CN104447167A - New process for preparing high-purity isobutene from tertiary butanol - Google Patents
New process for preparing high-purity isobutene from tertiary butanol Download PDFInfo
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- CN104447167A CN104447167A CN201410752628.7A CN201410752628A CN104447167A CN 104447167 A CN104447167 A CN 104447167A CN 201410752628 A CN201410752628 A CN 201410752628A CN 104447167 A CN104447167 A CN 104447167A
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Abstract
The invention belongs to the field of chemical industry and relates to a preparation method of basic chemical organic raw material-isobutene, and particularly relates to a new process for preparing high-purity isobutene from tertiary butanol. The new process is used for various production devices for generating the isobutene by carrying out gas-phase catalysis on the tertiary butanol. The new process is characterized by adopting unique vaporization stripping process and structure, selecting the low-content industrial product tertiary butanol as a raw material, being ingeniously combined with an isobutene rectifying tower and achieving the purposes of tertiary butanol recovery and process wastewater separation by directly delivering residual liquid inside the rectifying tower into a vaporization stripping tower. The new process is also characterized in that a crude isobutene product is directly placed into the rectifying tower under the condition without being condensed for purification, and the process flow can achieve further energy conservation on the basis of the vaporization stripping process.
Description
Technical field
The invention belongs to chemical field, relate to the preparation method of a kind of basic chemical industry organic raw material-iso-butylene, be specially and prepare high-purity iso-butylene novel process by the trimethyl carbinol.
Background technology
The main method of current industrial production iso-butylene has three kinds: the first is from C
4sulfuric acid absorption method is adopted in cut; The second is that the trimethyl carbinol dewaters production under the catalysis such as activated alumina, sulfonic acid, ion exchange resin; The third uses physisorphtion separation of C
4cut.
The method preparing high-purity isobutylene mainly contains 2 kinds: methyl tertiary butyl ether (MTBE) cracking process and tert-butyl alcohol dehydration method.MTBE cracking process is the technique that after the eighties in last century, countries in the world generally adopt, and product purity is high, and unit scale handiness is large, can produce MTBE or iso-butylene according to the market requirement.Shortcoming is because etherification method side reaction is many, and for obtaining high-purity isobutylene product, separation and purification complex process, energy consumption is larger.
Domestic usual employing tert-butyl alcohol dehydration prepares iso-butylene production technique, and this technique is mainly divided into reactor class intermittent type and continuous two types of catalytic distillation.Adopt batch process, the trimethyl carbinol and catalyzer is disposable adds in reaction unit, under the dehydration of catalyzer, thermal degradation becomes iso-butylene.Product iso-butylene leaves reaction system with gas phase from venting port, and water byproduct is still stayed in system.The feature of this production method is that in system, water content constantly increases along with reaction is carried out, and raw material trimethyl carbinol density loss, causes iso-butylene generating rate significantly to decline.Continuous print catalytic rectification process, needs to be entered in reactive distillation column by catalyst loading in advance.What generally adopt at present has two kinds of types of feed: one is by bulk for granules of catalyst in the reaction tower being designed to special construction, to guarantee catalyst loading, to change conveniently, not easily leaks.Other method is filled out by granules of catalyst to be placed on to form catalyst structure by the sack that inert material is made, catalyst structure be separated noggin piece and form catalytic distillation element together, catalytic distillation element is arranged in catalytic rectifying tower more in some way.This filling mode has the advantages such as liquid phase resistance is little, catalyzer not easily leaks, but catalyzer is installed and is changed inconvenience in use procedure, simultaneously owing to there is resistance to mass transfer inside and outside catalyzer mesh bag, the granules of catalyst of catalytic distillation element internal can not be fully used.
Summary of the invention
The object of the invention is to for above technical problem, provide a kind of less investment, energy consumption low, simple to operate prepare high-purity iso-butylene novel process by the trimethyl carbinol.
The object of the invention is realized by following technical proposals:
Prepare high-purity iso-butylene novel process by the trimethyl carbinol, the method comprises the steps:
A, content are 70-99.5%(Wt), the raw material trimethyl carbinol of impurity based on water heating up in a steamer vaporization in tower be separated with from carrying in vaporization with the trimethyl carbinol and the water mixed solution that is major ingredient of iso-butylene tower bottom of rectifying tower extraction, send into tert-butyl alcohol dehydration reactive system from the tower top trimethyl carbinol out and water mixing steam, processing wastewater is carried by vaporization and is heated up in a steamer tower tower reactor and get rid of continuously.
B, dehydration reaction system obtain based on the reaction product of iso-butylene, water, the trimethyl carbinol, therefrom, bottom enters iso-butylene rectifying tower, just exporting extraction purity from iso-butylene rectifying tower tower top is 90-99.9%(Wt) iso-butylene product, mixed solution in iso-butylene tower bottom of rectifying tower is sent into vaporization and is carried and heat up in a steamer tower and carry out trimethyl carbinol recovery and separating technology waste water.
The raw material trimethyl carbinol is carried from vaporization and is heated up in a steamer top of tower, and the tower bottoms from iso-butylene rectifying tower is carried in vaporization the middle part opening for feed heating up in a steamer tower and entered in tower, and the upper and lower part of middle part opening for feed is all provided with the tower joint with separating power.
From step b obtain the thick product of iso-butylene without condensation, point liquid phase from iso-butylene rectifying tower, bottom is sent into, and is 99-99.9%(Wt from overhead extraction mouth extraction purity) iso-butylene product.
The steam of iso-butylene rectifying tower tower top is through iso-butylene water cooler condensation rear portion or all pass back in tower from trim the top of column mouth, non-refluxing portion as the extraction of iso-butylene product, with mass ratio range, quantity of reflux: produced quantity is (0.5-5): 1.
Pressure is 0.1-0.3Mpa(G) water vapour directly enter vaporization and carry and heat up in a steamer tower tower reactor and heat with mixing of materials wherein, or to be carried by the vaporization of reboiler indirect heating with water vapour or other thermal barrier and heat up in a steamer material in tower tower reactor, tower reactor get rid of t butanol content in liquid be 100PPm once.
Vaporization is carried and is heated up in a steamer tower and iso-butylene rectifying tower is packing tower or tray column, and its operating pressure is 0.1-0.8Mpa(G).
Positively effect of the present invention is embodied in:
(1), the present invention adopts the water had concurrently in the vaporization raw material trimethyl carbinol and isobutylene separation tower bottom of rectifying tower mixed solution, the vaporization of trimethyl carbinol dual-use function carries and heat up in a steamer tower, not only save the investment of trimethyl carbinol recovery tower and support equipment thereof, also make the trimethyl carbinol energy consumption in recovery iso-butylene tower bottom of rectifying tower mixed solution significantly reduce, solve the difficult problem that existing tert-butyl alcohol dehydration preparing isobutene still reaction and catalytic rectification process processing wastewater are difficult to deviate from.
(2), vaporization carries that to heat up in a steamer tower be that carrying of two section feedings heats up in a steamer tower.The raw material trimethyl carbinol is carried by vaporization and is heated up in a steamer top of tower charging, and the mixed solution obtained from iso-butylene tower bottom of rectifying tower is carried by vaporization and heated up in a steamer (this position all has the tower of centrifugation to save up and down, is not middle) charging in the middle part of tower.The water that raw material brings and all put forward the tower reactor of heating up in a steamer tower and discharge continuously from the water iso-butylene rectifying tower 3 tower reactor mixed solution from vaporization.The trimethyl carbinol after vaporization, water mixing steam are then carried from vaporization and are heated up in a steamer the raw material of column overhead discharge as gas-phase dehydration reaction.Vaporization is carried and is heated up in a steamer tower process process and can realize vaporizing and carry in the tower reactor mixed solution heating up in a steamer tower Separation and Recovery iso-butylene rectifying tower needed for the trimethyl carbinol heat energy just needed for the vaporization trimethyl carbinol, the energy consumption of heating up in a steamer the trimethyl carbinol in tower Separation and Recovery iso-butylene tower bottom of rectifying tower mixed solution is put forward in visible the present invention's vaporization, significantly reduces compared with existing production iso-butylene method.Compared with existing autoclave or catalytic rectification process, take material purity as 70-99.5%(Wt), impurity is with water for the main moral trimethyl carbinol prepares iso-butylene, and product iso-butylene per ton can save steam about 0.5 ton.
(3), vaporization of the present invention carry heat up in a steamer the another feature of tower be tower reactor heating can adopt water vapour and the direct Hybrid Heating of tower reactor liquid, in this process, water vapour directly mixes with tower reactor liquid, the condensing temperature of water vapour is equal with bottom temperature, compared with use reboiler, the condensing temperature of water vapour is lower, its latent heat is larger, and sensible heat can utilize completely.While reducing facility investment, reduce further water vapour consumption.Condensed water vapour to be carried with vaporization together with processing wastewater and is heated up in a steamer tower tower reactor and discharge system continuously.
(4), the steam of iso-butylene rectifying tower tower top is through iso-butylene water cooler condensation rear portion or all pass back in tower from trim the top of column mouth, non-refluxing portion as the extraction of iso-butylene product, quantity of reflux: produced quantity is (0.5-5): 1, weight ratio.Can generate a small amount of as by products such as normal butane, cis-2-butene, Trans-2-butenes in tert-butyl alcohol dehydration reaction process, its boiling point is all higher than target product iso-butylene.The present invention is provided with the above component of side take-off mouth extraction at iso-butylene rectifier, avoids these intermediate components circulative accumulation in systems in which, ensure that the purity of iso-butylene product.
(5), the thick product of iso-butylene that obtains of dehydration reaction system without condensation, point liquid phase from iso-butylene rectifying tower, bottom sends into.Compared with traditional technology, this process takes full advantage of system heat energy, significantly can reduce the water vapour consumption of iso-butylene rectifying tower, saves the facility investment of the thick product condenser of iso-butylene and preheater simultaneously.
Accompanying drawing explanation
Fig. 1 is the process flow sheet adopted in present method.
Wherein, 1---vaporization is carried and is heated up in a steamer tower, 2------iso-butylene condenser, 6-15 are pipeline circuit to iso-butylene rectifying tower, 4---reboiler, 5---to tert-butyl alcohol dehydration reactive system, 3.
Embodiment
Arbitrary feature disclosed in this specification sheets (comprising any accessory claim, summary), unless specifically stated otherwise, all can be replaced by other equivalences or the alternative features with similar object.That is, unless specifically stated otherwise, each feature is an example in a series of equivalence or similar characteristics.
As shown in process flow sheet, the raw material trimethyl carbinol is carried from vaporization the tower top 6 heating up in a steamer tower and is entered vaporization and carry and heat up in a steamer tower 1, iso-butylene rectifying tower 3 tower reactor mixed solution enters vaporization and carries and heat up in a steamer tower 1 from middle part 14, the trimethyl carbinol in these two bursts of chargings is discharged from tower top 7 and entered tert-butyl alcohol dehydration reactive system 2 after vaporization is separated.
Vaporization is carried and is heated up in a steamer tower 1 tower reactor and adopt water vapour directly and kettle material Hybrid Heating, and condensed water vapour to be carried with vaporization together with processing wastewater and heated up in a steamer tower 1 tower reactor and discharge system continuously.
The thick product of iso-butylene from tert-butyl alcohol dehydration reactive system 2 is entered by iso-butylene rectifying tower 3 middle and lower part 8 without condensation, iso-butylene rectifying tower 3 overhead vapours enters tower through iso-butylene condenser 5 condensation rear portion from trim the top of column, and a part obtains through 11 high-purity iso-butylene product that purity is greater than 99.9.The intermediate by-products component (as normal butane, cis-2-butene, Trans-2-butene) of boiling point between the trimethyl carbinol (82.42 DEG C) and iso-butylene (-6.9 DEG C) is from side line 12,13 extraction.
embodiment 1:
Vaporization is carried and is heated up in a steamer tower 1 theoretical plate number 25, working pressure 0.5Mpa (G).Raw material trimethyl carbinol 3000kg/h, wherein trimethyl carbinol 2400kg/h, water 600kg/h, t butanol content is 80%(Wt).
The raw material trimethyl carbinol is carried from vaporization and is heated up in a steamer the charging of tower 1 tower top.Trimethyl carbinol 240kg/h in iso-butylene tower bottom of rectifying tower mixed solution, water 1183.8kg/h, feed entrance point is carried in vaporization and is heated up in a steamer tower 1 tower reactor number and play the 15th block of theoretical tray, tower top exhaust vapour 7 sends into dehydration reaction system, wherein trimethyl carbinol 2639.8kg/h, water 293.3kg/h, t butanol content 89.98%(Wt).T butanol content 0.01%(Wt in the water that tower reactor is discharged).
Iso-butylene rectifying tower is tray column, and working pressure is 0.45Mpa (G), theoretical plate number 28 pieces, trimethyl carbinol 240kg/h in charging 8, water 876.8kg/h, iso-butylene 1814.24kg/h.Feed tray number is liquid phase feeding 6 blocks of theoretical trays, gas phase 13 theoretical tray from tower reactor number.Overhead condensation liquid by tower top 11 extraction, reflux ratio 0.8:1, extraction iso-butylene product 1810.8kg/h, product purity 99.91%(Wt).
embodiment 2:
Vaporization is carried and is heated up in a steamer tower 1 theoretical plate number 20, working pressure 0.5Mpa (G).Raw material trimethyl carbinol 2000kg/h, wherein trimethyl carbinol 1900kg/h, water 100kg/h, the content 95%(Wt of the trimethyl carbinol).
The raw material trimethyl carbinol is carried from vaporization and is heated up in a steamer the charging of tower 1 tower top.Trimethyl carbinol 152kg/h in iso-butylene tower bottom of rectifying tower mixed solution, water 525.2kg/h, feed entrance point is carried in vaporization and is heated up in a steamer tower 1 tower reactor number and play the 10th block of theoretical tray, tower top exhaust vapour 7 sends into dehydration reaction system, wherein trimethyl carbinol 1853kg/h, water 18.7kg/h, t butanol content 99.0%(Wt).T butanol content 0.008%(Wt in the water that tower reactor is discharged).
Iso-butylene rectifying tower is tray column, and working pressure is 0.45Mpa (G), theoretical plate number 15 pieces, trimethyl carbinol 152kg/h, 432.45kg/h in charging 8, iso-butylene 1287.24kg/h.Feed tray number is liquid phase feeding 5 blocks of theoretical trays, gas phase 11 theoretical tray from tower reactor number.Overhead condensation liquid by tower top 11 extraction, reflux ratio 0.7:1, extraction iso-butylene product 1285.55kg/h, product purity 99.93%(Wt).
Claims (7)
1. prepare high-purity iso-butylene novel process by the trimethyl carbinol, it is characterized in that comprising the steps:
A, the raw material trimethyl carbinol heating up in a steamer vaporization in tower be separated with from carrying in vaporization with the trimethyl carbinol and the water mixed solution that is major ingredient of iso-butylene tower bottom of rectifying tower extraction, send into tert-butyl alcohol dehydration reactive system from the tower top trimethyl carbinol out and water mixing steam, processing wastewater is carried by vaporization and is heated up in a steamer tower tower reactor and get rid of continuously;
B, dehydration reaction system obtain based on the reaction product of iso-butylene, water, the trimethyl carbinol therefrom, bottom enters iso-butylene rectifying tower, be 90-99.9%(Wt from iso-butylene rectifying tower tower top outlet extraction purity) iso-butylene product, the mixed solution in iso-butylene tower bottom of rectifying tower is sent into vaporization and is carried and heat up in a steamer tower and carry out trimethyl carbinol recovery and separating technology waste water.
2. according to claim 1ly prepare high-purity iso-butylene novel process by the trimethyl carbinol, it is characterized in that: the content in step a in mixed solution shared by the trimethyl carbinol is 70-99.5%(Wt), impurity is based on water.
3. according to claim 1ly prepare high-purity iso-butylene novel process by the trimethyl carbinol, it is characterized in that: the raw material trimethyl carbinol is carried from vaporization and heated up in a steamer top of tower, tower bottoms from iso-butylene rectifying tower is carried in vaporization the middle part opening for feed heating up in a steamer tower and is entered in tower, and the upper and lower part of middle part opening for feed is all provided with the tower joint with separating power.
4. according to claim 1ly prepare high-purity iso-butylene novel process by the trimethyl carbinol, it is characterized in that: from step b obtain the thick product of iso-butylene without condensation, point liquid phase from iso-butylene rectifying tower, bottom is sent into, and is 99-99.9%(Wt from overhead extraction mouth extraction purity) iso-butylene product.
5. according to claim 1ly prepare high-purity iso-butylene novel process by the trimethyl carbinol, it is characterized in that: the steam of iso-butylene rectifying tower tower top is through iso-butylene water cooler condensation rear portion or all pass back in tower from trim the top of column mouth, non-refluxing portion as the extraction of iso-butylene product, quantity of reflux: produced quantity take mass ratio range as 0.5-5:1.
6. according to claim 1ly prepare high-purity iso-butylene novel process by the trimethyl carbinol, it is characterized in that: pressure is 0.1-0.3Mpa(G) water vapour directly enter vaporization and carry and heat up in a steamer tower tower reactor and heat with mixing of materials wherein, or to be carried by the vaporization of reboiler indirect heating with water vapour or other thermal barrier and heat up in a steamer material in tower tower reactor, it is below 100PPm that tower reactor gets rid of t butanol content in liquid.
7. according to claim 1ly prepare high-purity iso-butylene novel process by the trimethyl carbinol, it is characterized in that: vaporization is carried and heated up in a steamer tower and iso-butylene rectifying tower is packing tower or tray column, and its operating pressure is 0.1-0.8Mpa(G).
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109096026A (en) * | 2018-08-28 | 2018-12-28 | 宁波昊德化学工业股份有限公司 | A kind of production method of isobutene |
| CN111635290A (en) * | 2020-07-03 | 2020-09-08 | 天津科技大学 | Method for preparing isobutene by dehydration of tertiary butanol |
| CN113680087A (en) * | 2021-08-27 | 2021-11-23 | 重庆山巨化工机械股份有限公司 | Double-tower efficient energy-saving rectification process |
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| CN102344336A (en) * | 2011-08-03 | 2012-02-08 | 天津市泰源工业气体有限公司 | Preparation of isobutylene by using direct hydration method |
| CN102372567A (en) * | 2010-08-23 | 2012-03-14 | 中国石油化工股份有限公司 | Method for producing ethene by ethanol dehydration |
| CN102633588A (en) * | 2012-03-30 | 2012-08-15 | 北京化工大学 | Method for preparing high-purity isobutene from raffinate C4 by means of separation |
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2014
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102372567A (en) * | 2010-08-23 | 2012-03-14 | 中国石油化工股份有限公司 | Method for producing ethene by ethanol dehydration |
| CN102344336A (en) * | 2011-08-03 | 2012-02-08 | 天津市泰源工业气体有限公司 | Preparation of isobutylene by using direct hydration method |
| CN102633588A (en) * | 2012-03-30 | 2012-08-15 | 北京化工大学 | Method for preparing high-purity isobutene from raffinate C4 by means of separation |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109096026A (en) * | 2018-08-28 | 2018-12-28 | 宁波昊德化学工业股份有限公司 | A kind of production method of isobutene |
| CN109096026B (en) * | 2018-08-28 | 2021-07-06 | 宁波昊德化学工业股份有限公司 | Production method of isobutene |
| CN111635290A (en) * | 2020-07-03 | 2020-09-08 | 天津科技大学 | Method for preparing isobutene by dehydration of tertiary butanol |
| CN113680087A (en) * | 2021-08-27 | 2021-11-23 | 重庆山巨化工机械股份有限公司 | Double-tower efficient energy-saving rectification process |
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