CN101735025B - Method and device for separating dimethyl ether from one-step synthesis dimethyl ether gas phase - Google Patents
Method and device for separating dimethyl ether from one-step synthesis dimethyl ether gas phase Download PDFInfo
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- CN101735025B CN101735025B CN 200910194375 CN200910194375A CN101735025B CN 101735025 B CN101735025 B CN 101735025B CN 200910194375 CN200910194375 CN 200910194375 CN 200910194375 A CN200910194375 A CN 200910194375A CN 101735025 B CN101735025 B CN 101735025B
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Abstract
The invention provides a method and a device for separating dimethyl ether from a one-step synthesized dimethyl ether gas phase. Soft water is used as an absorbing liquid for absorbing dimethyl ether in the mixed gas after reaction at the pressure of 1.0-2.0 MPa. The device comprises an absorbing tower. The upper part of the absorbing tower is provided with a circulatory absorbing liquid inlet, the middle part is provided with a soft water inlet, the bottom is provided with an absorbing liquid outlet, the middle lower part is provided with a mixed gas inlet, and the top is provided with a tail outlet after absorption. A soft water groove is communicated with the soft water inlet by a pressurizing pump and a pressure meter through pipelines, and is further communicated with a soft water spraying opening in the absorbing tower to form an absorbing liquid supplying system. The absorbing liquid outlet is sequentially connected with a circulatory pump, an absorbing liquid sampling outlet and an absorbing liquid circulatory inlet through pipelines, and is communicated with a circulatory liquid spraying opening in the absorbing tower to form an absorbing liquid circulatory utilizing loop. The absorbing liquid sampling opening is communicated with a rectifying tower by a pipeline and a pump. The invention has the advantages of simple structure, easy operation and mature technology, and solves the problem of dimethyl ether separating and purifying technology in the prior art.
Description
Technical field
The present invention relates to coal/biomass chemical field, relate in particular to a kind of from single stage method dimethyl ether synthesis gas phase the device of separation of dimethyl ether.
Technical background
Dme is a kind of broad-spectrum Chemicals, can the replacement fluorine chlorocarbon, and to do the molten sprays of gas and environment friendly refrigerating fluid and use, it easily compresses, easily stores, efficiency of combustion is high, it is low to pollute, and alternative coal gas, LPG make domestic fuel.Dme has higher cetane value simultaneously, can directly be used as the automobile fuel diesel oil substitute.Therefore, the potential market of dme is huge.
At present, industrial production dme adopts the two-step approach preparation, and this process using is by the synthetic gas synthesizing methanol, and then dimethyl ether preparation by dehydrating, and its unit scale is little, and production cost is higher.One-step technology has that flow process is short, reduced investment, low power consumption and other advantages, thereby and breaks thermodynamic(al)equilibrium and obtain higher per pass conversion.
Synthetic gas is converted into dme and mainly contains following two reactions:
2CO+4H
2＝CH
3OCH
3+H
2O ΔH＝-218.4KJ/mol(250℃)
3CO+3H
2＝CH
3OCH
3+CO
2 ΔH＝-257.9KJ/mol(250℃)
As seen, synthesis of dimethyl ether with synthesis gas one-step is the mixture of multiple gases through reacted gas, and in gas mixture, dme content is lower.Traditional carries out purifying to dme, and two kinds of methods can be arranged.A kind of is directly dme to be separated by filtering membrane, but present method is not mature enough, and there is no special filtering membrane for gas of dimethyl ether; Another is to adsorb dme under certain condition by certain medium, take out after absorption discharge or carry out separating-purifying by other simple method, but the method can not maturation be utilized suite of equipment at present, can't implement high efficiency operation.
Therefore, prior art from the technique of single stage method dimethyl ether synthesis, in the urgent need to supporting can be from low levels dme gas phase the method and apparatus of separation of dimethyl ether.
Summary of the invention
The object of the invention is to solve the difficult point of dme purification technique in prior art, method and the device of a kind of simple, easy to operate, technology maturation ground separation of dimethyl ether from single stage method dimethyl ether synthesis gas phase is provided.
For realizing above purpose, the inventive method comprises the following steps:
1) utilize the character of dme solubleness in water large (under normal temperature approximately 34%), utilize soft water to make absorption liquid, the dme in gas mixture after absorption reaction under 1.0-2.0MPa pressure in the absorption tower;
2) the tail gas circulation after after the absorption of top, absorption tower, the tail gas outlet is discharged after absorbing enters synthetic tower and recycles or enter gas driven generator and carry out the emission power generation utilization, absorption liquid is in the absorption liquid outlet extraction of bottom, absorption tower, to partially absorb liquid by recycle pump and again squeeze into the absorption tower through the absorption liquid loop head, circulation absorbs, and improves dme concentration in absorption liquid;
3) absorption liquid extraction part is carried out rectification and purification by pipeline and pump delivery in rectifying tower.
Soft water of the present invention refers to the softening water after the industrial soft water treatment unit is processed, and refers to that calcium salt and magnesium salts content are lower than the softening water of 10 mg/litre.
Soft water absorption cycle of the present invention uses flow process to belong to one-step catalytic dimethyl ether synthesis purification techniques field and uses first.
Apparatus of the present invention comprise the absorption tower, and filler or multilayer column plate are equipped with in this inside, absorption tower; Be provided with absorption liquid circulation import above described absorption tower, there is the soft water import at the middle part, and the bottom is provided with the absorption liquid outlet, and mixed gas inlet is established in middle below, tail gas outlet after the top is provided with and absorbs; Mixed gas inlet is communicated with to come the pipeline to synthetic tower; The soft water storage tank is communicated to the soft water import by pipeline through topping-up pump, tensimeter, and further is communicated to the soft water spout formation absorption liquid plenum system of being located at inside, absorption tower; Absorption liquid outlet connects recycle pump, absorption liquid extraction mouth, absorption liquid loop head successively by pipeline, and is communicated to the circulation fluid spout of inside, absorption tower, consists of absorption liquid recycle loop; Absorption liquid extraction mouth is communicated to rectifying tower by pipeline and pump.
After absorbing, generator or recycle pipeline are removed in tail gas outlet connection.
The further improvement of apparatus of the present invention is as follows:
Outside lower end, absorption tower is provided with the liquidometer that is communicated with the internal space, absorption tower.
The soft water storage tank is communicated with soft water treatment unit pipeline, and is furnished with liquidometer at soft water storage tank one end.
Absorption liquid plenum system pipeline is provided with safety valve.
After absorbing, the tail gas outlet is removed generator or recycle pipeline through tensimeter, under meter, reducing valve connection successively.
The absorption liquid loop head attaches under meter.
Absorption liquid recycle loop is provided with safety valve.
during apparatus of the present invention work, whole absorption process is under pressure, soft water enters the absorption tower by the soft water import after the topping-up pump supercharging, gas after synthetic enters the absorption tower through inlet mouth, whole absorption process absorbs exchange between filler top layer, absorption tower or column plate, then the tail gas after absorbing is discharged through the venting port with regard to the top, absorption liquid is in the absorption liquid outlet extraction of bottom, absorption tower, lower owing to absorbing dme concentration under circulation of absorption liquid, again squeeze into the absorption tower through the absorption liquid loop head so will partially absorb liquid by recycle pump, circulation absorbs increases dme concentration in absorption liquid with this, partially absorb liquid and carry out rectification and purification by pipeline and pump delivery in the extraction of absorption liquid extraction mouth in rectifying tower.
The inventive method and device are the brand-new design of carrying out on the prior art basis, and easy to operate, technique is simple, and efficient is high, and because absorption agent adopts industrial soft water, the while can recycle, has greatly improved assimilated efficiency, and has reduced cost.Ripe design provided by the invention has solved the technical problem of one-step method from syngas catalytic synthesising dimethyl ether separating-purifying aspect, is also that one-step catalytic dimethyl ether synthesis commercialization progress solves another engineering problem.
Description of drawings
Fig. 1 is apparatus of the present invention structural representation;
Fig. 2 is absorption tower structural representation in Fig. 1;
description of reference numerals: 1, the absorption tower, 2, mixed gas inlet, 3, tail gas outlet after absorbing, 4, the absorption liquid loop head, 5, the soft water import, 6, the absorption liquid outlet, 7, the circulation fluid spout, 8, the soft water spout, 9, filler or column plate, 10, liquidometer, 11, recycle pump, 12, safety valve, 13, under meter, 14, absorption liquid extraction mouth, 15, remove rectifying tower, 16, come to the synthetic tower pipeline, 17, tensimeter, 18, under meter, 19, reducing valve, 20, remove generator or recycle pipeline, 21, come to soft water treatment unit pipeline, 22, the soft water storage tank, 23, topping-up pump, 24, tensimeter, 25, safety valve, 26, liquidometer.
Embodiment
Below in conjunction with drawings and Examples, content of the present invention is described in further detail.
The separation of dimethyl ether device from single stage method dimethyl ether synthesis gas phase of the present embodiment is to carry out system's restructuring in the chemical industry equipment unit basis of maturation to optimize, adopt soft water to absorb the dme that synthesizes in gas phase as absorption agent, thereby make dme and other gas delivery, absorption liquid enters and carries out rectification and purification in rectifying tower.
As illustrated in fig. 1 and 2, comprise absorption tower 1, interior laterally parallel multiple filling layers or the column plate 9 of being distributed with in this absorption tower 1.Outside lower end, absorption tower 1 is provided with the liquidometer 10 that is communicated with 1 internal space, absorption tower.The middle and lower part on absorption tower 1 is provided with the rear mixed gas inlet 2 of reaction, the pipelines 16 that mixed gas inlet 2 connects to come to synthetic tower.
After being provided with absorption near 1 top, absorption tower, tail gas exports 3, and after absorbing, tail gas exports 3 and removes generator or recycle pipeline 20 through tensimeter 17, under meter 18, reducing valve 19 connections successively.
1 bottom, absorption tower is provided with absorption liquid outlet 6, absorption liquid outlet 6 connects recycle pump 11, absorption liquid extraction mouth 14, absorption liquid loop head 4 successively by pipeline, the subsidiary under meter 13 of absorption liquid loop head 4, absorption liquid loop head 4 also is communicated to the circulation fluid spout 7 of 1 inside, absorption tower, consist of absorption liquid recycle loop, absorption liquid recycle loop is provided with safety valve 12.
The interior soft water of soft water storage tank 22 is used for supplying with absorption tower 1 and absorbs the required soft water of dme that is synthesized.Soft water storage tank 22 is communicated to the soft water import 5 of being located at 1 middle and upper part, absorption tower through topping-up pump 23, tensimeter 24 by pipeline, and further be communicated to the soft water spout 8 formation absorption liquid plenum systems of being located at 1 inside, absorption tower, and described pipeline is provided with safety valve 25.Soft water storage tank 22 is communicated with soft water treatment unit pipeline 21, and is furnished with liquidometer 26 at soft water storage tank 22 1 ends.
During this device operation beginning, be 3.8-4.6MPa by the synthetic rear gaseous tension to synthetic tower pipeline 16, enter absorption tower 1 by reacting rear mixed gas inlet 2 by Pressure Drop after reducing valve to 1.2-2.0MPa, simultaneously soft water at topping-up pump 23 adherence pressures to a little more than absorption tower 1 pressure, by soft water import 5, spray in absorption tower 1 through soft water spout 8.After absorption liquid and reaction, gas mixture 1 interior filler or column plate 9 surfaces carries out gas-liquid mass transfer on the absorption tower, after dme is absorbed by liquid absorption, enter rectifying tower 15 by pipeline and pump by recycle pump 11 through absorption liquid outlet 6 after the 14 part extraction of absorption liquid extraction mouth and carry out rectification and purification, another part reenters absorption tower 1 through under meter 13 by absorption liquid loop head 4, spray into circulation absorption in absorption tower 1 through circulation fluid spout 7, further promote dme concentration in absorption liquid.After absorbing, tail gas is gone out from absorbing rear tail gas outlet 3, by tensimeter 17, under meter 18, reducing valve 19 rear past go generator or recycle pipeline 20.
Results of experimental operation is as shown in the table:
Can be found out by above-mentioned experimental data, before and after absorbing, DME (dme) all has been absorbed through dme in tail gas after absorption system by original 8.4-11.4% (volume content), illustrates that the present invention has the advantages such as assimilated efficiency is high, cost absorption is low.
Claims (8)
1. the method for separation of dimethyl ether from single stage method dimethyl ether synthesis gas phase, is characterized in that comprising the steps:
1) utilize the large character of dme solubleness in water, utilize soft water to make absorption liquid, the dme in gas mixture after absorption reaction under 1.0-2.0MPa pressure in the absorption tower, described soft water refer to that calcium salt and magnesium salts content are lower than the softening water of 10 mg/litre;
2) the tail gas outlet after the absorption of top, absorption tower of the tail gas after the absorption is discharged, absorption liquid is in the absorption liquid outlet extraction of bottom, absorption tower, to partially absorb liquid by recycle pump and again squeeze into the absorption tower through the absorption liquid loop head, circulation absorbs, and increases dme concentration in absorption liquid;
3) absorption liquid extraction part is carried out rectification and purification by pipeline and pump delivery in rectifying tower.
2. the device of a separation of dimethyl ether from single stage method dimethyl ether synthesis gas phase, comprise the absorption tower, filler or multilayer column plate are equipped with in this inside, absorption tower, it is characterized in that: be provided with the circulating absorption solution import above described absorption tower, there is the soft water import at the middle part, the bottom is provided with the absorption liquid outlet, and mixed gas inlet is established in middle below, tail gas outlet after the top is provided with and absorbs; Mixed gas inlet is communicated with to come the pipeline to synthetic tower; The soft water storage tank is communicated to the soft water import by pipeline through topping-up pump, tensimeter, and further is communicated to the soft water spout formation absorption liquid plenum system of being located at inside, absorption tower; Absorption liquid outlet connects recycle pump, absorption liquid extraction mouth, absorption liquid loop head successively by pipeline, and described absorption liquid loop head is communicated to the circulation fluid spout of inside, absorption tower, consists of absorption liquid recycle loop; Described absorption liquid extraction mouth is communicated to rectifying tower by pipeline and pump; After absorbing, generator or recycle pipeline are removed in tail gas outlet connection.
As claimed in claim 2 from single stage method dimethyl ether synthesis gas phase the device of separation of dimethyl ether, it is characterized in that: outside lower end, described absorption tower is provided with the liquidometer that is communicated with the internal space, absorption tower.
As claimed in claim 2 from single stage method dimethyl ether synthesis gas phase the device of separation of dimethyl ether, it is characterized in that: described soft water storage tank is communicated with soft water treatment unit pipeline, and is furnished with liquidometer at soft water storage tank one end.
As claimed in claim 2 from single stage method dimethyl ether synthesis gas phase the device of separation of dimethyl ether, it is characterized in that: described absorption liquid plenum system pipeline is provided with safety valve.
As claimed in claim 2 from single stage method dimethyl ether synthesis gas phase the device of separation of dimethyl ether, it is characterized in that: after described absorption, the tail gas outlet is communicated with through tensimeter, under meter, reducing valve successively and removes generator or recycle pipeline.
As claimed in claim 2 from single stage method dimethyl ether synthesis gas phase the device of separation of dimethyl ether, it is characterized in that: described absorption liquid loop head attaches under meter.
As claimed in claim 2 from single stage method dimethyl ether synthesis gas phase the device of separation of dimethyl ether, it is characterized in that: described absorption liquid recycle loop is provided with safety valve.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200910194375 CN101735025B (en) | 2009-12-02 | 2009-12-02 | Method and device for separating dimethyl ether from one-step synthesis dimethyl ether gas phase |
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|---|---|---|---|
| CN 200910194375 CN101735025B (en) | 2009-12-02 | 2009-12-02 | Method and device for separating dimethyl ether from one-step synthesis dimethyl ether gas phase |
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| CN101735025A CN101735025A (en) | 2010-06-16 |
| CN101735025B true CN101735025B (en) | 2013-11-06 |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1215716A (en) * | 1998-08-12 | 1999-05-05 | 中国科学院大连化学物理研究所 | Process for preparing dimethyl ether from synthetic gas |
| CN1293178A (en) * | 2000-10-21 | 2001-05-02 | 天津市新天进科技开发有限公司 | Catalytic process for preparing ethylbenzene from dry gas |
| US6458856B1 (en) * | 2001-11-07 | 2002-10-01 | Air Products And Chemicals, Inc. | Separation process for one-step production of dimethyl ether from synthesis gas |
| CN1548411A (en) * | 2003-05-21 | 2004-11-24 | 中国石油化工集团公司 | Separation method of dimethyl ether prepared with synthetic gas through one-step process |
| CN201574123U (en) * | 2009-12-02 | 2010-09-08 | 中国科学院广州能源研究所 | Device for separating dimethyl ether from dimethyl ether synthesized by one-step method |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1215716A (en) * | 1998-08-12 | 1999-05-05 | 中国科学院大连化学物理研究所 | Process for preparing dimethyl ether from synthetic gas |
| CN1293178A (en) * | 2000-10-21 | 2001-05-02 | 天津市新天进科技开发有限公司 | Catalytic process for preparing ethylbenzene from dry gas |
| US6458856B1 (en) * | 2001-11-07 | 2002-10-01 | Air Products And Chemicals, Inc. | Separation process for one-step production of dimethyl ether from synthesis gas |
| CN1548411A (en) * | 2003-05-21 | 2004-11-24 | 中国石油化工集团公司 | Separation method of dimethyl ether prepared with synthetic gas through one-step process |
| CN201574123U (en) * | 2009-12-02 | 2010-09-08 | 中国科学院广州能源研究所 | Device for separating dimethyl ether from dimethyl ether synthesized by one-step method |
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