CN104941388A - Method for separating chloroethylene from acetylene - Google Patents
Method for separating chloroethylene from acetylene Download PDFInfo
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- CN104941388A CN104941388A CN201410857063.9A CN201410857063A CN104941388A CN 104941388 A CN104941388 A CN 104941388A CN 201410857063 A CN201410857063 A CN 201410857063A CN 104941388 A CN104941388 A CN 104941388A
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- activated carbon
- acetylene
- modified activated
- chloroethylene
- separating
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Abstract
The invention discloses a method for separating chloroethylene from acetylene. According to the method, a pressure swing adsorption technology is adopted, modified activated carbon is taken as a separation adsorbent, and chloroethylene is separated from acetylene. The method is characterized in that activated carbon taken as the adsorbent is prepared by modification by adopting inert gases, specifically, is prepared by baking activated carbon at high temperature under protection of inert atmosphere and cooling to room temperature. The separation coefficient of the adopted modified activated carbon for chloroethylene and acetylene is obviously improved compared with the activated carbon which is modified, can achieve 6.86 under pressure of 0.1MPa and can achieve 4.62 under pressure of 0.5 MPa, the adsorption capacity of the modified activated carbon for chloroethylene is also improved to a certain extent, can achieve 0.591mmlol/g under pressure of 0.1MPa and can achieve 0.761mmol/g under pressure of 0.5MPa, and therefore, a good path is provided for separating chloroethylene from acetylene.
Description
Technical field
The invention belongs to adsorption technology field, is a kind of method for carrying out being separated containing vinyl chloride and the mist of acetylene specifically.
Background technology
Vinyl chloride and acetylene are extensively present in calcium carbide process PVC tail gas, as not treated direct discharge not only contaminated environment, are detrimental to health, and cause a large amount of C
2h
3cl, C
2h
2the waste of resource, increases Production of PVC cost.
In PVC Industry, tail gas clean-up processing mode generally adopts membrane separation process and absorption method (Temp .-change adsorptive process and pressure swing adsorption method) at present.Membrane separation process easily occurs that acetylene and oxygen concentration etc. jeopardize the phenomenon of safety in production, when there is tail gas band material in addition in actual production, can cause the permanent damage of film, replacing of must stopping, and there is film and changes the problems such as frequent, operating cost is high.Temp .-changing adsorption rule needs the external world to provide thermal source and low-temperature receiver because of regeneration of adsorbent beds, causes energy ezpenditure, and plant running cost is higher, C in purified gas
2h
3cl and C
2h
2the defects such as content often not exclusively exceedes environmental protection index because of regeneration of adsorbent beds, causes environmental pollution, the vinyl chloride water content height of recovery.
Pressure swing adsorption (PSA) due to there is investment and operating cost low, non-environmental-pollution and equipment corrosion, many remarkable advantages such as automaticity is high and save energy and reduce the cost and be used to the reclaiming clean of calcium carbide process PVC tail gas.C is reclaimed by adsorbent and corresponding technique
2h
3cl, C
2h
2, the good adsorbent of separating property is by C
2h
2and C
2h
3cl recycles respectively, capable of reducing energy consumption, obtains the C that purity is higher
2h
3cl and C
2h
2gas product, not only can reduce the pollution to environment, and can economize energy and resource, reduces production cost.
Summary of the invention
The object of this invention is to provide a kind of method of separating chlorine ethene and acetylene, can significantly improve vinyl chloride and acetylene adsorbing separation ability, and to vinyl chloride, there is high-adsorption-capacity.The invention is characterized in that its preparation method comprises the steps: with the high temperature modified active carbon of inert gas for adsorbent
1,30-80 order active carbon is placed in tube furnace, at room temperature passes into inert gas purge.
2, in an inert atmosphere in 120 DEG C of dry activated carbon 2h;
3, by the high-temperature roasting in noble gas atmosphere of dried active carbon, and be cooled to room temperature and namely obtain modified activated carbon under noble gas protection.
Modified activated carbon can be the one in carbo lignius, ature of coal charcoal, coconut husk charcoal and nucleocapsid charcoal.
Inert gas can be He, Ar and N
2in one.
Active carbon sintering temperature is 300-1000 DEG C, and roasting time is 2-12h, and inert gas flow velocity is 50-300mL/min.
The present invention has following advantages and effect:
1. operation is simple in the present invention, and can improve active carbon to vinyl chloride and acetylene separation at various pressures, separation can reach 4.62 can reach 6.86,0.5MPa under 0.1MPa under.
2. the modified adsorbent of the present invention's use is all high than unmodified active carbon to the adsorption capacity of vinyl chloride, and the adsorption capacity of vinyl chloride can reach 0.591mmol/g at 0.1MPa, can reach 0.761mmol/g under 0.5MPa.
Detailed description of the invention
Vinyl chloride is carry out on dynamic method experimental provision with being separated of acetylene.Vinyl chloride/acetylene/He gaseous mixture under a constant by being equipped with the adsorption bed of modified activated carbon absorbent, by the gas concentration of gas-chromatography on-line analysis adsorption bed outlet, measures the breakthrough curve of vinyl chloride and acetylene with regime flow.Absorption test condition: adsorbent 4.00g, adsorption temp 40 DEG C, adsorptive pressure is 0.1-0.5MPa.Embodiment 1-4 is shown in the preparation of modified activated carbon.
Embodiment 1:
30-80 order coconut husk charcoal is placed in tube furnace, passes into N
230min is swept in air-blowing, is then being warming up at 120 DEG C after dry coconut husk charcoal 2h, roasting 6h, N at 800 DEG C
2flow velocity is 120mL/min, and at N
2be cooled to room temperature under protection and namely obtain modified activated carbon.
Embodiment 2:
30-80 order coconut husk charcoal is placed in tube furnace, passes into Ar air-blowing and sweep 30min, be then warming up at 120 DEG C after dry coconut husk charcoal 2h, at 600 DEG C, roasting 8h, Ar flow velocity is 150mL/min, and is cooled to room temperature and namely obtains modified activated carbon under Ar protection.
Embodiment 3:
30-80 order ature of coal charcoal is placed in tube furnace, passes into N
230min is swept in air-blowing, is then being warming up at 120 DEG C after dry coconut husk charcoal 2h, roasting 6h, N at 800 DEG C
2flow velocity is 200mL/min, and at N
2be cooled to room temperature under protection and namely obtain modified activated carbon.
Embodiment 4:
30-80 order nucleocapsid charcoal is placed in tube furnace, passes into He air-blowing and sweep 30min, be then warming up at 120 DEG C after dry coconut husk charcoal 2h, at 900 DEG C, roasting 6h, He flow velocity is 120mL/min, and is cooled to room temperature and namely obtains modified activated carbon under He protection.
Embodiment 5:
Unmodified active carbon and embodiment 1-4 are prepared the mensuration that modified activated carbon carries out vinyl chloride and acetylene breakthrough curve, the separation of vinyl chloride/acetylene and the adsorption capacity of vinyl chloride as shown in table 1.
The desorption balance data of table 1 activated carbon modified front and back vinyl chloride and acetylene and separation
Visible: for various active carbon, modified through inert gas shielding high-temperature roasting, compared with respective fresh activity charcoal, be all significantly improved without the separation of vinyl chloride/acetylene under pressure, and the adsorption capacity of vinyl chloride also increases to some extent.N in embodiment 1
2as inert gas, flow velocity is 120mL/min, 800 DEG C of roasting 6h gained modification coconut husk charcoals, and it is 0.591mmol/g to the adsorption capacity of vinyl chloride at 0.1MPa, and separation is 6.86; During 0.5MPa, the adsorption capacity of vinyl chloride is 0.761mmol/g at 0.1MPa, and separation is 4.62.
Claims (5)
1. a method for separating chlorine ethene and acetylene, it is characterized in that being to adopt pressure swing adsorption technique, take modified activated carbon as separating adsorbent.
2. the method for a kind of separating chlorine ethene according to claim 1 and acetylene, is characterized in that the preparation method of modified activated carbon comprises the following steps:
1. 30-80 order active carbon is placed in tube furnace, under room temperature, passes into inert gas purge 30min;
2. in an inert atmosphere in 120 DEG C of dry activated carbon 2h;
3. continue the dried active carbon of high-temperature roasting in an inert atmosphere, and be cooled to room temperature and namely obtain modified activated carbon under noble gas protection.
3. the preparation method of modified activated carbon according to claim 2, is characterized in that used active carbon can be the one in carbo lignius, ature of coal charcoal, coconut husk charcoal and nucleocapsid charcoal.
4. the preparation method of modified activated carbon according to claim 2, is characterized in that inert gas can be He, Ar and N
2in one.
5. the preparation method of modified activated carbon according to claim 2, it is characterized in that the sintering temperature of modified activated carbon is 300-1000 DEG C, roasting time is 2-12h, and inert gas flow velocity is 50-300mL/min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410857063.9A CN104941388B (en) | 2013-12-23 | 2014-12-23 | A method of separation vinyl chloride and acetylene |
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310713967X | 2013-12-23 | ||
| CN201310713967 | 2013-12-23 | ||
| CN201410857063.9A CN104941388B (en) | 2013-12-23 | 2014-12-23 | A method of separation vinyl chloride and acetylene |
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| Publication Number | Publication Date |
|---|---|
| CN104941388A true CN104941388A (en) | 2015-09-30 |
| CN104941388B CN104941388B (en) | 2019-10-15 |
Family
ID=54156779
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410857063.9A Active CN104941388B (en) | 2013-12-23 | 2014-12-23 | A method of separation vinyl chloride and acetylene |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109422265A (en) * | 2017-09-01 | 2019-03-05 | 中国科学院大连化学物理研究所 | A kind of high temperature modified processing method of activated carbon raw material |
Citations (7)
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|---|---|---|---|---|
| CN1594251A (en) * | 2004-07-09 | 2005-03-16 | 张双永 | Method for separating and recovering chloroethylene by pressure swing adsorption method |
| CN1597053A (en) * | 2004-08-27 | 2005-03-23 | 四川天一科技股份有限公司 | Pressure-varying adsorption method for recovering vinyl chloride and acetylene from gas mixture |
| CN1597052A (en) * | 2004-08-27 | 2005-03-23 | 四川天一科技股份有限公司 | Pressure-varying adsorption method for concentrating and recovering chlorethylene from chlorethylene containing gas mixture |
| CN1850751A (en) * | 2005-11-28 | 2006-10-25 | 四川开元科技有限责任公司 | Pressure-variation adsorption separation recovering method for mixd gas containing chloroethylene and acetylene |
| EP1716907A1 (en) * | 2005-04-26 | 2006-11-02 | Air Products and Chemicals, Inc. | Pressure swing adsorption method |
| CN101531365A (en) * | 2009-03-18 | 2009-09-16 | 重庆大学 | Preparation method of pressed active carbon for pressure swing adsorption/separation of methane/nitrogen |
| CN101653721A (en) * | 2009-09-15 | 2010-02-24 | 重庆大学 | Preparation method of coal-based granular activated carbon with molecular sieving effect and application thereof in pressure-transformation adsorption and separation concentrated gas |
-
2014
- 2014-12-23 CN CN201410857063.9A patent/CN104941388B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1594251A (en) * | 2004-07-09 | 2005-03-16 | 张双永 | Method for separating and recovering chloroethylene by pressure swing adsorption method |
| CN1597053A (en) * | 2004-08-27 | 2005-03-23 | 四川天一科技股份有限公司 | Pressure-varying adsorption method for recovering vinyl chloride and acetylene from gas mixture |
| CN1597052A (en) * | 2004-08-27 | 2005-03-23 | 四川天一科技股份有限公司 | Pressure-varying adsorption method for concentrating and recovering chlorethylene from chlorethylene containing gas mixture |
| EP1716907A1 (en) * | 2005-04-26 | 2006-11-02 | Air Products and Chemicals, Inc. | Pressure swing adsorption method |
| CN1850751A (en) * | 2005-11-28 | 2006-10-25 | 四川开元科技有限责任公司 | Pressure-variation adsorption separation recovering method for mixd gas containing chloroethylene and acetylene |
| CN101531365A (en) * | 2009-03-18 | 2009-09-16 | 重庆大学 | Preparation method of pressed active carbon for pressure swing adsorption/separation of methane/nitrogen |
| CN101653721A (en) * | 2009-09-15 | 2010-02-24 | 重庆大学 | Preparation method of coal-based granular activated carbon with molecular sieving effect and application thereof in pressure-transformation adsorption and separation concentrated gas |
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| 刘包生: "采用变压吸附技术回收氯乙烯精馏尾气", 《中国氯碱》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109422265A (en) * | 2017-09-01 | 2019-03-05 | 中国科学院大连化学物理研究所 | A kind of high temperature modified processing method of activated carbon raw material |
| CN109422265B (en) * | 2017-09-01 | 2021-12-31 | 中国科学院大连化学物理研究所 | High-temperature modification treatment method for activated carbon raw material |
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|---|---|
| CN104941388B (en) | 2019-10-15 |
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