CN100575319C - Circulating solvent uses the method for azeotropic dehydration in the C5 extraction separation diene - Google Patents
Circulating solvent uses the method for azeotropic dehydration in the C5 extraction separation diene Download PDFInfo
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- CN100575319C CN100575319C CN200610171044A CN200610171044A CN100575319C CN 100575319 C CN100575319 C CN 100575319C CN 200610171044 A CN200610171044 A CN 200610171044A CN 200610171044 A CN200610171044 A CN 200610171044A CN 100575319 C CN100575319 C CN 100575319C
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Abstract
Circulating solvent uses the method for azeotropic dehydration in the C5 extraction separation diene, belongs in DMF extracting and separating isoprene preparation technology.It is characterized in that: circulating solvent is dimethyl formamide DMF, adopts single tower, and circulating solvent DMF enters a collection stripping tower (1) from opening for feed (6), is 90～120 ℃ in temperature, under the tower top pressure 0.02MPa, carries out azeotropic dehydration, from discharge port (7) discharging.In DMF method separation of C 5 components in the process of diolefin, use the method for azeotropic dehydration to guarantee that a collection circulating solvent water-content reaches requirement, water content is less than 500PPm, a tower system and attached interchanger, pump, lime set jar have been reduced, reduced facility investment, reduce technique controlling difficulty, and guarantee that the circulating solvent water content reaches requirement, assurance C5 separation processes engineering can be carried out smoothly.
Description
Technical field
Circulating solvent uses the method for azeotropic dehydration in the C5 extraction separation diene, belongs in DMF extracting and separating isoprene preparation technology.
Background technology
The a considerable amount of C 5 fractions of by-product in the process of petroleum cracking system ethene, contain 40～60% the diolefins such as isoprene, cyclopentadiene and m-pentadiene of having an appointment in the C 5 fraction, these diolefin chemical property are active, it is the important source material of a lot of fine chemical products, therefore, the separation utilization of C 5 fraction is for the economic benefit that improves ethylene unit, and the comprehensive utilization petroleum resources are extremely meaningful.But C 5 fraction is close by more than 30 kinds of boiling points, the component that easily forms azeotrope is each other again formed, in order to isolate each diolefin of higher degree, industrial general employing rectifying separation is purified with the separation that the means that technologies such as extracting rectifying separates combine are carried out C 5 fraction at present, and its complex process and flow process are longer.
In the technology of C5 extraction separation diene, the DMF method is most widely used a kind of method, this be because 1, dimethyl formamide (DMF) is big to the solubleness of isoprene, selectivity is good, consumption is few, process cost is low; 2, solvent is to the carbon steel equipment non-corrosiveness, and whole process can be used plain carbon stool; 3, dimethyl formamide toxicity is little, and boiling point and isoprene difference are bigger, separate easily.
In the process of DMF method separation of C 5 cut diolefins, the water content of circulating solvent is an important controlling index.The problem that circulating solvent water-content height causes mainly contains two: the one, and circulating solvent and water generation hydrolysis reaction generate formic acid.Formic acid is understood etching apparatus on the one hand and is caused reduce equipment life, and produced simultaneously ferrous ion is a redox initiator, easily causes the polymerization of diolefin, and ferrous ion also can consume stopper.Formic acid and the Sodium Nitrite generation sodium formiate that can react on the other hand, sodium formiate is insoluble object, it is the main component of black slag in the circulating solvent, cause the obstruction of extraction tower column plate and pump easily, the circulating solvent water content has substantial connection with the generation quantity of black slag, the water content height, the solvent amount of hydrolysis is big, and it is many to generate black slag.The bad adaptability of stopper on the other hand, to moisture-sensitive, water-content exceeds standard and causes the inactivation of stopper easily.
Existing technology is in the technological process of DMF method separation of C 5 cut diolefins, the method that reduces the water-content of a collection circulating solvent is that two stripping towers are set, materials such as moisture, the hydro carbons that is steamed by the first stripping tower cat head, solvent are sent into second stripping tower, are extracted out by the second stripping Tata still and send the solvent treatment unit refining dehydration.In the prior art, facility investment is big, extracts solvent out by the second stripping Tata still and goes to make with extra care, and the load of refined unit is big, the solvent loss height that causes.
Summary of the invention
Problem to be solved by this invention is: will guarantee that not only a collection circulating solvent water content reaches sealed system requirement, reduce facility investment simultaneously, the circulating solvent in the C5 extraction separation diene that reduces the solvent loss amount uses the method for azeotropic dehydration.
The technical solution adopted for the present invention to solve the technical problems is: the method for being somebody's turn to do circulating solvent use azeotropic dehydration in the C5 extraction separation diene, it is characterized in that: circulating solvent is dimethyl formamide DMF, adopt single tower, material enters a collection stripping tower from opening for feed, in temperature is 90～120 ℃, under the tower top pressure 0.02MPa, carry out azeotropic dehydration, from discharge hole for discharge.
One collection is provided with 50～60 blocks of plates in the stripping tower, in be provided with guide float-valve, the 28th block of plate is temperature control point.
The bottom land of one collection stripping tower cat head condensate tank is provided with the dehydration bag.Dehydration is according to the liquid level timing drainage.
Because the solvent DMF Heat stability is good, toxicity is low, and discord carbon five any components form azeotrope, and water and hydro carbons can form azeotrope, therefore provide feasibility for azeotropic dehydration.
Process analog calculation: after isoprene-water reaches the vapor liquid equilibrium state, the variation of its equilibrium constant K is relevant with the water-content in the liquid phase, and equilibrium constant K is a function with temperature, pressure, is not moisture in the liquid phase in equilibrium constant K 〉=1.125 therefore.And under constant pressure (P=1.2000kg/cm2), after isoprene-water reached the vapor liquid equilibrium state, temperature was greater than 110 ℃, and the water-content in the gas phase just can account for to mix forms 100% of interior all water.The boiling point of water hydrocarbon azeotrope is well below the boiling point of DMF, so azeotropic dehydration is fully feasible.
Compared with prior art, the present invention's circulating solvent in the C5 extraction separation diene uses the beneficial effect that method had of azeotropic dehydration to be: a collection stripping tower is designed to 50～60 blocks of column plates, use guide float-valve to improve tray efficiency, the 28th plate temperature value of this tower is designed to the technology controlling and process point, this plate temperature is controlled at the 90-120 ℃ of purpose that can realize azeotropic dehydration, tower still aqueous solvent content reaches the control requirement, with the suitable amplification of cat head condensate tank design margin and at dehydration bag of bottom land design, make the hydrocarbon water mixture that be arranged enough rest times, and remove moisture content from the dehydration bag.After device was driven, through adjusting T602 tower the 28th plate temperature value, moisture can be deviate from from cat head fully, and tower still circulating solvent is reached＜requirement of 500PPm.
Description of drawings
Fig. 1 is the structural representation of stripping tower of the present invention;
Fig. 2 is isoprene of the present invention-water balance coefficient (K) figure;
Fig. 3 is isoprene of the present invention-water system T-X-Y (temperature-liquid phase composition-gas phase is formed) figure.
Fig. 1-the 3rd, most preferred embodiment of the present invention, wherein: 1 one collection stripping towers, 2 lime set pumps, 3 dehydration bags, 4 condensate tanks, 5 overhead condensers, 6 opening for feeds, 7 discharge ports.
Embodiment
Below in conjunction with accompanying drawing 1-3 to of the present invention in the C5 extraction separation diene circulating solvent use the method for azeotropic dehydration to be described further:
With reference to Fig. 1:
Material enters a collection stripping tower 1 through opening for feed 6, and this tower is designed to 50～60 blocks of plates, and tower top pressure 0.02MPa uses guide float-valve with the raising tray efficiency, or adopts common float valve.The 28th plate temperature value of one collection stripping tower 1 is designed to the technology controlling and process point, be controlled at＞90 ℃ of purposes that can realize azeotropic dehydration through calculating this plate temperature, therefore temperature is 90～120 ℃ in the collection stripping tower 1, tower still aqueous solvent content reaches the control requirement, with a collection stripping tower suitable amplification of 1 cat head condensate tank, 4 design margins and at dehydration bag 3 of bottom land design, make the hydrocarbon water mixture that be arranged enough rest times, and remove moisture content from dehydration bag 3.
After device was driven, through adjusting a collection stripping tower 1 the 28th plate temperature value, moisture can be deviate from from cat head fully, and tower still circulating solvent is reached＜requirement of 500PPm.
Tower still circulating solvent water-content and the 28th plate temperature relation see Table 1:
Table 1
| Time | The 28th plate temperature value, ℃ | Tower top pressure, MPaG | Tower still aqueous solvent content, ppm |
| 2006.6.2 | 112.3 | 0.022 | 120 |
| 2006.6.5 | 90.6 | 0.02 | 89 |
| 2006.6.10 | 98 | 0.021 | 76 |
| 2006.6.15 | 120.3 | 0.02 | 45 |
| 2006.6.20 | 95.6 | 0.02 | 70 |
Therefore, control one collection stripping tower the 28th plate temperature value is at 90～120 ℃, and tower top pressure 0.02MPa can accomplish to keep tower still circulating solvent water-content＜500PPm fully.Simultaneously, according to the liquid level timing drainage, can realize the purpose of azeotropic dehydration to the dehydration bag 3 of cat head condensate tank 4 fully.
Fig. 2-the 3rd passes through analog calculation water hydrocarbon under 0.02MPaG pressure, the azeotropic situation of isoprene and water.
With reference to Fig. 2:
Being isoprene--the implication of water balance coefficient (K) figure is: after isoprene-water reaches the vapor liquid equilibrium state, the variation of its equilibrium constant K is relevant with the water-content in the liquid phase, and equilibrium constant K be one with temperature, the relevant function of pressure, therefore be not moisture in the liquid phase in equilibrium constant K 〉=1.125.
With reference to Fig. 3:
The implication that is isoprene-water system T-X-Y (temperature-liquid phase composition-gas phase is formed) figure is: under constant pressure (P=1.2000kg/cm2), after isoprene-water reaches the vapor liquid equilibrium state, temperature is greater than 110 ℃, and the water-content in the gas phase just can account for to mix forms 100% of interior all water.
Claims (3)
1, the method for circulating solvent use azeotropic dehydration in the C5 extraction separation diene, it is characterized in that: circulating solvent is dimethyl formamide DMF, adopt single tower, material enters a collection stripping tower (1) from opening for feed (6), in temperature is 90～120 ℃, under the tower top pressure 0.02MPa, carry out azeotropic dehydration, from discharge port (7) discharging.
2, according to claim 1 in the C5 extraction separation diene circulating solvent use the method for azeotropic dehydration, it is characterized in that: in the collection stripping tower (1) 50～60 blocks of plates are set, in be provided with guide float-valve, the 28th block of plate is temperature control point.
3, according to claim 1 in the C5 extraction separation diene circulating solvent use the method for azeotropic dehydration, it is characterized in that: the bottom land of collection stripping (a 1) column overhead condensate tank (4) is provided with dehydration bag (3).
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| Application Number | Priority Date | Filing Date | Title |
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| CN200610171044A CN100575319C (en) | 2006-12-31 | 2006-12-31 | Circulating solvent uses the method for azeotropic dehydration in the C5 extraction separation diene |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200610171044A CN100575319C (en) | 2006-12-31 | 2006-12-31 | Circulating solvent uses the method for azeotropic dehydration in the C5 extraction separation diene |
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| CN101209950A CN101209950A (en) | 2008-07-02 |
| CN100575319C true CN100575319C (en) | 2009-12-30 |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB585211A (en) * | 1943-08-17 | 1947-02-03 | Standard Oil Dev Co | An improved process for the separation of diolefins from mixtures thereof with other hydrocarbons |
| GB586474A (en) * | 1943-11-01 | 1947-03-20 | Standard Oil Dev Co | Improvements in or relating to the separation of hydrocarbons from mixtures thereof |
| GB587241A (en) * | 1944-07-04 | 1947-04-18 | Standard Oil Dev Co | Process for the treatment of mixtures of hydrocarbons to effect segregation of desired hydrocarbons |
| GB588037A (en) * | 1944-07-18 | 1947-05-13 | Standard Oil Dev Co | Process for the separation of c diolefins from mixtures thereof with other hydrocarbons |
| US3038315A (en) * | 1958-10-02 | 1962-06-12 | Scient Design Co | Chemical process |
| GB1556962A (en) * | 1977-11-10 | 1979-12-05 | Sterlitamax Opytpromysh Neftek | Method for recovering formaldehyde from aqueous solutions thereof |
-
2006
- 2006-12-31 CN CN200610171044A patent/CN100575319C/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB585211A (en) * | 1943-08-17 | 1947-02-03 | Standard Oil Dev Co | An improved process for the separation of diolefins from mixtures thereof with other hydrocarbons |
| GB586474A (en) * | 1943-11-01 | 1947-03-20 | Standard Oil Dev Co | Improvements in or relating to the separation of hydrocarbons from mixtures thereof |
| GB587241A (en) * | 1944-07-04 | 1947-04-18 | Standard Oil Dev Co | Process for the treatment of mixtures of hydrocarbons to effect segregation of desired hydrocarbons |
| GB588037A (en) * | 1944-07-18 | 1947-05-13 | Standard Oil Dev Co | Process for the separation of c diolefins from mixtures thereof with other hydrocarbons |
| US3038315A (en) * | 1958-10-02 | 1962-06-12 | Scient Design Co | Chemical process |
| GB1556962A (en) * | 1977-11-10 | 1979-12-05 | Sterlitamax Opytpromysh Neftek | Method for recovering formaldehyde from aqueous solutions thereof |
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Assignee: Maoming Luhua Chemical Co., Ltd. Assignor: Zibo Luhua Hongjin Chemical Co.,Ltd. Contract record no.: 2011440000312 Denomination of invention: Method for using azeotropy dehydration for circulation solvent in C5 extraction separation diene Granted publication date: 20091230 License type: Exclusive License Open date: 20080702 Record date: 20110407 |
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Address after: 255411 No. 3, Feng Bei Road, Zhangdian District, Shandong, Zibo Patentee after: ZIBO LUHUA HONGJIN NEW MATERIAL CO., LTD. Address before: 255411 No. 3, Feng Bei Road, Zhangdian District, Shandong, Zibo Patentee before: Zibo Luhua Hongjin Chemical Co.,Ltd. |
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Address after: 255411 No. 3, Feng Bei Road, Zhangdian District, Shandong, Zibo Patentee after: Zibo luhuahongjin New Material Group Co.,Ltd. Address before: 255411 No. 3, Feng Bei Road, Zhangdian District, Shandong, Zibo Patentee before: ZIBO LUHUA HONGJIN NEW MATERIAL Co.,Ltd. |
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