CN201358217Y - Reactor for producing dimethyl ether from methanol through vapor-phase dehydration under pressurization - Google Patents
Reactor for producing dimethyl ether from methanol through vapor-phase dehydration under pressurization Download PDFInfo
- Publication number
- CN201358217Y CN201358217Y CNU2009200665372U CN200920066537U CN201358217Y CN 201358217 Y CN201358217 Y CN 201358217Y CN U2009200665372 U CNU2009200665372 U CN U2009200665372U CN 200920066537 U CN200920066537 U CN 200920066537U CN 201358217 Y CN201358217 Y CN 201358217Y
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- conversion zone
- reactor
- methyl alcohol
- methanol
- dme
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Abstract
The utility model relates to a reactor for producing dimethyl ether from methanol through vapor-phase dehydration under pressurization. The reactor comprises an upper sealing head, a methanol gasifying section, reaction sections and a lower sealing head, wherein a cylinder body is formed by connecting the methanol gasifying section at upper part with one to three reaction sections at lower part in series; a catalytic agent layer and a cooling coil are arranged in each reaction section; the cooling coils are connected with the inlet and the outlet of cooling media; the reaction sections are separated by catalytic agent supporting plates; catalytic agents filled in the reaction sections from the top down have the same volume, or increase gradually or decrease gradually; and the reaction products enter separation procedure through a reactant outlet. The utility model provides a reactor for producing dimethyl ether from methanol through vapor-phase dehydration under pressurization, has the advantages of small occupied area, simple structure and full and reasonable use of heat, and is easy for large scalization of equipment.
Description
[technical field]
The utility model relates to the chemical reaction device technical field, specifically, relates to the production equipment of dme (DME), relates in particular to the reactor that methyl alcohol gas-phase dehydration under pressurized conditions generates dme.
[background technology]
Dme is a kind of ideal clean fuel, can be used as domestic fuel and automobile fuel, is the surrogate of fluorochlorohydrocarbon class, can reduce the destruction to atmospheric ozone layer; The sprays carrier that dme also can be used as aerosol industry uses, as the raw material of producing low-carbon alkene.Dme is as the raw material of clean fuel and low-carbon alkene, and its market is huge.
At present, the type of reactor that is used for producing dimethyl ether by dehydrating methanol mainly contains:
(1) methanol liquid-phase dehydration continuous stir reactor reactor is traditional liquid-phase dehydration method of catalyzer with the vitriol oil because separation difficulty, waste liquor contamination be serious etc. problem substantially need not now.Chinese patent literature CN1322704A has reported the technology with complex and dewatering and catalyzing process to produce dimethyl ether, and it adopts common continuous stir reactor as reactor.But, because the characteristic of continuous stir reactor reactor makes the methyl alcohol that adds to react away rapidly, cause a lot of methyl alcohol to volatilize, therefore, need to increase rectifier unit and separate and reclaim methyl alcohol with dme, the complex manufacturingization that this just makes dme has increased production cost.
(2) Chinese patent literature CN1194257 has proposed under nearly methanol critical state the reaction process equipment of dimethyl ether synthesis in the slurry bed, because it has proposed harsh requirement to production unit, yet there are no and implements report.
(3) Chinese patent literature CN1907932A has reported a kind of method of methanol production dme, but, because its reaction is carried out under 120～220 ℃, and methyl alcohol enters reactor with liquid phase or gas-liquid phase admixture under this temperature, the contact area of methyl alcohol and catalyzer is less, therefore, the throughput of single reactor is limited.
(4) Chinese patent literature CN2900523Y has proposed the reactor that a kind of methanol vapor phase that has heat exchanging segment is produced dme, because the exothermic heat of reaction amount of producing dimethyl ether by dehydrating methanol is very little, under the little situation of dme turnout, the reaction process liberated heat not only is difficult to heat import gas phase methanol steam, even can reason causes the gas-phase methanol vapor condensation owing to the reactor heat insulation effect is bad etc.; Meanwhile, because this type reactor is operated under normal pressure, along with the increase of dme output, its volume is also huge day by day, can't satisfy the requirement that dme production is maximized.
Because the reactor of above producing dimethyl ether by dehydrating methanol is all operated under normal pressure, therefore, no matter be the preheating and the gasification of material benzenemethanol before the reaction, still react the recovery of after product reaction heat, all low potential energy heat under normal pressure, whole process flow needs a plurality of interchanger around reactor, therefore, has increased the investment on equipment greatly.
[utility model content]
The purpose of this utility model is to overcome the deficiency that prior art exists, provide a kind of floor space little, simple in structure, fully rationally utilize heat, be easy to the reactor of methyl alcohol gas-phase dehydration generation dme under pressurized conditions of equipment enlarging.
For achieving the above object, the technical scheme taked of the utility model is:
A kind of methyl alcohol gas-phase dehydration under pressurized conditions generates the reactor of dme, contain cylindrical shell, upper cover, the methanol gasifying section, conversion zone and lower cover, on upper cover, be provided with the import of liquid phase methyl alcohol and be convenient to the uniform spray thrower of liquid phase methyl alcohol, in the methanol gasifying section, be provided with the heating coil that makes the liquid phase methanol gasifying, one end of heating coil is connected in the heating medium import that is arranged at methanol gasifying section below, the other end of heating coil is connected with the heating medium outlet that is arranged on methanol gasifying section top, between heating coil, load inert filler, inert filler is the porcelain ring of Φ 5 * 5, and the porcelain ring is supported by the inert filler back up pad; On lower cover, be provided with the reactant outlet, it is characterized in that, simplifiedly be composed in series by the methanol gasifying section on top and 1～3 conversion zone of bottom, in each conversion zone, be provided with catalyst layer and spiral coil cooling tube, the lower end of spiral coil cooling tube is connected on the cooling medium inlet that is arranged at conversion zone below, the upper end of spiral coil cooling tube be arranged at conversion zone intermediary heat-eliminating medium and export and be connected; Separate by the catalyzer back up pad between conversion zone and the conversion zone; The catalyst volume that each conversion zone loaded from top to bottom identical (1: 1: 1), correspondingly, the ratio of the cooling area of spiral coil cooling tube identical (1: 1: 1); Reaction product enters separation circuit by reactant outlet 18 at last.
The described catalyst volume that each conversion zone loaded from top to bottom increases (1: 1～3: 1～4) gradually, and correspondingly, the ratio of the cooling area of spiral coil cooling tube increases (1: 1～3: 1～4) gradually.
The described catalyst volume that each conversion zone loaded from top to bottom reduces (1: 1/3～1: 1/4～1) gradually, and correspondingly, the ratio of the cooling area of spiral coil cooling tube reduces (1: 1/3～1: 1/4～1) gradually.
The caliber of described heating coil is φ 16～35mm, and medium-pressure or high pressure steam is led in the heating medium import.
The internal diameter of described spiral coil cooling tube is Φ 18～60mm, and the cold pipe area of unit volume is 20～120m
2/ m
3
The heat-eliminating medium of described conversion zone is 104～140 ℃ of medium pressure boiler water, or material benzenemethanol.
Described cooling medium inlet or be arranged on the bottom of each conversion zone, or be arranged on the middle part of each conversion zone.
A kind of aforesaid methyl alcohol gas-phase dehydration under pressurized conditions generates the reactor of dme, it is characterized in that, the cooling segment of reactor is the direct cold shock of material benzenemethanol, do not establish the outlet of spiral coil cooling tube and heat-eliminating medium in the conversion zone, material benzenemethanol enters the import of liquid phase methyl alcohol by a sparger part, another part or uniform distribution flow (1: 1: 1), or increase (1: 1～3: 1～4) gradually, or minimizing (1: 1/3～1: 1/4～1) enters conversion zone by the heat-eliminating medium inlet gradually, mix with reacted logistics, reaction product enters separation circuit by the reactant outlet at last.
Positively effect of the present utility model is:
(1) reactor of methyl alcohol gas-phase dehydration generation dme under pressurized conditions comprises methanol gasifying section and methanol dehydration section, place same reactor to produce by two processes with liquid phase methyl alcohol heating and gasifying and methyl alcohol reaction dimethyl ether synthesis, not only reduced outside reaction unit and heated, the energy waste that causes in pressurization methyl alcohol and the pipeline transmission process, and overcome methyl alcohol and depressed easy liquefaction adding, under high-temperature and high-pressure conditions, easily be decomposed to form the shortcoming of by product, improved reaction preference, the reaction operation under high pressure that makes methanol dehydration generate dme becomes a reality.And, because the increase of reaction pressure can reduce reactor volume under the situation of equivalent production capacity greatly, but the transformation efficiency of reaction does not descend, realization reduces the purpose of design of equipment size, productivity gain, and can realize the maximization of producing dimethyl ether by dehydrating methanol technology.
(2) dme that adopts pressurized operation to produce under producing times over the atmospheric operation condition under the identical situation of reactor volume helps the maximization of producing dimethyl ether by dehydrating methanol reactor.
(3) reactor that adopts of the utility model makes methanol gasifying and methanol dehydration integrated, simultaneously according to the little characteristics of producing dimethyl ether by dehydrating methanol exothermic heat of reaction amount, taken into full account the heat effect that may form after reactor maximizes, adopted the pattern of intersegmental coil pipe cooling or material benzenemethanol cold shock, avoided adopting complicated heat transfer tube, can not only reclaim the heat of high potential, and greatly reduce the cost that equipment is made.
[description of drawings]
Accompanying drawing 1 is the structural representation that the utility model methyl alcohol gas-phase dehydration under pressurized conditions generates the reactor of dme;
Accompanying drawing 3 is that the utility model is at the structural representation and the flow graph that adopt under the direct cold shock mode of material benzenemethanol.
Label among the figure is respectively:
1, cylindrical shell, 2, upper cover, 3, the import of liquid phase methyl alcohol,
4, spray thrower, 5, gasification section, 6, the heating medium outlet,
7, heating coil, 8, inert filler, 9, the heating medium import,
10, inert filler back up pad, 11, conversion zone, 12, catalyst layer,
13, heat-eliminating medium outlet, 14, spiral coil cooling tube, 15, cooling medium inlet,
16, catalyzer back up pad, 17, lower cover, 18, the reactant outlet.
[embodiment]
Below specifically introduce the embodiment that the utility model methyl alcohol gas-phase dehydration under pressurized conditions generates the reactor of dme by accompanying drawing, still, enforcement of the present utility model is not limited to following form.
Referring to accompanying drawing 1.
A kind of methyl alcohol gas-phase dehydration under pressurized conditions generates the reactor of dme, and its cylindrical shell 1 comprises upper cover 2, methanol gasifying section 5, conversion zone 10 and lower cover 17.
The internal diameter of cylindrical shell 1 is 3.8 meters (can adjust according to the DESIGN OF REACTOR scale), and top is methanol gasifying section 5, and liquid phase methyl alcohol import 3 is set on arcual upper cover 2, below liquid phase methyl alcohol import 3 spray thrower 4 is set; Upper cover 2 is connected with methanol gasifying section 5, and heating coil 5 is set in methanol gasifying section 5, and adopting caliber is the heating coil 7 of φ 16～35mm, meet the requirement of logical medium-pressure or high pressure steam; One end of heating coil 7 is connected in the heating medium import 9 that is arranged at methanol gasifying section 5 belows, the other end is connected with the heating medium outlet 6 that is arranged on methanol gasifying section 5 tops, filling inert filler 8 between heating coil 5, inert filler is the porcelain ring of Φ 5 * 5, and the porcelain ring is supported by inert filler back up pad 10.
The below of methanol gasifying section 5, the middle and lower part that is cylindrical shell 1 is composed in series by 1～3 conversion zone 11, in each conversion zone 11, be provided with catalyst layer 12, in the middle and lower part of conversion zone 11 spiral coil cooling tube 14 is set, adopting internal diameter is the spiral coil cooling tube 14 of Φ 18～60mm, the cold pipe area of unit volume is 20～120m2/m3, the lower end of spiral coil cooling tube 14 is connected on the cooling medium inlet 15 that is arranged at conversion zone 11 belows, the upper end of spiral coil cooling tube 14 be arranged at conversion zone 11 intermediary heat-eliminating mediums outlet 13 and be connected; Separate by catalyzer back up pad 16 between conversion zone 11 and the conversion zone 11;
The catalyst volume that three conversion zones 11 are from top to bottom loaded can identical (1: 1: 1), can increase (1: 1～3: 1～4) gradually, also can reduce (1: 1/3～1: 1/4～1) gradually, correspondingly, the ratio of the cooling area of spiral coil cooling tube 14 also can identical (1: 1: 1), can increase (1: 1～3: 1～4) gradually, also can reduce (1: 1/3～1: 1/4～1) gradually; At last, reaction product enters separation circuit by reactant outlet 18.
The heat-eliminating medium of conversion zone 11 can adopt 100～140 ℃ of medium pressure boiler water, and at this moment reactor can the by-product middle pressure steam.
The heat-eliminating medium of conversion zone 11 also can adopt material benzenemethanol, if adopt the words of material benzenemethanol, through the material benzenemethanol of pressurization by sparger in each conversion zone 11 from top to bottom or uniform distribution flow (1: 1: 1), or increase (1: 1～3: 1～4) gradually, or minimizing (1: 1/3～1: 1/4～1) enters cooling medium inlet 13 gradually, through deriving from heat-eliminating medium outlet 13 after spiral coil cooling tube 9 heat exchange, merging enters reaction unit from liquid phase methyl alcohol import 3 and reacts, and reaction product enters separation circuit (referring to accompanying drawing 2) by reactant outlet 18 at last.
If the cooling segment of reactor adopts the direct cold shock of material benzenemethanol, do not establish spiral coil cooling tube 14 and heat-eliminating medium outlet 13 in the conversion zone 11, material benzenemethanol enters liquid phase methyl alcohol import 3 by a sparger part, another part or uniform distribution flow (1: 1: 1) or increase (1: 1～3: 1～4) gradually or reduce (1: 1/3～1: 1/4～1) gradually and enter conversion zone 11 by heat-eliminating medium inlet 15, mix with reacted logistics, reaction product enters separation circuit (referring to accompanying drawing 3) by reactant outlet 18 at last.
The reactor that adopts the utility model methyl alcohol gas-phase dehydration under pressurized conditions to generate dme has carried out relevant enforcement checking, and its result is as follows:
Employing is with γ-Al
2O
3It is main methanol dehydration catalyst, granularity is Φ 3 * (15～25), imported raw material is a refined methanol, flow is 140kg/h, and refined methanol is through methanol gasifying section 5, and temperature is elevated to 270 ℃, pressure is elevated to 5.0Mpa, enter conversion zone 11 reactions, hot(test)-spot temperature is elevated to 385 ℃, enters separation system after temperature are reduced to 250 ℃ after spiral coil cooling tube 14 coolings; Get reaction product dme 82.6kg/h, water 32.5kg/h, residue methyl alcohol 25kg/h.
Employing is with γ-Al
2O
3Be main methanol dehydration catalyst, granularity is Φ 3 * (15～25), and imported raw material is thick methyl alcohol, and flow is 140kg/h, and wherein quantity of methyl alcohol is 126kg/h, and water is 14kg/h; Thick methyl alcohol is through methanol gasifying section 5, and temperature is elevated to 270 ℃, and pressure is elevated to 5.0Mpa, enters conversion zone 11 reactions, and hot(test)-spot temperature is elevated to 375 ℃, enters separation system after temperature are reduced to 250 ℃ after spiral coil cooling tube 14 coolings; Get dme 80.5kg/h in the reaction product, water 39.4kg/h, residue methyl alcohol 14kg/h.
Employing is with γ-Al
2O
3It is main methanol dehydration catalyst, granularity is Φ 3 * (15～25), and imported raw material is a refined methanol, and flow is 2800kg/h, refined methanol is through methanol gasifying section 5, temperature is elevated to 270 ℃, and pressure is elevated to 5.0Mpa, enters 11 reactions of first conversion zone, hot(test)-spot temperature is elevated to 385 ℃, enter 11 reactions of second conversion zone by after temperature are reduced to 270 ℃ after spiral coil cooling tube 14 coolings, hot(test)-spot temperature is elevated to 380 ℃, enters separation system after temperature are reduced to 255 ℃ after spiral coil cooling tube 14 coolings; Get reaction product dme 1652kg/h, water 646.5kg/h, residue methyl alcohol 501.5kg/h.
Employing is with γ-Al
2O
3It is main methanol dehydration catalyst, granularity is Φ 3 * (15～25), imported raw material is a refined methanol, flow is 28000kg/h, refined methanol is through methanol gasifying section 5, temperature is elevated to 280 ℃, pressure is elevated to 6.0Mpa, enter 11 reactions of first conversion zone, hot(test)-spot temperature is elevated to 390 ℃, enters 11 reactions of second conversion zone by after temperature are reduced to 270 ℃ after spiral coil cooling tube 14 coolings, hot(test)-spot temperature is elevated to 385 ℃, enter 11 reactions of the 3rd conversion zone by after temperature are reduced to 285 ℃ after spiral coil cooling tube 14 coolings, hot(test)-spot temperature is elevated to 380 ℃, enters separation system after temperature are reduced to 250 ℃ after spiral coil cooling tube 14 coolings; Get reaction product dme 16732kg/h, water 6547.3kg/h, residue methyl alcohol 4718kg/h.
Claims (7)
1, a kind of methyl alcohol gas-phase dehydration under pressurized conditions generates the reactor of dme, contain cylindrical shell (1), upper cover (2), methanol gasifying section (5), conversion zone (10) and lower cover (17), on upper cover (2), be provided with liquid phase methyl alcohol import (3) and be convenient to the uniform spray thrower of liquid phase methyl alcohol (4), in methanol gasifying section (5), be provided with the heating coil (5) that makes the liquid phase methanol gasifying, one end of heating coil (7) is connected in the heating medium import (9) that is arranged at methanol gasifying section (5) below, the other end of heating coil (7) is connected with the heating medium outlet (6) that is arranged on methanol gasifying section (5) top, between heating coil (5), load inert filler (8), inert filler is the porcelain ring of φ 5 * 5, and the porcelain ring is supported by inert filler back up pad (10); On lower cover (17), be provided with reactant outlet (18), it is characterized in that, cylindrical shell (1) is composed in series by the methanol gasifying section (5) on top and 1～3 conversion zone (11) of bottom, in each conversion zone (11), be provided with catalyst layer (12) and spiral coil cooling tube (14), the lower end of spiral coil cooling tube (14) is connected on the cooling medium inlet (15) that is arranged at conversion zone (11) below, the upper end of spiral coil cooling tube (14) be arranged at conversion zone (11) intermediary heat-eliminating medium and export (13) and be connected; Separate by catalyzer back up pad (16) between conversion zone (11) and the conversion zone (11); Identical 1: 1: 1 of the catalyst volume that each conversion zone (11) is from top to bottom loaded, correspondingly, identical 1: 1: 1 of the ratio of the cooling area of spiral coil cooling tube (14); Reaction product enters separation circuit by reactant outlet (18) at last.
2, methyl alcohol according to claim 1 gas-phase dehydration under pressurized conditions generates the reactor of dme, it is characterized in that, the catalyst volume that described each conversion zone (11) is from top to bottom loaded increases by 1: 1～3: 1～4 gradually, correspondingly, the ratio of the cooling area of spiral coil cooling tube (14) increases by 1: 1～3: 1～4 gradually.
3, methyl alcohol according to claim 1 gas-phase dehydration under pressurized conditions generates the reactor of dme, it is characterized in that, the catalyst volume that described each conversion zone (11) is from top to bottom loaded reduces 1: 1/3 gradually～and 1: 1/4～1, correspondingly, the ratio of the cooling area of spiral coil cooling tube (14) reduce 1: 1/3 gradually～1: 1/4～1.
4, methyl alcohol according to claim 1 gas-phase dehydration under pressurized conditions generates the reactor of dme, it is characterized in that the caliber of described heating coil (7) is φ 16～35mm, and medium-pressure or high pressure steam is led in heating medium import (9).
5, methyl alcohol according to claim 1 gas-phase dehydration under pressurized conditions generates the reactor of dme, it is characterized in that the internal diameter of described spiral coil cooling tube (14) is φ 18～60mm, and the cold pipe area of unit volume is 20～120m
2/ m
3
6, methyl alcohol according to claim 1 gas-phase dehydration under pressurized conditions generates the reactor of dme, it is characterized in that the heat-eliminating medium of described conversion zone (11) is 104～140 ℃ of medium pressure boiler water, or material benzenemethanol.
7, methyl alcohol according to claim 1 gas-phase dehydration under pressurized conditions generates the reactor of dme, it is characterized in that, and described cooling medium inlet (15) or be arranged on the bottom of each conversion zone, or be arranged on the middle part of each conversion zone.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNU2009200665372U CN201358217Y (en) | 2009-01-06 | 2009-01-06 | Reactor for producing dimethyl ether from methanol through vapor-phase dehydration under pressurization |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNU2009200665372U CN201358217Y (en) | 2009-01-06 | 2009-01-06 | Reactor for producing dimethyl ether from methanol through vapor-phase dehydration under pressurization |
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| Publication Number | Publication Date |
|---|---|
| CN201358217Y true CN201358217Y (en) | 2009-12-09 |
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|---|---|---|---|
| CNU2009200665372U Expired - Lifetime CN201358217Y (en) | 2009-01-06 | 2009-01-06 | Reactor for producing dimethyl ether from methanol through vapor-phase dehydration under pressurization |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101768054A (en) * | 2009-01-06 | 2010-07-07 | 华东理工大学 | Method and device for producing dimethyl ether by gaseous phase dehydration of methanol under pressurized conditions |
| CN103797096A (en) * | 2011-04-01 | 2014-05-14 | 赫多特普索化工设备公司 | Process for preparing a fuel for automotive applications, stationary engines and marine applications by catalytic liquid phase alcohol conversion and a compact device for carrying out the process |
| CN108067162A (en) * | 2016-11-17 | 2018-05-25 | 中国石油化工股份有限公司 | A kind of hydrogenation reactor and hydrogenation method |
-
2009
- 2009-01-06 CN CNU2009200665372U patent/CN201358217Y/en not_active Expired - Lifetime
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101768054A (en) * | 2009-01-06 | 2010-07-07 | 华东理工大学 | Method and device for producing dimethyl ether by gaseous phase dehydration of methanol under pressurized conditions |
| CN101768054B (en) * | 2009-01-06 | 2013-10-16 | 华东理工大学 | Method and device for producing dimethyl ether by gaseous phase dehydration of methanol under pressurized conditions |
| CN103797096A (en) * | 2011-04-01 | 2014-05-14 | 赫多特普索化工设备公司 | Process for preparing a fuel for automotive applications, stationary engines and marine applications by catalytic liquid phase alcohol conversion and a compact device for carrying out the process |
| CN108067162A (en) * | 2016-11-17 | 2018-05-25 | 中国石油化工股份有限公司 | A kind of hydrogenation reactor and hydrogenation method |
| CN108067162B (en) * | 2016-11-17 | 2020-12-08 | 中国石油化工股份有限公司 | Hydrogenation reactor and hydrogenation process method |
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| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CX01 | Expiry of patent term |
Granted publication date: 20091209 |
|
| CX01 | Expiry of patent term |