CN102516029A - Method for synthesising methanol by complete cycle of carbon monoxide, carbon dioxide and hydrogen - Google Patents
Method for synthesising methanol by complete cycle of carbon monoxide, carbon dioxide and hydrogen Download PDFInfo
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- CN102516029A CN102516029A CN2011104261948A CN201110426194A CN102516029A CN 102516029 A CN102516029 A CN 102516029A CN 2011104261948 A CN2011104261948 A CN 2011104261948A CN 201110426194 A CN201110426194 A CN 201110426194A CN 102516029 A CN102516029 A CN 102516029A
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Abstract
The invention discloses a method for synthesising methanol by the complete cycle of carbon monoxide, carbon dioxide and hydrogen, comprising the following steps of: adjusting the content of carbon dioxide in raw material gases for synthesising methanol to control the intensity of heat release in a reaction for synthesising methanol, so as to achieve the matching of heat released from the synthesis reaction and the heat transfer of a methanol synthesis tower, wherein the concentration in mole percentage of carbon dioxide in the synthesising gases is 10.0-20.5%; performing gas-liquid separation and boosting on the unreacted carbon monoxide, carbon dioxide and hydrogen after catalytic reaction on the raw material gases consisting of carbon monoxide, carbon dioxide and hydrogen, and then returning all the unreacted gases to the inlet of the synthesis tower; and adjusting the ratio of the carbon monoxide to the carbon dioxide to the hydrogen in a fresh gas, and enabling the synthesising gases entering in the synthesis tower to satisfy a hydrogen-carbon ratio of 2.00-2.80. The method disclosed by the invention realizes the complete cycle of carbon monoxide, carbon dioxide and hydrogen, reduces energy and the losses of non-renewable resources, optimizes the process technology for synthesising methanol, and decreases production cost.
Description
Technical field
The present invention relates to the process method of synthetic gas synthesizing methanol in the chemical field, relate in particular to the synthetic gas methanol synthetizing technology of mesolow (not containing inert nitrogen gas) high carbon dioxide content.
Background technology
Along with rapid economy development and petroleum resources are petered out, substitute energy has become one of center of gravity of China's science and technology and industry development.In the face of the resources supplIes and the national conditions of China's " oil starvation, weak breath, coal resources are abundant relatively ", alcohol-ether fuel has become a kind of substitute energy that has development prospect.
Mesolow synthesizing methanol technology is one of important Technology of coal chemical technology.In recent years, China's mesolow synthesizing methanol industrial development is rapid, and production capacity and demand all increase simultaneously and rapidly.Synthesizing methanol full scale plant scale effect is apparent in view, and methyl alcohol maximizes and produces is the inexorable trend of following domestic methanol industry development.The maximization production of methyl alcohol proposes higher requirement to catalst for synthesis of methanol, and the while also requires further to improve the synthesizing methanol reaction process, to guarantee normally carrying out of methanol industry production.
Existing methyl alcohol maximization production equipment mainly adopts the synthetic gas synthesizing methanol of the carbon monoxide that contains nitrogen, carbonic acid gas, hydrogen.The reaction of co hydrogenation synthesizing methanol is a strong exothermal reaction; Response intensity is big more; Liberated heat is just many more; Thereby the amplitude that causes the catalst for synthesis of methanol bed temperature to raise is big more, causes catalst for synthesis of methanol overheated and sintering takes place to a certain extent, thereby causes catalyzer to lose activity fast.For guaranteeing life of catalyst, add a large amount of nitrogen in the synthetic gas, reduce the intensity of reaction, be moved out of to guarantee reaction heat.
CO+2H
2→CH
3OH +90.64KJ/mol
CO
2+3H
2→CH
3OH+H
2O +48.02KJ/mol
In traditional synthesizing methanol full scale plant because the existence of inert nitrogen gas in the synthetic gas; And the synthetic gas recycle ratio is relatively large; A nitrogen content in the circulation synthetic gas raises along with the increase of cycle index; Therefore, need regularly give off in process of production to speed to exit and satisfy the requirement of building-up reactions hydrogen-carbon ratio with the composition that guarantees the raw material inlet tower gas.In the full scale plant, the synthetic gas that contains nitrogen that gives off system generally arrives more than 10% of circulating flow rate.Not only cause the pollution of environment, and wasted resource.
Summary of the invention
The main purpose of patent of the present invention is to overcome the problem of above existence; The method of a kind of carbon monoxide, carbonic acid gas and hydrogen recycle to extinction synthesizing methanol is provided; To realize the recycle to extinction of virgin gas carbon monoxide, carbonic acid gas, hydrogen; Reduce the loss of energy and Nonrenewable resources, optimize the methanol synthetizing technology technology, and reduce production costs.
In order to reach above purpose, the present invention adopts following technical scheme:
The method of a kind of carbon monoxide, carbonic acid gas and hydrogen recycle to extinction synthesizing methanol; The content that is adjusted in carbonic acid gas in the virgin gas of synthesizing methanol is controlled the intensity of synthesizing methanol exothermic heat of reaction, reaches the coupling of the transfer of heat of building-up reactions liberated heat and methyl alcohol synthetic reactor; Wherein, the mole percent concentration ratio of carbonic acid gas in synthetic gas is 10.0～20.5%;
Virgin gas carbon monoxide, carbonic acid gas and hydrogen all return the inlet of synthetic tower through gas-liquid separation, after boosting through unreacted carbon monoxide, carbonic acid gas and hydrogen after the catalyzed reaction;
It is 2.00～2.80 that the ratio of regulating carbon monoxide, carbonic acid gas and hydrogen in the virgin gas makes the synthetic gas that gets into synthetic tower satisfy hydrogen-carbon ratio.
Preferably, to satisfy hydrogen-carbon ratio be 2.67 to synthetic gas.
Preferably, the mole percent concentration ratio of carbonic acid gas in synthetic gas is 20.0%.
The mole percent concentration ratio of carbon monoxide in synthetic gas is 6.0～18.0%.
Preferably, the mole percent concentration ratio of carbon monoxide in synthetic gas is 10.0%.
The temperature that building-up reactions is suitable for is 200～280 ℃; The pressure that is suitable for is 4.5～8.5MPa; The gas phase air speed is 5000～12000h
-1
Preferably, the suitable temperature of building-up reactions is 250 ℃; The pressure that is suitable for is 8.0MPa; The gas phase air speed is 10000h
- 1
The catalyzer main ingredient that building-up reactions is suitable for is CuO/ZnO/Al
2O
3
Can find out from the chemical reaction of carbon monoxide, synthesizing methanol by hydrogenating carbon dioxide; Carbon dioxide-synthesized methanol exothermic heat of reaction amount is less relatively, and, because the chemical reaction inertia of carbonic acid gas is stronger; Therefore in the synthesizing methanol reaction; Concentration of carbon dioxide changes can regulate the heat that the synthesizing methanol reaction generates, and in addition, the reaction that carbonic acid gas can well shift the carbon monoxide synthesizing methanol generates heat; Reduce the temperature rise amplitude of beds, thus the catalytic activity and the work-ing life that have well kept catalyzer.
Reach the coupling of the transfer of heat of building-up reactions liberated heat and methyl alcohol synthetic reactor, the reaction that can effectively migrate out beds generates heat, reduces beds temperature rise amplitude, thereby well keeps activity of such catalysts and stability; Unreacted carbon monoxide, carbonic acid gas and hydrogen all return the inlet of synthetic tower through gas-liquid separation, after boosting; Because nonnitrogenous gas in the reaction cycle gas; Therefore, reduced the loss of carbon monoxide, carbonic acid gas in the virgin gas that the bleed air exhaust of speeding in traditional methanol synthetizing technology causes;
Synthetic gas satisfies the requirement of hydrogen-carbon ratio, can keep the intensity of synthesizing methanol reaction and methanol output stable.
The beneficial effect of the said technology of the application is:
The method of the invention has realized the recycle to extinction of virgin gas carbon monoxide, carbonic acid gas, hydrogen, has reduced the loss of energy and Nonrenewable resources, has optimized the methanol synthetizing technology technology, and has reduced production cost.
Embodiment
Below in conjunction with embodiment foregoing invention content of the present invention is done further to describe in detail.
But should this be interpreted as that the scope of the above-mentioned theme of the present invention only limits to following embodiment.Not breaking away under the above-mentioned technological thought situation of the present invention, according to ordinary skill knowledge and customary means, make various replacements and change, all should comprise within the scope of the invention.
Embodiment 1
Raw material inlet tower gas body consists of in the synthesizing methanol reaction: CO8.0%, CO
215.13%, H
276.87%, raw material inlet tower gas hydrogen-carbon ratio is 2.67, and temperature of reaction is 250 ℃, and reaction pressure is 8.0MPa, and reaction velocity is 10000h
-1, adopt 200mlCuO/ZnO/Al
2O
3The industry catalst for synthesis of methanol carries out fixed bed catalyst.Exhaust gas consists of after gas-liquid separation: CO, 3.00%; CO
2, 17.92%; H
2, 79.08%, the exhaust gas amount is 1.60Nm
3/ h.Under existing industrial catalst for synthesis of methanol effect, the per pass conversion of carbon monoxide is 70.00%, and the per pass conversion of carbonic acid gas is 5.19%, and it is 676.84kj/h that heat is emitted in reaction.Average temperature rising is 5 ℃ in the reaction process, and unreacted raw material and gaseous products methyl alcohol, water etc. are taken away heat and is about 13.25kj/h, and the ratio that shared reaction generates heat is about 1.96%.The amount of replenishing virgin gas is 0.40Nm
3/ h, the consisting of of virgin gas: CO, 28.08%; CO
2, 3.94%; H
2, 67.98%, the hydrogen-carbon ratio of adjusted inlet tower gas is 2.67.The mixing of reaction exhaust gas and virgin gas is after get into synthetic tower and recycle again after boosting.
Embodiment 2
Raw material inlet tower gas body consists of in the synthesizing methanol reaction: CO, 6.0%; CO
2, 20.5%; H
2, 73.50%.Raw material inlet tower gas hydrogen-carbon ratio is 2.0, and temperature of reaction is 240 ℃, and reaction pressure is 8.5MPa, and reaction velocity is 10000h
-1, adopt 200mlCuO/ZnO/Al
2O
3The industry catalst for synthesis of methanol carries out fixed bed catalyst.Exhaust gas consists of after gas-liquid separation: CO, 2.51%; CO
2, 23.11%; H
2, 74.37%, the exhaust gas amount is 1.67Nm
3/ h.Under existing industrial catalst for synthesis of methanol effect, the per pass conversion of carbon monoxide is 65.00%, and the per pass conversion of carbonic acid gas is 5.8%, and it is 422.38kj/h that heat is emitted in reaction.Average temperature rising is 2 ℃ in the reaction process, and unreacted raw material and gaseous products methyl alcohol, water etc. are taken away heat and is about 8.30kj/h, and the ratio that shared reaction generates heat is about 2.02%.The amount of replenishing virgin gas is 0.33Nm
3/ h, the consisting of of virgin gas: CO, 23.70%; CO
2, 7.22%; H
2, 69.07%, the hydrogen-carbon ratio of adjusted inlet tower gas is 2.0.Reaction exhaust gas and virgin gas mixing get into synthetic tower again and recycle after boosting.
Embodiment 3
Raw material inlet tower gas body consists of in the synthesizing methanol reaction: CO, 10.0%; CO
2, 12.90%; H
2, 77.10%.Raw material inlet tower gas hydrogen-carbon ratio is 2.8, and temperature of reaction is 200 ℃, and reaction pressure is 8.0MPa, and reaction velocity is 5000h
-1, adopt 200mlCuO/ZnO/Al
2O
3The industry catalst for synthesis of methanol carries out fixed bed catalyst.Exhaust gas consists of after gas-liquid separation: CO, 6.06%; CO
2, 14.88%; H
2, 79.06%, the exhaust gas amount is 0.82Nm
3/ h.Under existing industrial catalst for synthesis of methanol effect, the per pass conversion of carbon monoxide is 50.00%, and the per pass conversion of carbonic acid gas is 4.93%, and it is 170.24kj/h that heat is emitted in reaction.Average temperature rising is 2.5 ℃ in the reaction process, and unreacted raw material and gaseous products methyl alcohol, water etc. are taken away heat and is about 3.28kj/h, and the ratio that shared reaction generates heat is about 1.93%.The amount of replenishing virgin gas is 0.18Nm
3/ h, the consisting of of virgin gas: CO, 28.52%; CO
2, 3.61%; H
2, 67.87%, the hydrogen-carbon ratio of adjusted inlet tower gas is 2.8.Reaction exhaust gas and virgin gas mixing get into synthetic tower again and recycle after boosting.
Embodiment 4
Raw material inlet tower gas body consists of in the synthesizing methanol reaction: CO, 18.0%; CO
2, 11.50%; H
2, 70.50%.Raw material inlet tower gas hydrogen-carbon ratio is 2.0, and temperature of reaction is 250 ℃, and reaction pressure is 8.0MPa, and reaction velocity is 12000h
-1, adopt 200mlCuO/ZnO/Al
2O
3The industry catalst for synthesis of methanol carries out fixed bed catalyst.Exhaust gas consists of after gas-liquid separation: CO, 13.45%; CO
2, 14.91%; H
2, 71.64%, the exhaust gas amount is 1.77Nm
3/ h.Under existing industrial catalst for synthesis of methanol effect, the per pass conversion of carbon monoxide is 45.00%, and the per pass conversion of carbonic acid gas is 4.60%, and it is 1174.8kj/h that heat is emitted in reaction.Average temperature rising is 8 ℃ in the reaction process, and unreacted raw material and gaseous products methyl alcohol, water etc. are taken away heat and is about 24.48kj/h, and the ratio that shared reaction generates heat is about 2.08%.The amount of replenishing virgin gas is 0.63Nm
3/ h, the consisting of of virgin gas: CO, 30.66%; CO
2, 2.00%; H
2, 67.33%, the hydrogen-carbon ratio of adjusted inlet tower gas is 2.0.Reaction exhaust gas and virgin gas mixing get into synthetic tower again and recycle after boosting.
Embodiment 5
Raw material inlet tower gas body consists of in the synthesizing methanol reaction: CO, 15.0%; CO
2, 10.00%; H
2, 75.00%.Raw material inlet tower gas hydrogen-carbon ratio is 2.6, and temperature of reaction is 210 ℃, and reaction pressure is 4.5MPa, and reaction velocity is 12000h
-1, adopt 200mlCuO/ZnO/Al
2O
3The industry catalst for synthesis of methanol carries out fixed bed catalyst.Exhaust gas consists of after gas-liquid separation: CO, 11.31%; CO
2, 11.81%; H
2, 76.88%, the exhaust gas amount is 1.91Nm
3/ h.Under existing industrial catalst for synthesis of methanol effect, the per pass conversion of carbon monoxide is 40.00%, and the per pass conversion of carbonic acid gas is 6.00%, and it is 870.22kj/h that heat is emitted in reaction.Average temperature rising is 6.0 ℃ in the reaction process, and unreacted raw material and gaseous products methyl alcohol, water etc. are taken away heat and is about 18.44kj/h, and the ratio that shared reaction generates heat is about 2.12%.The amount of replenishing virgin gas is 0.49Nm
3/ h, the consisting of of virgin gas: CO, 29.41%; CO
2, 2.94%; H
2, 67.65%, the hydrogen-carbon ratio of adjusted inlet tower gas is 2.6.Reaction exhaust gas and virgin gas mixing get into synthetic tower again and recycle after boosting.
Embodiment 6
Raw material inlet tower gas body consists of in the synthesizing methanol reaction: CO, 11.0%; CO
2, 15.00%; H
2, 74.00%.Raw material inlet tower gas hydrogen-carbon ratio is 2.27, and temperature of reaction is 250 ℃, and reaction pressure is 5.5MPa, and reaction velocity is 10000h
-1, adopt 200mlCuO/ZnO/Al
2O
3The industry catalst for synthesis of methanol carries out fixed bed catalyst.Exhaust gas consists of after gas-liquid separation: CO, 7.13%; CO
2, 17.47%; H
2, 75.40%, the exhaust gas amount is 1.60Nm
3/ h.Under existing industrial catalst for synthesis of methanol effect, the per pass conversion of carbon monoxide is 48.00%, and the per pass conversion of carbonic acid gas is 6.50%, and it is 638.16kj/h that heat is emitted in reaction.Average temperature rising is 5 ℃ in the reaction process, and unreacted raw material and gaseous products methyl alcohol, water etc. are taken away heat and is about 13.26kj/h, and the ratio that shared reaction generates heat is about 2.08%.The amount of replenishing virgin gas is 0.39Nm
3/ h, the consisting of of virgin gas: CO, 26.75%; CO
2, 4.94%; H
2, 68.31%, the hydrogen-carbon ratio of adjusted inlet tower gas is 2.27.Reaction exhaust gas and virgin gas mixing get into synthetic tower again and recycle after boosting.
Embodiment 7
Raw material inlet tower gas body consists of in the synthesizing methanol reaction: CO, 8.0%; CO
2, 18.00%; H
2, 74.00%.Raw material inlet tower gas hydrogen-carbon ratio is 2.15, and temperature of reaction is 280 ℃, and reaction pressure is 4.5MPa, and reaction velocity is 5000h
-1, adopt 200mlCuO/ZnO/Al
2O
3The industry catalst for synthesis of methanol carries out fixed bed catalyst.Exhaust gas consists of after gas-liquid separation: CO, 3.99%; CO
2, 20.76%; H
2, 75.25%, the exhaust gas amount is 0.80Nm
3/ h.Under existing industrial catalst for synthesis of methanol effect, the per pass conversion of carbon monoxide is 60.00%, and the per pass conversion of carbonic acid gas is 7.40%, and it is 394.96kj/h that heat is emitted in reaction.Average temperature rising is 6 ℃ in the reaction process, and unreacted raw material and gaseous products methyl alcohol, water etc. are taken away heat and is about 8.10kj/h, and the ratio that shared reaction generates heat is about 2.05%.The amount of replenishing virgin gas is 0.20Nm
3/ h, the consisting of of virgin gas: CO, 24.33%; CO
2, 6.75%; H
2, 68.92%, the hydrogen-carbon ratio of adjusted inlet tower gas is 2.15.Reaction exhaust gas and virgin gas mixing get into synthetic tower again and recycle after boosting.
Comparative Examples
Raw material inlet tower gas body consists of in the synthesizing methanol reaction: CO, 16.23%; CO
2, 6.74%; N
2, 8.35%; H
2, 68.08%.Hydrogen-carbon ratio is 2.67, and temperature of reaction is 250 ℃, and reaction pressure is 8.0MPa, and reaction velocity is 10000h
-1, adopt 200mlCuO/ZnO/Al
2O
3The industry catalst for synthesis of methanol carries out fixed bed catalyst.Exhaust gas consists of after gas-liquid separation: CO, 8.77%; CO
2, 9.50%; N
2, 12.55%; H
2, 69.18%, the exhaust gas amount is 1.33Nm
3/ h.Under existing industrial catalst for synthesis of methanol effect, the per pass conversion of carbon monoxide is 64.06%, and the per pass conversion of carbonic acid gas is 6.19%, and it is 1256.59kj/h that heat is emitted in reaction.Average temperature rising is 10 ℃ in the reaction process, and unreacted raw material and gaseous products methyl alcohol, water etc. are taken away heat and is about 121.82kj/h, and the ratio that shared reaction generates heat is about 1.94%.The amount of replenishing virgin gas is 0.67Nm
3/ h, the consisting of of virgin gas: CO, 31.64%; CO
2, 1.27%; H
2, 67.09%, the hydrogen-carbon ratio of adjusted inlet tower gas is 2.67.Reaction exhaust gas and virgin gas mixing get into synthetic tower again and carry out after boosting.Consisting of after one hour gas-liquid separator separates of synthetic gas circulation: CO, 6.18%; CO
2, 10.79%; N
2, 23.39%; H
2, 59.64%;～2.5% methyl alcohol;～0.5% water.The bleed air exhaust of speeding amount is :～0.2Nm
3/ h wherein loses methyl alcohol 7.24g/h, carbon monoxide 0.01236Nm
3/ h.
Claims (8)
1. the method for a carbon monoxide, carbonic acid gas and hydrogen recycle to extinction synthesizing methanol is characterized in that:
The content that is adjusted in carbonic acid gas in the virgin gas of synthesizing methanol is controlled the intensity of synthesizing methanol exothermic heat of reaction, reaches the coupling of the transfer of heat of building-up reactions liberated heat and methyl alcohol synthetic reactor; Wherein, the mole percent concentration ratio of carbonic acid gas in synthetic gas is 10.0～20.5%;
Virgin gas carbon monoxide, carbonic acid gas and hydrogen all return the inlet of synthetic tower through gas-liquid separation, after boosting through unreacted carbon monoxide, carbonic acid gas and hydrogen after the catalyzed reaction;
It is 2.00～2.80 that the ratio of regulating carbon monoxide, carbonic acid gas and hydrogen in the virgin gas makes the synthetic gas that gets into synthetic tower satisfy hydrogen-carbon ratio.
2. the method for carbon monoxide according to claim 1, carbonic acid gas and hydrogen recycle to extinction synthesizing methanol is characterized in that: it is 2.67 that synthetic gas satisfies hydrogen-carbon ratio.
3. the method for carbon monoxide according to claim 2, carbonic acid gas and hydrogen recycle to extinction synthesizing methanol is characterized in that: the mole percent concentration ratio of carbonic acid gas in synthetic gas is 20.0%.
4. the method for carbon monoxide according to claim 3, carbonic acid gas and hydrogen recycle to extinction synthesizing methanol is characterized in that: the mole percent concentration ratio of carbon monoxide in synthetic gas is 6.0～18.0%.
5. the method for carbon monoxide according to claim 4, carbonic acid gas and hydrogen recycle to extinction synthesizing methanol is characterized in that: the mole percent concentration ratio of carbon monoxide in synthetic gas is 10.0%.
6. the method for carbon monoxide according to claim 5, carbonic acid gas and hydrogen recycle to extinction synthesizing methanol is characterized in that: the temperature that building-up reactions is suitable for is 200～280 ℃; The pressure that is suitable for is 4.5～8.5MPa; The gas phase air speed is 5000～12000h
-1
7. according to the method for any described carbon monoxide of claim 6, carbonic acid gas and hydrogen recycle to extinction synthesizing methanol, it is characterized in that: the temperature that building-up reactions is suitable for is 250 ℃; The pressure that is suitable for is 8.0MPa; The gas phase air speed is 10000h
-1
8. the method for carbon monoxide according to claim 7, carbonic acid gas and hydrogen recycle to extinction synthesizing methanol is characterized in that: the catalyzer main ingredient that building-up reactions is suitable for is CuO/ZnO/Al
2O
3
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|---|---|---|---|---|
| CN104672056A (en) * | 2013-11-30 | 2015-06-03 | 崔胜民 | Automatic carbon supplementing product-increasing and consumption-reducing process of methanol production |
| CN112142558A (en) * | 2020-08-31 | 2020-12-29 | 南京聚拓化工科技有限公司 | Single-power double-circulation methanol production method |
| CN112194566A (en) * | 2020-09-29 | 2021-01-08 | 浙江工业大学 | Device and process for synthesizing methanol based on carbon dioxide hydrogenation |
| CN108779051B (en) * | 2016-02-16 | 2022-01-04 | 加泰罗尼亚化学研究学院（Iciq） | Methanol preparation method |
| CN114907186A (en) * | 2022-04-24 | 2022-08-16 | 中国成达工程有限公司 | Method for directly preparing methanol from carbon dioxide and hydrogen |
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| CN102264679A (en) * | 2008-12-22 | 2011-11-30 | 国际壳牌研究有限公司 | Process to prepare methanol and/or dimethylether |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104672056A (en) * | 2013-11-30 | 2015-06-03 | 崔胜民 | Automatic carbon supplementing product-increasing and consumption-reducing process of methanol production |
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| CN112194566A (en) * | 2020-09-29 | 2021-01-08 | 浙江工业大学 | Device and process for synthesizing methanol based on carbon dioxide hydrogenation |
| CN114907186A (en) * | 2022-04-24 | 2022-08-16 | 中国成达工程有限公司 | Method for directly preparing methanol from carbon dioxide and hydrogen |
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| Publication number | Publication date |
|---|---|
| CN102516029B (en) | 2014-07-23 |
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