~014.8 |
| Pressure Mpag | ??0.87 | ??0.87 | ??0.85 | ??0.78 | ??0.20 |
| Molar flow kmol/h | ??14.29 | ??32.50 | ??32.50 | ??12.89 | ??19.61 |
| Mass rate kg/h | ??446.12 | ??1018.78 | ??1018.78 | ??374.43 | ??644.34 |
| Volumetric flow rate Nm3/h | ??337.87 | ??768.41 | ??768.41 | ??304.67 | ??463.74 |
Claims (5)
1. the method for an enriching and recovering methyl chloride by membrane separation method and device is characterized in that: this device is provided with the compression decorum (1), shallow cooling system (2), strainer (3), well heater (4), membrane separation apparatus (5) from left to right successively.The connection situation of each several part is as follows: the inlet end of compression system (1) is connected with the refining cat head tail gas discharging pipe of organosilicon synthesis unit methyl chloride, compression system (1) outlet side is connected with the inlet end of shallow cooling system (2), the outlet side of shallow cooling system (2) is connected with the inlet end of strainer (3), the outlet end of shallow cooling system (2) is connected with the methyl chloride withdrawing can, the outlet side of strainer (3) is connected with the inlet end of well heater (4), the outlet side of well heater (4) is connected with the inlet end of membrane separation apparatus (5), the per-meate side outlet of membrane separation apparatus (5) is connected with the inlet end of compression system (1), and the retentate side outlet of membrane separation apparatus (5) is connected with other exhaust gas processing devices.
2. the method for an enriching and recovering methyl chloride by membrane separation method and device, it is characterized in that: the recovery method of methyl chloride is to adopt membrane separation apparatus (5) and compression system (1), shallow cooling system (2), strainer (3) and well heater (4) to carry out the coupled method in the described waste gas, and concrete steps are:
1) mixed gas enters under certain pressure and temp in the compression system (1), and gas is compressed in the certain pressure scope;
2) mixed gas that comes out from compression system enters in the shallow cooling system and is condensed, and most methyl chloride and aqueous vapor are condensed recycling;
3) all the other condensation tail gas are introduced in the multistage accurate filter, have removed part drop and the aerosol that membrane module is polluted at this;
4) condensation tail gas enters heater heats in certain temperature range subsequently, removes remainder drop and aerosol;
5) tail gas after being heated is incorporated in the membrane separation apparatus, obtains the enrichment methyl chloride gas in per-meate side and returns the compression system recovery that circulates, and removes other exhaust gas processing devices and be mainly components such as the nitrogen that is trapped, methane at retentate side gas.
3. according to the method and the device of the described enriching and recovering methyl chloride by membrane separation method of claim 1, it is characterized in that: the preferred organic vapor film separator of the membrane separation apparatus that this device adopted.
4. according to the method and the device of enriching and recovering methyl chloride by membrane separation method in the described waste gas of claim 2, it is characterized in that: mixed gas is compressed into the certain pressure scope in compression system, the preferred 1.0～1.3MPa of this pressure range.
5. according to the method and the device of enriching and recovering methyl chloride by membrane separation method in the described waste gas of claim 2, it is characterized in that: condensation tail gas enters heater heats to certain temperature range, preferred 5～20 ℃ of this temperature range.
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| CN106008150A (en) * | 2016-05-27 | 2016-10-12 | 崔贤长 | Chloromethane dehydration purifying apparatus and method thereof |
| CN106008150B (en) * | 2016-05-27 | 2018-11-09 | 江苏金纳多生物科技有限公司 | A kind of device and method that chloromethanes dehydration is refined |
| CN106542960A (en) * | 2016-09-30 | 2017-03-29 | 无锡市张舍化工有限公司 | A kind of method of liquid in removing methyl chloride gas |
| CN107837654A (en) * | 2017-10-26 | 2018-03-27 | 上海安居乐环保科技股份有限公司 | Waste gas containing fluoride recovery and processing system based on UF membrane principle |
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