CN104941388B - A method of separation vinyl chloride and acetylene - Google Patents
A method of separation vinyl chloride and acetylene Download PDFInfo
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- CN104941388B CN104941388B CN201410857063.9A CN201410857063A CN104941388B CN 104941388 B CN104941388 B CN 104941388B CN 201410857063 A CN201410857063 A CN 201410857063A CN 104941388 B CN104941388 B CN 104941388B
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- vinyl chloride
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- activated carbon
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Abstract
The invention discloses a kind of methods for separating vinyl chloride and acetylene.This method separates vinyl chloride and acetylene using modified activated carbon as separating adsorbent using pressure swing adsorption technique.The invention is characterized in that the active carbon as adsorbent is prepared through inert gas modification, the preparation method is as follows: the high-temperature roasting under inert atmosphere protection by active carbon, is cooled to room temperature up to modified activated carbon.The modified activated carbon that this method uses is significantly raised to the more unmodified active carbon of the separation of vinyl chloride and acetylene, up under 6.86,0.5MPa reachable 4.62 at 0.1MPa；And also increase to the adsorption capacity of vinyl chloride, 0.1MPa up to 0.761mmol/g under 0.5MPa, provides good approach for the separation of vinyl chloride and acetylene up to 0.591mmol/g.
Description
Technical field
It is specifically a kind of to be carried out for the mixed gas containing vinyl chloride and acetylene the invention belongs to adsorption technology field
Isolated method.
Background technique
Vinyl chloride and acetylene are widely present in calcium carbide process PVC tail gas, such as not only pollute environment without processing direct emission,
It is detrimental to health, and causes a large amount of C2H3Cl、C2H2The waste of resource increases Production of PVC cost.
Tail gas clean-up processing mode generally uses membrane separation process and absorption method (temp.-changing adsorption in PVC Industry at present
Method and pressure swing adsorption method).Easily there is the phenomenon that acetylene and oxygen concentration etc. jeopardize safety in production in membrane separation process, furthermore actual production
When middle generation tail gas strip, the permanent damage of film will cause, it is necessary to which parking replacement, there are film replacements frequently, operating cost is high
The problems such as.Temp.-changing adsorption rule causes energy consumption, device operating cost because regeneration of adsorbent beds needs extraneous offer heat source and cold source
It is higher, C in purified gas2H3Cl and C2H2Content is often more than environmental protection index because regeneration of adsorbent beds is incomplete, causes environment dirty
The defects of dye, the vinyl chloride water content of recycling is high.
Pressure swing adsorption (PSA) invests, non-environmental-pollution and equipment corrosion low with operating cost, automation due to having
Degree height and many remarkable advantages such as energy-saving and the reclaiming clean for being used for calcium carbide process PVC tail gas.Pass through adsorbent and phase
Technique is answered to recycle C2H3Cl、C2H2, the good adsorbent of separating property is by C2H2And C2H3Utilization is separately recovered in Cl, can reduce energy consumption,
Obtain the higher C of purity2H3Cl and C2H2Product gas, can not only reduce the pollution to environment, and can energy saving and resource,
Reduce production cost.
Summary of the invention
The object of the present invention is to provide a kind of methods for separating vinyl chloride and acetylene, can significantly improve to vinyl chloride and acetylene
Adsorbing separation ability, and there is high-adsorption-capacity to vinyl chloride.The present invention is characterized in that the work high temperature modified with inert gas
Property charcoal be adsorbent, preparation method includes the following steps:
1,30-80 mesh active carbon is placed in tube furnace, is passed through inert gas purge at room temperature.
2, in an inert atmosphere in 120 DEG C of dry activated carbon 2h；
3, the active carbon after drying is roasted in noble gas atmosphere high temperature, and is cooled to room temperature under noble gas protection and changes to obtain the final product
Property active carbon.
Modified activated carbon can be one of carbo lignius, coal quality charcoal, coconut husk charcoal and nucleocapsid charcoal.
Inert gas can be He, Ar and N2One of.
Active carbon maturing temperature is 300-1000 DEG C, calcining time 2-12h, inert gas flow velocity 50-300mL/
min。
The present invention has following advantages and effect:
1. operation of the present invention is simple and easy, the segregative line of active carbon at various pressures to vinyl chloride and acetylene can be improved
Number, separation is at 0.1MPa up under 6.86,0.5MPa reachable 4.62.
2. the modified adsorbent that the present invention uses is higher than unmodified active carbon to the adsorption capacity of vinyl chloride, vinyl chloride
Adsorption capacity in 0.1MPa up to 0.591mmol/g, up to 0.761mmol/g under 0.5MPa.
Specific embodiment
The separation of vinyl chloride and acetylene is carried out on dynamic method experimental provision.Vinyl chloride/acetylene/He gaseous mixture is with stabilization
Flow by being equipped with the adsorption bed of modified activated carbon absorbent, passes through gas-chromatography on-line analysis adsorbent bed under a constant
The gas concentration of layer outlet, measures the breakthrough curve of vinyl chloride and acetylene.Adsorb test condition: adsorbent 4.00g, adsorption temp
40 DEG C, adsorptive pressure 0.1-0.5MPa.Embodiment 1-4 is shown in the preparation of modified activated carbon.
Embodiment 1:
30-80 mesh coconut husk charcoal is placed in tube furnace, N is passed through230min is swept in air-blowing, then dry in the case where being warming up to 120 DEG C
After coconut husk charcoal 2h, 6h, N are roasted at 800 DEG C2Flow velocity is 120mL/min, and in N2It is cooled to room temperature under protection and lives up to modified
Property charcoal.
Embodiment 2:
30-80 mesh coconut husk charcoal is placed in tube furnace, Ar air-blowing is passed through and sweeps 30min, it is then dry in the case where being warming up to 120 DEG C
After coconut husk charcoal 2h, 8h is roasted at 600 DEG C, Ar flow velocity is 150mL/min, and is cooled to room temperature under Ar protection and lives up to modified
Property charcoal.
Embodiment 3:
30-80 mesh coal quality charcoal is placed in tube furnace, N is passed through230min is swept in air-blowing, then dry in the case where being warming up to 120 DEG C
After coconut husk charcoal 2h, 6h, N are roasted at 800 DEG C2Flow velocity is 200mL/min, and in N2It is cooled to room temperature under protection and lives up to modified
Property charcoal.
Embodiment 4:
30-80 mesh nucleocapsid charcoal is placed in tube furnace, He air-blowing is passed through and sweeps 30min, it is then dry in the case where being warming up to 120 DEG C
After coconut husk charcoal 2h, 6h is roasted at 900 DEG C, He flow velocity is 120mL/min, and is cooled to room temperature under He protection and lives up to modified
Property charcoal.
Embodiment 5:
Unmodified active carbon and embodiment 1-4 are prepared into the survey that modified activated carbon carries out vinyl chloride and acetylene breakthrough curve
Fixed, the adsorption capacity of vinyl chloride/acetylene separation and vinyl chloride is as shown in table 1.
The desorption balance data and separation of table 1 activated carbon modified front and back vinyl chloride and acetylene
It can be seen that: it is modified through inert gas shielding high-temperature roasting for various active carbons, with respective fresh activity charcoal phase
Than being significantly improved without vinyl chloride/acetylene separation under pressure, and the adsorption capacity of vinyl chloride also increased.
N in embodiment 12As inert gas, it is modified coconut husk charcoal obtained by flow velocity 120mL/min, 800 DEG C of roasting 6h, to vinyl chloride
Adsorption capacity 0.1MPa be 0.591mmol/g, separation 6.86；The adsorption capacity of vinyl chloride exists when 0.5MPa
0.1MPa is 0.761mmol/g, separation 4.62.
Claims (4)
1. a kind of method for separating vinyl chloride and acetylene is with modified activated carbon it is characterized in that being to use pressure swing adsorption technique
Separating adsorbent；1. the preparation method of modified activated carbon is the following steps are included: be placed in tube furnace, room temperature for 30-80 mesh active carbon
Under be passed through inert gas purge 30min；2. in an inert atmosphere in 120 DEG C of dry activated carbon 2h；3. continuing in an inert atmosphere
Active carbon after 300-1000 DEG C of roasting is dry, and be cooled to room temperature under inert gas protection up to modified activated carbon.
2. the method for separation vinyl chloride and acetylene according to claim 1, it is characterised in that used active carbon is wood
One of matter charcoal, coal quality charcoal, coconut husk charcoal and nucleocapsid charcoal.
3. the method for separation vinyl chloride and acetylene according to claim 1, it is characterised in that inert gas He, Ar and N2
One of.
4. the method for separation vinyl chloride and acetylene according to claim 1, it is characterised in that the roasting temperature of modified activated carbon
Degree is 300-1000 DEG C, calcining time 2-12h, inert gas flow velocity 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 |
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| CN201310713967 | 2013-12-23 | ||
| CN201310713967X | 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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| CN104941388A CN104941388A (en) | 2015-09-30 |
| CN104941388B true CN104941388B (en) | 2019-10-15 |
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| 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 |
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 |
| 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 |
| 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 |
| 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 |
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- 2014-12-23 CN CN201410857063.9A patent/CN104941388B/en active Active
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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 |
| 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 |
| 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 |
| 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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| 采用变压吸附技术回收氯乙烯精馏尾气;刘包生;《中国氯碱》;20091231(第12期);第39至42页 * |
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