CN103910601B - Method for producing monohydric alcohol from water and olefins - Google Patents
Method for producing monohydric alcohol from water and olefins Download PDFInfo
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- CN103910601B CN103910601B CN201410162624.3A CN201410162624A CN103910601B CN 103910601 B CN103910601 B CN 103910601B CN 201410162624 A CN201410162624 A CN 201410162624A CN 103910601 B CN103910601 B CN 103910601B
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/03—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by addition of hydroxy groups to unsaturated carbon-to-carbon bonds, e.g. with the aid of H2O2
- C07C29/04—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by addition of hydroxy groups to unsaturated carbon-to-carbon bonds, e.g. with the aid of H2O2 by hydration of carbon-to-carbon double bonds
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Abstract
The invention provides a method for producing monohydric alcohol from water and olefins, which comprises the following steps: reacting demineralized water and olefins subjected to pressurization and heating in a multistage superimposed fixed-bed reactor at 130-250 DEG C under the pressure of 4.0-8.0 MPaG; and reducing the pressure of the reacted mixture to 0.5-1.0 MPaA, cooling to 40-60 DEG C, and separating to obtain the unreacted olefins, process water and monohydric alcohol product. The multistage superimposed fixed-bed reactor is formed by superimposing a plurality of stages or sections of fixed beds, wherein the number of beds N is greater than or equal to 2 and smaller than or equal to 20. The technique adopts the one-step alcohol synthesis method by multistage superimposed fixed-bed reaction, thereby simplifying the synthesis route and greatly lowering the production cost; the equipment has the advantages of simple structure and low investment; and the catalyst can use a resin catalyst which is nontoxic, harmless and pollution-free, so the production process is environment-friendly.
Description
Technical field
The present invention relates to chemical production technical field, be specifically related to a kind of water and the alkene processing method through multistage folded type fixed bed generation unit alcohol.
Background technology
Alcohols chemical is a kind of important organic solvent and industrial chemicals, can be applicable to the industries such as medicine, fine chemistry industry, spices, clean-out system, is widely used, wide market.
The method of water and olefine reaction generation unit alcohol adopts sulfuric acid indirect hydration method the earliest, make catalyzer with sulfuric acid, reaction is carried out in the liquid phase, and main drawback is that equipment corrosion is serious, operational condition is severe, plant investment is large and environmental pollution serious, and production cost is high.Current unit alcohol production method is alkene direct hydration method under resin catalysis mainly: be by adverse current by olefin generation unit alcohol or be floating bed productive unit alcohol; Or single-stage following current fixed bed production unit alcohol.The relative merits of this method are: advantage adopts resin catalyst relative to indirect hydration method, and nontoxic, production environment is friendly; Shortcoming is that structure of reactor is more complicated, and facility investment is higher, and conversion rate of products is low, and production cost is higher.
Summary of the invention
The object of the invention is to: provide a kind of water and alkene through the processing method of multistage folded type fixed bed reaction generation unit alcohol, device structure is simple, and technical process is simple, reduces facility investment, reduces production cost, reduces environmental pollution.
In order to achieve the above object, the present invention is by the following technical solutions:
A kind of method of water and olefine reaction productive unit alcohol is provided, react in multistage superimposed fixed-bed reactor after de-mineralized water and alkene boosting are heated up, temperature of reaction 130-250 DEG C, reaction pressure 4.0-8.0MPaG, reacted mixture is decompressed to 0.5-1.0MPaA, is cooled to 40-60 DEG C, then obtains unreacted alkene, process water and unit alcohol product through separating technology; Described multistage superimposed fixed-bed reactor are formed by fixed bed that is multistage or multistage is superimposed, and bed number N is: 2≤N≤20.
In technical solution of the present invention, described unit alcohol can be ethanol, Virahol, all butanols, all amylalcohols, all hexanols, all enanthol, all octanols or decyl alcohol etc.
In technical solution of the present invention, described raw material olefin can be carbonatoms be 2 ~ 30 all normal olefines or isomeric olefine.
In technical solution of the present invention, described raw material warming temperature preferably reaches 130-250 DEG C.
In technical solution of the present invention, described raw material boost pressure preferably reaches 4.0-8.0MPaG.
In technical solution of the present invention, the reaction conditions in described multistage superimposed fixed-bed reactor is preferably: working pressure 7.0MPaG, service temperature 150 DEG C.
In technical solution of the present invention, described multistage superimposed fixed-bed reactor bed number N is preferably 4≤N≤6.
In technical solution of the present invention, described separating technology preferably includes: reacted mixture isolates unreacted alkene and tower bottoms through separation of olefins tower; Unreacted alkene is recovered or enters torch net; Tower bottoms enters azeotrope column and isolates unit alcohol and process water; Process water is recycled.
The described preferred 0.5-1.0MPaG of separation of olefins tower working pressure, service temperature is preferred: tower top temperature 35-60 DEG C, bottom temperature 130-150 DEG C.
The described preferred 0.15-1.0MPaA of azeotrope column working pressure, service temperature is preferred: tower top temperature 95-99 DEG C, bottom temperature 110-130 DEG C.
The present invention is preferred technical scheme further, uses instrument and supplies flow process as shown in Figure 1, comprises the following steps:
Raw material de-mineralized water is purified by the incoming stock de-mineralized water cleaner 2 of raw material de-mineralized water feed-pipe 1, incoming stock demineralized-water preheater 3 preheating again of the raw material de-mineralized water after purification, and temperature mentions 130-250 DEG C, raw material olefin enters alkene preheater 5 through raw material olefin feed-pipe 4 and is preheated to 130-250 DEG C, in raw material parallel feeding pipe 6 and from after the raw material de-mineralized water mixing of raw material demineralized-water preheater 3 from top to bottom sectional type enter multistage superimposed fixed-bed reactor 10 and react, described multistage superimposed fixed-bed reactor 10 are formed by fixed bed that is multistage or multistage is superimposed, bed number N is 4≤N≤6, temperature of reaction 130-250 DEG C, reaction pressure 4.0-8.0MPaG, reacted mixture is decompressed to 0.5-1.0MPaA, enter separation of olefins tower 12 through separation of olefins tower feed-pipe 11 after being cooled to 40-60 DEG C to be separated, the gas phase of separation of olefins tower 12 tower top enters separation of olefins column overhead condenser 14 through separation of olefins column overhead outlet pipe 13, after cooling, mixture enters separation of olefins column overhead return tank 16 through separation of olefins column overhead return tank inlet pipe 15, a phlegma part is back to separation of olefins tower 12, another part olefin recovery recycles, noncondensable gas enters torch pipe network through torch net inlet pipe 17, the liquid phase mixture of separation of olefins tower 12 tower reactor enters azeotrope column 19 by azeotrope column feed pipe 18 and is separated, the gas phase of azeotrope column 19 tower top enters azeotrope column overhead condenser 21 condensation through azeotrope column tower top outlet pipe 20, the unit alcohol product obtained enters azeotrope column return tank of top of the tower 23 through azeotrope column return tank of top of the tower inlet pipe 22, part unit alcohol product reflux is to azeotrope column, and the extraction of another part unit alcohol product is to storage tank, the process water that azeotrope column 19 tower reactor obtains is recycled through process water recovery tube 24.
In technical solution of the present invention, the feedstock direction of all reaction masses is all from top to bottom, can be sectional feeding, also can combined feed total feed from top to bottom.
The present invention has the following advantages compared with the prior art:
(1) this technique adopts multistage folded type fixed bed reaction one-step synthesis alcohol method, simplifies synthetic route, production cost is significantly reduced.
(2) device structure is simple, and floor space is little, and facility investment is low.
(3) catalyzer can use resin catalyst, and olefin conversion is high, nontoxic pollution-free, and production process environment is good.
Accompanying drawing explanation
Fig. 1 is water of the present invention and the alkene process flow diagram through multistage folded type fixed bed reaction generation unit alcohol.
In Fig. 1: 1, raw material de-mineralized water feed-pipe; 2, raw material de-mineralized water cleaner; 3, raw material demineralized-water preheater; 4, raw material olefin feed-pipe; 5, alkene preheater; 6, raw material parallel feeding pipe; 10, multistage superimposed fixed-bed reactor; 11, separation of olefins tower feed-pipe; 12, separation of olefins tower; 13, separation of olefins column overhead outlet pipe; 14, separation of olefins column overhead condenser; 15, separation of olefins column overhead return tank inlet pipe; 16, separation of olefins column overhead return tank; 17, torch net inlet pipe; 18, azeotrope column feed pipe; 19, azeotrope column; 20, azeotrope column tower top outlet pipe; 21, azeotrope column overhead condenser; 22, azeotrope column return tank of top of the tower inlet pipe; 23, azeotrope column return tank of top of the tower; 24, process water recovery tube.
Embodiment
Embodiment 1
To purify rear de-mineralized water and n-butene for raw material, prepare sec-butyl alcohol and the trimethyl carbinol with the device systems shown in Fig. 1 and technical process, concrete steps are as follows:
Raw material de-mineralized water is purified by the incoming stock de-mineralized water cleaner 2 of raw material de-mineralized water feed-pipe 1, and the raw material de-mineralized water pressure after purification brings up to 7.0MPaG, more incoming stock demineralized-water preheater 3 preheating, and temperature mentions 150 DEG C, enter alkene preheater 5 through raw material olefin feed-pipe 4 after raw material olefin pressure brings up to 7.0MPaG and be preheated to 150 DEG C, in raw material parallel feeding pipe 6 and from after the raw material de-mineralized water mixing of raw material demineralized-water preheater 3 from top to bottom sectional type enter multistage superimposed fixed-bed reactor 10 and react, described multistage superimposed fixed-bed reactor 10 are formed by fixed bed that is multistage or multistage is superimposed, bed number N is 5, temperature of reaction 150 DEG C, reaction pressure 7.0MPaG, reacted mixture is decompressed to 0.5-1.0MPaA, enter separation of olefins tower 12 through separation of olefins tower feed-pipe 11 after being cooled to 40-60 DEG C to be separated, the gas phase of separation of olefins tower 12 tower top enters separation of olefins column overhead condenser 14 through separation of olefins column overhead outlet pipe 13, after cooling, mixture enters separation of olefins column overhead return tank 16 through separation of olefins column overhead return tank inlet pipe 15, a phlegma part is back to separation of olefins tower 12, another part olefin recovery recycles, noncondensable gas enters torch pipe network through torch net inlet pipe 17, the liquid phase mixture of separation of olefins tower 12 tower reactor enters azeotrope column 19 by azeotrope column feed pipe 18 and is separated, the gas phase of azeotrope column 19 tower top enters azeotrope column overhead condenser 21 condensation through azeotrope column tower top outlet pipe 20, the unit alcohol product obtained enters azeotrope column return tank of top of the tower 23 through azeotrope column return tank of top of the tower inlet pipe 22, part unit alcohol product reflux is to azeotrope column, and the extraction of another part unit alcohol product is to storage tank, the process water that azeotrope column 19 tower reactor obtains is recycled through process water recovery tube 24.
Claims (1)
1. a method for water and olefine reaction productive unit alcohol, is characterized in that, comprise the following steps:
Raw material de-mineralized water is by incoming stock de-mineralized water cleaner (2) purification of raw material de-mineralized water feed-pipe (1), and the raw material de-mineralized water after purification is incoming stock demineralized-water preheater (3) preheating again, and temperature mentions 130-250 DEG C, raw material olefin enters alkene preheater (5) through raw material olefin feed-pipe (4) and is preheated to 130-250 DEG C, after raw material parallel feeding pipe (6) neutralization is from the raw material de-mineralized water mixing of raw material demineralized-water preheater (3), sectional type enters the reaction of multistage superimposed fixed-bed reactor (10) from top to bottom, described multistage superimposed fixed-bed reactor (10) are formed by fixed bed that is multistage or multistage is superimposed, bed number N is 4≤N≤6, temperature of reaction 130-250 DEG C, reaction pressure 4.0-8.0MPaG, reacted mixture is decompressed to 0.5-1.0MPaA, enter separation of olefins tower (12) through separation of olefins tower feed-pipe (11) after being cooled to 40-60 DEG C to be separated, the gas phase of separation of olefins tower (12) tower top enters separation of olefins column overhead condenser (14) through separation of olefins column overhead outlet pipe (13), after cooling, mixture enters separation of olefins column overhead return tank (16) through separation of olefins column overhead return tank inlet pipe (15), a phlegma part is back to separation of olefins tower (12), another part olefin recovery recycles, noncondensable gas enters torch pipe network through torch net inlet pipe (17), the liquid phase mixture of separation of olefins tower (12) tower reactor enters azeotrope column (19) by azeotrope column feed pipe (18) and is separated, the working pressure of azeotrope column is 0.15-1.0MPaA, tower top temperature 95-99 DEG C, bottom temperature is 110-130 DEG C, the gas phase of azeotrope column (19) tower top enters azeotrope column through azeotrope column tower top outlet pipe (20), overhead condenser (21) condensation, the unit alcohol product obtained enters azeotrope column return tank of top of the tower (23) through azeotrope column return tank of top of the tower inlet pipe (22), part unit alcohol product reflux is to azeotrope column, and the extraction of another part unit alcohol product is to storage tank, the process water that azeotrope column (19) tower reactor obtains is recycled through process water recovery tube (24).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410162624.3A CN103910601B (en) | 2014-04-22 | 2014-04-22 | Method for producing monohydric alcohol from water and olefins |
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| CN201410162624.3A CN103910601B (en) | 2014-04-22 | 2014-04-22 | Method for producing monohydric alcohol from water and olefins |
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| CN103910601A CN103910601A (en) | 2014-07-09 |
| CN103910601B true CN103910601B (en) | 2015-07-22 |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105523888A (en) * | 2015-12-31 | 2016-04-27 | 天津天中福大科技发展有限公司 | Method for using cation exchange resin for catalytic synthesis of isopropanol |
| CN114505017B (en) * | 2020-10-28 | 2022-11-11 | 中国石油化工股份有限公司 | Olefin hydration reaction device and olefin hydration method |
| CN114478185B (en) * | 2020-10-28 | 2024-02-09 | 中国石油化工股份有限公司 | Olefin hydration process |
| CN114507116B (en) * | 2020-10-28 | 2024-03-08 | 中国石油化工股份有限公司 | Olefin hydration reaction method |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4476333A (en) * | 1980-10-31 | 1984-10-09 | Deutsche Texaco Aktiengesellschaft | Process for the continuous production of secondary butyl alcohol |
| CN1670006A (en) * | 2004-03-15 | 2005-09-21 | 中国科学院大连化学物理研究所 | Process for producing lower alcohol by direct hydration of low carbon olefin |
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2014
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4476333A (en) * | 1980-10-31 | 1984-10-09 | Deutsche Texaco Aktiengesellschaft | Process for the continuous production of secondary butyl alcohol |
| CN1670006A (en) * | 2004-03-15 | 2005-09-21 | 中国科学院大连化学物理研究所 | Process for producing lower alcohol by direct hydration of low carbon olefin |
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Address after: 062451 Cangzhou City, Hebei Province Hejian City Gu Xian Xiang Xi Liu Zhuang Applicant after: Kai Rui environmental protection Science and Technology Co., Ltd. Address before: 062451, Hebei City, Cangzhou Province Hejian City West Zhuang Industrial Zone Applicant before: Kairui Chemical Co., Ltd. |
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