CN201848255U - Catalyst reduction device for one-step catalytic synthesis of dimethyl ether gas - Google Patents
Catalyst reduction device for one-step catalytic synthesis of dimethyl ether gas Download PDFInfo
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- CN201848255U CN201848255U CN2010205032400U CN201020503240U CN201848255U CN 201848255 U CN201848255 U CN 201848255U CN 2010205032400 U CN2010205032400 U CN 2010205032400U CN 201020503240 U CN201020503240 U CN 201020503240U CN 201848255 U CN201848255 U CN 201848255U
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Abstract
The utility model discloses a catalyst reduction device for one-step catalytic synthesis of dimethyl ether gas, which mainly comprises a fixed-bed reactor, a heat conduction oil furnace, a compressor, an online hydrogen analyzer and a corresponding test system. A plurality of reaction tubes are arranged in parallel in the fixed-bed reactor, heat exchanger is carried out between catalysts in the reaction tubes and heat conduction oil outside the reaction tubes, and reduction reaction of reducing gases is carried out in the reaction tubes. Hydrogen and nitrogen are mixed in a pipeline to produce the reducing gases of a certain proportion, the reducing gases flow into a synthesis tower for catalyst reduction, online analysis of the hydrogen content in the mixed gases is carried out through the online hydrogen analyzer, the heat conduction oil furnace heats the heat conduction oil, the heat conduction oil reaches the shell pass of the reactor for heating to realize the temperature control of the fixed-bed reactor, the heat conduction oil after being heated circulates into the heat conduction oil furnace to be reheated, and tail gases generated in reduction flow into the compressor to boost pressure and then circulates into the fixed-bed reactor through a one-way valve. The catalyst reduction device is optimized and integrated based on the traditional chemical unit for catalyst reduction, and the waste of the hydrogen and nitrogen is greatly reduced during catalyst reduction. The system can be applied in chemical reaction for reduction prior to various types of reaction, and can be scaled in systems for one-step catalytic synthesis of the dimethyl ether so as to promote commercial operation of the one-step catalytic synthesis of the dimethyl ether.
Description
Technical field
The utility model relates to a kind of catalyst reduction reaction technology field, specially refers to the reduction apparatus of one-step method synthesizing dimethyl ether catalyst, belongs to coal/living beings chemical field.
Background technology
Because petroleum resources is day by day deficient, environmental pollution and greenhouse problem are serious day by day, obtain the high-grade liquid fuel and chemicals becomes a kind of development trend just gradually from living beings agriculture and forestry organic waste material resource (as stalk etc.), at home and abroad cause and show great attention to.The synthetic high-grade liquid fuel (as dimethyl ether, methyl alcohol, LPG etc.) of living beings gasification catalysis, be by after the directed gasification of living beings, through catalyst synthetic liquid fuel, chemicals, therefore, improve the technological core that activity of such catalysts has become whole catalysis synthesis system.The market prospects of biomass-based liquid fuel and chemicals finally depend on the competitiveness of cost, become the key link of its economy thereby reduce cost.Simultaneously, dimethyl ether can be used as the use that directly acts as a fuel of liquefied petroleum gas and diesel oil substitute.
At present, the synthetic production major part of one-step method dimethyl ether rests on laboratory and pilot scale stage, and its scale is less relatively, and production cost is higher.The large-scale production dimethyl ether adopts the direct conversion process of synthesis gas.Lab scale and pilot-scale are less demanding to reduction tolerance, and cost can manifest, and in the large industrialized process, saving cost will become the synthetic principal economic indicators of dimethyl ether.Therefore, the saving of reducing gases also will be the important component part of the synthetic cost of dimethyl ether in the catalyst reduction.
The reduction of one-step catalytic synthesizing dimethyl ether catalyst mainly contains following two reactions:
CuO+H
2＝Cu
2O+H
2O；Cu
2O+H
2＝Cu+H
2O；
As seen, one-step method from syngas catalytic synthesising dimethyl ether catalyst reduction reaction only needs H
2As reaction gas.But in reduction process, if with pure H
2Carry out catalyst reduction, can make the Cu crystal grain that restores become big, the active and life-span reduces greatly, therefore need utilize N
2As inert gas to H
2Dilute, thereby reduce the speed of reducing, reach the best reduction effect of catalyst.
The utility model content
The purpose of this utility model is at reducing gas H in the synthesizing dimethyl ether catalyst reduction process
2And N
2Waste and the optimization system of carrying out design, under the situation that does not influence the dimethyl ether synthetic catalyst reduction effect, hydrogen content is 0～25%, 0.3～0.5MPa, the catalyst reduction reaction is carried out in normal temperature to 270 ℃ temperature programming, provide a kind of simple, easy to operate, technology is reliable, can save 80% N
2With 50% H
2, simultaneously system is optimized integrated one-step catalytic synthesis gas dimethyl ether catalyst reduction apparatus.
For realizing above purpose, the utility model has been taked following technical scheme: one-step catalytic synthesizing dimethyl ether catalyst reduction apparatus, include fixed bed reactors, many reaction tubes of parallel distribution in these fixed bed reactors, have point for measuring temperature in the tubulation in described fixed bed reactors bottom, the top is provided with the reducing gases import, and the bottom is provided with the tail gas outlet of reduction back, the below, side is provided with the heat conductive oil inlet of two symmetries, and the top, side is provided with the conduction oil outlet; Be used to store and heat-conducting oil furnace that heat-conducting oil heating heats up, heat-conducting oil furnace is connected with fixed bed reactors by heat conductive oil inlet, the conduction oil outlet is connected to heat-conducting oil furnace by pipeline, the conduction oil of heat-conducting oil furnace is imported and exported is furnished with temperature point, simultaneously control conduction oil and enter fixed bed reactors shell side temperature according to program setting, conduction oil carries out heat exchange in fixed bed reactors after, flow out, reenter heat-conducting oil furnace and heat from the conduction oil outlet; Include the compressor of compressor inlet and compressor outlet, it is the recycling supercharging of reducing gases for a compressor, thereby it is recycling that reducing gases can be carried out, described compressor inlet is connected with the tail gas outlet of described reduction back by pipeline, described compressor outlet is connected with described reducing gases import by pipeline, all is equipped with the Pressure gauge that is used to control the check valve of reducing gases refluence and measures the compressor inlet and outlet pressure on above-mentioned pipeline; Also include the reducing gases H that on-line monitoring enters fixed bed reactors
2Content, whether need in the system to determine to replenish H with this
2So that the On-line Hydrogen Analyser of the normal operation of reduction process, H
2Gas content reduces, need be from H
2Provide H by import
2, H
2Content reaches requirement, stops to increase H
2On described compressor outlet and pipeline that described reducing gases import is connected, also be connected with H respectively
2Import and N
2Import; With also be provided with the tail gas emptying outlet on the pipeline that the tail gas outlet of described reduction back is connected, this system also comprises the compressor cooling water recirculation system, check valve prevents gas refluence, auxiliary equipment such as temperature measurement on-line pressure measurement.
In the tube side of fixed bed reactors dimethyl ether synthetic catalyst is housed, synthesis gas carries out catalytic synthesis through the catalyst after reducing under the condition of certain pressure, temperature, and the conduction oil of shell side for flowing is furnished with point for measuring temperature in the fixed bed reactors tubulation simultaneously; Many reaction tubes of parallel distribution in the fixed bed reactors, the outer conduction oil of reaction tube inner catalyst and reaction tube carries out heat exchange, and reducing gases is carried out reduction reaction in reaction tube.Hydrogen and nitrogen are mixed into a certain proportion of reducing gases in pipeline, enter synthetic tower and carry out the catalyst reduction reaction, hydrogen content carries out on-line analysis by On-line Hydrogen Analyser in the gaseous mixture, the control of fixed bed reaction actuator temperature arrives the reactor shell side by heat-conducting oil furnace heating conduction oil through pipeline and heats, conduction oil circulation after the heating enters heat-conducting oil furnace and heats, reduction tail gas enters compressor and carries out supercharging, enters fixed bed reactors by the check valve circulation.Whole catalyst reduction process be, hydrogen content is 0～25%, 0.3～0.5MPa carries out under normal temperature to the 270 ℃ condition, thereby dimethyl ether synthetic catalyst is reduced.
The utility model compared with prior art has following advantage: the utility model is optimized integrated on traditional catalyst reduction chemical unit basis, takes recycling inert gas N
2To H
2Reduce after the dilution, under the situation that does not reduce the catalyst reduction effect, save N
2And H
2Significantly reduce the waste of nitrogen and hydrogen in the catalyst reduction process; this system can use needs the chemical reaction that reduces before the various reactions, but scale simultaneously use in the one-step catalytic dimethyl ether synthesis system, advance the commercialized running of one-step catalytic dimethyl ether synthesis.
Description of drawings
Fig. 1 is the utility model one-step catalytic synthesizing dimethyl ether catalyst reduction apparatus schematic diagram;
Fig. 2 is H in the utility model temperature control program and the reduction process
2Content figure;
Description of reference numerals: 1, H
2Import, 2, N
2Import, 3, the reducing gases import, 4, the tail gas outlet of reduction back, 5, check valve, 6, compressor inlet, 7, compressor outlet, 8, tail gas emptying outlet, 9, fixed bed reactors, 10, On-line Hydrogen Analyser, 11, compressor, 12, heat-conducting oil furnace, 13, heat conductive oil inlet, 14, conduction oil outlet, 15, cooling water inlet, 16, coolant outlet, 17, Pressure gauge, 18, point for measuring temperature.
The specific embodiment
Below in conjunction with the drawings and specific embodiments content of the present utility model is described in further details.
Embodiment:
The one-step catalytic synthesizing dimethyl ether catalyst reduction apparatus of present embodiment and method are by utilizing ripe chemical industry equipment unit, carry out system's reorganization and optimize, adopt the method for recycling reducing gases, thereby reduce the waste of reducing gases, reducing production costs.
As shown in Figure 1, present embodiment provides one-step catalytic synthesizing dimethyl ether catalyst reduction apparatus, include fixed bed reactors 9, many reaction tubes of parallel longitudinal distribution in these fixed bed reactors 9, dimethyl ether catalyst is equipped with in tubulation inside, tubulation is full of the conduction oil that circulates outward, has point for measuring temperature 18 in the tubulation in fixed bed reactors 9 bottoms, and the bottom has the temperature thermocouple jack directly to insert tubulation middle part to carry out thermometric; The top is provided with reducing gases import 3 and connects tubulation, and the bottom is provided with reduction back tail gas outlet 4, and the below, side is provided with the heat conductive oil inlet 13 of two symmetries, and the top, side is provided with conduction oil outlet 14; Heat-conducting oil furnace 12, it is used to store and heat-conducting oil heating is heated up, conduction oil heats in heat-conducting oil furnace 12, provide the conduction oil of high temperature to enter the fixed bed reactors tube side, provide reduction reaction needed temperature, enter fixed bed reactors 9 shell sides by heat conductive oil inlet 13 and carry out heat exchange fixed bed reactors 9 heating, the conduction oil outlet 14 of conduction oil after the heat exchange by top, fixed bed reactors 9 side flowed out, and flows into heat-conducting oil furnace 12 heating that circulates by pipeline then; Include the compressor 11 of compressor inlet 6 and compressor outlet 7, compressor carries out supercharging circulation to the gas that reduced, and makes the reducing gases repeated use that circulates with this; Be provided with cooling water inlet 15 near on the compressor 11 of compressor outlet 7, be provided with coolant outlet 16 near on the compressor 11 of compressor inlet 6; Compressor inlet 6 is connected with reduction back tail gas outlet 4 by pipeline, compressor outlet 7 is connected with reducing gases import 3 by pipeline, Pressure gauge 17 and check valve 5 on above-mentioned pipeline, all be equipped with, check valve 5 is used to control reducing gases and flows backwards, and Pressure gauge 17 is measured compressor 11 inlet and outlet pressures, made its energy recycling for reducing gases provides power; Also include the reducing gases H that on-line monitoring enters fixed bed reactors 9
2Content, whether need in the system to determine to replenish H with this
2So that the On-line Hydrogen Analyser 10 of the normal operation of reduction process, On-line Hydrogen Analyser 10 is connected on the pipeline between compressor outlet 7 and the reducing gases import 3; On compressor outlet 7 and pipeline that reducing gases import 3 is connected, also be connected with H respectively
2Import 1 and N
2Import 2; With also be provided with tail gas emptying outlet 8 on reduction back tail gas outlet 4 pipelines that are connected, and the pressure measurement temperature measuring equipment of being correlated with.
Reduction reaction is carried out early stage, need utilize N
2Carry out system's displacement, guarantee that oxygen content is lower in the system, N
2Import 2 charges into nitrogen, opens compressor 11, makes system reach 0.3MPa, opens tail gas emptying outlet 8 then and discharges the substitution gas that contains oxygen, makes the N in the system
2Circulation is got up, and with this triplicate, makes that oxygen content is lower than 0.5% in the system, opens N then
2Import 2 makes system pressure reach 0.3MPa, opens compressor 11, makes gas circulation in the system, opens 12 pairs of fixed bed reactors 9 of heat-conducting oil furnace and heats, and when temperature reaches 50 ℃, opens H
21 pair of whole system of import is carried out hydrogenation, and beginning catalyst reduction reaction utilizes On-line Hydrogen Analyser 10 to carry out field monitoring, and heat-conducting oil furnace 12 heats up then, along with the H that carries out of reduction
2Content is kept within the specific limits by On-line Hydrogen Analyser, and along with the adding of hydrogen, pressure surpasses 0.5MPa in the system, need open the tail gas emptying outlet and come systems stabilisation pressure with this; Complete until reduction reaction; Heating schedule is set in reduction: by room temperature through 110 ℃ (1h), 140 ℃ (1h), 160 ℃ (3h), (1h～3h) reduce heats in the restoring system H in the temperature control program and reduction process in the actual motion for 220 ℃ (3h) and 270 ℃
2Content as shown in Figure 2.
Catalyst system therefor in the present embodiment is that the patent No. is: the bifunctional catalyst of the one-step method dimethyl ether synthesis of CN1785519.Fixed bed reactors in the present embodiment are number of patent application: the fixed bed reactors that design among the 200810218978.X.After the reduction of one-step method synthesizing dimethyl ether catalyst is finished, promptly carry out the dimethyl ether building-up process, its synthesis gas average group becomes:
V (H
2): V (CO): V (CO
2): V (O
2): V (N
2): V (CH
4)=28.63: 28.19: 29.19: 0.06: 11.54: 2.45, H wherein
2/ CO=0.98～1.17, C
2Above gas content is lower than 0.05%, synthetic operation continuously, and synthetic result such as following table:
Further, in the present embodiment in the fixed bed reactors 9 the tubulation size can design as required;
Heat-conducting oil furnace 12 can provide the relevant apparatus of heat for homogeneous solution-type reactor or electrical heating cover etc.;
The H that contains after the reduction tail gas outlet 4
2Equally can be recycling;
The compressor cooling water can be the soft water that running water or demineralized water treatment device were handled.
Above-listed detailed description is at the specifying of the utility model possible embodiments, and this embodiment is not in order to limiting claim of the present utility model, does not allly break away from the equivalence that the utility model does and implements or change, all should be contained in the claim of this case.
Claims (2)
1. one-step catalytic synthesis gas dimethyl ether catalyst reduction apparatus, it is characterized in that: include fixed bed reactors (9), many reaction tubes of parallel distribution in these fixed bed reactors (9), have point for measuring temperature (18) in the tubulation in described fixed bed reactors (9) bottom, the top is provided with reducing gases import (3), the bottom is provided with reduction back tail gas outlet (4), and the below, side is provided with the heat conductive oil inlet (13) of two symmetries, and the top, side is provided with conduction oil outlet (14);
The heat-conducting oil furnace (12) that is used to store and heat-conducting oil heating is heated up, heat-conducting oil furnace (12) is connected with fixed bed reactors (9) by heat conductive oil inlet (13), and conduction oil exports (14) and is connected to heat-conducting oil furnace (12) by pipeline;
Include the compressor (11) of compressor inlet (6) and compressor outlet (7), described compressor inlet (6) is connected with described reduction back tail gas outlet (4) by pipeline, described compressor outlet (7) is connected with described reducing gases import (3) by pipeline, all is equipped with the Pressure gauge (17) that is used to control the check valve (5) of reducing gases refluence and measures compressor (11) inlet and outlet pressure on above-mentioned pipeline;
Also include the reducing gases H that on-line monitoring enters fixed bed reactors (9)
2Content, whether need in the system to determine to replenish H with this
2So that the On-line Hydrogen Analyser (10) of the normal operation of reduction process;
On described compressor outlet (7) and pipeline that described reducing gases import (3) is connected, also be connected with H respectively
2Import (1) and N
2Import (2); With also be provided with tail gas emptying outlet (8) on the pipeline that described reduction back tail gas outlet (4) is connected.
2. one-step catalytic synthesis gas dimethyl ether catalyst reduction apparatus as claimed in claim 1 is characterized in that: described heat-conducting oil furnace (12) can be superheated steam boiler or electrical heating cover simultaneously.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010205032400U CN201848255U (en) | 2010-08-23 | 2010-08-23 | Catalyst reduction device for one-step catalytic synthesis of dimethyl ether gas |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010205032400U CN201848255U (en) | 2010-08-23 | 2010-08-23 | Catalyst reduction device for one-step catalytic synthesis of dimethyl ether gas |
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| Publication Number | Publication Date |
|---|---|
| CN201848255U true CN201848255U (en) | 2011-06-01 |
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ID=44090670
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2010205032400U Expired - Lifetime CN201848255U (en) | 2010-08-23 | 2010-08-23 | Catalyst reduction device for one-step catalytic synthesis of dimethyl ether gas |
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|---|---|
| CN (1) | CN201848255U (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101966472A (en) * | 2010-08-23 | 2011-02-09 | 中国科学院广州能源研究所 | Device and method for reducing catalyst for catalytic synthesis of dimethyl ether by one-step method |
| CN105709858A (en) * | 2014-12-01 | 2016-06-29 | 神华集团有限责任公司 | Catalyst continuous reducing apparatus and method |
| CN107096577A (en) * | 2017-06-21 | 2017-08-29 | 南通金源催化剂有限公司 | The reduction of low temperature isomerization catalyst, chlorination integrated apparatus |
-
2010
- 2010-08-23 CN CN2010205032400U patent/CN201848255U/en not_active Expired - Lifetime
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101966472A (en) * | 2010-08-23 | 2011-02-09 | 中国科学院广州能源研究所 | Device and method for reducing catalyst for catalytic synthesis of dimethyl ether by one-step method |
| CN101966472B (en) * | 2010-08-23 | 2012-06-20 | 中国科学院广州能源研究所 | Device for reducing catalyst for catalytic synthesis of dimethyl ether by one-step method |
| CN105709858A (en) * | 2014-12-01 | 2016-06-29 | 神华集团有限责任公司 | Catalyst continuous reducing apparatus and method |
| CN105709858B (en) * | 2014-12-01 | 2018-09-14 | 国家能源投资集团有限责任公司 | A kind of device and method of continuous reducing catalyst |
| CN107096577A (en) * | 2017-06-21 | 2017-08-29 | 南通金源催化剂有限公司 | The reduction of low temperature isomerization catalyst, chlorination integrated apparatus |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| AV01 | Patent right actively abandoned |
Granted publication date: 20110601 Effective date of abandoning: 20120620 |
|
| AV01 | Patent right actively abandoned |
Granted publication date: 20110601 Effective date of abandoning: 20120620 |