CN103910601A - 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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- CN103910601A CN103910601A CN201410162624.3A CN201410162624A CN103910601A CN 103910601 A CN103910601 A CN 103910601A CN 201410162624 A CN201410162624 A CN 201410162624A CN 103910601 A CN103910601 A CN 103910601A
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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
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, and market outlook are wide.
The method of water and olefine reaction generation unit alcohol adopts the indirect hydration method of sulfuric acid the earliest, make catalyzer with sulfuric acid, reaction is carried out in liquid phase, and main drawback is that equipment corrosion is serious, operational condition is severe, plant investment is large and environmental pollution is serious, and production cost is high.Unit alcohol production method is mainly alkene direct hydration method under resin catalysis at present: be by adverse current or be floating bed productive unit alcohol by olefin production unit alcohol; Or single-stage following current fixed bed production unit alcohol.The relative merits of this method are: advantage is to adopt resin catalyst with respect to indirect hydration method, nontoxic, production environment close friend; 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: a kind of water and the alkene processing method through multistage folded type fixed bed reaction generation unit alcohol is provided, and device structure is simple, and technical process is simple, reduce facility investment, reduce production costs, reduce 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, that de-mineralized water and alkene are boosted after heating up and reacted in multistage superimposed fixed-bed reactor, temperature of reaction 130-250 ℃, reaction pressure 4.0-8.0MPaG, reacted mixture is decompressed to 0.5-1.0MPaA, is cooled to 40-60 ℃, then obtains unreacted alkene, process water and unit alcohol product through separating technology; Described multistage superimposed fixed-bed reactor form by the fixed bed of multistage or multistage is superimposed, and bed is counted N and 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 that carbonatoms is 2～30 all normal olefines or isomeric olefine.
In technical solution of the present invention, described raw material intensification temperature preferably reaches 130-250 ℃.
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, 150 ℃ of service temperatures.
In technical solution of the present invention, described multistage superimposed fixed-bed reactor bed is counted N and is preferably 4≤N≤6.
In technical solution of the present invention, described separating technology preferably includes: reacted mixture is isolated 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 ℃, tower reactor temperature 130-150 ℃.
The described preferred 0.15-1.0MPaA of azeotrope column working pressure, service temperature is preferred: tower top temperature 95-99 ℃, tower reactor temperature 110-130 ℃.
The further preferred technical scheme of the present invention, is used equipment and technical process as shown in Figure 1, comprises the following steps:
Raw material de-mineralized water purifies 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 after purification is incoming stock demineralized-water preheater 3 preheatings again, and temperature is mentioned 130-250 ℃, raw material olefin enters alkene preheater 5 through raw material olefin feed-pipe 4 and is preheated to 130-250 ℃, raw material parallel feeding pipe 6 neutralize mix from the raw material de-mineralized water of raw material demineralized-water preheater 3 after from top to bottom sectional type enter multistage superimposed fixed-bed reactor 10 and react, described multistage superimposed fixed-bed reactor 10 form by the fixed bed of multistage or multistage is superimposed, it is 4≤N≤6 that bed is counted N, temperature of reaction 130-250 ℃, reaction pressure 4.0-8.0MPaG, reacted mixture is decompressed to 0.5-1.0MPaA, after being cooled to 40-60 ℃, entering separation of olefins tower 12 through separation of olefins tower feed-pipe 11 separates, the gas phase of separation of olefins tower 12 tower tops enters separation of olefins column overhead condenser 14 through separation of olefins column overhead outlet pipe 13, cooling rear 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 reactors enters azeotrope column 19 by azeotrope column feed pipe 18 and separates, the gas phase of azeotrope column 19 tower tops enters 21 condensations of azeotrope column overhead condenser through azeotrope column tower top outlet pipe 20, the unit alcohol product obtaining 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 alcohol product extraction of another part unit is to storage tank, the process water that azeotrope column 19 tower reactors obtain 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 combined feed total feed from top to bottom.
The present invention has the following advantages compared with the prior art:
(1) the multistage folded type fixed bed reaction of this process using one-step synthesis alcohol method, has simplified synthetic route, and 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 as 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 purifies 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 is brought up to 7.0MPaG, then 3 preheatings of incoming stock demineralized-water preheater, and temperature is mentioned 150 ℃, raw material olefin pressure is brought up to and is entered alkene preheater 5 through raw material olefin feed-pipe 4 after 7.0MPaG and be preheated to 150 ℃, raw material parallel feeding pipe 6 neutralize mix from the raw material de-mineralized water of raw material demineralized-water preheater 3 after from top to bottom sectional type enter multistage superimposed fixed-bed reactor 10 and react, described multistage superimposed fixed-bed reactor 10 form by the fixed bed of multistage or multistage is superimposed, it is 5 that bed is counted N, 150 ℃ of temperature of reaction, reaction pressure 7.0MPaG, reacted mixture is decompressed to 0.5-1.0MPaA, after being cooled to 40-60 ℃, entering separation of olefins tower 12 through separation of olefins tower feed-pipe 11 separates, the gas phase of separation of olefins tower 12 tower tops enters separation of olefins column overhead condenser 14 through separation of olefins column overhead outlet pipe 13, cooling rear 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 reactors enters azeotrope column 19 by azeotrope column feed pipe 18 and separates, the gas phase of azeotrope column 19 tower tops enters 21 condensations of azeotrope column overhead condenser through azeotrope column tower top outlet pipe 20, the unit alcohol product obtaining 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 alcohol product extraction of another part unit is to storage tank, the process water that azeotrope column 19 tower reactors obtain is recycled through process water recovery tube 24.
Claims (10)
1. the method for a water and olefine reaction productive unit alcohol, it is characterized in that: de-mineralized water and alkene are boosted after heating up and reacted in multistage superimposed fixed-bed reactor, temperature of reaction 130-250 ℃, reaction pressure 4.0-8.0MPaG, reacted mixture is decompressed to 0.5-1.0MPaA, is cooled to 40-60 ℃, then obtains unreacted alkene, process water and unit alcohol product through separating technology; Described multistage superimposed fixed-bed reactor form by the fixed bed of multistage or multistage is superimposed, and bed is counted N and is: 2≤N≤20.
2. method claimed in claim 1, is characterized in that: described raw material olefin is that carbonatoms is 2～30 all normal olefines or isomeric olefine.
3. method claimed in claim 1, is characterized in that: described raw material intensification temperature reaches 130-250 ℃.
4. method claimed in claim 1, is characterized in that: described raw material boost pressure reaches 4.0-8.0MPaG.
5. method claimed in claim 1, is characterized in that: the reaction conditions in described multistage superimposed fixed-bed reactor is: working pressure 7.0MPaG, 150 ℃ of service temperatures.
6. method claimed in claim 1, is characterized in that: it is 4≤N≤6 that described multistage superimposed fixed-bed reactor bed is counted N.
7. method claimed in claim 1, is characterized in that: described separating technology preferably includes: reacted mixture is isolated 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.
8. method claimed in claim 7, is characterized in that: described separation of olefins tower working pressure is 0.5-1.0MPaG, and service temperature is: tower top temperature 35-60 ℃, tower reactor temperature 130-150 ℃.
9. method claimed in claim 7, is characterized in that: described azeotrope column working pressure is 0.15-1.0MPaA, and service temperature is: tower top temperature 95-99 ℃, tower reactor temperature 110-130 ℃.
10. method claimed in claim 1, is characterized in that, comprises the following steps:
Raw material de-mineralized water purifies by the incoming stock de-mineralized water cleaner of raw material de-mineralized water feed-pipe (1) (2), incoming stock demineralized-water preheater (3) preheating again of the raw material de-mineralized water after purification, and temperature is mentioned 130-250 ℃, raw material olefin enters alkene preheater (5) through raw material olefin feed-pipe (4) and is preheated to 130-250 ℃, after raw material parallel feeding pipe (6) neutralization mixes from the raw material de-mineralized water of raw material demineralized-water preheater (3), sectional type enters multistage superimposed fixed-bed reactor (10) reaction from top to bottom, described multistage superimposed fixed-bed reactor (10) form by the fixed bed of multistage or multistage is superimposed, it is 4≤N≤6 that bed is counted N, temperature of reaction 130-250 ℃, reaction pressure 4.0-8.0MPaG, reacted mixture is decompressed to 0.5-1.0MPaA, after being cooled to 40-60 ℃, entering separation of olefins tower (12) through separation of olefins tower feed-pipe (11) separates, 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), cooling rear 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 separates, 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 obtaining 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 alcohol product extraction of another part unit 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 |
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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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| CN201410162624.3A CN103910601B (en) | 2014-04-22 | 2014-04-22 | Method for producing monohydric alcohol from water and olefins |
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| CN103910601A true CN103910601A (en) | 2014-07-09 |
| CN103910601B CN103910601B (en) | 2015-07-22 |
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Cited By (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 |
| WO2022089530A1 (en) * | 2020-10-28 | 2022-05-05 | 中国石油化工股份有限公司 | Liquid-liquid mixer, liquid-liquid reaction apparatus comprising liquid-liquid mixer, and liquid-liquid reaction method using liquid-liquid mixer |
| CN114478185A (en) * | 2020-10-28 | 2022-05-13 | 中国石油化工股份有限公司 | Olefin hydration process |
| CN114507116A (en) * | 2020-10-28 | 2022-05-17 | 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 |
-
2014
- 2014-04-22 CN CN201410162624.3A patent/CN103910601B/en active Active
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 |
Cited By (8)
| 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 |
| WO2022089530A1 (en) * | 2020-10-28 | 2022-05-05 | 中国石油化工股份有限公司 | Liquid-liquid mixer, liquid-liquid reaction apparatus comprising liquid-liquid mixer, and liquid-liquid reaction method using liquid-liquid mixer |
| CN114478185A (en) * | 2020-10-28 | 2022-05-13 | 中国石油化工股份有限公司 | Olefin hydration process |
| CN114507116A (en) * | 2020-10-28 | 2022-05-17 | 中国石油化工股份有限公司 | Olefin hydration reaction method |
| CN114505017A (en) * | 2020-10-28 | 2022-05-17 | 中国石油化工股份有限公司 | Olefin hydration reaction device and olefin hydration method |
| 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 |
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