CN1226262C - Separation method of dimethyl ether prepared with synthetic gas through one-step process - Google Patents

Separation method of dimethyl ether prepared with synthetic gas through one-step process Download PDF

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Publication number
CN1226262C
CN1226262C CN 03134277 CN03134277A CN1226262C CN 1226262 C CN1226262 C CN 1226262C CN 03134277 CN03134277 CN 03134277 CN 03134277 A CN03134277 A CN 03134277A CN 1226262 C CN1226262 C CN 1226262C
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gas
tower
separation method
dimethyl ether
product
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CN1548411A (en
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唐宏青
房鼎业
唐锦文
郑明峰
苏明
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Sinopec Ningbo Engineering Co Ltd
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China Petrochemical Corp
Sinopec Lanzhou Design Institute
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Abstract

The present invention mainly relates to a separation method for preparing dimethyl ether in one step, particularly to a separation method for preparing dimethyl ether from synthetic gas in one step. The separation method for preparing dimethyl ether from synthetic gas in one step comprises: reacted gas is condensed by a conderser; non-condensed gas is filled into the lower part of an absorption tower and is absorbed by soft water; products of tail gas from the tower top of the absorption tower are filled into a gas cabinet. The separation method is mainly characterized in that products of crude dimethyl ether solution at the bottom flow of the condenser and/or products of ether water solution are filled into a flash pot; gas evaporated in flash is filled into the bottom part of the absorption tower; a product of pure ethereal solution at the bottom flow of the flash pot is filled into a dimethyl ether rectifying tower; a product at the tower top is refined dimethyl ether, and a product at the bottom flow is crude methanol solution. By using the present invention, the purity of the product of dimethyl ether reaches over 98%; the recovery rate of dimethyl ether in the synthetically reacted crude dimethyl ether solution reaches over 98% (99%). The present invention is suitable for technical processes for preparing dimethyl ether from various raw materials by synthetic gas under the condition of the one-step method of synthetic gas. Raw materials for preparing synthetic gas are unrestricted. The proportion of H2 to CO in the synthetic gas is unrestricted. The present invention is particularly suitable for gas containing CO2, etc. The kinds of synthesis reactors are unrestricted.

Description

The separation method of one-step method from syngas preparing dimethy ether
Technical field:
The present invention relates generally to the separation method of single stage method preparing dimethy ether, relates in particular to the separation method of one-step method from syngas preparing dimethy ether.
Background technology:
Dme is the important green Industrial products that meet current environmental requirement, and its main application is: the intermediate of clean fuel, aerosol, cooling agent, whipping agent, organic synthesis etc.Dme has natural gas, methyl alcohol, ethanol, the incomparable comprehensive advantage of hydrogen as automobile-used and general fuel substitute.Both at home and abroad The experimental results shows, can directly substitute diesel oil after the dme liquefaction and be used as automobile fuel, and its fuel effect is better than methanol fuel, except that having the advantage that methanol fuel has, has also overcome the shortcoming of its cold starting performance and acceleration characteristics difference.Studies show that the cost of scale operation dme can not be higher than diesel oil, cost and pollution all are lower than low pollution alternative fuel such as propane and compressed natural gas.Therefore, dme is extremely tempting as the automobile fuel development prospect.The technology of producing dme just is converted into basic chemical industry from fine chemistry industry.
The conventional separation method of the single stage method preparing dimethy ether (DME) of prior art is seen Fig. 1.Reaction back gas 6 condensation in condenser 1 (40 ℃), phlegma is thick dme solution.Do not coagulate in the gas 16 and contain noncondensable gas H 2, CO, CO 2Reach a small amount of gas of dimethyl ether and enter absorption tower 2, absorb at 2.0MPa and 20-35 ℃ of following water, its underflow product is the ether aqueous solution 8, and absorption tail gas 15 returns gas holder and makes fuel.After mixing, the ether aqueous solution 8 and thick dme solution 7 enters rectifying tower 4.The distillation operation condition is 0.5-0.8MPa, and tower top temperature is 20 ℃, and product is an extractive dimethyl ether 12.Tower still temperature is 150 ℃, and its underflow product is a soft water 13, returns absorption tower 2 and makes absorption agent.
The subject matter that this technology exists is: though this method adopts in the kiloton testing apparatus at home at present, can not steady running, and do not reach design objective, gap is bigger.Though the method for calculation of design will not be owing to will test equilibrium and method and simulate and combine, make simulated data and testing data to agree to have certain problem, but major cause is in the building-up reactions of one-step method from syngas preparing dimethy ether, because the synthesis material difference, behind gas after the building-up reactions and the methanol dehydration there be than big difference the gas ingredients of preparing dimethy ether.The former is except there being H 2, CO, DME, CH 3Outside the OH, also has a large amount of CO 2Exist.CO 2The relatively difficulty of separating with dme (DME) can not make these two kinds of components effectively separate with conventional separation method.
In addition under the condition that condensation or water absorb, some CO all 2Enter in the thick dme solution or the aqueous solution.And at rectifying tower top or cat head side line, with some CO 2Enter in the smart ether.The quality of product can't guarantee for this reason, is difficult to continuous production.
Simultaneously in the absorption tower, water is very low to the solubleness of dme, shows the dme concentration less than 2% in the aqueous solution in the data of 2.0Mpa and 20 ℃.Some dme enters gas holder with tail gas, causes the loss of dme.Therefore, the product purity of dme does not reach 98%, and the rate of recovery of dme does not reach more than 95% in the gas after the building-up reactions.
Summary of the invention:
The separation method that the objective of the invention is to avoid the deficiencies in the prior art part and a kind of one-step method from syngas preparing dimethy ether is provided.On the basis of test equilibrium, set up a new method, the purity of dme is reached more than 98%, the rate of recovery of dme reaches more than 98% in the thick methyl ether solution after the building-up reactions, and can steady running.
Purpose of the present invention can be by realizing by the following technical solutions: a kind of separation method of one-step method from syngas preparing dimethy ether, include reacted gas (6) through condenser (1) condensation, do not coagulate gas (16) and enter bottom, absorption tower (2), absorb with soft water (13), the overhead product tail gas (15) on absorption tower (2) enters gas holder, its principal feature is that the underflow product ether aqueous solution (8) of the thick dme solution of the underflow product of condenser (1) (7) and/or absorption tower (2) enters flash tank (3), and gas after the flash distillation (9) is sent into bottom, absorption tower (2); The pure ethereal solution of flash tank (3) underflow product (10) enters dme rectifying tower (4), and overhead product is extractive dimethyl ether (12); The underflow product is thick methanol solution (11).
The pressure that the ether aqueous solution (8) of the separation method of described one-step method from syngas preparing dimethy ether enters flash tank (3) is 0.1-0.9MPa, and the temperature of flash tank is 40-100 ℃.The temperature that the pure ethereal solution of flash tank (3) underflow product (10) enters dme rectifying tower (4) is 80-150 ℃.
The pressure of described dme rectifying tower (4) is 0.2-2.2MPa.Tower top temperature is 20-90 ℃, and tower still temperature is 150-220 ℃.
The thick methanol solution of underflow product (11) that the separation method of one-step method from syngas preparing dimethy ether of the present invention also includes dme rectifying tower (4) enters methanol distillation column (5), and its underflow product is soft water (13), and tower side line product is refined methanol (14).
The pressure of described methanol distillation column (5) is 0.1-0.8Mpa; Tower still temperature is 80-150 ℃, and tower top temperature is 40-90 ℃.The temperature that the thick methanol solution of underflow product (11) enters methanol distillation column (5) is 80-150 ℃.
The present invention has comprised that also tail gas from absorption tower (15) goes transformation absorption or membrane sepn to extract useful composition CO and H 2After, return the dme synthesis unit and do synthesis material.
The invention has the beneficial effects as follows:
1. the present invention reaches more than 98% the product purity of dme, and the rate of recovery of dme reaches (99%) more than 98% in the thick dme solution after the building-up reactions.
2. be suitable for adopting under the situation of one-step method from syngas, various raw materials are through the technological process of synthetic gas preparing dimethy ether, and the raw material of producing synthetic gas is unrestricted.
3. the H in the synthetic gas 2Unrestricted with the ratio of CO, be particularly suitable for containing in the gas CO 2Deng gas.The kind of synthesis reactor is unrestricted.
Description of drawings:
Fig. 1 is the conventional separation method of the single stage method preparing dimethy ether of prior art;
The separation method of Fig. 2 one-step method from syngas preparing dimethy ether of the present invention.
Embodiment:
The invention will be further described below by embodiment, but the present invention is not limited to embodiment.
Embodiment: accompanying drawing 2 is a kind of for the separation method of one-step method from syngas preparing dimethy ether of the present invention.Reacted gas 6 is 200-300 ℃ in temperature, and pressure is 1.5-6.0Mpa, and through condenser 1 condensation (40 ℃), most of dme steam is in this condensation, and methanol vapor also is condensed.Contain noncondensable gas H 2, CO, CO 2, small amounts of inert gas CH 4, N 2What reach uncooled gas of dimethyl ether does not coagulate gas 16 through being decompressed to 0.6-4.8MPa, enter 2 bottoms, absorption tower, at 2.0MPa, 20-35 ℃ absorbs with soft water 13 down, the underflow product ether aqueous solution 8 on thick dme solution 7 of the underflow product of condenser 1 and absorption tower 2 enters flash tank 3, and the temperature of flash tank is 40-100 ℃.Gas 9 is sent into 2 bottoms, absorption tower after the flash distillation; The pure ethereal solution 10 of flash tank 3 underflow products enters dme rectifying tower 4, and overhead product is an extractive dimethyl ether 12; The underflow product is thick methanol solution 11.The pressure that the ether aqueous solution 8 enters flash tank 3 is 0.1-0.9MPa.The temperature that the pure ethereal solution 10 of flash tank 3 underflow products enters dme rectifying tower 4 is 80-150 ℃.The pressure of dme rectifying tower 4 is 0.2-2.2MPa.Tower top temperature is 20-90 ℃, and tower still temperature is 150-220 ℃.The thick methanol solution 11 of the underflow product of dme rectifying tower 4 enters methanol distillation column 5, and its underflow product is a soft water 13, and tower side line product is a refined methanol 14.The higher alcohols side line extraction on the rectifier bottoms column plate of concentrating.The pressure of methanol distillation column 5 is 0.1-0.8Mpa; Tower still temperature is 80-150 ℃, and tower top temperature is 40-90 ℃.The temperature that the thick methanol solution 11 of underflow product enters methanol distillation column 5 is 80-150 ℃.Tail gas from absorption tower 15 goes transformation absorption or membrane sepn to extract useful composition CO and H 2After, return the dme synthesis unit and do synthesis material.
Embodiment 1: table 1 is the data of each logistics product in raw material 1 sepn process.
Embodiment 2: table 2 is the data of each logistics product in raw material 2 sepn processes.
Logistics 12 is a dme in above-mentioned two tables, reaches 99.16%, 99.39% respectively.
Table 1:
The logistics sequence number 6 7 8 9 10 11 12 13 14 15 16
Component V% H 2 .0591 .0003 0 .0024 0 0 0 0 0 .0851 .0776
N 2 .0527 .0003 0 .0021 0 0 0 0 0 .0758 .0691
CO .1851 .0018 .0001 .0101 0 0 0 0 0 .2664 .2426
CO 2 .1926 .0288 .0021 .2053 .0002 0 .0083 0 0 .2752 .2440
CH 4 .2040 .0031 .0001 .0164 0 0 0 0 0 .2937 .2671
DME .1619 .3671 .0245 .7225 .0289 0 .9916 0 .0073 0 .0976
CH 3OH .0432 .1777 .0002 .0027 .0077 .0080 0 0 .9945 0 .0010
H 2O .1014 .4209 .9730 .0385 .9631 .9920 0 1.0000 .0018 .0038 .0011
Flow Kmol 37.956 9.065 205.506 3.110 211.460 205.297 6.163 200.000 1.643 26.371 28.892
Table 2
Patent number 6 7 8 9 10 11 12 13 14 15 16
Component V% H 2 .1797 .0005 .0001 .0098 0 0 0 0 0 .3204 .2870
N 2 .0059 0 0 .0003 0 0 0 0 0 .0105 .0094
CO .0929 .0003 0 .0058 0 0 0 0 0 .1656 .1483
CO 2 .1101 .0084 .0015 .1566 .0002 0 .0061 0 0 .1946 .1709
CH 4 .1711 .0009 .0001 .0152 0 0 0 0 0 .3051 .2730
DME .1526 .2243 .0243 .7722 .0307 0 .9939 0 .0069 0 .1097
CH 3OH .0217 .0573 .0001 .0015 .0043 .0045 0 0 .9851 0 .0004
H 2O .2660 .7083 .9739 .0386 .9648 .9955 0 1.0000 .0080 .0038 .0013
Flow Kmol 44.247 16.568 205.318 2.556 219.323 212.566 6.764 200.000 .971 24.817 27.679
Comparative Examples
Comparative Examples is the conventional separation method of single stage method preparing dimethy ether shown in Figure 1.Reaction back gas 6 condensation in condenser 1 (40 ℃), phlegma is thick dme solution.Do not coagulate in the gas 16 and contain noncondensable gas H 2, CO, CO 2Reach a small amount of gas of dimethyl ether and enter absorption tower 2, absorb at 2.0MPa and 20-35 ℃ of following water, its underflow product is the ether aqueous solution 8, and absorption tail gas 15 returns gas holder and makes fuel.After mixing, the ether aqueous solution 8 and thick dme solution 7 enters rectifying tower 4.The distillation operation condition is 0.5-0.8MPa, and tower top temperature is 20 ℃, and product is an extractive dimethyl ether 12.Tower still temperature is 150 ℃, and its underflow product is a soft water 13, returns absorption tower 2 and makes absorption agent.The difference of this method and embodiment is not set up flash tank 3 between absorption tower 2 and rectifying tower 4, directly enter rectifying tower 4 after the ether aqueous solution 8 and thick dme solution 7 mix for this reason, rather than enter flash tank 3, and lack the method that gas 9 after the flash distillation is sent into 2 bottoms, absorption tower.And the flash tank 3 underflow products among the embodiment are pure ethereal solution 10, through flash tank 3, and the CO of pure ethereal solution 10 2Reduce Deng gas, entering dme rectifying tower 4, the dme product purity reaches more than 98%.The rate of recovery of dme reaches (99%) more than 98% in the thick dme solution after the building-up reactions.
Table 3 is the data of each logistics product in raw material 3 sepn processes.
Logistics 12 is a dme in the above-mentioned table, only can reach 90.26%,
Table 4 is the effect comparison of embodiment and Comparative Examples.
Table 3
Patent number 6 7 8 12 13 15 16
Component V% H 2 .0618 .0004 0 .0005 0 .0920 .0818
N 2 .0537 .0004 0 .0003 0 .0799 .0710
CO .1892 .0018 .0001 .0021 0 .2813 .2501
CO 2 .1751 .0266 .0019 .0905 0 .2362 .2233
CH 4 .2069 .0032 .0001 .0040 0 .3069 .2731
DME .1656 .3717 .0136 .9026 0 0 .0986
CH 3OH .0442 .1770 .0001 0 0 0 .0010
H 2O .1036 .4188 .9841 0 1.0000 .0038 .0011
Flow Kmol 37.083 9.095 203.158 6.623 200.000 24.8304 24.830
Table 4
Embodiment 1 Embodiment 2 Comparative Examples
The concentration % of dme in the product 99.16 99.39 90.26
Dme rate of recovery % in the thick dme solution 99.42 99.57 97.36

Claims (9)

1. the separation method of an one-step method from syngas preparing dimethy ether, include reacted gas (6) through condenser (1) condensation, do not coagulate gas (16) and enter bottom, absorption tower (2), absorb with soft water (13), absorption tower (2) overhead product tail gas (15) enters gas holder, it is characterized in that the thick dme solution of underflow product (7) of condenser (1) and the underflow product ether aqueous solution (8) of absorption tower (2) enter flash tank (3), gas after the flash distillation (9) is sent into bottom, absorption tower (2); The pure ethereal solution of flash tank (3) underflow product (10) enters dme rectifying tower (4), and overhead product is extractive dimethyl ether (12); The underflow product is thick methanol solution (11).
2. the separation method of one-step method from syngas preparing dimethy ether as claimed in claim 1 is characterized in that the pressure that the ether aqueous solution (8) enters flash tank (3) is 0.1-0.9Mpa; The temperature of flash tank is 40-100 ℃.
3. the separation method of one-step method from syngas preparing dimethy ether as claimed in claim 1 is characterized in that the temperature that the pure ethereal solution of flash tank (3) underflow product (10) enters dme rectifying tower (4) is 80-150 ℃.
4. the separation method of one-step method from syngas preparing dimethy ether as claimed in claim 1, the pressure that it is characterized in that dme rectifying tower (4) is 0.2-2.2MPa.
5. the separation method of one-step method from syngas preparing dimethy ether as claimed in claim 1, the tower top temperature that it is characterized in that dme rectifying tower (4) is 20-90 ℃, tower still temperature is 150-220 ℃.
6. as claim 1 or 2 or 3 or the separation method of 4 or 5 described one-step method from syngas preparing dimethy ethers, it is characterized in that the thick methanol solution of underflow product (11) that also includes dme rectifying tower (4) enters methanol distillation column (5), its underflow product is soft water (13), and tower side line product is refined methanol (14).
7. the separation method of one-step method from syngas preparing dimethy ether as claimed in claim 6, the pressure that it is characterized in that methanol distillation column (5) are that 0.1-0.8Mpa tower still temperature is 80-150 ℃, and tower top temperature is 40-90 ℃.
8. the separation method of one-step method from syngas preparing dimethy ether as claimed in claim 7 is characterized in that the temperature that the thick methanol solution of underflow product (11) enters methanol distillation column (5) is 80-150 ℃.
9. the separation method of one-step method from syngas preparing dimethy ether as claimed in claim 8 is characterized in that also including tail gas from absorption tower (15) and goes transformation absorption or membrane sepn to extract useful component CO and H 2After, return the dme synthesis unit and do synthesis material.
CN 03134277 2003-05-21 2003-05-21 Separation method of dimethyl ether prepared with synthetic gas through one-step process Expired - Lifetime CN1226262C (en)

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Publication number Priority date Publication date Assignee Title
CN1331833C (en) * 2005-06-23 2007-08-15 昆山市迪昆精细化工公司 Process for preparing dimethyl ether
ATE514669T1 (en) * 2007-08-23 2011-07-15 Haldor Topsoe As METHOD FOR PRODUCING DIMETHYL ETHER
CN101735025B (en) * 2009-12-02 2013-11-06 中国科学院广州能源研究所 Method and device for separating dimethyl ether from one-step synthesis dimethyl ether gas phase
US8835517B2 (en) * 2012-05-30 2014-09-16 Cool Planet Energy Systems, Inc. Method for producing dimethyl ether using a separator
WO2015104290A1 (en) * 2014-01-07 2015-07-16 Linde Aktiengesellschaft Processing by a separation technique of a gas mixture formed from a product stream of a dimethyl reactor
CN104258588B (en) * 2014-09-03 2016-02-24 中国科学院广州能源研究所 A kind of integrated and method of living beings dimethyl ether rectification and purification device
CN107382680A (en) * 2017-06-12 2017-11-24 中国科学院青岛生物能源与过程研究所 A kind of carbon dioxide eliminating method and its system
CN108707064B (en) * 2018-06-28 2024-01-02 鹤壁宝发能源科技股份有限公司 Production method for co-producing dimethyl ether by using blast furnace gas
CN112441890A (en) * 2020-11-25 2021-03-05 武汉理工大学 Method and system for preparing dimethyl ether by garbage gasification

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