CN1349841A - Pressure swing absorption process of separating relieved gas from methanol synthesis to prepare high-purity hydrogen and CO2 - Google Patents

Pressure swing absorption process of separating relieved gas from methanol synthesis to prepare high-purity hydrogen and CO2 Download PDF

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CN1349841A
CN1349841A CN00116188A CN00116188A CN1349841A CN 1349841 A CN1349841 A CN 1349841A CN 00116188 A CN00116188 A CN 00116188A CN 00116188 A CN00116188 A CN 00116188A CN 1349841 A CN1349841 A CN 1349841A
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gas
pressure
adsorption
hydrogen
methanol
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曾迪琰
薛立震
杜华成
王俊昌
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HUATAI INVESTMENT CO Ltd SICHUAN
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HUATAI INVESTMENT CO Ltd SICHUAN
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Abstract

The method for preparing high-purity hydrogen and CO2 by means of variable pressure adsorption type separation of gas discharged from methyl alcohol synthesis process is characterized by that the described discharged gas at least is passed through 4 adsorption beds, every bed possesses the steps of adsorption, uniform pressure reduction, forward pressure reduction, backward pressure reduction, replacement, vacuum pumping, uniform pressure step-up and final step-up, in which the pressure of adsorption process is 1.8-4.8 MPa, temp. is 30-45 deg.C, and the pressure of vacuum pumping step is -0.05--0.075 MPa.

Description

Separate the method for producing high-purity hydrogen and carbonic acid gas with the transformation suction type by the methanol synthesizing process off-gas
The present invention relates to be a kind of be in the technological process of raw material production methyl alcohol with Sweet natural gas, heavy hydrocarbons compound, coal, acetylene tail gas etc., adopt multi-bed vacuum pressure swing adsorption process that the component of methanol technics off-gas is separated, remove discarded composition and export highly purified hydrogen simultaneously and purity greater than the method for 98.0% carbonic acid gas.According to different methanol feedstock gas preparation technologies, this hydrogen and/or carbonic acid gas can return system for methanol synthesis and be used for tuning to the methyl alcohol synthetic raw gas, also can be used as independent product output.This method both can with the supporting enforcement of newly-built methanol device, also can transform and perfect the methanol device of having built.
With coal, heavy hydrocarbons compound, acetylene tail gas etc. is in the raw material production methanol technics, except that various waste compositions, also contains the hydrogen of different ratios and carbonic acid gas etc. and is the needed material composition of its synthesis technique in the methanol technics off-gas.On the one hand, all as exhaust gas emission, obviously be a kind of wasting of resources with off-gas.On the other hand, the hydrogen-carbon ratio value R for the methyl alcohol synthetic raw gas is formed H/C(H 2-CO 2/ CO+CO 2) adjust to suitable or best scope, in synthetic gas, replenish the hydrogen and/or the carbonic acid gas of requirement again with suitable mode.
Adopt pressure swing adsorption process from hydrogeneous mixed gas separation purifying hydrogen of hydrogen, successfully be widely used in fields such as chemical industry, electronics.United States Patent (USP) 3,564 has been narrated four two equal adiabatic pressure swing adsorption techniques of a kind of employing in 816, is widely used in from the gaseous mixture of impurity such as hydrogeneous, carbonic acid gas, methane, carbon monoxide, for example separation of hydrogen in the petroleum naphtha steam reforming gas.But this technology is subjected to the restriction of maximum bed size, causes adsorption bed throughput to be restricted.If adopt the method head it off that is equipped with two cover systems, but the low and big problem of sorbent material consumption of the hydrogen rate of recovery appears.For this reason, at United States Patent (USP) 3,986, having proposed the adiabatic pressure swing adsorption process that adopts many to select absorption in 849 again, is a kind ofly to extract hydrogen and release ten three equal processing methodes of PSA of all the other compositions from unstripped gas.The main ingredient of its raw materials used gas:
Component ??H 2 ??CO ??CO 2 ?CH 4
??V% 69.22 ?3.57 ?20.92 ?6.29
Above-mentioned raw materials gas is at pressure 2.5Mpa, enters the pressure swing adsorption system of its ten three equal technologies under 40 ℃ of the temperature.Each adsorption bed experiences absorption A, once all pressure drop E1D, the equal voltage rise E2D of secondary, three equal pressure drop E3D, forward step-down PP, reverse step-down RD, flushing P, three equal voltage rise E3R, the equal voltage rise E2R of secondary, once all voltage rise E1R, final 11 steps of FR of boosting in a loop cycle.When ten bed operatings, be carved with the step that three adsorption beds are in product when any, all the other seven adsorption beds are in the regenerated different step.This technology is optionally adsorbed CH from the rich hydrogen unstripped gas with elevated pressures 4, CO and CO 2Deng impurity, obtain high purity product hydrogen.Improvement through this patent, product recovery rate is increased, and the rate of recovery of hydrogen can be brought up to about 84% by 80%, and output is not subjected to the restriction of adsorption bed size simultaneously, and the cumulative volume of adsorption bed and sorbent material consumption all reduce to some extent than the method in past, can also make transformation absorption realize maximizing.But this patent adopts product hydrogen process of washing to finish to the regeneration of the sorbent material that adsorbed impurity.Therefore this part hydrogen can't reclaim, and the yield of product hydrogen can not further be improved.Simultaneously, only can provide a kind of product of hydrogen, can't provide the carbon dioxide product of higher degree simultaneously again by this patented method.
Given this, the object of the present invention is to provide a kind of method of producing high-purity hydrogen and two kinds of products of carbonic acid gas by the methanol synthesizing process off-gas with the separation of transformation suction type, to realize further improving the rate of recovery of product hydrogen, reduce the sorbent material consumption, both can return system for methanol synthesis easily and be used for tuning, also can be used as independent product output methanol feedstock gas.
The present invention separates the method for producing high-purity hydrogen and carbonic acid gas by the methanol synthesizing process off-gas with the transformation suction type, be to make said off-gas successively through at least 4 adsorption beds, experience absorption successively, all pressure drop, forward step-down, the reverse step-downs in a loop cycle of each adsorption bed, replace, vacuumize, all voltage rise and the step of finally boosting, wherein the control pressure of adsorption step is 1.8~4.8Mpa, temperature is 30 ℃~45 ℃, the pressure that vacuumizes step is-0.05~-0.075Mpa.
In aforesaid method of the present invention, the usage quantity of adsorption bed in the said pressure swing adsorption system can be selected in 4~10 scopes that do not coexist according to tolerance, pressure, but wherein should have four adsorption beds to be in normal working order at least.Can be equipped to secondary to five time equal pressure drop and all voltage rises in pressure swing adsorption system, can be secondary, three times, four times, five times equal pressure drops and all voltage rises for example, constitutes many repeatedly equal compression technologies.Form circulation by many repeatedly equal compression technology steps, make the intermittent process serialization of adsorbent reactivation.Its each adsorption bed experiences following steps successively in a loop cycle:
(1) absorption (A):
Unstripped gas constantly enters adsorption bed under the constant adsorptive pressure, simultaneously output products hydrogen.In adsorption step, the sorbent material in the adsorption bed is passed in time the adsorptive capacity of impurity composition beyond the hydrogen and is progressively increased.Stop incoming stock gas when reaching the adsorptive capacity of regulation, absorption stops.Still be reserved with the sorbent material that a part is not adsorbed impurity this moment in the adsorption bed.
(2) all pressure drop is that pressure equalization is fallen:
Enter the direction of exporting with product hydrogen along unstripped gas and reduce pressure, effluent air is a product hydrogen still, is used for boosting of other adsorption bed.This eluting gas can be respectively applied for different several adsorption beds and boost, thereby can form repeatedly the equal pressure drop stage, for example can be once all pressure drops (E1D), the equal pressure drop of secondary (E2D), three equal pressure drops (E3D), four equal pressure drops (E4D), five equal pressure drops (E5D) etc.In this process, constantly descend with the implantation internal pressure, impurity on the sorbent material is by constantly desorb, and it is adsorbed that the impurity after the desorb continues not adsorbed the sorbent material of impurity again, so impurity does not leave adsorption bed.Along with step-down is carried out, the agent of final bed internal adsorption is all taken by impurity.
(3) forward step-down (PP): along unstripped gas enter, the step-down of product hydrogen outbound course.
(4) reverse step-down (BD): enter the direction of exporting with product hydrogen against unstripped gas and reduce pressure, until barometric point, the impurity of most of absorption is with outside the air-flow discharge adsorption bed in the adsorption bed.Utilize the pressure rating difference can adopt repeatedly step-down to finish according to stripping gas.
(5) displacement: after reverse step-down finished, carbon dioxide content was about 80% in the bed, needed to use the higher degree carbon dioxide replacement, to guarantee to vacuumize acquisition product carbon dioxide purity.
(6) vacuumize (VC): utilize vacuum pump to vacuumize, reduce the dividing potential drop of carbonic acid gas in the bed, make the carbonic acid gas desorb that is adsorbed agent absorption, and make sorbent material obtain regeneration, obtain the higher degree carbonic acid gas simultaneously.
(7) all voltage rise is the pressure equalization liter: the adsorption bed after vacuumizing desorption and regeneration is in the minimal pressure of technological process.Under this pressure condition, utilize product hydrogen that the corresponding adsorption bed that is in equal voltage drop step discharges to enter adsorption bed and make it progressively high pressure from the product end of this adsorption bed.All voltage rise can be finished several times, forms repeatedly all voltage rise steps, can be described as five equal voltage rises (E5R), four equal voltage rises (E4R), three equal voltage rises (E3R), the equal voltage rise of secondary (E2R), once all voltage rises (E1R) etc. respectively.
(8) (FR) finally boosts: because all the voltage rise step can't make adsorbent beds arrive adsorptive pressure, therefore the part of the product hydrogen that need export with the adsorption bed that is in adsorption step is boosted to this adsorption bed from the product output terminal.
In aforesaid method, the sorbent material that uses in the pressure swing adsorption system can be sorbent material form commonly used at present, for example can use the compound adsorbent of forming by zeolite molecular sieve, gac, Kiselgel A and activated alumina commonly used, can obtain comparatively satisfied treatment effect.
Aforesaid method of the present invention is on the basis of existing pressure swing adsorption, employing vacuumizes step, substitute the rinse step in the prior art, not only make the present invention from the off-gas of methanol synthesizing process, extract hydrogen, and cancellation rinse step, help reducing the loss of bed being washed the product hydrogen that causes, can also obtain the higher degree carbonic acid gas simultaneously.The purity of hydrogen can reach 99.0%~99.999% in its products obtained therefrom, and the purity of product carbonic acid gas can reach 98.0%~99.5%.According to the difference of synthesizing methanol raw material route, pressure-swing adsorption process handle before the converter that carbonic acid gas in the products obtained therefrom of back can return system for methanol synthesis or behind the stove to improve the R of synthetic gas H/CValue also can become independent product output for using it for anything else; Equally, the hydrogen in the product both can return system for methanol synthesis to improve the R of synthetic gas H/CValue also can be used as independent product output and uses for other purposes.For example, be in the raw material production methanol technics with coal, heavy hydrocarbons compound, acetylene tail gas, the R of synthetic virgin gas hydrogen-carbon ratio H/C(H 2-CO 2/ CO+CO 2) value is less than 2.05, can adopt aforesaid method that the hydrogen in the off-gas is separated and returns in the synthetic gas, improves hydrogen-carbon ratio in the gas, optimizes synthetic technological condition, the purity of the hydrogen when it returns system for methanol synthesis should be greater than 99.0%; Products C O 2Then can be used as independent product output.When adopting one section of gas water steam to transform system gas synthesizing methanol, aforesaid method is handled carbonic acid gas in the products obtained therefrom and be can be used for returning before the converter or behind the stove, product hydrogen then can be according to the requirement of methyl methanol syngas hydrogen-carbon ratio value, or partly or entirely return, or all outer failing used for downstream user.The stripping gas that separation has been removed behind most of hydrogen and the carbonic acid gas then can be used as the burning gas use.
The present invention's multi-bed vacuum pressure swing absorption process of separation of hydrogen and carbonic acid gas from methanol purge gas is compared with above-mentioned prior art, can have following tangible advantage and significant effect:
One, the present invention replaces the rinse step of prior art and constitutes the multi-bed vacuum pressure swing adsorption technique with vacuumizing step.This improved benefit is to have avoided the product loss that causes because of flushing, has improved the rate of recovery of product hydrogen, has improved the effective adsorption capacity of sorbent material, reduces the consumption of sorbent material.
Two, the present invention adopts and vacuumizes the rinse step that step replaces prior art, separate the outer stripping gas of most of dehydrogenation and carbonic acid gas, obtaining purity respectively is that 99.0%~99.999% hydrogen and purity are two kinds of high purity products of 98.0%~99.5% carbonic acid gas.
Therefore, adopt aforesaid method of the present invention to be matched in the methyl alcohol product installation, can be according to the difference of methanol feedstock gas circuit line, with the off-gas of making fuel gas originally comprehensively, be used efficiently.
Below in conjunction with foregoing of the present invention being described in further detail, but this should be interpreted as that the scope of the above-mentioned theme of the present invention is confined to following example by specific embodiment shown in the drawings.
Fig. 1 is to be that a kind of the present invention of representative separates the method that obtains high-purity hydrogen and carbonic acid gas from methanol purge gas with four Vacuum Pressure Swing Adsorption technical process.
Fig. 2 is to be that a kind of the present invention of representative separates the method that obtains high-purity hydrogen and carbonic acid gas from methanol purge gas with eight Vacuum Pressure Swing Adsorption technical process.
Embodiment 1:
This example is a kind of method of extracting hydrogen and carbonic acid gas with four Vacuum Pressure Swing Adsorption technologies from the methanol purge gas of the synthetic gas synthesizing methanol system of one section conversion preparation of Sweet natural gas steam, the mutual relationship that its four adsorption beds respectively go on foot preface is as shown in table 1, and is composed as follows as the off-gas of unstripped gas:
Form H 2 ?N 2 +CH 4 ?CO ?CO 2 ?CH 3OH
?V% 75.72 ?16.44 ?3.09 ?4.02 ?0.63
Unstripped gas is at pressure 1.8Mpa, and temperature enters native system for 40 ℃, by inlet end from bottom to up by being in each adsorption bed of adsorption step.System operation can require to finish switching to each sequencing valve by the computer control follow procedure.The loop cycle of each adsorption bed by absorption (A), once all pressure drops (E1D), the equal pressure drop of secondary (E2D), forward decompression (PP), displacement (S), vacuumize (V), the equal voltage rise of secondary (E2R), isolate (OO), once all voltage rises (E1R), (FR) 11 steps of finally boosting are formed.The sorbent material that uses in variable-pressure adsorption bed is the compound adsorbent of being made up of zeolite molecular sieve, gac, Kiselgel A and activated alumina commonly used.In operational process, always there is an adsorption bed to be in the adsorption step of incoming stock gas and output hydrogen, its excess-three adsorption bed is in the different step of adsorbent reactivation; The step of finally boosting adopts product gas from the product end adsorption bed finally to be boosted.Component beyond the dehydrogenation in the adsorbents adsorb unstripped gas of filling in the adsorption bed, the pressure of output products hydrogen is 1.70Mpa, temperature≤40 ℃.The stripping gas of vacuum pressure swing adsorption system is from forward step-down, reverse step-down and displacement step, under temperature≤40 ℃, is sent to the fuel gas pipe network.The product carbonic acid gas comes the self-evacuating vacuum step, and pressure is 100~300mm H 2O, purity is greater than 99.0%.The purity of the product hydrogen that present embodiment obtains is greater than 99.9%, and the rate of recovery of hydrogen is greater than 85%; The purity of carbonic acid gas is greater than 99.0%, and the rate of recovery of carbonic acid gas is greater than 50%.
Embodiment 2;
This example is to make the method for separation of hydrogen and carbonic acid gas the methanol purge gas of raw material production methyl alcohol with eight Vacuum Pressure Swing Adsorption technologies from acetylene tail gas, and the mutual relationship that its eight adsorption beds respectively go on foot preface is as shown in table 2, and is composed as follows as the off-gas of unstripped gas:
Component ??H 2 ??CO ??CO 2 ??CH 4+Ar ?CH 3OH
??V% ??63.06 ??11.5 ??7.8 ??17.0 ??0.64
Unstripped gas is at pressure 3.5Mpa, and temperature enters native system for 40 ℃, and from bottom to up by being in each adsorption bed of adsorption step, system's operation can require to finish switching to each sequencing valve by the computer control follow procedure by inlet end.The loop cycle of each adsorption bed by absorption (A), once all pressure drops (E1D), the equal pressure drop of secondary (E2D), three equal pressure drops (E3D), four equal pressure drops (E4D), forward step-down (PP), reverse step-down (BD), displacement (S), vacuumize (V), four equal voltage rises (E4R), isolate (OO), three equal voltage rises (E3R), the equal voltage rise of secondary (E2R), once all voltage rises (E1R), (FR) 15 steps of finally boosting are formed.The sorbent material that uses in the pressure swing adsorption system still is the compound adsorbent of being made up of zeolite molecular sieve, gac, Kiselgel A and activated alumina commonly used.In operational process, always there are two adsorption beds to be in the adsorption step of incoming stock gas and output hydrogen, all the other six adsorption beds are in the different step of adsorbent reactivation; The step of finally boosting adopts product gas from the product end adsorption bed finally to be boosted.Component beyond the dehydrogenation in the adsorbents adsorb unstripped gas of filling in the adsorption bed, the pressure of output products hydrogen is 3.4Mpa, under temperature≤45 ℃.The product carbonic acid gas comes from evacuation step, and pressure is 100~300mm H 2O, purity is greater than 99%.The purity of the hydrogen that present embodiment obtains is greater than 99.9%, and the rate of recovery of hydrogen is greater than 87%; The purity of carbonic acid gas is greater than 99.0%, and the rate of recovery of carbonic acid gas is greater than 70%.Four Vacuum Pressure Swing Adsorption technology steps of table 1 preface
Figure A0011618800081
Eight Vacuum Pressure Swing Adsorption technology steps of table 2 preface
Figure A0011618800082

Claims (5)

1. separate the method for producing high-purity hydrogen and carbonic acid gas with the transformation suction type by the methanol synthesizing process off-gas, it is characterized in that making said off-gas successively through at least 4 adsorption beds, experience absorption successively, all pressure drop, forward step-down, the reverse step-downs in a loop cycle of each adsorption bed, replace, vacuumize, all voltage rise and the step of finally boosting, wherein the pressure of adsorption step is 1.8~4.8Mpa, temperature is 30 ℃~45 ℃, the pressure that vacuumizes step is-0.05~-0.075Mpa.
2. the method for claim 1 is characterized in that the adsorption bed in the said pressure-swing adsorption process is 4~10, but should have four beds to be in normal operating conditions at least.
3. the method for claim 1 is characterized in that the compound adsorbent of sorbent material for being made up of zeolite molecular sieve, gac, Kiselgel A and activated alumina that uses in the pressure-swing adsorption process.
4. as the described method of one of claim 1 to 3, it is characterized in that carbon dioxide gas in the product returns before the converter of Sweet natural gas steam reforming methanol synthetizing technology system or behind the stove, to improve the R of methyl methanol syngas H/CValue.
5. as the described method of one of claim 1 to 3, it is characterized in that the hydrogen in the product returns system for methanol synthesis to improve the R of methyl methanol syngas H/CValue, the purity of returning system for methanol synthesis hydrogen should be greater than 99.0%.
CN00116188A 2000-10-19 2000-10-19 Pressure swing absorption process of separating relieved gas from methanol synthesis to prepare high-purity hydrogen and CO2 Pending CN1349841A (en)

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Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100338360C (en) * 2004-12-23 2007-09-19 上海交通大学 Vacuuming method for container by gas associating exchanging principle
CN102172463A (en) * 2011-02-28 2011-09-07 四川同盛科技有限责任公司 Pressure swing adsorption method comprising pump-out and replacement steps
CN102343196A (en) * 2011-07-08 2012-02-08 杭州普菲科空分设备有限公司 Method and device for one-stage pressure swing adsorption hydrogen extraction and carbon-rich gas recovery
CN102351147A (en) * 2011-07-15 2012-02-15 清华大学 Moderate temperature pressure swing adsorption method for CO2, H2S and H2 mixed gas separation
CN102391898A (en) * 2011-10-08 2012-03-28 广西大学 Method for separating and purifying carbon dioxide in marsh gas by adopting pressure swing adsorption
CN104128073A (en) * 2014-08-09 2014-11-05 湖南三箭自控科技有限公司 Novel saturation adsorption process of pressure swing adsorption decarburization and device thereof
CN105176612A (en) * 2015-07-31 2015-12-23 赛鼎工程有限公司 Technology for preparing low-carbon alcohol and by-products of natural gas and hydrogen from coke oven gas
CN106744686A (en) * 2017-01-19 2017-05-31 上海华西化工科技有限公司 A kind of VPSA for improving hydrogen yield carries hydrogen methods and device
CN108472573A (en) * 2016-01-13 2018-08-31 乔治洛德方法研究和开发液化空气有限公司 Change the H2 PSA of gas feed rate

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100338360C (en) * 2004-12-23 2007-09-19 上海交通大学 Vacuuming method for container by gas associating exchanging principle
CN102172463A (en) * 2011-02-28 2011-09-07 四川同盛科技有限责任公司 Pressure swing adsorption method comprising pump-out and replacement steps
CN102343196A (en) * 2011-07-08 2012-02-08 杭州普菲科空分设备有限公司 Method and device for one-stage pressure swing adsorption hydrogen extraction and carbon-rich gas recovery
CN102351147A (en) * 2011-07-15 2012-02-15 清华大学 Moderate temperature pressure swing adsorption method for CO2, H2S and H2 mixed gas separation
CN102391898A (en) * 2011-10-08 2012-03-28 广西大学 Method for separating and purifying carbon dioxide in marsh gas by adopting pressure swing adsorption
CN104128073A (en) * 2014-08-09 2014-11-05 湖南三箭自控科技有限公司 Novel saturation adsorption process of pressure swing adsorption decarburization and device thereof
CN104128073B (en) * 2014-08-09 2017-02-01 湖南三箭自控科技有限公司 Saturation adsorption process of pressure swing adsorption decarburization and device thereof
CN105176612A (en) * 2015-07-31 2015-12-23 赛鼎工程有限公司 Technology for preparing low-carbon alcohol and by-products of natural gas and hydrogen from coke oven gas
CN108472573A (en) * 2016-01-13 2018-08-31 乔治洛德方法研究和开发液化空气有限公司 Change the H2 PSA of gas feed rate
CN106744686A (en) * 2017-01-19 2017-05-31 上海华西化工科技有限公司 A kind of VPSA for improving hydrogen yield carries hydrogen methods and device

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