CN105175210A - Method for preparing isobutylene by tert butyl alcohol - Google Patents

Method for preparing isobutylene by tert butyl alcohol Download PDF

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Publication number
CN105175210A
CN105175210A CN201510565660.9A CN201510565660A CN105175210A CN 105175210 A CN105175210 A CN 105175210A CN 201510565660 A CN201510565660 A CN 201510565660A CN 105175210 A CN105175210 A CN 105175210A
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China
Prior art keywords
trimethyl carbinol
slurry
butylene
iso
prepares
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CN201510565660.9A
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Chinese (zh)
Inventor
张国华
姜立新
王纪伟
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Shandong Chengtai Chemical Co Ltd
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Shandong Chengtai Chemical Co Ltd
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Priority to CN201510565660.9A priority Critical patent/CN105175210A/en
Publication of CN105175210A publication Critical patent/CN105175210A/en
Pending legal-status Critical Current

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    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/10Process efficiency

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  • Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The invention is applicable to the technical field of preparation of isobutylene, and provides a method for preparing the isobutylene by tert butyl alcohol. The method comprises the following steps: preparing deionized water and a catalyst into slurry in a slurry mixer; pumping the slurry into a catalytic distillation column by using a pump; performing a dehydrating reaction on the slurry and an isobutylene raw material, wherein the material discharged from the catalytic distillation column is a mixture of a small amount of the isobutylene, the water and the catalyst; circulating the mixture back to the slurry mixer; enabling distillate at the top of the column to enter a reflux tank after the distillate is condensed by a condenser; enabling part of the distillate to reflux to the catalytic distillation column; pumping part of the distillate into a purification rectifying column, wherein high-purity isobutylene is distilled from the top of the purification rectifying column. Therefore, slurry catalytic distillation is adopted, so that the efficiency of the catalyst is improved; an original catalyst is not required to be prepared; catalytic distillation equipment is simplified; the catalyst can be replaced without stopping; the production efficiency is improved.

Description

The trimethyl carbinol prepares the method for iso-butylene
Technical field
The present invention relates to a kind of preparation method of iso-butylene, specifically, relate to a kind of method that trimethyl carbinol prepares iso-butylene, belong to technical field of chemistry and chemical engineering.
Background technology
At present, ion exchange process is utilized to mainly contain two kinds by the method for tert-butyl alcohol dehydration preparing isobutene, one is under the catalyst actions such as sulfonic acid ion exchange resin, in fixed-bed reactor, dehydration generates iso-butylene, because per pass conversion is low, often adopt the mode of plural parallel stage or series connection, equipment is many and complicated, energy consumption is also corresponding higher, needs to stop to change after catalyst failure; Another kind fills sulfonic acid ion exchange resin in rectifying tower, and make rectifying tower form multi-segment structure and realize tert-butyl alcohol dehydration reaction, rectifying tower structure is complicated, wayward, needs to stop to change after catalyst failure.
In summary, obviously there is inconvenience and defect in actual use in prior art, so be necessary to be improved.
Summary of the invention
The technical problem to be solved in the present invention is for above-mentioned defect, and provide a kind of trimethyl carbinol to prepare the method for iso-butylene, it can simplify catalytic distillation equipment, structure is simple, and energy consumption is low, achieves the more catalyst changeout that do not stop, thus enhance productivity, the transformation efficiency of the trimethyl carbinol is high.
To achieve these goals, the invention provides a kind of method that trimethyl carbinol prepares iso-butylene, deionized water and catalyzer make slurry in slurry mixer, described slurry is squeezed in catalytic rectifying tower by pump, described slurry and trimethyl carbinol raw material carry out dehydration reaction, the discharging of described catalytic rectifying tower tower reactor is a small amount of trimethyl carbinol, water and catalyst mixture, loop back slurry mixer, overhead product enters return tank after condenser condenses, described overhead product is partly refluxed to catalytic rectifying tower, part pumps into purification rectifying tower, described purification rectifying tower tower top distillates high-purity isobutylene.
The trimethyl carbinol according to the present invention prepares the method for iso-butylene, and described catalyzer is sulfonic acid ion exchange resin particulate or ultrafine particle.
The trimethyl carbinol according to the present invention prepares the method for iso-butylene, and described catalytic rectifying tower working pressure is 0.1 ~ 0.25MPa, and temperature controls at 80 ° ~ 150 °.
The trimethyl carbinol according to the present invention prepares the method for iso-butylene, and the interpolation concentration of described catalyzer controls at 20Kg/m 3~ 39Kg/m 3.
The trimethyl carbinol according to the present invention prepares the method for iso-butylene, it is characterized in that, described overhead product control of reflux ratio is 1.2 ~ 1.8.
The present invention adopts above technical scheme, compared with prior art, have the following advantages: the present invention realizes catalytic distillation by ion exchange resin is made slurry, with conventional distillation technique, there is outstanding feature: without the need to making catalyzer original paper, simplify catalytic distillation equipment, achieve the more catalyst changeout that do not stop, catalyst efficiency is high, trimethyl carbinol transformation efficiency 95%-99%, do not need the mode adopting plural parallel stage or series connection, structure is simple, and energy consumption is low, be easy to suitability for industrialized production, there is the prospect of further research and development.
Be described further below in conjunction with drawings and Examples contrast invention.
Accompanying drawing explanation
Accompanying drawing 1 is the process flow diagram that in the embodiment of the present invention, the trimethyl carbinol prepares iso-butylene;
In figure,
A-ionized water, b-catalyzer, the c-trimethyl carbinol, e-iso-butylene, 1-slurry mixer, 2-catalytic rectifying tower, 3-condenser, 4-return tank, 5-purification rectifying tower, 6-condenser, 7-return tank.
Embodiment
In order to make object of the present invention, technical scheme and advantage clearly understand, below in conjunction with drawings and Examples, the present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explain the present invention, be not intended to limit the present invention.
See Fig. 1, the invention provides a kind of method that trimethyl carbinol prepares iso-butylene, deionized water and catalyzer are incorporated in slurry mixer 1, evenly make slurry by magnetic stirrer, squeeze in catalytic rectifying tower 2 by pump; Slurry flows fully in catalytic rectifying tower 2 and trimethyl carbinol contact raw catalysis tert-butyl alcohol dehydration reacts.After dehydration reaction, the discharging of catalysis tower reactor is a small amount of trimethyl carbinol, water and catalyst mixture, loops back slurry mixer 1, recycle through recycle pump.Overhead product is thick iso-butylene, return tank 4 is entered after condenser 3 condensation, catalytic rectifying tower 2 is partly refluxed in return tank 4, part pumps into purification rectifying tower 5, purification rectifying tower 5 tower top distillates high-purity isobutylene and enter return tank 7 after condenser 6 condensation, return tank 7 discharging is high-purity isobutylene, is partly refluxed to purification rectifying tower 5.
Preferably, catalyzer of the present invention is the strong acid ion exchange resin particulate or ultrafine particle that particle diameter is very little, forms slurry with liquid phase, flows in catalytic rectifying tower 2, and catalytic efficiency improves.
In test, find that catalytic rectifying tower 2 working pressure is 0.1 ~ 0.25MPa, temperature controls at 80 ° ~ 150 °, when pressure is raised to 0.25MPa by 0.1MPa, trimethyl carbinol transformation efficiency slightly improves, but when pressure is more than 0.25MPa, raise with pressure, trimethyl carbinol transformation efficiency reduces gradually.
Find, the interpolation concentration of catalyzer controls at 20Kg/m simultaneously 3~ 39Kg/m 3, practice result shows the increase along with catalyst concn in charging, and the transformation efficiency of the trimethyl carbinol raises gradually, when concentration is higher than 20Kg/m 3time, trimethyl carbinol transformation efficiency is higher than 95%, and special concentration of working as reaches 39Kg/m 3time, trimethyl carbinol transformation efficiency can reach 99%.
Find that overhead product reflux ratio 1.2 ~ 1.8 facts have proved the increase along with reflux ratio, the transformation efficiency of the trimethyl carbinol raises gradually, but becomes downtrending after 1.5 simultaneously, and simultaneously for reducing energy consumption, rational reflux ratio should be 1.2 ~ 1.8, and preferably 1.5.
In sum, the present invention realizes catalytic distillation by ion exchange resin is made slurry, with conventional distillation technique, there is outstanding feature: without the need to making catalyzer original paper, simplify catalytic distillation equipment, achieve the more catalyst changeout that do not stop, catalyst efficiency is high, is easy to suitability for industrialized production, has the prospect of further research and development.
Certainly; the present invention also can have other various embodiments; when not deviating from the present invention's spirit and essence thereof; those of ordinary skill in the art are when making various corresponding change and distortion according to the present invention, but these change accordingly and are out of shape the protection domain that all should belong to the claim appended by the present invention.

Claims (7)

1. the trimethyl carbinol prepares a method for iso-butylene, it is characterized in that, deionized water and catalyzer make slurry in slurry mixer, and described slurry is squeezed in catalytic rectifying tower by pump, and described slurry and trimethyl carbinol raw material carry out dehydration reaction;
The discharging of described catalytic rectifying tower tower reactor is the mixture of a small amount of trimethyl carbinol, water and catalyzer, and described mixture loops back slurry mixer, and overhead product enters return tank after condenser condenses;
A part for described overhead product is back to catalytic rectifying tower, and another part pumps into purification rectifying tower, and described purification rectifying tower tower top distillates high-purity isobutylene.
2. the trimethyl carbinol according to claim 1 prepares the method for iso-butylene, it is characterized in that, described catalyzer is strong acid ion exchange resin particulate or ultrafine particle.
3. the trimethyl carbinol according to claim 1 prepares the method for iso-butylene, it is characterized in that, described catalytic rectifying tower working pressure is 0.1 ~ 0.25MPa, and temperature controls at 80 ° ~ 150 °.
4. the trimethyl carbinol according to claim 1 prepares the method for iso-butylene, it is characterized in that, the interpolation concentration of described catalyzer controls at 20Kg/m 3~ 39Kg/m 3.
5. the trimethyl carbinol according to claim 1 prepares the method for iso-butylene, it is characterized in that, described overhead product control of reflux ratio is 1.2 ~ 1.8.
6. the trimethyl carbinol according to claim 1 prepares the method for iso-butylene, it is characterized in that, described overhead product control of reflux ratio is 1.5.
7. the trimethyl carbinol according to claim 1 prepares the method for iso-butylene, it is characterized in that, described trimethyl carbinol transformation efficiency 95%-99%.
CN201510565660.9A 2015-09-08 2015-09-08 Method for preparing isobutylene by tert butyl alcohol Pending CN105175210A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
CN110354519A (en) * 2019-08-19 2019-10-22 凯瑞环保科技股份有限公司 A kind of device and method that catalytic distillation process produces isobutene polymer grade
CN110776389A (en) * 2019-11-29 2020-02-11 万华化学集团股份有限公司 Compound catalyst and method for preparing styrene
CN112094192A (en) * 2019-06-18 2020-12-18 天津华信化工技术有限公司 Novel method for preparing dimethyl carbonate by catalytic reaction and rectification of slurry

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105152844A (en) * 2015-08-17 2015-12-16 山东成泰化工有限公司 Method for preparing isobutylene from tert-butyl alcohol

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105152844A (en) * 2015-08-17 2015-12-16 山东成泰化工有限公司 Method for preparing isobutylene from tert-butyl alcohol

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
CN112094192A (en) * 2019-06-18 2020-12-18 天津华信化工技术有限公司 Novel method for preparing dimethyl carbonate by catalytic reaction and rectification of slurry
CN110354519A (en) * 2019-08-19 2019-10-22 凯瑞环保科技股份有限公司 A kind of device and method that catalytic distillation process produces isobutene polymer grade
CN110776389A (en) * 2019-11-29 2020-02-11 万华化学集团股份有限公司 Compound catalyst and method for preparing styrene
CN110776389B (en) * 2019-11-29 2022-08-05 万华化学集团股份有限公司 Compound catalyst and method for preparing styrene

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Application publication date: 20151223