CN102908880A - Pre-dewatering method for reducing load of high-water-content methyl chloride drying apparatus - Google Patents
Pre-dewatering method for reducing load of high-water-content methyl chloride drying apparatus Download PDFInfo
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- CN102908880A CN102908880A CN2012104138948A CN201210413894A CN102908880A CN 102908880 A CN102908880 A CN 102908880A CN 2012104138948 A CN2012104138948 A CN 2012104138948A CN 201210413894 A CN201210413894 A CN 201210413894A CN 102908880 A CN102908880 A CN 102908880A
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Abstract
The invention discloses a pre-dewatering method for reducing the load of a high-water-content methyl chloride drying apparatus, which belongs to the technical field of chemical industry. The pre-dewatering method is characterized in that water in methyl chloride gas is removed efficiently through the adoption of a film separation and compression condensing method. The method comprises the steps of: implementing compression condensing treatment on the methyl chloride gas firstly to remove the water of the methyl chloride gas preliminarily, filtering to remove liquid drops and impurities and preheating to a proper temperature, then further pre-removing the water vapor in the gas by using a film separation method. The osmosis gas generated by the film separation is methyl chloride containing concentrated water vapor, wherein the methyl chloride reflows to a feeding place for circular treatment so as not to be lost. The osmosis residual gas is methyl chloride which is pre-dehumidified, and the water content is less than 200ppm. The dehumidifying rate can be up to greater than 90% by using the pre-dewatering method which can be used as a pre-dewatering system of a plurality of methyl chloride drying apparatus; and the method is flexible in operation, stable in product quality and remarkable in economic benefit.
Description
Technical field
The invention belongs to chemical technology field, relate to a kind of method of organic vapor dehydration, particularly the coupling of compression condensation and membrane separating method removes the technique of water vapour in the methyl chloride gas.
Background technology
Chloromethanes is monochloro methane, is widely used as diluent and solvent in the butyl rubber production process in industry.
Industrial chloromethanes water content is about 2000ppm, water can be brought into the butyl rubber paradigmatic system when chloromethanes water content is too high, not only can produce the possibility that initator freezes in heat exchanger, also can destroy the stability of initiator solution activity fully, when serious even cause completely and stop.In addition, moisture methyl chloride gas has extremely strong corrosivity, can cause pipeline, equipment etc. to have a strong impact on, and increases maintenance cost; Extremely strong corrosivity also makes chloromethanes/aqueous systems easily polymeric film material be caused irreversible destruction, makes the polymer film dewater unit can't directly apply to the methyl chloride gas dehydration.So the requirement to the methyl chloride gas water content in the industrial production is very strict, China's chemical industry standard regulation chloromethanes high-class product water content should be lower than and requires the chloromethanes water content to need below 20ppm in 100ppm, the butyl rubber polymerization reaction system.
Traditional handicraft adopts absorption method to remove moisture in the methyl chloride gas, because water content is higher in the raw material, product purity requires very harsh again, and adsorbent capacity can't infinitely be enlarged by the cost restriction, so that the adsorbent in the drying tower can be saturated fast in dehydration.Do must be warming up to more than 200 ℃ when adsorbent is regenerated behaviour, not only energy consumption is very large, and high temperature can cause loss to device, adsorbent etc., the increase maintenance cost.For keeping continuous production, in the general factory a plurality of adsorption towers are installed, switch to another tower when Dang Yita is saturated and process.Chloromethanes high-moisture adsorption tower must be regenerated/handover operation frequently, not only increased the operating cost of adsorption tower, also make chloromethanes dry gas quality can't keep stable.
Summary of the invention
For solve the drying tower adsorbent operation cycle that prior art exists short, the adsorption tower regeneration cost is too high, unstable product quality and film separating and dehydrating device are difficult to directly apply to the problems such as chloromethanes-aqueous systems, the invention provides a kind of predrainage method that reduces high moisture chloromethanes drying equipment load, the characteristics of the method are to adopt film separation and the integrated method of compression condensation that methyl chloride gas is processed, remove the water vapour in the methyl chloride gas, realize low-cost methyl chloride gas dehydration, reduce the effect of chloromethanes drying device load, prolong operation cycle.The method dehumidification efficient is high, can produce continuously, need not handover operation, and additive-free, can significantly reduce drying cost and increase economic efficiency.
A kind of predrainage method that reduces high moisture chloromethanes drying equipment load of the present invention, its process characteristic is mainly: by supercharging makes the wherein easier condensation of moisture to methyl chloride gas, thereby remove most of moisture by compression condensation, make methyl chloride gas reach the condition of suitable membrane separation, the recycling membrane separating method further removes in advance to moisture.
This technique mainly is comprised of following system: compression condensation system, film separation system.Wherein the compression condensation system mainly comprises the devices such as compressor, condenser, minute flow container; Film separation system mainly comprises the devices such as accurate filter, preheater, membrane separation assemblies.Each installs Main Function: the compression condensation system is mainly removes most of water vapor in the methyl chloride gas, reduces raw material to the corrosivity of membrane separation device; Accurate filter act as impurity such as filter removing liquid foam, particle, guarantee the gas free from admixture, to film without destruction; The effect of membrane separation assemblies is further to remove in advance moisture in the methyl chloride gas, reduces moisture concentration in the methyl chloride gas.
The technical solution adopted in the present invention is: methyl chloride gas A at first enters the compression condensation system, through compressor pressurizes to 0.05 ~ 2.0MPag, processes by entering the separatory tank behind condenser condenses to 0 ~ 40 ℃ again.Divide flow container that condensed mixture is separated, liquefied mixture B discharges from the bottom and reclaims, and top gas enters accurate filter and filters removal impurity, enters film separation system again.Gas at first is preheated to 10 ~ 60 ℃ through preheater in film separation system, make gas temperature away from dew point, and guaranteeing does not have droplets agglomerate; Gas enters membrane separation assemblies and processes afterwards.Membrane separation assemblies further removes moisture in the methyl chloride gas in advance, and moisture concentration is down to below the 200ppm.The infiltration gas C that membrane separation assemblies produces is water and the chloromethanes that is removed, ooze residual air D and be finish pre-dehumidification chloromethanes.Infiltration gas C is back to methyl chloride gas A place to be mixed, and reenters compressor; Ooze residual air D separating device.
Contain a large amount of chloromethanes among the infiltration gas C that membrane separation assemblies produces in the technical solution of the present invention, infiltration gas C returns methyl chloride gas A place to be mixed with it, returns to compressor and processes, and makes to permeate that chloromethanes is reclaimed fully among the gas C; Oozing residual air D is the chloromethanes of finishing pre-dehumidification, discharger.
Membrane separation assemblies can adopt flat, spiral wound or doughnut formula membrane separator in the technical solution of the present invention; The per-meate side of film can be taked the discharge of the method guiding infiltration gas such as sweeping method, vacuum method, and is preferred according to specific embodiments; Separation membrane material is preferred high molecular polymer dehumidification film, and membrane material can be the polymeric materials such as polysulfones, polyimides, PEI.
Effect of the present invention with benefit is: the present invention separates by film and the compression condensation dewater unit is efficient, non-additive has removed moisture in the methyl chloride gas, and the dehumidification rate reaches more than 90%, and vapour content is minimum in the product chloromethanes reaches below the 200ppm.The present invention has the coupling of height, is suitable as the pretreatment system of high-moisture methyl chloride gas, can reduce the load of former dewater unit more than 80%, prolong 4.5 ~ 9 times of regeneration periods, significantly reduce running cost, improve adsorbent service life, guarantee simultaneously the stable of product quality.
Description of drawings
Accompanying drawing is the process chart of minor amount of water in the film separation removal methyl chloride gas.
Among the figure: the A methyl chloride gas; The B liquefied mixture; C permeates gas; D oozes residual air; 1 compressor; 2 condensers; 3 minutes flow containers; 4 accurate filters; 5 preheaters; 6 membrane separation assemblies.
The specific embodiment
Be described in detail the specific embodiment of the present invention below in conjunction with technical scheme and accompanying drawing, following embodiment will help the understanding of the present invention more, but not consist of the restriction to content of the present invention.
Please by reference to the accompanying drawings, methyl chloride gas A water content is 2000ppmw, and temperature is 18 ℃, after at first entering compressor 1 and being forced into 0.3MPag, is condensed to 14 ℃ by condenser 2.Condensed liquid-vapor mixture enters minute flow container 3 separatory, liquefied mixture B is discharged to other devices by a minute flow container and processes, gas enters accurate filter 4 and filters to remove and enter preheater 5 behind the impurity and be preheated to 20 ℃ in minute flow container 3, enters membrane separation assemblies 6 again and carries out dehumidification and process.Gas is divided into two strands after membrane separation assemblies 5 is processed, one is for oozing residual air D, and main component is chloromethanes, and vapour content is 183ppmw; Another strand is infiltration gas C, and main component still is chloromethanes, but wherein contains by the water vapour of enrichment, and content is 1674ppmw.Infiltration gas C is back to compressor 1 porch to be mixed with methyl chloride gas A, re-starts dehumidification and processes.Membrane separation assemblies 6 adopts hollow fiber membrane separators in the present embodiment, and membrane material is ps hollow fiber uf membrane, takes raw material to make the mode of operation that tube side, infiltration are made shell side leave with rage leave with rage, wherein 20% ooze residual air as sweep gas.The dehumidification rate is 91.44% in the present embodiment, the chloromethanes drying adsorption tower regeneration period can be prolonged 6 times, and its material balance is as shown in table 1:
Table 1 embodiment 1 material balance table
Claims (10)
1. one kind is reduced the predrainage method that high moisture chloromethanes drying equipment is loaded, it is characterized in that, by supercharging makes the wherein easier condensation of moisture to methyl chloride gas, thereby remove most of moisture by compression condensation, make methyl chloride gas reach the condition of suitable membrane separation, the recycling membrane separating method further removes in advance to moisture; It is characterized in that the method comprises compression condensation system and film separation system, wherein the compression condensation system comprises compressor (1), condenser (2), minute flow container (3); Film separation system comprises accurate filter (4), preheater (5), membrane separation assemblies (6);
Methyl chloride gas A at first enters the compression condensation system, is forced into 0.05 ~ 2.0MPag through compressor 1, enters separatory tank (3) after being condensed to 0 ~ 40 ℃ by condenser (2) again to process; Divide flow container (3) that condensed mixture is separated, liquefied mixture B discharges from the bottom and reclaims, and top gas enters accurate filter (4) and filters removal impurity, enters film separation system again; Gas at first passes through preheater (5) and is preheated to 10 ~ 60 ℃ in film separation system, make gas temperature away from dew point, and guaranteeing does not have droplets agglomerate; Gas enters membrane separation assemblies (6) and processes afterwards; Membrane separation assemblies (6) further removes moisture in the methyl chloride gas in advance, and moisture concentration is down to below the 200ppm; The infiltration gas C that membrane separation assemblies (6) produces is water and the chloromethanes that is removed, ooze residual air D and be finish pre-dehumidification chloromethanes.
2. predrainage method according to claim 1 is characterized in that, infiltration gas C is back to methyl chloride gas A place to be mixed, and reenters compressor; Ooze residual air D separating device.
3. predrainage method according to claim 1 and 2 is characterized in that, that membrane separation assemblies adopts is flat, spiral wound or doughnut formula membrane separator.
4. predrainage method according to claim 1 and 2 is characterized in that, the per-meate side of film is taked sweeping method, vacuum method.
5. predrainage method according to claim 1 and 2 is characterized in that, the separation membrane material of described membrane separation assemblies (6) is high molecular polymer dehumidification film.
6. predrainage method according to claim 3 is characterized in that, the separation membrane material of described membrane separation assemblies (6) is high molecular polymer dehumidification film.
7. predrainage method according to claim 4 is characterized in that, the separation membrane material of described membrane separation assemblies (6) is high molecular polymer dehumidification film.
8. predrainage method according to claim 5 is characterized in that, membrane material is polysulfones, polyimides, PEI.
9. predrainage method according to claim 6 is characterized in that, membrane material is polysulfones, polyimides, PEI.
10. predrainage method according to claim 7 is characterized in that, membrane material is polysulfones, polyimides, PEI.
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| CN2012104138948A CN102908880A (en) | 2012-10-24 | 2012-10-24 | Pre-dewatering method for reducing load of high-water-content methyl chloride drying apparatus |
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| CN2012104138948A CN102908880A (en) | 2012-10-24 | 2012-10-24 | Pre-dewatering method for reducing load of high-water-content methyl chloride drying apparatus |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106008150A (en) * | 2016-05-27 | 2016-10-12 | 崔贤长 | Chloromethane dehydration purifying apparatus and method thereof |
| 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 |
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| US5089033A (en) * | 1989-11-07 | 1992-02-18 | Membrane Technology & Research, Inc. | Process for removing condensable components from gas streams |
| CN101450890A (en) * | 2007-11-30 | 2009-06-10 | 山东方兴科技开发有限公司 | Removal method for recovery of water in dichloroethane |
| CN101633600A (en) * | 2009-08-21 | 2010-01-27 | 江苏三星化工有限公司 | Method and device for enriching and recovering methyl chloride by membrane separation method |
| CN102451619A (en) * | 2010-10-15 | 2012-05-16 | 中国石油化工股份有限公司 | Y-shaped molecular sieve film and removal method for moisture in dichloromethane |
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2012
- 2012-10-24 CN CN2012104138948A patent/CN102908880A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5089033A (en) * | 1989-11-07 | 1992-02-18 | Membrane Technology & Research, Inc. | Process for removing condensable components from gas streams |
| US5089033B1 (en) * | 1989-11-07 | 1995-02-21 | Membrane Tech & Res Inc | Process for removing condensable components from gas streams |
| CN101450890A (en) * | 2007-11-30 | 2009-06-10 | 山东方兴科技开发有限公司 | Removal method for recovery of water in dichloroethane |
| CN101633600A (en) * | 2009-08-21 | 2010-01-27 | 江苏三星化工有限公司 | Method and device for enriching and recovering methyl chloride by membrane separation method |
| CN102451619A (en) * | 2010-10-15 | 2012-05-16 | 中国石油化工股份有限公司 | Y-shaped molecular sieve film and removal method for moisture in dichloromethane |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
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Application publication date: 20130206 |