CN103030493B - Method for preparing ethylene and acetylene from ethane - Google Patents
Method for preparing ethylene and acetylene from ethane Download PDFInfo
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- CN103030493B CN103030493B CN201210537307.6A CN201210537307A CN103030493B CN 103030493 B CN103030493 B CN 103030493B CN 201210537307 A CN201210537307 A CN 201210537307A CN 103030493 B CN103030493 B CN 103030493B
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Abstract
The invention relates to a method for preparing ethylene and acetylene from ethane, belonging to the technical field of chemical industry. The method comprises steps as follows: ethane or low-carbon alkane mixture containing rich ethane and oxygen are respectively preheated to 200-700 DEG C, and enter a mixer to be quickly mixed; the mixture is ignited by a burner, and enters a combustion chamber to react, thereby obtaining a 700-1500 DEG C high-temperature product; and the high-temperature product is quenched by a quenching agent at the outlet of the combustion chamber to terminate the further reaction consumption of ethylene and acetylene in time. Compared with the traditional process of preparing ethylene from ethane by vapor pyrolytic cracking, the invention directly utilizes heat generated by oxidation of partial ethane to generate high temperature, so that the ethane is cracked to prepare the ethylene and acetylene. Under different operating conditions, the ethylene selectivity is 30-70%, the acetylene selectivity is 10-30%, and the total selectivity of ethylene and acetylene is 50-85%.
Description
Technical field
The present invention relates to a kind of method utilizing ethane to prepare ethene and acetylene, belong to technical field of chemical material preparation.
Background technology
Ethene and acetylene are important basic organic chemical raw materials, and its Downstream processing product mainly contains polyethylene, oxyethane, ethylene glycol, polyacrylonitrile, polyvinyl chloride, polyvinyl alcohol etc.Ethylene industry is produced and is mainly comprised high-temperature vapor cracking ethane and petroleum naphtha Pintsch process two kinds of techniques, and it is large that the former high-temperature vapor produces difficulty, and energy consumption is large and thermo-efficiency is low, and the latter relies on serious to petroleum resources.Acetylene is produce by calcium carbide route the earliest, and the advantage that the method produces acetylene is that product purity is high, and easy and simple to handle, shortcoming is that consuming electric power is high, and environmental pollution is severe; Gas by partial oxidation of natural method is produced acetylene and is not produced solid waste, goes back by-product synthetic gas.
Ethane non-catalytic partial oxidation technology is not owing to adopting catalyzer, and the route that possesses skills is simple, can the advantage such as long-period stable operation.The advantage of partial oxidation process is: raw material is easy to get, low price, the ethane that oxidizing reaction does not occur in the heat cracking directly utilizing ethane partial oxidation to produce prepares ethene and acetylene, greatly can improve heat utilization ratio, and by-product tail gas can be used for producing synthetic ammonia or methyl alcohol.This process relates to high temperature, short mix, strong turbulence, Millisecond reaction and Quick stop reaction etc., is proposed very high requirement to Optimizing operation and safety control, and wherein, ethane and oxygen short mix and high-temperature product chilling are the keys realizing this process.
The a large amount of high-temperature vapor cracking ethane that adopts in by-product ethane area produces ethene in the Middle East etc., although there is larger cost advantage than petroleum naphtha Pintsch process, but it is large that this process high-temperature vapour produces difficulty, the volume ratio of water vapour and ethane is the highest close to 3, by coil pipe heat transfer cracking ethane, belong to indirect heat exchange, heating efficiency is low, and has higher requirements to reactor material.,
But ethane partial oxidation ethene and acetylene also exist some problems, and such as temperature has a significant impact reactive behavior, due to the restriction of ethane ignition delay time, preheating temperature can not be too high; When preheating temperature is lower, the amount of oxygen needed for reaction increases, and this can cause the ethane ratio of participating in partial oxidation reaction to rise, thus reduces the selectivity that ethane generates ethene and acetylene.Along with the increase in reaction times, the ratio generating methane also can rise.
The existing patented technology for ethane partial oxidation process of producing ethylene at present.Major part patent concentrates on catalyzing part oxidation field.US 3541179 temperature of reaction 600 ~ 1000 ° of C, the reaction generating ethene is carried out quickly, and water vapour indirect heat exchange efficiency is difficult to ensure; Have chlorine element to exist in US 3080435 reaction process, the olefin purification difficulty of generation, and under hot conditions, chlorine is very serious to the corrosion of reactor; US 4524236 and US 4568790 temperature of reaction reduce greatly, are only 200 ° of C, and ethylene selectivity is up to 70 ~ 90%, but ethane per pass conversion is lower than 30%.Non-catalytic partial oxidation technology also has patent open, CN 1269341A temperature of reaction is 700 ~ 900 ° of C, inert gas content 10 ~ 80%, and ethylene selectivity can reach more than 70%, this patented method still needs external heat to provide high temperature to carry out to maintain stable reaction, and energy consumption is higher.
Summary of the invention
The object of this invention is to provide a kind of method utilizing ethane to prepare ethene and acetylene, the route that possesses skills be simple, can the advantage of long-period stable operation.
Technical scheme of the present invention is as follows:
The invention provides the method that the low-carbon alkanes mixture utilizing ethane or be rich in ethane prepares ethene and acetylene, for the production of ethene and acetylene, be achieved through the following technical solutions.
Ethane or be rich in the low-carbon alkanes mixture of ethane and oxygen accurately controls flow by quantifier, the volume ratio of the two is 10 ~ 1, ethane or to be rich in the pressure that the low-carbon alkanes mixture of ethane and oxygen enters mixing tank be 1 ~ 5atm.The heating of ethane or the low-carbon alkanes mixture and oxygen that are rich in ethane by fireplace direct heating to 200 ~ 700 ° C, can enter mixing tank short mix, to be lighted enter combustion chamber and react at mixer outlet by the pilot burner flammule that auxiliary oxygen is formed.
Ethane or enter mixing tank short mix after being rich in the low-carbon alkanes mixture of ethane and oxygen heating, mixture ignition time of lag after preheating shortens, ethane or be rich in the low-carbon alkanes mixture of ethane and oxygen mixture is 10 ~ 500ms by the residence time of mixing tank.For the low-carbon alkanes mixture realizing ethane or be rich in ethane mixes cmpletely with oxygen, the length of mixing tank is 0.5 ~ 10m.For ensureing that the abnormal flow phenomenon such as back-mixing, backflow does not occur mixing process, mixing tank needs the structure being designed to diameter flaring, and mixing tank is 0 ~ 15 ° along the flaring angle α of gas flow direction.Gaseous mixture is 30 ~ 150m/s by the via hole gas speed of burner.
The high-temperature product of combustor exit needs within several milliseconds of times, be chilled to 80 ~ 200 ° of C, the anxious water as refrigerant of ejection needs to keep an angle obliquely with horizontal plane at a high speed, the distance vertically that this structure can shorten chilling high-temperature product, stop required for product deep pyrolytic completely, chilling agent injection direction is for being 0 ~ 45 ° with horizontal plane angle obliquely.Product after chilling enters separation system, is separated and obtains ethene, acetylene and synthetic gas.
The raw material sources of ethane are the rich ethane Sweet natural gas and refinery gas, the coal-seam gas that contain the saturated alkanes such as methane, ethane, propane, butane, and through desulphurization and denitration process, do not need further purification, oxygen purity is technical purity.
Being stainless steel for processing the material of mixing tank, is high temperature material for processing the material of burner and combustion chamber, as quartz, pottery, stainless steel etc.
The problem that difficulty is large, indirect heat exchange thermo-efficiency is low is produced in order to solve water vapour Pintsch process ethane to ethylene indirect heat exchange water vapour, the present invention proposes and prepare ethene and acetylene with method for partical oxidation by ethane or the low-carbon alkanes mixture that is rich in ethane, the heat that the ethane utilizing generating portion to be oxidized generates produces high temperature to be carried out cracking ethane and prepares ethene and acetylene.
The present invention compared with prior art, has following outstanding advantage and effect.
1. ethane or be rich in low-carbon alkanes mixture and oxygen preheat to the 200 ~ 700 ° C of ethane, ethane activity improves, and ethane generates the selectivity of ethene and acetylene up to 50 ~ 85%.
2. the ratio passing through the low-carbon alkanes mixture and oxygen regulating ethane or be rich in ethane can control to generate ethene and acetylene, increases industrial product production controllability.
3. reaction product is except ethene and acetylene, also has a large amount of synthetic gas, can be used for synthetic ammonia or synthesizing methanol industry, improves industrial competitiveness.
4. because this process does not use catalyzer, there is not Catalysts Deactivation Problems, there is the feature of long-term operation.
Accompanying drawing explanation
Fig. 1 is a kind of structural principle schematic diagram utilizing ethane to prepare the method for ethene and acetylene provided by the invention.
Fig. 2 a is cyclone-type mixing tank longitudinal section schematic diagram, Fig. 2 b cyclone-type mixing tank schematic cross section.
Fig. 3 a is distribution type mixing tank longitudinal section schematic diagram, Fig. 3 b distribution type mixing tank schematic cross section.
Fig. 4 is nozzle structure schematic diagram.
Fig. 5 a is the front view (employing open-celled structure) of annular quencher, and Fig. 5 b is the sectional view of Fig. 5 a.
In figure: 1-oxygen intake; 1a-cyclone-type mixing tank oxygen intake; 1b-distribution type mixing tank oxygen intake; 1c-distribution type mixing tank oxygen jet; 2-ethane entrance; 2a-cyclone-type mixing tank first ethane entrance, 2b-cyclone-type mixing tank second ethane entrance, 2c-cyclone-type mixing tank the 3rd ethane entrance, 2d-cyclone-type mixing tank the 4th ethane entrance; 2e-distribution type mixing tank first ethane entrance, 2f-distribution type mixing tank second ethane entrance, 2g-distribution type mixing tank ethane nozzle; 3-mixing tank; 3a-cyclone-type mixing tank; 3b-distribution type mixing tank; 4-burner; 5-oxygen auxiliary tube; 6-combustion chamber; 7-quencher; 8-gaseous product exporter; 9-annular quencher; 10-chilling agent entrance; The perforate of 11-annular quencher medial surface.
Embodiment
Prepare the principle of work of ethene and acetylene, structure of reactor and processing method to the present invention by ethane or the low-carbon alkanes mixture that is rich in ethane below in conjunction with accompanying drawing to be explained in detail.
Fig. 1 is a kind of structural principle schematic diagram utilizing ethane to prepare the method for ethene and acetylene provided by the invention.Normal temperature ethane or be rich in the low-carbon alkanes mixture of ethane and normal temperature oxygen accurately controls flow by gauger, be heated to 200 ~ 700 ° of C with interchanger heat exchange or by process furnace respectively, enter into mixing tank 3 via oxygen intake 1 and ethane entrance 2 and carry out fast fully mixing; Ethane after mixing or be rich in pilot burner flammule that the low-carbon alkanes mixture of ethane and the oxygen auxiliary tube 5 of oxygen at burner 4 place formed and light and enter combustion chamber 6 and react, generates the high-temperature product of temperature 700 ~ 1500 ° of C.In the agent of combustor exit annular quencher 7 high speed ejection chilling, chilling is carried out to high-temperature product according to one embodiment of the present invention and be cooled to 80 ~ 200 ° of C, the deep pyrolytic reaction terminating of ethene, acetylene.According to another embodiment of the invention, first 700 ~ 1500 ° of C high-temperature products are chilled to 500 ~ 600 ° of C, then indirect heat exchange reclaims heat.Gaseous mixture enters ethene, acetylene cryogenic separation device by gaseous product take-up gear 8 connection, obtains product ethene, acetylene and synthetic gas.
Be that the cyclone-type mixing tank oxygen intake 1a that inserted by cyclone-type mixing tank 3a top of oxygen after heating is sprayed from centre shown in Fig. 2, mix with from cyclone-type mixing tank first ethane entrance 2a, cyclone-type mixing tank second ethane entrance 2b, cyclone-type mixing tank the 3rd ethane entrance 2c, ethane that cyclone-type mixing tank the 4th ethane entrance 2d sprays into or the low-carbon alkanes mixture that is rich in ethane.Oxygen is by the uniform aperture radiation ejection of intervalve, and ethane or the low-carbon alkanes mixture being rich in ethane are close to mixing tank wall by four branch roads and are sprayed into, and form eddy flow, mix cmpletely in the mixing tank of diameter flaring.To be oxygen after heating realize mixing by the ethane after gas and heating or the low-carbon alkanes mixture distribution type mixing tank 3b structure that is rich in ethane to Fig. 3, oxygen after heating is connected with uniform distribution type mixing tank oxygen jet 1c by distribution type mixing tank oxygen intake 1b, ethane after heating or be rich in ethane low-carbon alkanes mixture by distribution type mixing tank first ethane entrance 2e, distribution type mixing tank second ethane entrance 2f is connected with uniform distribution type mixing tank ethane nozzle 2g, oxygen jet and ethane or the low-carbon alkanes mixture nozzle being rich in ethane are spaced, the realization that this arrangement mode shortens oxygen and ethane or the low-carbon alkanes mixture that is rich in ethane mixes required diffusion length completely, realize at short notice mixing completely fast.
The intake pressure of ethane or the low-carbon alkanes mixture and oxygen that are rich in ethane is 1 ~ 5atm, preferably 1 ~ 3atm, more preferably 1 ~ 2atm.
Ethane or be rich in the low-carbon alkanes mixture of ethane and oxygen accurately controls flow by quantifier, the volume ratio of ethane or the low-carbon alkanes mixture and oxygen that are rich in ethane is 10 ~ 1.0, preferably 5 ~ 1.5, more preferably 3 ~ 2.
The heating of ethane or the low-carbon alkanes mixture and oxygen that are rich in ethane can, by fireplace direct heating, also can use the high-temperature residual heat after high-temperature product chilling to heat; The preheating temperature of ethane or the low-carbon alkanes mixture and oxygen that are rich in ethane is 200 ~ 700 ° of C, preferably 450 ~ 700 ° of C, and oxygen is 600 ~ 700 ° of C more preferably, ethane or be rich in low-carbon alkanes mixture more preferably 450 ~ 550 ° of C of ethane.
Ethane or enter mixing tank short mix after being rich in the low-carbon alkanes mixture of ethane and oxygen heating, mixture ignition shortening time of lag after preheating, need the low-carbon alkanes mixture and the complete composition mixing of oxygen that realize ethane at short notice or be rich in ethane, its residence time is 10 ~ 500ms, preferably 30 ~ 300ms, more preferably 80 ~ 150ms.
Ethane or be rich in the low-carbon alkanes mixture of ethane and oxygen mixture is 30 ~ 150m/s, preferably 50 ~ 120m/s, more preferably 80 ~ 100m/s by the gas speed of burner.
For realizing ethane or being rich in the low-carbon alkanes mixture of ethane and the quick and complete abundant mixing of oxygen, the length of mixing tank is 0.5 ~ 10m, preferably 1 ~ 8m, more preferably 2 ~ 5m.
For ensureing that the abnormal flow phenomenon such as back-mixing, backflow does not occur mixing process, mixing tank needs the structure being designed to diameter flaring, and mixing tank is 0 ~ 15 ° along the flaring angle α of gas flow direction, preferably 3 ~ 12 °, more preferably 5 ~ 10 °.
The high-temperature product of combustor exit needs within several milliseconds of times, be chilled to 80 ~ 200 ° of C, the chilling agent needs sprayed at a high speed and horizontal plane keep an angle obliquely, the distance vertically that this structure can shorten chilling high-temperature product, stop required for product deep pyrolytic completely, quencher jet orifice is 0 ~ 45 ° with horizontal plane angle obliquely, preferably 10 ~ 30 °, more preferably 15 ~ 20 °.
According to one embodiment of the present invention, the mixture being chilled to 80 ~ 200 ° of C enters product separation device, obtains product ethene, acetylene and synthesis synthetic gas.
According to one embodiment of the present invention, the mixture being chilled to 500 ~ 600 ° of C enters after interchanger indirect heat exchange reclaims heat, enters product separation device, obtains product ethene, acetylene and synthesis synthetic gas.
The definition of product carbon back selectivity and ethane conversion:
S
ithe selectivity of a certain carbonaceous material, C
ithe volumetric molar concentration of this carbonaceous material, n
ithe carbonatoms of this carbonaceous material, ∑ C
i× n
iconcentration and its carbonatoms sum of products of all carbonaceous materials detected,
ethane conversion,
it is ethane volumetric molar concentration.
Below in conjunction with preferred specific examples, describe the method for ethane partial oxidation ethene and acetylene in detail.
Embodiment 1:
Preheating temperature directly affects ethane and oxygen reaction is active, and preheating temperature is higher, and ethane and the residence time required for oxygen reaction will be shorter, and the selectivity of target product ethene and acetylene will be higher, has therefore investigated the impact of preheating temperature on this process.Reaction system pressure is 1atm, and the volume ratio of ethane and oxygen is 3.3:1, and the reaction gas residence time is 10ms, and preheating temperature 200 ~ 600 ° of C, reaction result lists in table 1.
Table 1 various preheat temperature is on the impact of ethane oxidative cracking ethene and acetylene
Embodiment 2:
Ethane or the severe degree being rich in the low-carbon alkanes mixture of ethane and oxygen volume comparison reactive behavior especially reaction process have a significant impact, volume ratio is lower, reaction process Shaoxing opera is strong, and the residence time required for reaction is shorter, is conducive to the total recovery improving target product ethene and acetylene; But volume ratio is too low, temperature of reaction can be too high, has more ethylene synthesis acetylene in the same residence time, even deep pyrolytic becomes carbon black, volume ratio reduces simultaneously, also greatly can increase the selectivity of oxycarbide, therefore investigate the impact of ethane and this process of oxygen volume comparison.Reaction system pressure is 1atm, and ethane and oxygen preheat temperature are 500 ° of C, reaction gas residence time 10ms, and ethane and oxygen volume are 10 ~ 2, and reaction result lists in table 2.
The impact of the different ethane of table 2 and oxygen volume comparison ethane oxidative cracking ethene and acetylene
Embodiment 3:
With the increase of the residence time, the transformation efficiency of ethane can increase, but under hot conditions, target product ethene and acetylene understand deep pyrolytic and methanation, and overall selectivity can decline, and has therefore investigated the impact of the residence time on this process.Reaction system pressure is 1atm, and the volume ratio of ethane and oxygen is 3.3, and preheating temperature 500 ° of C, the residence time 5 ~ 20ms, reaction result lists in table 3.
The table 3 different residence time is on the impact of ethane oxidative cracking ethene and acetylene
Embodiment 4:
Be rich in the methane in the low-carbon alkanes mixture of ethane, propane, butane generate ethene and acetylene to ethane and produce and have Different Effects, identical preheating temperature propane, butane activity are higher than methane, more be conducive to reacting under ethane generates the reaction conditions of ethene, therefore investigated in ethane and contained same ratio methane, propane, butane to the impact of ethylene synthesis.Reaction system pressure is 1atm, the ratio of methane or propane or butane and ethane is 1:9, ethane and methane or propane or butane mixture and oxygen preheat temperature are 500 ° of C, reaction gas residence time 10ms, ethane and methane or propane or butane mixture and oxygen volume are 3.3, and reaction result lists in table 4.
Table 4 methane, propane, butane are on the impact of ethane oxidative cracking ethene and acetylene
Claims (7)
1. utilize ethane to prepare a method for ethene and acetylene, it is characterized in that the method is carried out as follows:
1) by ethane or be rich in the low-carbon alkanes mixture of ethane and oxygen is heated to 200 ~ 700 DEG C respectively, wherein the volume ratio of ethane or the low-carbon alkanes mixture and oxygen that are rich in ethane is 10:2, enter mixing tank in 10 ~ 500ms short mix, light via burner and enter combustion chamber and react, produce 700 ~ 1500 DEG C of high-temperature products;
2) utilize anxious water as refrigerant in combustor exit ejection at a high speed, form trim, high-temperature product is chilled to 80 ~ 200 DEG C;
3) product after chilling enters centrifugal station, obtains ethene, acetylene and synthetic gas.
2. a kind of method utilizing ethane to prepare ethene and acetylene according to claim 1, is characterized in that: be 30 ~ 150m/s by the gas speed of burner after ethane or the low-carbon alkanes mixture being rich in ethane fully mix with oxygen.
3. a kind of method utilizing ethane to prepare ethene and acetylene according to claim 2, is characterized in that: ethane or to be rich in the pressure that the low-carbon alkanes mixture of ethane and oxygen enters mixing tank be 1 ~ 5atm.
4. a kind of method utilizing ethane to prepare ethene and acetylene according to claim 1, it is characterized in that: the hybrid mode of ethane or the low-carbon alkanes mixture and oxygen that are rich in ethane be heat after ethane or the low-carbon alkanes mixture that is rich in ethane from mixing tank surrounding obliquely eddy flow spray into, the oxygen after heating inserts inner pipe by mixing tank top and sprays from centre.
5. a kind of method utilizing ethane to prepare ethene and acetylene according to claim 1, it is characterized in that: the hybrid mode of ethane or the low-carbon alkanes mixture and oxygen that are rich in ethane be heat after ethane and oxygen after heat is connected with spaced gas distributor nozzle by pipeline, spray abundant mixing downwards.
6. a kind of method utilizing ethane to prepare ethene and acetylene according to claim 1, it is characterized in that: described mixing tank length of mixing 0.5 ~ 10m, mixing tank is 0 ~ 15 ° along the flaring angle α of gas flow direction.
7. a kind of method utilizing ethane to prepare ethene and acetylene according to claim 5, is characterized in that: described chilling agent emission direction is for being 0 ~ 45 ° with horizontal plane angle obliquely.
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| CN105272796B (en) * | 2014-06-27 | 2017-09-15 | 中国石油化工集团公司 | A kind of method that use natural gas non-catalytic partial oxidation prepares acetylene |
| CN106854127B (en) * | 2015-12-08 | 2021-03-12 | 清华大学 | Method and device for preparing acetylene and/or synthesis gas from hydrocarbon |
| CN105879806B (en) * | 2016-06-13 | 2018-01-19 | 北京凯瑞英科技有限公司 | Hydrocarbon partial oxidation prepares the large-scale reactor of acetylene and synthesis gas |
| WO2020097751A1 (en) | 2018-11-12 | 2020-05-22 | 清华大学 | Apparatus and method for preparing ethylene and/or acetylene using hydrocarbon |
| CN109821495B (en) * | 2019-03-01 | 2021-02-09 | 清华大学 | Multistage reaction device for preparing ethylene and/or acetylene from hydrocarbon and preparation method |
| CN111747809B (en) * | 2019-03-27 | 2023-03-24 | 中国石油化工股份有限公司 | Olefin preparation process by coupling methane oxidation coupling and ethane cracking |
| CN113231003A (en) * | 2021-05-11 | 2021-08-10 | 清华大学 | Device for preparing ethylene and/or acetylene from hydrocarbon and preparation method |
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| CN1131190C (en) * | 1999-04-07 | 2003-12-17 | 中国科学院大连化学物理研究所 | Ethane oxidizing and cracking process to produce ethylene |
| DE102005018981A1 (en) * | 2005-04-23 | 2006-10-26 | Basf Ag | Preparing acetylene by partial thermal oxidation in a reactor exhibiting a burner with execution holes, comprises mixing an use material for bringing it to the reaction directly before the flame reaction zone in the holes of the burner |
| CN100404485C (en) * | 2005-05-31 | 2008-07-23 | 中国石油化工集团公司 | Method for producing more ethyne through technique of partial oxidation of hydrocarbon |
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