CN105712820A - Novel technology for concentrating post-MTBE C4 - Google Patents
Novel technology for concentrating post-MTBE C4 Download PDFInfo
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Abstract
The invention discloses a novel technology for concentrating post-MTBE C4. The technology comprises that a C4 raw material is introduced into an extraction absorbing tower through the lower part of the extraction absorbing tower, absorbents are introduced into the extraction absorbing tower through the upper part and the middle part of the extraction absorbing tower and are respectively used as an absorbent 1 and an absorbent 2, the material at the top of the extraction absorbing tower is butane, the material at the bottom of the extraction absorbing tower enters the upper part of an desorption tower 1, the material at the top of the desorption tower 1 enters the upper part of an desorption tower 2, a part of the material at the tower bottom is used as the absorbent 2 for recycle, a part of the material at the tower bottom enters the lower part of the desorption tower 2, the material at the top of the desorption tower 2 is a butene product, the material collected from the middle of the desorption tower 2 is circulated to the lower part of the desorption tower 1 and the material at the desorption tower 2 bottom as the absorbent 1 is recycled. The technology can produce a high-purity butane product and a butylene product under conditions of a low tower bottom temperature and a low liquid-gas ratio and has a butylene recovery rate of 99% or more and an n-butene concentration greater than or equal to 99.9%.
Description
Technical field
The present invention relates to the concentration new technology of carbon four after a kind of ether, particularly to the extraction rectifying method of a kind of butylene Yu butane.
Background technology
The method n-butene method of the unique large-scale production of butanone process units in current global range, after ether, carbon four is as the raw material of n-butene legal system butanone technique, the fresh n-butene concentration (wt%) >=97% of its technological requirement, and in carbon four, n-butene concentration (wt%) is generally 40～50% after ether, other great majority are butane, so needing n-butene and alkane are easily separated, it is achieved the concentration of butylene.
Owing to the boiling point of butane Yu butylene is close, relative volatility is close to 1, it is difficult to separate with conventional distillation, need to be easily separated with extraction fractional distillation, namely one or more polar compounds are added on the top of rectifying column as solvent, make the relative volatility of butane and butylene in extractive distillation column increase, improve the efficiency separated.Can be used for the extractant of extracting rectifying and have a lot, such as the mixture etc. of N-N-formyl morpholine N, morpholine, N-N-formyl morpholine N and morpholine mixtures, sulfolane, N-Methyl pyrrolidone, butanone and N-N-formyl morpholine N, morpholine and N-N-formyl morpholine N.The separating of butylene and butane is generally two towers and carries out, and a tower is for extracting absorption tower, and another tower is desorber.
There are problems in the extraction absorption technique of existing separating butane and butylene: (1) Conventional solvents is little to the dissolubility of C4 alkene, causes common extraction absorption tower inner transmission matter efficiency low.(2) Solvent quantity is too big, in order to improve mass-transfer efficiency, it is ensured that the response rate of butane and butylene, it is necessary to increase considerably liquid-gas ratio, existing absorbent liquid-gas ratio have even as high as 20～22, corresponding equipment is huge, and energy consumption is also high, very uneconomical.(3) purpose of desorber and solvent recovery tower is that tower top to obtain qualified butylene, and tower reactor obtains qualified extractant or pressurized operation or atmospheric operation.If pressurized operation, bottom temperature is higher, and during as used morpholine and N-N-formyl morpholine N mixture as solvent, desorber column bottom temperature, up to 210～230 DEG C, can cause decomposition or the coking of solvent；If atmospheric operation, butylene under the normal pressure of tower top about 45 DEG C cannot realize condensation, it is necessary to deep cooling or compression, energy consumption increases a lot.(4) butylene yield is relatively low, and especially industrial when butylene purity reaches more than 95%, butylene yield only has about 75%, loses bigger.
CN101050159A proposes method and the device of a kind of separating butane and butylene, this process have employed four-column process flow, including pretreatment of raw material tower, heavy constituent extractive distillation column, weight component extracting rectifying column and degassing tower, extractant adopts conventional extraction agent, one or more mixture in morpholine, N-N-formyl morpholine N, butanone, N-Methyl pyrrolidone.The effect of the shortcoming of this technique employing conventional extraction agent on the one hand is very not notable, yet suffer from the problems that existing extraction absorbent exists, four-column process flow relatively two towers or three-column process flow are complicated a lot of on the other hand, and investment, material consumption and energy consumption double substantially, but effect is without too big improvement.
Prior art from separating butane and butylene, on the one hand preferably new suitable dicyandiamide solution is still the important goal of technological development, significant for improving the purity of butylene and concentration, reduction material consumption and energy consumption, the economy that develops skill by optimization technological process on the other hand.
Summary of the invention
For the deficiency of currently available technology, the present invention provides the concentration new technology of carbon four after a kind of ether.Two-stage is adopted to extract the technological process of absorption, two stage rectification desorbing, two-stage Matter Transfer, obtaining highly purified butane product and butylene product when and low liquid-gas ratio relatively low at column bottom temperature, the response rate of butylene reaches more than 99%, n-butene concentration >=99.9%.
The concentration new technology of carbon four after a kind of ether of the present invention, including following content: carbon four raw material is introduced by the bottom extracting absorption tower, absorbent introduces from the top and middle part that extract absorption tower and is designated as absorbent 1, absorbent 2 respectively, introduce position 2～15 blocks of column plates of difference, preferably 5～12 blocks of column plates, the volume ratio of introduction volume is 1:1～1:30, it is preferable that 1:5～1:20；The tower top material extracting absorption tower is butane, and the materials at bottom of tower extracting absorption tower enters the top of desorber 1；The tower top material of desorber 1 enters the top of desorber 2, and materials at bottom of tower recycles partly as absorbent 2, is partially into the bottom of desorber 2；The tower top material of Analytic Tower 2 is butylene product, and in the middle part of Analytic Tower 2, extraction material loops back the bottom of desorber 1, and materials at bottom of tower recycles as absorbent 1.
In present invention process, absorbent can adopt existing absorbent can also adopt homemade absorbent, it is preferred to use homemade absorbent.Absorbent 1, absorbent 2 composition can be the same or different, it is preferable that the latter.
In present invention process, absorbent 1, absorbent 2 contain dimethyl sulfoxide that mass content is 60%～90%, 5%～30% respectively, preferably contain the dimethyl sulfoxide that mass content is 65%～80%, 10%～25% respectively, surplus is one or more in morpholine, N-N-formyl morpholine N, butanone, N-Methyl pyrrolidone, sulfolane, preferred morpholine and N-N-formyl morpholine N, mass ratio 1:0.1～the 1:8 of morpholine and N-N-formyl morpholine N, it is preferable that 1:1～1:2.
In present invention process, it is 1:0.5～1::10 that desorber 1 materials at bottom of tower recycles the mass ratio with entrance desorber 2 bottom as absorbent 2, it is preferable that 1:1～1:4.
In the inventive method, extracting absorption tower and desorber is packed tower, extracting absorption tower number of theoretical plate is 5～28 pieces, and desorber 1 number of theoretical plate is 4～10 pieces, and desorber 2 number of theoretical plate is 5～15 pieces.The introducing position of absorbent 1, for extracting absorption tower the 2nd～6 block of plate from top to bottom, extracts and absorbs materials at bottom of tower to enter the position of desorber 1 be the 2nd～5 block of plate from top to bottom；It is the 2nd～5 block of plate from top to bottom that the tower top material of desorber 1 enters the position of desorber 2, and the position of desorber 1 part materials at bottom of tower portion entrance desorber 2 is the 6th～10 block of plate from top to bottom；In the middle part of desorber 2, extraction material loops back the position of desorber 1 is the 6th～10 block of plate from top to bottom.
In present invention process, the operating condition extracting absorption tower is as follows: total liquid-gas ratio is 2～15, the tower top temperature extracting absorption tower is 40～45 DEG C, tower top pressure is 0.5～0.6MPa(G), column bottom temperature is 80～130 DEG C, and reflux ratio is 1～5, preferably total liquid-gas ratio is 4～8,, column bottom temperature is 95～115 DEG C, and reflux ratio is 2～4。
In present invention process, the operating condition of desorber 1 is as follows: tower top temperature is 40～45 DEG C, and tower top pressure is 0.3～0.4MPa(G), column bottom temperature is 80～100 DEG C, and reflux ratio is 1～5.Preferred column bottom temperature is 85～95 DEG C, and reflux ratio is 2～4.
In present invention process, the operating condition of desorber 2 is as follows: tower top temperature 80～100 DEG C, and tower top pressure is 0.3～0.4MPa(G), column bottom temperature is 110～140 DEG C, and reflux ratio is 1～5.Preferred tower top temperature is 85～95 DEG C, and column bottom temperature is 115～125 DEG C, and reflux ratio is 2～4.
The advantage of present invention process is as follows:
(1) extracting absorption technique and adopt efficient combination absorbent, assimilation effect improves 10%～30% than prior art, it is possible to reduce liquid-gas ratio.
(2) this technique is provided with two-stage and extracts absorption technique, further increases extraction assimilation effect, and reduces liquid-gas ratio further.
(3) according to extracting the butene concentration of differing heights in absorption tower, combination is extracted absorbent and introduces from the diverse location of tower, be favorably improved assimilation effect；
(4) for desorption process feature and energy consumption bottleneck, adopt the technological process of two stage rectification desorbing, make the butylene of 65%～85% realize desorbing when the comparison mitigation of desorber (), it is possible to reduce total power consumption during desorbing.
(5) absorbed by Optimized Extraction, Matter Transfer between one-level desorbing and three processes of two grades of desorbings, it is achieved technique effect, energy consumption and material consumption than existing four towers and above technique effect more preferably.
(6) butylene yield >=99% that the present invention obtains, butylene purity >=99.9%.
Accompanying drawing explanation
Fig. 1 is the process flow diagram of the present invention
Wherein, 2 is absorbent 1；3 is carbon four mixed gas feed；4 is absorbent 2；5 is butane material；6 for extracting absorption tower；7 is desorber 1 top charging；8 is desorber 1 bottom charging；9 is desorber 1；10 is desorber 2 top charging；11 is desorber 2 bottom charging；12 is butylene material；13 is desorber 2；14 is the desorber 2 recycle stock to extraction absorption tower, and 15 is absorbent discharges material.
Detailed description of the invention
Illustrate with embodiment, this technological invention scheme to be described in detail below in conjunction with accompanying drawing, but be not so limited the present invention.
Present invention process is realized by such mode: first carbon four mixed gas feed 3 is introduced by the bottom extracting absorption tower 6, absorbent 24 introduces from the middle part extracting absorption tower, absorbent 12 introduces from the top extracting absorption tower, butylene in carbon four raw material is extracted absorption step by step by absorbent 1 and absorbent 2, materials at bottom of tower is the top that desorber 1 top charging 7 introduces desorber 19, the material of desorber 1 is after a desorbing, gas phase is that desorber 2 top charging 10 introduces the top of desorber 2 and carries out secondary desorbing, Partial Liquid Phase loops back and reuses in the middle part of extraction absorption tower, another part enters desorber 213 as the charging of desorber 2 bottom and carries out secondary desorbing；It is butylene product 12 that desorber 2 solves the gas phase of sucking-off, and in the middle part of tower, extraction material returns to the bottom of desorber 1, and materials at bottom of tower is back to extraction top, absorption tower, reuses as absorbent 1.
The raw material that embodiment and comparative example use is carbon four after ether, and composition is in Table 1.
Table 1
Embodiment 1
Containing the dimethyl sulfoxide that mass content is 65%～80%, 10%～25% in absorbent 1, absorbent 2 respectively, surplus is morpholine and N-N-formyl morpholine N, the mass ratio 1:1 of morpholine and N-N-formyl morpholine N.First composite absorber, the second composite absorber introduction volume volume ratio be 1:5, desorber 1 materials at bottom of tower as absorbent 2 recycle with enter desorber 2 bottom mass ratio be 1:1.Extracting absorption tower and desorber is packed tower, extracting absorption tower number of theoretical plate is 10 pieces, and desorber 1 number of theoretical plate is 6 pieces, and desorber 2 number of theoretical plate is 8 pieces.The introducing position of absorbent 1 is the 2nd layer from top to bottom of absorption tower of extraction, and the introducing position of absorbent 2 is for extracting the 5th layer from top to bottom of absorption tower, and extracting the position absorbing materials at bottom of tower entrance desorber 1 is the 2nd layer from top to bottom；It is the 2nd layer from top to bottom that the tower top material of desorber 1 enters the position of desorber 2, and it is the 7th layer from top to bottom that desorber 1 part materials at bottom of tower portion enters the position of desorber 2；In the middle part of desorber 2, extraction material loops back the position of desorber 1 is the 6th layer from top to bottom.Operating condition is in Table 2, and separating resulting is in Table 3, and butane purity is 99%, and butylene purity reaches 99.9%.
Table 2
Table 3
Embodiment 2
Containing the dimethyl sulfoxide that mass content is 65%～80%, 10%～25% in absorbent 1, absorbent 2 respectively, surplus is morpholine and N-N-formyl morpholine N, the mass ratio 1:2 of morpholine and N-N-formyl morpholine N.First composite absorber, the second composite absorber introduction volume volume ratio be 1:1～1:30, desorber 1 materials at bottom of tower as absorbent 2 recycle with enter desorber 2 bottom mass ratio be 1:4.Extracting absorption tower and desorber is packed tower, extracting absorption tower number of theoretical plate is 22 pieces, and desorber 1 number of theoretical plate is 10 pieces, and desorber 2 number of theoretical plate is 15 pieces.The introducing position of absorbent 1 is the 6th layer from top to bottom of absorption tower of extraction, and the introducing position of absorbent 2 is for extracting absorption tower 11th layer from top to bottom, and extracting the position absorbing materials at bottom of tower entrance desorber 1 is the 5th layer from top to bottom；It is the 5th layer from top to bottom that the tower top material of desorber 1 enters the position of desorber 2, and it is the 10th layer from top to bottom that desorber 1 part materials at bottom of tower portion enters the position of desorber 2；In the middle part of desorber 2, extraction material loops back the position of desorber 1 is the 9th layer from top to bottom.Operating condition is in Table 4, and separating resulting is in Table 5, and butane purity is 99%, and butylene purity reaches 99.9%.Operating condition is in Table 6, and separating resulting is in Table 7, and butane purity is 99%, and butylene purity reaches 99.9%.
Table 4
Table 5
Embodiment 3
The biabsorption agent adopting the present invention extracts and absorbs flow process and two grades of desorbing flow processs, by the C4 raw material of table 1 by the bottom extracting absorption tower, first absorbent adopts the sulfolane containing 50wt% and the mixture that mass ratio is the morpholine of 1:1, N-N-formyl morpholine N, second absorbent adopts containing the mixture that 25wt% sulfolane and mass ratio are the morpholine of 1:1, N-N-formyl morpholine N, after absorption tower absorption and desorption tower desorbing, complete the purification of C4 raw material, absorption tower, desorber 1, Analytic Tower 2 operating condition identical with embodiment 1.Separating resulting is in Table 6.
Table 6
Comparative example 1
Adopting device and the operating condition of embodiment 1, simply top, absorption tower does not introduce absorbent 2, and absorbent does not recycle.Separating resulting is in Table 7.
Table 7
| Component | Iso-butane | Butene-1 | Normal butane | Trans-butene-2 | Cis-butene-2 |
| Butane material, wt% | 62.97 | 9.56 | 22.37 | 2.54 | 2.56 |
| Butylene material, wt% | 1.85 | 48.45 | 11.72 | 23.61 | 14.37 |
Claims (14)
1. the concentration new technology of carbon four after an ether, it is characterized in that: include following content: carbon four raw material is introduced by the bottom extracting absorption tower, absorbent introduces from the top and middle part extracting absorption tower, it is designated as absorbent 1, absorbent 2 respectively, introducing position 2～15 blocks of column plates of difference, the volume ratio of introduction volume is 1:1～1:30；The tower top material extracting absorption tower is butane, and the materials at bottom of tower extracting absorption tower enters the top of desorber 1；The tower top material of desorber 1 enters the top of desorber 2, and materials at bottom of tower recycles partly as absorbent 2, is partially into the bottom of desorber 2；The tower top material of Analytic Tower 2 is butylene product, and in the middle part of Analytic Tower 2, extraction material loops back the bottom of desorber 1, and materials at bottom of tower recycles as absorbent 1.
2. technique according to claim 1, it is characterised in that: absorbent 1, absorbent 2 introduce position 5～12 blocks of column plates of difference, and the volume ratio of introduction volume is 1:5～1:20.
3. technique according to claim 1, it is characterized in that: contain the dimethyl sulfoxide that mass content is 60%～90%, 5%～30% in absorbent 1, absorbent 2 respectively, surplus is one or more in morpholine, N-N-formyl morpholine N, butanone, N-Methyl pyrrolidone, sulfolane.
4. the technique according to claim 1 or 3, it is characterized in that: absorbent 1, absorbent 2 contain dimethyl sulfoxide that mass content is 65%～80%, 10%～25% respectively, surplus is morpholine and N-N-formyl morpholine N, the mass ratio 1:0.1～1:8 of morpholine and N-N-formyl morpholine N.
5. technique according to claim 1, it is characterised in that: it is 1:0.5～1::10 that desorber 1 materials at bottom of tower recycles the mass ratio with entrance desorber 2 bottom as absorbent 2.
6. technique according to claim 5, it is characterised in that: it is 1:1～1:4 that desorber 1 materials at bottom of tower recycles the mass ratio with entrance desorber 2 bottom as absorbent 2.
7. technique according to claim 1, it is characterised in that: extracting absorption tower and desorber is packed tower, extracting absorption tower number of theoretical plate is 5～28 pieces, and desorber 1 number of theoretical plate is 4～10 pieces, and desorber 2 number of theoretical plate is 5～15 pieces.
8. technique according to claim 1, it is characterised in that: the introducing position of absorbent 1 is for extracting absorption tower the 2nd～6 block of plate from top to bottom；Extract and absorb materials at bottom of tower to enter the position of desorber 1 be the 2nd～5 block of plate from top to bottom；It is the 2nd～5 block of plate from top to bottom that the tower top material of desorber 1 enters the position of desorber 2, and the position of desorber 1 part materials at bottom of tower portion entrance desorber 2 is the 6th～10 block of plate from top to bottom；In the middle part of desorber 2, extraction material loops back the position of desorber 1 is the 6th～10 block of plate from top to bottom.
9. technique according to claim 1, it is characterized in that: the operating condition extracting absorption tower is as follows: total liquid-gas ratio is 2～15, and the tower top temperature extracting absorption tower is 40～45 DEG C, and tower top pressure is 0.5～0.6MPa(G), column bottom temperature is 80～130 DEG C, and reflux ratio is 1～5。
10. technique according to claim 9, it is characterised in that: total liquid-gas ratio is 4～8, column bottom temperature is 95～115 DEG C, and reflux ratio is 2～4。
11. technique according to claim 1, it is characterised in that: the operating condition of desorber 1 is as follows: tower top temperature is 40～45 DEG C, and tower top pressure is 0.3～0.4MPa(G), column bottom temperature is 80～100 DEG C, and reflux ratio is 1～5.
12. technique according to claim 11, it is characterised in that: column bottom temperature is 85～95 DEG C, and reflux ratio is 2～4.
13. technique according to claim 1, it is characterised in that: the operating condition of desorber 2 is as follows: tower top temperature 80～100 DEG C, and tower top pressure is 0.3～0.4MPa(G), column bottom temperature is 110～140 DEG C, and reflux ratio is 1～5.
14. technique according to claim 13, it is characterised in that: tower top temperature is 85～95 DEG C, and column bottom temperature is 115～125 DEG C, and reflux ratio is 2～4.
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| CN108929188A (en) * | 2017-05-23 | 2018-12-04 | 中国石油化工股份有限公司 | From mixing C4The method of separation of extractive distillation butane and butylene in hydrocarbon raw material |
| CN115340439A (en) * | 2021-05-14 | 2022-11-15 | 浙江蓝天环保高科技股份有限公司 | Absorption purification method of hexafluorobutadiene |
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