CN203648128U - Rectification device capable of reducing energy consumption of azeotropic distillation in sec-butyl acetate separating process - Google Patents
Rectification device capable of reducing energy consumption of azeotropic distillation in sec-butyl acetate separating process Download PDFInfo
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- CN203648128U CN203648128U CN201320844163.9U CN201320844163U CN203648128U CN 203648128 U CN203648128 U CN 203648128U CN 201320844163 U CN201320844163 U CN 201320844163U CN 203648128 U CN203648128 U CN 203648128U
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- tower
- rectifying column
- return tank
- column
- overhead
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- DCKVNWZUADLDEH-UHFFFAOYSA-N sec-butyl acetate Chemical compound CCC(C)OC(C)=O DCKVNWZUADLDEH-UHFFFAOYSA-N 0.000 title claims abstract description 26
- 238000010533 azeotropic distillation Methods 0.000 title claims abstract description 15
- 238000005265 energy consumption Methods 0.000 title claims abstract description 11
- 238000000034 method Methods 0.000 title abstract description 8
- 230000008569 process Effects 0.000 title abstract description 6
- 239000000463 material Substances 0.000 claims abstract description 24
- 238000000605 extraction Methods 0.000 claims abstract description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 150000002148 esters Chemical class 0.000 claims abstract description 15
- 239000007791 liquid phase Substances 0.000 claims abstract description 15
- 238000000926 separation method Methods 0.000 claims abstract description 13
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 30
- 238000010992 reflux Methods 0.000 claims description 27
- 239000002994 raw material Substances 0.000 claims description 6
- 238000002360 preparation method Methods 0.000 claims description 3
- 238000007670 refining Methods 0.000 abstract 3
- 238000010438 heat treatment Methods 0.000 abstract 1
- 239000012808 vapor phase Substances 0.000 abstract 1
- 239000012071 phase Substances 0.000 description 8
- 239000000306 component Substances 0.000 description 5
- 238000009833 condensation Methods 0.000 description 4
- 230000005494 condensation Effects 0.000 description 4
- 239000004215 Carbon black (E152) Substances 0.000 description 3
- 150000001336 alkenes Chemical class 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 229930195733 hydrocarbon Natural products 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- VXNZUUAINFGPBY-UHFFFAOYSA-N 1-Butene Chemical compound CCC=C VXNZUUAINFGPBY-UHFFFAOYSA-N 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- BTANRVKWQNVYAZ-UHFFFAOYSA-N butan-2-ol Chemical compound CCC(C)O BTANRVKWQNVYAZ-UHFFFAOYSA-N 0.000 description 2
- 239000000470 constituent Substances 0.000 description 2
- 150000002430 hydrocarbons Chemical class 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- DURPTKYDGMDSBL-UHFFFAOYSA-N 1-butoxybutane Chemical group CCCCOCCCC DURPTKYDGMDSBL-UHFFFAOYSA-N 0.000 description 1
- -1 C12 hydrocarbon Chemical class 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000004939 coking Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000003623 enhancer Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000032050 esterification Effects 0.000 description 1
- 238000005886 esterification reaction Methods 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000012429 reaction media Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 235000013599 spices Nutrition 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 238000011144 upstream manufacturing Methods 0.000 description 1
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- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The utility model discloses a rectification device capable of reducing energy consumption of azeotropic distillation in a sec-butyl acetate separating process. The device comprises a rectifying tower (1), an overhead condenser (2), an overhead return tank (3), an overhead ester return pump (4), a side-draw condenser (5) and a tower bottom reboiler (6). The device is characterized in that 1-10 side-draw liquid phase material extraction lines (7) are drawn from the upper part of the rectifying tower (1) to be connected with the overhead return tank (3). According to the device disclosed by the utility model, the vapor phase load of an azeotropic distillation tower is reduced, the heat exchange area of the overhead condenser is reduced and the equipment investment is lowered, and meanwhile, the use level of circulating water of the overhead condenser is reduced and the use level of feedstock pre-heating steam of a subsequent refining tower is reduced, so that the energy consumption is saved. The content of C4 entering into the feedstock of the refining tower is reduced, thereby facilitating the separation efficiency of the refining tower.
Description
Technical field
The utility model relates to a kind of rectifier unit that reduces azeotropic distillation energy consumption in sec-butyl acetate separation process.
Background technology
Sec-butyl acetate is a kind of novel dissolvent, there is the features such as low toxic and environment-friendly, solvability be strong, can be used as spices, solvent, drug absorption enhancer, reaction medium component, extractant component, metal cleaner etc., of many uses, be subject to gradually people and more and more pay close attention to.At present, domestic sec-butyl acetate mainly adopts the technique of alkene addition process one-step synthesis to produce, and utilizes n-butene in acetic acid and refinery's hybrid C 4 to produce for raw material.With respect to the traditional handicraft of alcohol esterification process, acetic acid and n-butene synthetic method have that raw material sources are extensive, cost is little, the feature of good in economic efficiency, environmental protection.
In existing alkene addition process one-step synthesis sec-butyl acetate preparation technology, because the boiling point of acetic acid and sec-butyl acetate is more approaching, need to carry out azeotropic distillation with separating acetic acid and sec-butyl acetate.In existing azeotropic distillation separating technology, the raw material of coming from upstream equipment is undertaken entering azeotropy rectification column preheating by feed preheater, in azeotropy rectification column, the azeotropic mixture azeotropic of the azeotropic mixture of acetic acid and water, C8 alkene and water is to tower top, after overhead condenser condensation, enter return tank of top of the tower and carry out layering, part water enters respectively overhead reflux mutually with partial solvent, and another part solvent phase enters treating column and refines after preheating.Mainly there is following problem in existing technique: 1, azeotropic distillation column overhead vapour phase load is large, and it is large that what overhead condenser was required change area; 2, the cold rear temperature of tower top material is low, and heat utilization rate is lower; 3, C4 dissolves morely in overhead condensation liquid, brings into and affects treating column operation after treating column.
Utility model content
The purpose of this utility model is to provide a kind of novel sec-butyl acetate azeotropic distillation device, and high for overcoming existing azeotropic distillation process energy consumption, thermal efficiency utilization rate is low, the problem that overhead materials feed collet band C4 is many.
The utility model provides a kind of rectifier unit that reduces azeotropic distillation energy consumption in sec-butyl acetate separation process, described rectifier unit comprises rectifying column, overhead condenser, return tank of top of the tower, tower top ester reflux pump, side line extraction condenser and tower bottom reboiler, rectifying column has charging aperture, top exit, outlet at bottom, the top exit of rectifying column is connected with overhead condenser and return tank of top of the tower successively by pipeline, an outlet (preferably side outlet) of return tank of top of the tower is connected with the top of tower top ester reflux pump and rectifying column successively by pipeline, the side line extraction line of rectifying column bottom is connected with side line extraction condenser, the bottom of rectifying column is provided with tower bottom reboiler, the top of rectifying column is drawn 1-10 bar and (is preferably 1-8 bar, more preferably 1-5 bar, more preferably 1-3 bar) side line liquid phase material extract out line be connected with return tank of top of the tower.
In the utility model, the charging of introducing from the charging aperture of described rectifying column is that the mixture acetic acid and C4 raw material reaction removes light component (after de-light component rectifying column rectifying) product afterwards, in this product, the part by weight of acetic acid is generally 20～80 % by weight, the part by weight of sec-butyl acetate is generally 20～75 % by weight, optional other accessory substances of 0～15 % by weight that exist, described other accessory substances include but not limited to sec-butyl alcohol, secondary butyl ether, C5 hydrocarbon, C8 hydrocarbon, one or more in C12 hydrocarbon, their ratios in tower bottom product are respectively 0.01～1.0 % by weight, 0.01～1.0 % by weight, 0.01～1.0 % by weight, 0.01～5.0 % by weight, 0.01～10.0 % by weight, in this product, also may contain the water of 0.1-20%.
In the utility model, the rectifying section of described rectifying column is preferably plank frame, and this side line liquid phase material that is conducive to rectifier is extracted out.
In the utility model, the theoretical cam curve of described rectifying column is preferably 30-150 piece, more preferably 35-120 piece, more preferably 40-100 piece, more preferably 45-80 piece.
In the utility model, described side line liquid phase material is extracted line out and is preferably disposed on more than rectifying column charging aperture 5 positions more than column plate, more preferably more than charging aperture 8 positions more than column plate, the more preferably position of the above 10 blocks of column plates of charging aperture.In the utility model, in order not reduce the purity of sec-butyl acetate in return tank of top of the tower, guarantee separative efficiency and the effect of follow-up treating column, need to select the tower tray that azeotropy rectification column rectifying section is suitable to carry out the extraction of side line liquid phase.The present utility model people finds, has a sec-butyl acetate Heng Nong district, the region that the concentration that so-called " Heng Nong district " is exactly certain material substantially can not change in rectifying column at the rectifying section of azeotropy rectification column.So, in the utility model, the position that side line liquid phase material is extracted line out should be arranged at sec-butyl acetate in rectifying section Heng Nong district, find after deliberation, sec-butyl acetate Heng Nong district is 5 positions more than tower tray more than charging aperture, be preferably 8 positions more than column plate, more preferably the position of the above 10 blocks of column plates of charging aperture.
In the utility model, preferably, the outlet at bottom of described rectifying column is connected with drawing pump at the bottom of tower by pipeline.In order to prevent heavy constituent (component more than C12) enrichment at the bottom of tower, cause the concentration of materials at bottom of tower to reduce, heat transfer effect variation at the bottom of tower, and the generation of the phenomenon such as the coking of bottom reboiler, drawing pump at the bottom of can tower being set at the bottom of azeotropy rectification column tower, discharges the heavy constituent at the bottom of tower.
In the utility model, preferably, the feeding line of described rectifying column is provided with feed preheater.In order to increase the separative efficiency of tower, reduce the load of azeotropy rectification column bottom reboiler, a feed preheater can be set on the feeding line of azeotropy rectification column, by the feeding preheating of azeotropy rectification column to 80-100 ℃.
In the utility model, preferably, another outlet of described return tank of top of the tower (preferably outlet at bottom) is connected with the top of overhead water reflux pump and rectifying column successively by pipeline.In order to save energy consumption, reduce costs, the water after return tank of top of the tower water-oil separating can be back in azeotropy rectification column and be recycled by overhead water reflux pump.
In the utility model, preferably, the side line extraction condenser being connected with the side line extraction line of rectifying column bottom is further connected in the mixer entrance before the reactor reacting with C4 raw material for the preparation of the acetic acid of sec-butyl acetate, for recycling of acetic acid.
In the utility model, preferably, pipeline after an outlet (side outlet) of return tank of top of the tower is connected with tower top ester reflux pump separates two arms, an arm is connected with the top of rectifying column, another arm connects the treating column of later separation, for the further separating-purifying of the thick product of sec-butyl acetate, and/or the pipeline that another outlet (outlet at bottom) of return tank of top of the tower is connected with overhead water reflux pump afterwards separates two arms, an arm is connected with the top of rectifying column, another arm is connected in the treating column of later separation, with the charging as treating column together with the thick product of the oil phase sec-butyl acetate in return tank of top of the tower, enter treating column and carry out further separating-purifying.
In the utility model, another return tank of top of the tower also can be set, the top of rectifying column is drawn to the material of the side line liquid phase material extraction line of 1-10 bar and introduce newly-installed return tank of top of the tower, the liquid phase of tower top lateral line withdrawal function is carried out overhead reflux through tower top ester reflux pump and water reflux pump respectively after water-oil separating.Tower top ester reflux pump and water reflux pump can utilize existing equipment, also can set up new equipment.
Advantage of the present utility model and effect: the utility model has overcome azeotropic distillation column overhead vapour phase in prior art and loaded large, it is large that what overhead condenser was required change area, the cold rear temperature of tower top material is low, heat utilization rate is lower, C4 dissolves more in overhead condensation liquid, after bringing treating column into, affect the shortcoming that treating column operates, extract by the side line liquid phase material of drawing 1-10 bar on the top of rectifying column the mode that line is connected with return tank of top of the tower out, a kind of rectifier unit that reduces azeotropic distillation energy consumption in sec-butyl acetate separation process is provided, realize the reduction of azeotropy rectification column vapour phase load, due to vapour phase load reduction, overhead condenser heat exchange area reduces, reduce equipment investment, simultaneously, reduce overhead condenser recirculated water consumption.
Owing to directly directly entering return tank of top of the tower from the sec-butyl acetate Heng Nong district Extract phase materials of azeotropy rectification column rectifying section without condensation, in return tank of top of the tower, temperature of charge improves, and in return tank of top of the tower, material part can enter treating column and refines, therefore, treating column feeding temperature improves, and has reduced treating column feeding preheating steam consumption.Meanwhile, the liquid phase material of rectifying section Heng Nong district's extraction is because temperature is higher, and the C4 amount in liquid phase material of being dissolved in is also less, and the C4 amount entering in return tank of top of the tower reduces, and the C4 content entering in treating column charging reduces, and is conducive to improve treating column separative efficiency.
Accompanying drawing explanation
Fig. 1 is structural representation of the present utility model.
In figure, 1 is rectifying column, and 2 is overhead condenser, and 3 is tower top ester return tank, and 4 is tower top ester reflux pump, and 5 is side line extraction condenser, and 6 is tower bottom reboiler, and 7 is tower top side line extraction line, and 8 is water reflux pump, and 9 is drawing pump at the bottom of tower, and 10 is feed preheater.
The specific embodiment
Below in conjunction with the drawings and specific embodiments, preferred embodiment of the present utility model is further elaborated.
Fig. 1 shows the rectifier unit of azeotropic distillation energy consumption in reduction sec-butyl acetate of the present utility model separation process, it comprises rectifying column 1, overhead condenser 2, return tank of top of the tower 3, tower top ester reflux pump 4, side line extraction condenser 5 and tower bottom reboiler 6, rectifying column 1 has charging aperture, top exit, outlet at bottom, the top exit of rectifying column is connected with overhead condenser 2 and return tank of top of the tower 3 successively by pipeline, the side outlet of return tank of top of the tower 3 is connected with the top of tower top ester reflux pump 4 and rectifying column 1 successively by pipeline, the side line extraction line of rectifying column bottom is connected with side line extraction condenser 5, the bottom of rectifying column is provided with tower bottom reboiler 6, the side line liquid phase material extraction line 7 that 1-10 bar is drawn on the top of rectifying column 1 is connected with return tank of top of the tower 3.Material is extracted line 7 out and is arranged at more than rectifying column charging aperture 5 positions more than column plate, the rectifying section of rectifying column 1 is plank frame, the theoretical cam curve of rectifying column 1 is 30-150 piece, the bottom of rectifying column 1 is connected with drawing pump at the bottom of tower 9 by pipeline, the feeding line of rectifying column 1 is provided with feed preheater 10, and the outlet at bottom of return tank of top of the tower 3 is connected with the top of rectifying column 1 with overhead water reflux pump 8 successively by pipeline.Pipeline one end after the side outlet of return tank of top of the tower 3 is connected with tower top ester reflux pump 4 is connected with the top of rectifying column 1, the other end is connected in the treating column of later separation, for the further separating-purifying of the thick product of sec-butyl acetate, pipeline one end after the outlet at bottom of return tank of top of the tower 3 is connected with overhead water reflux pump 8 is connected with the top of rectifying column 1, the other end is connected in the treating column of later separation, with the charging as treating column together with the thick product of the oil phase sec-butyl acetate in return tank of top of the tower 3, enter treating column and carry out further separating-purifying.
More than show and described basic principle of the present utility model and principal character and advantage of the present utility model, the technical staff of the industry should understand, the utility model is not restricted to the described embodiments, that in above-described embodiment and description, describes just illustrates principle of the present utility model, do not departing under the prerequisite of the utility model spirit and scope, the utility model also has various changes and modifications, these changes and improvements all fall within the scope of claimed the utility model, the claimed scope of the utility model is defined by appending claims and equivalent thereof.
Claims (10)
1. one kind is reduced the rectifier unit of azeotropic distillation energy consumption in sec-butyl acetate separation process, it is characterized in that, described rectifier unit comprises rectifying column (1), overhead condenser (2), return tank of top of the tower (3), tower top ester reflux pump (4), side line extraction condenser (5) and tower bottom reboiler (6), rectifying column (1) has charging aperture, top exit, outlet at bottom, the top exit of rectifying column (1) is connected with overhead condenser (2) and return tank of top of the tower (3) successively by pipeline, an outlet of return tank of top of the tower (3) is connected with the top of tower top ester reflux pump (3) and rectifying column (1) successively by pipeline, the side line extraction line of rectifying column bottom is connected with side line extraction condenser (5), the bottom of rectifying column is provided with tower bottom reboiler (6), the side line liquid phase material extraction line (7) that 1-10 bar is drawn on the top of rectifying column is connected with return tank of top of the tower (3).
2. rectifier unit according to claim 1, is characterized in that, the rectifying section of described rectifying column (1) is plank frame, and preferably, the theoretical cam curve of described rectifying column (1) is 30-150 piece.
3. rectifier unit according to claim 1 and 2, is characterized in that, described material is extracted line (7) out and is arranged at more than rectifying column charging aperture 5 positions more than column plate.
4. rectifier unit according to claim 3, is characterized in that, described material extraction line (7) is arranged at the position of the above 10 blocks of column plates of rectifying column charging aperture.
5. rectifier unit according to claim 1 and 2, is characterized in that, the outlet at bottom of described rectifying column (1) is connected with drawing pump at the bottom of tower (9) by pipeline.
6. rectifier unit according to claim 1 and 2, is characterized in that, the feeding line of described rectifying column (1) is provided with feed preheater (10).
7. rectifier unit according to claim 1 and 2, is characterized in that, the outlet at bottom of described return tank of top of the tower (3) is connected with the top of rectifying column (1) with overhead water reflux pump (8) successively by pipeline.
8. rectifier unit according to claim 1 and 2, it is characterized in that, pipeline after an outlet of return tank of top of the tower is connected with tower top ester reflux pump separates two arms, and an arm is connected with the top of rectifying column, and another arm connects the treating column of later separation; And/or pipeline that another outlet of return tank of top of the tower is connected with overhead water reflux pump afterwards separates two arms, an arm is connected with the top of rectifying column, the treating column of another arm connection later separation.
9. rectifier unit according to claim 1 and 2, it is characterized in that, another return tank of top of the tower is set, the top of rectifying column is drawn to the material of the side line liquid phase material extraction line of 1-10 bar and introduce described another return tank of top of the tower, the liquid phase of tower top lateral line withdrawal function is carried out overhead reflux through tower top ester reflux pump and water reflux pump respectively after water-oil separating.
10. rectifier unit according to claim 1 and 2, it is characterized in that, the side line extraction condenser being connected with the side line extraction line of rectifying column bottom is further connected in the mixer entrance before the reactor reacting with C4 raw material for the preparation of the acetic acid of sec-butyl acetate.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201320844163.9U CN203648128U (en) | 2013-12-19 | 2013-12-19 | Rectification device capable of reducing energy consumption of azeotropic distillation in sec-butyl acetate separating process |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201320844163.9U CN203648128U (en) | 2013-12-19 | 2013-12-19 | Rectification device capable of reducing energy consumption of azeotropic distillation in sec-butyl acetate separating process |
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| CN203648128U true CN203648128U (en) | 2014-06-18 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104326505A (en) * | 2014-10-20 | 2015-02-04 | 洛阳双瑞万基钛业有限公司 | Deep separation method for reducing tin content in titanium tetrachloride |
| CN104844444A (en) * | 2015-03-26 | 2015-08-19 | 南京师范大学 | Method for extracting acetic acid in salt-containing acetic acid aqueous solution by one-sided line heat integration azeotropic rectification method |
| CN107158731A (en) * | 2017-07-03 | 2017-09-15 | 长兴化学（天津）有限公司 | A kind of condensing reflux system |
| CN113599851A (en) * | 2021-08-19 | 2021-11-05 | 南通百川新材料有限公司 | Novel light component removal and rectification system and method for propylene glycol methyl ether acetate |
| CN115724715A (en) * | 2022-12-07 | 2023-03-03 | 湖南中创化工股份有限公司 | Sec-butyl alcohol refining method and device |
-
2013
- 2013-12-19 CN CN201320844163.9U patent/CN203648128U/en not_active Expired - Lifetime
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104326505A (en) * | 2014-10-20 | 2015-02-04 | 洛阳双瑞万基钛业有限公司 | Deep separation method for reducing tin content in titanium tetrachloride |
| CN104844444A (en) * | 2015-03-26 | 2015-08-19 | 南京师范大学 | Method for extracting acetic acid in salt-containing acetic acid aqueous solution by one-sided line heat integration azeotropic rectification method |
| CN107158731A (en) * | 2017-07-03 | 2017-09-15 | 长兴化学（天津）有限公司 | A kind of condensing reflux system |
| CN113599851A (en) * | 2021-08-19 | 2021-11-05 | 南通百川新材料有限公司 | Novel light component removal and rectification system and method for propylene glycol methyl ether acetate |
| CN115724715A (en) * | 2022-12-07 | 2023-03-03 | 湖南中创化工股份有限公司 | Sec-butyl alcohol refining method and device |
| CN115724715B (en) * | 2022-12-07 | 2024-03-08 | 湖南中创化工股份有限公司 | Refining method and device of sec-butyl alcohol |
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