CN116492937B - Methyl tertiary butyl ether schizolysis system isobutene device - Google Patents
Methyl tertiary butyl ether schizolysis system isobutene device Download PDFInfo
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- CN116492937B CN116492937B CN202310534036.7A CN202310534036A CN116492937B CN 116492937 B CN116492937 B CN 116492937B CN 202310534036 A CN202310534036 A CN 202310534036A CN 116492937 B CN116492937 B CN 116492937B
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- VQTUBCCKSQIDNK-UHFFFAOYSA-N Isobutene Chemical compound CC(C)=C VQTUBCCKSQIDNK-UHFFFAOYSA-N 0.000 title claims abstract description 110
- BZLVMXJERCGZMT-UHFFFAOYSA-N Methyl tert-butyl ether Chemical compound COC(C)(C)C BZLVMXJERCGZMT-UHFFFAOYSA-N 0.000 title claims abstract description 92
- 238000006243 chemical reaction Methods 0.000 claims abstract description 123
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 76
- 239000002994 raw material Substances 0.000 claims abstract description 68
- 238000005336 cracking Methods 0.000 claims abstract description 40
- 239000007788 liquid Substances 0.000 claims abstract description 23
- 238000010992 reflux Methods 0.000 claims abstract description 21
- 238000001704 evaporation Methods 0.000 claims abstract description 18
- 238000005070 sampling Methods 0.000 claims abstract description 18
- 230000008020 evaporation Effects 0.000 claims abstract description 17
- 238000009833 condensation Methods 0.000 claims abstract description 7
- 230000005494 condensation Effects 0.000 claims abstract description 7
- 239000003054 catalyst Substances 0.000 claims description 31
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 31
- 229910001220 stainless steel Inorganic materials 0.000 claims description 17
- 239000010935 stainless steel Substances 0.000 claims description 17
- 239000010410 layer Substances 0.000 claims description 13
- 238000010025 steaming Methods 0.000 claims description 12
- 238000006555 catalytic reaction Methods 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 10
- 239000011949 solid catalyst Substances 0.000 claims description 9
- 238000000197 pyrolysis Methods 0.000 claims description 4
- 238000011084 recovery Methods 0.000 claims description 4
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 claims description 3
- 229920005830 Polyurethane Foam Polymers 0.000 claims description 3
- 239000003063 flame retardant Substances 0.000 claims description 3
- 239000011229 interlayer Substances 0.000 claims description 3
- 239000011496 polyurethane foam Substances 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 40
- 238000005265 energy consumption Methods 0.000 abstract description 11
- 238000002360 preparation method Methods 0.000 abstract description 3
- 238000007599 discharging Methods 0.000 abstract 1
- 239000007789 gas Substances 0.000 description 46
- 238000000034 method Methods 0.000 description 21
- 239000012071 phase Substances 0.000 description 7
- 238000003556 assay Methods 0.000 description 6
- 238000009835 boiling Methods 0.000 description 6
- 238000012546 transfer Methods 0.000 description 6
- 230000008901 benefit Effects 0.000 description 5
- 238000002156 mixing Methods 0.000 description 5
- 239000000376 reactant Substances 0.000 description 5
- 229910000323 aluminium silicate Inorganic materials 0.000 description 4
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- 238000009434 installation Methods 0.000 description 4
- 239000007791 liquid phase Substances 0.000 description 4
- 230000008016 vaporization Effects 0.000 description 4
- DKGAVHZHDRPRBM-UHFFFAOYSA-N Tert-Butanol Chemical compound CC(C)(C)O DKGAVHZHDRPRBM-UHFFFAOYSA-N 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- RRHGJUQNOFWUDK-UHFFFAOYSA-N Isoprene Chemical compound CC(=C)C=C RRHGJUQNOFWUDK-UHFFFAOYSA-N 0.000 description 2
- 229920002367 Polyisobutene Polymers 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 229920005549 butyl rubber Polymers 0.000 description 2
- 239000013064 chemical raw material Substances 0.000 description 2
- 239000004020 conductor Substances 0.000 description 2
- 208000012839 conversion disease Diseases 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000003254 gasoline additive Substances 0.000 description 2
- NNPPMTNAJDCUHE-UHFFFAOYSA-N isobutane Chemical compound CC(C)C NNPPMTNAJDCUHE-UHFFFAOYSA-N 0.000 description 2
- 230000002441 reversible effect Effects 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 230000002194 synthesizing effect Effects 0.000 description 2
- YBRBMKDOPFTVDT-UHFFFAOYSA-N tert-butylamine Chemical compound CC(C)(C)N YBRBMKDOPFTVDT-UHFFFAOYSA-N 0.000 description 2
- YTZKOQUCBOVLHL-UHFFFAOYSA-N tert-butylbenzene Chemical compound CC(C)(C)C1=CC=CC=C1 YTZKOQUCBOVLHL-UHFFFAOYSA-N 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000009834 vaporization Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 206010019233 Headaches Diseases 0.000 description 1
- 206010061218 Inflammation Diseases 0.000 description 1
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 description 1
- 206010028813 Nausea Diseases 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000000711 cancerogenic effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 231100000315 carcinogenic Toxicity 0.000 description 1
- 238000004523 catalytic cracking Methods 0.000 description 1
- 238000012824 chemical production Methods 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000006356 dehydrogenation reaction Methods 0.000 description 1
- 230000003111 delayed effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 238000010574 gas phase reaction Methods 0.000 description 1
- 231100000869 headache Toxicity 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000007373 indentation Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000004054 inflammatory process Effects 0.000 description 1
- 239000001282 iso-butane Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000003808 methanol extraction Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
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- 238000000746 purification Methods 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
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- 238000007086 side reaction Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000004230 steam cracking Methods 0.000 description 1
- 229920003051 synthetic elastomer Polymers 0.000 description 1
- 239000005061 synthetic rubber Substances 0.000 description 1
- 230000026676 system process Effects 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/02—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds
- B01J8/04—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds the fluid passing successively through two or more beds
- B01J8/0446—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds the fluid passing successively through two or more beds the flow within the beds being predominantly vertical
- B01J8/0449—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds the fluid passing successively through two or more beds the flow within the beds being predominantly vertical in two or more cylindrical beds
- B01J8/0453—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds the fluid passing successively through two or more beds the flow within the beds being predominantly vertical in two or more cylindrical beds the beds being superimposed one above the other
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D5/00—Condensation of vapours; Recovering volatile solvents by condensation
- B01D5/0003—Condensation of vapours; Recovering volatile solvents by condensation by using heat-exchange surfaces for indirect contact between gases or vapours and the cooling medium
- B01D5/0012—Vertical tubes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D5/00—Condensation of vapours; Recovering volatile solvents by condensation
- B01D5/0057—Condensation of vapours; Recovering volatile solvents by condensation in combination with other processes
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention is suitable for the technical field of organic chemistry, and provides a methyl tertiary butyl ether cracking isobutene preparation device, which comprises a reaction tower and a diversion tower, wherein the reaction tower comprises a raw material feeding pipe, a steam feeding port, a gas evaporation port, a raw material reflux port and a plurality of baffle plates, the diversion tower comprises a gaseous interface, a product discharging port, a raw material diversion port, a sampling port, a methanol diversion port, a liquid interface and a condensation structure, the reaction tower is 8-10 m in height and 0.5-0.6 m in inner diameter, the diversion tower is 9-11 m in height and 0.3-0.4 m in inner diameter, and the diversion tower bottom is higher than the reaction tower bottom by 1-2 m. Therefore, the invention can effectively reduce the manufacturing cost of the device and the energy consumption of production on the premise of ensuring the production of high-purity isobutene products.
Description
Technical Field
The invention relates to the technical field of organic chemistry, in particular to a device for preparing isobutene by cracking methyl tertiary butyl ether.
Background
Isobutene is an important basic organic chemical raw material and is one of monomers of synthetic rubber. The method is mainly used for preparing butyl rubber and polyisobutene, and can be also used for synthesizing various organic chemical raw materials and fine chemicals such as methyl methacrylate, isoprene, tert-butylamine and the like. Currently, the world total demand for isobutene has exceeded 2000 ten thousand tons/year. Isobutene is an important chemical raw material, mainly from the four carbon fractions in steam cracking and catalytic cracking products. When the catalyst is used for synthesizing chemical products such as butyl rubber, polyisobutylene, tert-butylbenzene, tert-butylamine and the like, the purity requirement is quite high, and a large number of complicated separation processes or acid extraction, adsorption separation and the like are needed to be realized. In addition, the tert-butyl alcohol dehydration method, the isobutane dehydrogenation method, the MTBE cracking method and other methods are also commonly used, wherein the MTBE cracking method is used for preparing isobutene, and the method has the characteristics of no pollution and corrosion, high product purity, high single pass conversion rate, strong device independence and the like, so that the method is paid attention to, and great progress is made in research.
MTBE is a new petrochemical product that has been widely used for a long time as a gasoline additive. However, there has been a great deal of recent evidence that the use of MTBE is not safe, and that MTBE in the atmosphere and water can cause inflammation of the nose and throat, headache, nausea, and possibly carcinogenic. Thus, the united states has begun to promote ethanol as a gasoline additive instead of MTBE in 2000, and california has decided to completely prohibit the use of MTBE, and the fate of the MTBE industrial plant has attracted considerable attention. The scheme for preparing isobutene by MTBE cracking is a better way for MTBE in terms of the existing economic benefit and long-term development.
The cracking of methyl tert-butyl ether (MTBE) to produce isobutylene is currently the most widely used technical route to produce isobutylene. The method for preparing isobutene by cracking methyl tertiary butyl ether is a reversible reaction and an endothermic reaction, the reaction temperature and pressure have great influence on the conversion rate of reactants, and the contact area of the catalyst directly relates to the conversion rate and the purity of products.
According to the state of the reactant, the cracking process is divided into a gas-phase cracking process and a liquid-phase cracking reaction rectification process. In the current industrial production, the liquid phase method can effectively control the production cost because of low reaction temperature, but the reaction is difficult to push to the cracking direction because of low temperature, the pressure of the liquid phase method is also not well controlled, the contact area between reactants and a catalyst in the liquid phase is small, the factors directly lead the conversion rate of the reactants to stay below 90 percent, the reaction speed is low, the product content often does not reach high standard specification, and the production effect is not ideal; the conversion rate and the product purity of the methyl tertiary butyl ether can be effectively improved by the gas phase method, but a large amount of heat is required to be consumed in the process of vaporizing the methyl tertiary butyl ether, the energy consumption is high, the equipment requirement of the gas phase reaction is high, the compatibility is poor, the project carried out in the chemical production is not invariable, the compatibility is poor, the reconstruction equipment is required when the project is changed, the manufacturing cost of the gas phase equipment is high, and the equipment cost of the gas phase method production is greatly improved by the poor compatibility.
In summary, it is clear that the prior art has inconvenience and defects in practical use, so that improvement is needed.
Disclosure of Invention
Aiming at the defects, the invention aims to provide a device for preparing isobutene by cracking methyl tertiary butyl ether, which can effectively reduce the manufacturing cost of the device and the energy consumption of production on the premise of ensuring the production of high-purity isobutene products.
In order to achieve the aim, the invention provides a device for preparing isobutene by cracking methyl tertiary butyl ether, which comprises a reaction tower and a diversion tower, wherein the reaction tower is 8-10 m in height and 0.5-0.6 m in inner diameter, the diversion tower is 9-11 m in height and 0.3-0.4 m in inner diameter, and the diversion tower bottom is 1-2 m higher than the reaction tower bottom;
the reaction tower sequentially comprises a product steaming area, a catalytic reaction area and a heat exchange area from top to bottom, wherein a raw material feeding hole, a steam feeding hole, a gas steaming hole and a raw material reflux hole are formed in the reaction tower, a plurality of baffle plates are arranged in the reaction tower, the raw material feeding hole and the gas steaming hole are formed in the product steaming area, the steam feeding hole and the raw material reflux hole are formed in the heat exchange area, the baffle plates are arranged in the catalytic reaction area, a raw material feeding pipe is led into the reaction tower from the raw material feeding hole, and the raw material feeding pipe vertically penetrates through the product steaming area and the catalytic reaction area and is spirally arranged in the heat exchange area;
the baffles are round baffles, the baffles are horizontally arranged, the directions of the notches of two adjacent baffles are opposite, a catalyst containing net is arranged between the two adjacent baffles, and a solid catalyst is placed in the catalyst containing net;
the device comprises a diversion tower, a condensation structure, a gas interface, a product discharge port, a raw material diversion port, a sampling port, a methanol diversion port and a liquid interface, wherein the gas interface, the product discharge port, the raw material diversion port, the sampling port, the methanol diversion port and the liquid interface are arranged on the diversion tower;
the gas evaporation outlet is lower than the gas interface, the gas evaporation outlet is connected with the gas interface through a pipeline, the pipeline connecting the gas evaporation outlet and the gas interface is provided with a bottommost end which is bent downwards in the middle, and the bottommost end is provided with an opening which is connected with the liquid interface through a pipeline; the height of the raw material reflux port is lower than that of the raw material split-flow port, and the raw material split-flow port and the raw material reflux port are connected through a pipeline.
According to the isobutene preparation device by methyl tertiary butyl ether pyrolysis, the condensation structure comprises the guide plate and the cold water pipe, the guide plate is vertically downward, the drainage structure is arranged at the bottom end of the guide plate to facilitate flow gathering, the guide plate is welded at the outer side of the cold water pipe, and two ends of the cold water pipe penetrate through the diversion tower to be respectively connected with an external water pipe and a water recovery pipe.
According to the device for preparing isobutene by methyl tertiary butyl ether pyrolysis, the condensing structure comprises a condensing net, and the condensing net is arranged at the top end of the condensing structure and is abutted against the guide plate.
According to the device for preparing isobutene by cracking methyl tertiary butyl ether, a temperature measuring instrument is arranged above a gaseous interface in the splitting tower, and the temperature measuring instrument is connected with a display.
According to the device for preparing isobutene by cracking methyl tertiary butyl ether, the inner wall of the diversion tower is provided with the diversion trench, and the diversion trench extends spirally from one side of the gaseous interface (21) to the opposite side of the gaseous interface (21) from top to bottom.
According to the device for preparing isobutene by cracking methyl tertiary butyl ether, the height of the sampling port is 2-3 cm lower than that of the raw material shunt port.
According to the device for preparing isobutene by cracking methyl tertiary butyl ether, the catalyst containing net is perpendicular to the baffle plate, and the catalyst containing net is parallel to the notch of the baffle plate.
According to the methyl tertiary butyl ether cracking isobutene preparation device provided by the invention, the inner layer of the reaction tower body is a stainless steel tube of DN500 or a stainless steel tube of DN550, and the outer layer of the reaction tower body is a stainless steel tube of DN550 or a stainless steel tube of DN 600.
According to the device for preparing isobutene by cracking methyl tertiary butyl ether, a polyurethane foam material interlayer added with a flame retardant is arranged between the inner layer and the outer layer of the reaction tower body.
According to the device for preparing isobutene by cracking methyl tertiary butyl ether, a check valve is arranged in a pipeline between the raw material shunt opening and the raw material reflux opening, and the check valve is arranged in a direction which can circulate to the raw material reflux opening.
The invention aims to provide a device for preparing isobutene by cracking methyl tert-butyl ether, which increases the contact area of the methyl tert-butyl ether with a heat conductor and a catalyst by using a baffle plate and a catalyst holding net, and improves the heat exchange efficiency and the cracking efficiency; the high-pressure steam is utilized to conduct heat transfer and provide kinetic energy of mixed gas transportation and water separated from methanol, so that the production flow is effectively simplified, and the production energy consumption is reduced; the split-flow tower separates methyl tertiary butyl ether, isobutene and methanol by using one device by using the characteristics of low isobutene boiling point and water solubility of methanol, so that the installation of a subsequent production light component removing device and a subsequent heavy component removing device is avoided while the purity of the product is ensured, and the cost and the energy consumption of the device are reduced. In summary, the beneficial effects of the invention are as follows: can effectively reduce the manufacturing cost of the device and the energy consumption of the production on the premise of ensuring the production of high-purity isobutene products.
Drawings
FIG. 1 is a schematic view of the overall structure of the present invention;
FIG. 2 is a schematic view of a partial cross-sectional structure of the present invention;
FIG. 3 is a schematic cross-sectional view of the internal structure of the present invention;
FIG. 4 is a schematic view of a baffle arrangement of the present invention;
FIG. 5 is a first schematic diagram of a condensing structure;
FIG. 6 is a second schematic diagram of a condensing structure;
FIG. 7 is a graph of the assay gas phase of the product of example 1;
FIG. 8 is a graph of the assay gas phase of the product of example 2;
FIG. 9 is a chart of the assay of the product of example 3;
FIG. 10 is a graph of the assay gas phase of the product of example 4;
in the figure: 1-a reaction tower, 11-a raw material feeding pipe, 12-a steam feeding port, 13-a gas steaming outlet, 14-a raw material reflux port, 15-a baffle plate, 16-a catalyst holding net, 17-a product steaming zone, 18-a catalytic reaction zone and 19-a heat exchange zone; the device comprises a 2-diversion tower, a 21-gaseous interface, a 22-product discharge port, a 23-raw material diversion port, a 24-sampling port, a 25-methanol diversion port, a 26-liquid interface, a 27-temperature measuring instrument, a 28-display, a 29-guide plate, a 210-cold water pipe, a 211-condensing net and a 212-guide groove.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings, in order to make the objects, technical solutions and advantages of the present invention more apparent. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
In a reaction system for preparing isobutene by cracking methyl tertiary butyl ether, the following four reactions occur, and all the following four reactions are reversible reactions:
the reaction (1) is a main reaction, is a process for preparing isobutene by cracking methyl tertiary butyl ether, is an endothermic reaction, the higher the temperature is, the higher the reaction conversion rate is, the reactions (2) and (3) and (4) are side reactions, are further reactions of two products of the reaction (1), are exothermic reactions, the higher the temperature is, the lower the reaction conversion rate is, under the same pressure, the reaction temperature can be increased to effectively promote the reaction (1) to be carried out and prevent the reaction (2) and (3) and (4) from being carried out, when the reaction temperature is higher than 200 ℃, the conversion rate of the reaction (1) is higher than 70%, and the conversion rate of the reaction (2) and (3) and (4) is lower than 1%; the conversion rate is too low below 200 ℃, and the production efficiency is directly affected by the too low conversion rate; although the conversion rate can be improved to a certain extent by heating the material at the temperature exceeding 200 ℃, the benefit brought by the improvement of the conversion rate is not proportional to the heat consumed by the improvement of the temperature, and the significance is not great in terms of actual production, so that the production conditions need to ensure three points:
1. the whole temperature in the reaction system is not required to be above 200 ℃, but the reaction temperature for carrying out the cracking reaction when contacting with the catalyst is ensured to be above 200 ℃, and the reaction is pushed to the cracking direction as much as possible;
2. the contact area with the catalyst is increased as much as possible while the reaction exchanges heat, so that the conversion rate of reactants is improved;
3. the reaction system is removed from the reaction system as soon as possible after the reaction has taken place, preventing the reaction from moving to the left due to the increase in the product content.
Referring to fig. 1 to 3, the invention provides a device for preparing isobutene by cracking methyl tertiary butyl ether, which comprises a reaction tower 1 and a diversion tower 2, wherein the height of the reaction tower 1 is 8-10 m, the inner diameter of the reaction tower is 0.5-0.6 m, the height of the diversion tower 2 is 9-11 m, the inner diameter of the diversion tower is 0.3-0.4 m, and the bottom of the diversion tower 2 is 1-2 m higher than the bottom of the reaction tower 1.
The reaction tower 1 sequentially comprises a product evaporation zone 17, a catalytic reaction zone 18 and a heat exchange zone 19 from top to bottom, wherein a raw material feed inlet, a steam feed inlet 12, a gas evaporation outlet 13 and a raw material reflux outlet 14 are arranged on the reaction tower 1, a plurality of baffle plates 15 are arranged in the reaction tower 1, the raw material feed inlet and the gas evaporation outlet 13 are arranged in the product evaporation zone 17, the steam feed inlet 12 and the raw material reflux outlet 14 are arranged in the heat exchange zone 19, the baffle plates 15 are arranged in the catalytic reaction zone 18, a raw material feed pipe 11 is led into the reaction tower 1 from the raw material feed inlet, and the raw material feed pipe 11 vertically passes through the product evaporation zone 17 and the catalytic reaction zone 18 and is spirally arranged in the heat exchange zone 19;
the baffle plates 15 are round baffle plates, the baffle plates 15 are horizontally arranged, the directions of the notches of two adjacent baffle plates 15 are opposite, a catalyst containing net 16 is arranged between the two adjacent baffle plates 15, and a solid catalyst is placed in the catalyst containing net 16;
the liquid methyl tertiary butyl ether raw material is put into the raw material feeding pipe 11, flows along the raw material feeding pipe 11 to the heat exchange zone 19, the flow speed of the liquid methyl tertiary butyl ether is delayed by the spiral structure at the bottom, the raw material is preheated in the downward flowing process because the internal temperature of the reaction tower 1 is higher than the boiling point temperature of the methyl tertiary butyl ether, and the methyl tertiary butyl ether in the raw material feeding pipe 11 can be prevented from being overheated and evaporating upwards because the raw material at the upper part is continuously added and flows downwards, and the preheated methyl tertiary butyl ether flows into a reaction system in the reaction tower 1 after flowing out of the raw material feeding pipe 11.
The steam feed port 12 is filled with high-pressure steam, the steam transfers heat to methyl tertiary butyl ether in a reaction system, the heat exchange is in the meaning of vaporizing the methyl tertiary butyl ether and promoting the cracking reaction of the methyl tertiary butyl ether, the methyl tertiary butyl ether is in a liquid state and enters a production system, the steam exchanges heat, the pretreatment vaporization part of the methyl tertiary butyl ether is omitted, the steam becomes moisture in the subsequent cooling process, the product methanol can be smoothly extracted, and one step achieves two reaction effects; while the high-pressure steam is introduced to promote the vaporization of methyl tertiary butyl ether, the steam and the vaporized methyl tertiary butyl ether provide enough pressure in a limited space inside the reaction tower 1, mixed gas can be promoted to move upwards in a reaction system inside the reaction tower 1, and a gas evaporation outlet 13 at the top end of the reaction tower 1 is connected with a diversion tower 2, so that the pressure difference exists between the bottom and the top end of the reaction tower 1, the integral pressure inside the reaction tower 1 is higher than the atmospheric pressure, and the mixed gas rapidly passes through a baffle plate 15 and a catalyst containing net 16 through the pressure difference. Because methyl tertiary butyl ether belongs to endothermic reaction, high temperature is favorable to the reaction, and high pressure vapor still can reach more than 200 ℃ after carrying out heat transfer with methyl tertiary butyl ether, and the reaction demand is fully satisfied, and after methyl tertiary butyl ether heat transfer schizolysis, the molecular content in the mixed gas increases, high temperature and high pressure make the mixed gas in the reaction tower 1 diffuse to the gas evaporation mouth 13 at reaction tower 1 top fast, enter into the reposition of redundant personnel tower 2 through the pipeline, the heat consumption of heat transfer in this process, when the mixed gas enters into the reposition of redundant personnel tower 2 through the pipeline, the bulk temperature of mixed gas can drop to about 100 ℃.
The cost problem of the high-pressure steam in production is that the higher the temperature and the pressure are, the larger the cost is, in order to ensure that the mixed gas at the top of the reaction tower 1 still keeps more than 200 ℃ and the pressure of the reaction system is higher than the atmospheric pressure, the condition of the reaction tower 1 and the corresponding high-pressure steam temperature and pressure are in communication, the higher the tower height of the reaction tower 1 is, the higher the temperature requirement on the high-pressure steam is, the larger the volume in the reaction tower 1 is, the higher the pressure requirement on the high-pressure steam is, the higher the production cost is, otherwise, the temperature required by the reaction is difficult to reach, the conversion rate is low, and the production efficiency is low; if the volume and the tower height in the reaction tower 1 are too small, the temperature and the pressure of the high-pressure steam are required to be more approximate to the required overall conditions in the mixed gas at the top of the reaction tower 1, the required temperature is higher than 200 ℃ but not higher than the required pressure, the required pressure is higher than the atmospheric pressure but not higher than the atmospheric pressure, otherwise, the temperature is too high when the high-pressure steam enters the diversion tower 2, the diversion purification is difficult to realize, and the volume and the tower height in the reaction tower 1 are too small, so that the reaction conditions are more difficult to control, and the production efficiency is more seriously affected.
High-pressure steam commonly used in production, the temperature is 250-270 ℃ and the flow rate is 30-40 m 3 The steam is the most common high-pressure steam with lower cost, the conditions of 8-10 m high and 0.5-0.6 m inner diameter of the reaction tower 1 are more consistent with the reaction conditions of the high-pressure steam, the production efficiency is ensured while the cost is saved, and correspondingly, the height of 9-11 m high and 0.3-0.4 m inner diameter of the split-flow tower 2 are higher than the bottom 1-2 m of the reaction tower 2.
In the drawings, the state of the catalyst containing net 16 is only used for reference, in actual production, a plurality of catalyst containing nets 16 with different structures can be placed on each layer to increase the contact area between methyl tertiary butyl ether and the solid catalyst in the catalyst containing net 16, the mixed gas passes through gaps of the solid catalyst and fully contacts with the solid catalyst, and the methyl tertiary butyl ether is subjected to cracking reaction at a high temperature exceeding 200 ℃ to generate isobutene and methanol.
As a preferred mode, the catalyst holding net 16 can be used by placing a stack material and mixing with the solid catalyst, so that the contact area is increased and the material consumption of the solid catalyst can be saved.
The gas state interface 21, the product discharge port 22, the raw material diversion port 23, the sampling port 24, the methanol diversion port 25 and the liquid state interface 26 are arranged on the diversion tower 2, a condensation structure is arranged in the diversion tower 2, the gas state interface 21 is arranged above the liquid state interface 26, the liquid state interface 26 is arranged above the raw material diversion port 23, the methanol diversion port 25 is arranged at the bottom end of the diversion tower 2, and the sampling port 24 is arranged between the methanol diversion port 25 and the raw material diversion port 23; the gas evaporation outlet 13 is lower than the gas interface 21, the gas evaporation outlet 13 is connected with the gas interface 21 through a pipeline, the pipeline connecting the gas evaporation outlet 13 and the gas interface 21 is provided with a bottommost end which is bent downwards in the middle, the bottommost end is provided with an opening, and the opening is connected with the liquid interface 26 through the pipeline; the height of the raw material reflux mouth 14 is lower than that of the raw material split-flow mouth 23, and the raw material split-flow mouth 23 and the raw material reflux mouth 14 are connected through a pipeline.
Referring to fig. 5 and 6, the condensing structure comprises a guide plate 29, a cold water pipe 210 and a condensing net 211, the guide plate 29 is vertically downward, a drainage structure is arranged at the bottom end of the guide plate 29 to facilitate flow gathering, the guide plate 29 is welded at the outer side of the cold water pipe 210, two ends of the cold water pipe 210 penetrate through the splitting tower 2 to be respectively connected with an external water pipe and a water recovery pipe, and the condensing net 211 is arranged at the top end of the condensing structure to be abutted against the guide plate 29.
Circulating cold water flows through the cold water pipe 210, the ambient temperature is reduced to below 50 ℃ by heat conduction of the guide plate 29 and surrounding gas, methanol and water and only a small amount of residual methyl tertiary butyl ether are condensed into liquid at the temperature, the liquid is collected downwards along the guide plate 29 and the inner wall of the diversion tower 2, and low-boiling isobutene passes through the condensation net 211 and is collected along a pipeline connected with the product discharge hole 22; the fact that the temperature in the pipe connecting the gas outlet 13 and the gas port 21 is lower than 100 c results in condensation of a portion of the methanol in the water, which portion of the mixture flows into the splitter column 2 through the pipe between the feed split 23 and the feed return 14.
After the condensed mixed liquid is collected at the bottom of the splitting tower 2, as methanol is soluble in water, methyl tertiary butyl ether is insoluble in water, and the density of methyl tertiary butyl ether is smaller than that of water, the mixed liquid can be layered, when the liquid is enriched to a certain height, the methyl tertiary butyl ether at the upper part flows back into the reaction tower 1 through the raw material splitting port 23 to enter the reaction system again, the position of a splitting line is determined by controlling the liquid height through sampling of the sampling port 24, and after the high methanol content is detected by a sample taken out of the sampling port 24, the mixed liquid of the methanol and the water is collected from the methanol splitting port 25. The connecting pipeline between the raw material diversion port 23 and the raw material reflux port 14 is subjected to cooling treatment, so that the ambient temperature in the pipeline is ensured to be lower than the boiling point temperature of methyl tertiary butyl ether, and the reflux effect of the raw material is prevented from being influenced by the high temperature of water vapor in the reaction tower 1.
The reaction tower 1 is formed by splicing stainless steel pipes, and through practical production verification, the mixed gas can be fed into a diversion tower after the heat exchange reaction of high-pressure steam and methyl tertiary butyl ether can be fully satisfied under the conditions that the tower height is 8-10 m and the inner diameter is 0.5-0.6 m, if the tower height is lower than 8m and the inner diameter is lower than 0.5m, the mixed gas is difficult to ensure that the mixed gas can be quickly cooled to below 50 ℃ after entering the diversion tower 2 through the reaction tower, and part of methyl tertiary butyl ether enters a product collecting tank together with isobutene, so that the purity of a product is directly reduced; if the tower height is higher than 10m and the inner diameter is higher than 0.6m, the internal space of the reaction tower 1 is overlarge, more high-pressure steam is needed in the whole heat exchange reaction reflux system process, and the energy consumption is increased and the burden is also caused for the subsequent methanol extraction work. And stainless steel pipes of DN500, DN550 and DN600 are common commodity in the pipe market, the purchase cost is low, the stainless steel pipes are firm and durable, and the stainless steel pipes can be restarted by replacement installation only in two hours after partial fault occurs, so that the production efficiency is ensured.
The split-flow tower 2 separates methyl tertiary butyl ether, isobutene and methanol by using one device by utilizing the characteristics of low boiling point of isobutene and water solubility of methanol, so that the installation of a subsequent light component removing device and a heavy component removing device is avoided, and the device cost and the energy consumption are reduced.
The split-flow tower 2 is formed by splicing stainless steel pipes, the material and the advantages of the split-flow tower are the same as those of the reaction tower 1, the size of the tower height of 9-11 m and the inner diameter of 0.3-0.4 m corresponds to the size of the reaction tower 1, and the split-flow efficiency is highest on the premise of saving the cost by condensing split-flow recovery.
As a preferred mode, a temperature measuring instrument 27 is arranged above the gaseous interface 21 in the diversion tower 2, and the temperature measuring instrument 27 is connected with a display 28, so that the ambient temperature at the top of the diversion tower 2 can be conveniently controlled to make partial adjustment.
As a preferred mode, the inner wall of the diversion tower 2 is provided with a diversion trench 212, and the diversion trench is in a shape of spirally extending from one side of the gaseous interface 21 to the opposite side of the gaseous interface 21 from top to bottom.
As a preferred mode, the height of the sampling port 24 is 2-3 cm lower than the height of the raw material split-flow port 23.
As a preferred way, the catalyst holding net 16 is perpendicular to the baffle 15, and the catalyst holding net 16 is parallel to the indentations of the baffle 15.
In a preferred embodiment, the inner layer of the reaction column body is a stainless steel tube of DN500 or a stainless steel tube of DN550, and the outer layer of the reaction column body is a stainless steel tube of DN550 or a stainless steel tube of DN 600.
As a preferable mode, a polyurethane foam material interlayer added with a flame retardant is arranged between the inner layer and the outer layer of the reaction tower main body.
Preferably, a check valve is provided in the pipe between the material split port 23 and the material return port 14, and the check valve is provided so as to be capable of flowing toward the material return port 14.
The device for preparing isobutene by cracking methyl tertiary butyl ether provided by the invention has the advantages of high yield and high product purity, and is low in manufacturing cost, simple in structure and good in maintainability. The methyl tertiary butyl ether cracking process in the factory is continuous production, and the time required for producing 1t of isobutene by using the device is between 6 and 7 hours, and the production is stopped according to the time for changing the solid catalyst. The following description is made by way of several production examples.
In example 1, 32kg of aluminosilicate catalyst was charged and continuously produced for 57 hours, and the total yield of isobutylene was 8.73t, and the product mixing sampling test results were shown in fig. 7, and as seen in fig. 7, the total peak area was 82162.93, the main peak area was 82154.29, the impurity peak area was 8.64, the main peak was the product isobutylene peak, and the average purity of the batch product was 99.9895% as seen in the peak area.
In example 2, 27kg of aluminosilicate catalyst was charged and continuously produced for 53 hours, and 8.42t of isobutylene was produced in total, and the results of the product mixing sampling assay were shown in fig. 8, and as shown in fig. 8, the total peak area was 82209.13, the main peak area was 82200.05, the impurity peak area was 9.08, the main peak was the product isobutylene peak, and the average purity of the batch product was 99.9890% as shown in the peak area.
Example 3, 30kg of aluminosilicate catalyst was charged, the production was continued for 54 hours, the total yield of isobutylene was 8.56t, the result of the product mixing sampling assay was found in fig. 9, and it was found from fig. 9 that the total peak area was 85913.48, the main peak area was 85903.07, the impurity peak area was 10.41, the main peak was the product isobutylene peak, and the average purity of the batch product was 99.9879% from the peak area.
In example 4, 43kg of aluminosilicate catalyst was charged and continuously produced for 62 hours, and the total yield of isobutylene was 9.74t, and the product mixing sampling test results were shown in fig. 10, and as seen in fig. 10, the total peak area was 85597.47, the main peak area was 85589.17, the impurity peak area was 8.29, the main peak was the product isobutylene peak, and the average purity of the batch product was 99.9903% as seen in the peak area.
According to the invention, the contact area of methyl tertiary butyl ether, the heat conductor and the catalyst is increased by utilizing the baffle plate and the catalyst holding net, so that the heat exchange efficiency and the cracking efficiency are improved; the high-pressure steam is utilized to conduct heat transfer and provide kinetic energy of mixed gas transportation and water separated from methanol, so that the production flow is effectively simplified, and the production energy consumption is reduced; the split-flow tower separates methyl tertiary butyl ether, isobutene and methanol by using one device by using the characteristics of low isobutene boiling point and water solubility of methanol, so that the installation of a subsequent production light component removing device and a subsequent heavy component removing device is avoided while the purity of the product is ensured, and the cost and the energy consumption of the device are reduced. In summary, the beneficial effects of the invention are as follows: can effectively reduce the manufacturing cost of the device and the energy consumption of the production on the premise of ensuring the production of high-purity isobutene products.
Of course, the present invention is capable of other various embodiments and its several details are capable of modification and variation in light of the present invention, as will be apparent to those skilled in the art, without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (10)
1. The device for preparing isobutene by cracking methyl tertiary butyl ether comprises a reaction tower (1) and a diversion tower (2), and is characterized in that the height of the reaction tower (1) is 8-10 m, the inner diameter of the reaction tower is 0.5-0.6 m, the height of the diversion tower (2) is 9-11 m, the inner diameter of the diversion tower is 0.3-0.4 m, and the bottom of the diversion tower (2) is 1-2 m higher than the bottom of the reaction tower (1);
the reaction tower (1) sequentially comprises a product steaming area (17), a catalytic reaction area (18) and a heat exchange area (19) from top to bottom, wherein a raw material feeding hole, a steam feeding hole (12), a gas steaming outlet (13) and a raw material reflux opening (14) are formed in the reaction tower (1), a plurality of baffle plates (15) are arranged in the reaction tower (1), the raw material feeding hole and the gas steaming outlet (13) are formed in the product steaming area (17), the steam feeding hole (12) and the raw material reflux opening (14) are formed in the heat exchange area (19), the baffle plates (15) are formed in the catalytic reaction area (18), a raw material feeding pipe (11) is led into the reaction tower (1) from the raw material feeding hole, and the raw material feeding pipe (11) vertically penetrates through the product steaming area (17) and the catalytic reaction area (18) and is spirally arranged in the heat exchange area (19);
the baffle plates (15) are round baffle plates, the baffle plates (15) are horizontally arranged, the directions of the notches of two adjacent baffle plates (15) are opposite, a catalyst containing net (16) is arranged between the two adjacent baffle plates (15), and a solid catalyst is placed in the catalyst containing net (16);
the device is characterized in that a gaseous interface (21), a product discharge hole (22), a raw material splitting hole (23), a sampling hole (24), a methanol splitting hole (25) and a liquid interface (26) are arranged on the splitting tower (2), a condensation structure is arranged in the splitting tower (2), the gaseous interface (21) is arranged above the liquid interface (26), the liquid interface (26) is arranged above the raw material splitting hole (23), the methanol splitting hole (25) is arranged at the bottom end of the splitting tower (2), and the sampling hole (24) is arranged between the methanol splitting hole (25) and the raw material splitting hole (23);
the height of the gas evaporation outlet (13) is lower than that of the gas interface (21), the gas evaporation outlet (13) and the gas interface (21) are connected through a pipeline, the pipeline connecting the gas evaporation outlet (13) and the gas interface (21) is provided with a bottommost end which is bent downwards in the middle, and the bottommost end is provided with an opening which is connected with the liquid interface (26) through the pipeline; the height of the raw material reflux opening (14) is lower than that of the raw material split-flow opening (23), and the raw material split-flow opening (23) and the raw material reflux opening (14) are connected through a pipeline.
2. The device for preparing isobutene by methyl tertiary butyl ether pyrolysis according to claim 1, wherein the condensing structure comprises a guide plate (29) and a cold water pipe (210), the guide plate (29) is vertically downward, the guide plate (29) is welded on the outer side of the cold water pipe (210), and two ends of the cold water pipe (210) penetrate through the splitting tower (2) to be respectively connected with an external water pipe and a water recovery pipe.
3. The device for preparing isobutene by cracking methyl tertiary butyl ether according to claim 2, wherein the condensing structure comprises a condensing net (211), and the condensing net (211) is arranged at the top end of the condensing structure and is abutted against the guide plate (29).
4. The device for preparing isobutene by cracking methyl tertiary butyl ether according to claim 1, wherein a temperature measuring instrument (27) is arranged above the gaseous interface (21) in the splitting tower (2), and the temperature measuring instrument (27) is connected with a display (28).
5. The device for preparing isobutene by methyl tertiary butyl ether pyrolysis according to claim 1, wherein the inner wall of the diversion tower (2) is provided with a diversion trench (212), and the diversion trench (212) is spirally extended from one side of the gaseous interface (21) to the opposite side of the gaseous interface (21) from top to bottom.
6. The device for preparing isobutene by cracking methyl tertiary butyl ether according to claim 1, wherein the height of the sampling port (24) is 2-3 cm lower than the height of the raw material shunt port (23).
7. The apparatus for producing isobutene by cracking methyl tert-butyl ether according to claim 1, wherein the catalyst holding net (16) is perpendicular to the baffle plate (15), and the catalyst holding net (16) is parallel to the notch of the baffle plate (15).
8. The apparatus for preparing isobutene by cracking methyl tert-butyl ether according to claim 1, wherein the inner layer of the reaction tower body is a stainless steel tube of DN500 or a stainless steel tube of DN550, and the outer layer of the reaction tower body is a stainless steel tube of DN550 or a stainless steel tube of DN 600.
9. The apparatus for preparing isobutene by cracking methyl tert-butyl ether according to claim 1, wherein a polyurethane foam material interlayer added with a flame retardant is arranged between the inner layer and the outer layer of the reaction tower body.
10. The device for preparing isobutene by cracking methyl tertiary butyl ether according to claim 1, wherein a check valve is arranged in a pipeline between the raw material shunt port (23) and the raw material reflux port (14), and the check valve is arranged in a direction which can flow to the raw material reflux port (14).
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0302336A1 (en) * | 1987-08-04 | 1989-02-08 | Ec Erdölchemie Gmbh | Process for splitting alkyl-tert.-alkyl ethers |
| EP0860412A1 (en) * | 1997-02-21 | 1998-08-26 | Institut Francais Du Petrole | Process for the preparation of tertiary olefins by decomposition of tertiary alkyl ethers |
| US6049020A (en) * | 1997-04-02 | 2000-04-11 | Institut Francais Du Petrole | Process for producing an ether and an olefin from a hydrocarbon cut containing at least one tertiary olefin by synthesising then decomposing an ether, comprising a first step for purifying the olefin by fractionation |
| CN101134705A (en) * | 2006-08-29 | 2008-03-05 | 奥克森诺奥勒芬化学股份有限公司 | Process for the decomposition of methyl tertiary-butyl ether |
-
2023
- 2023-05-10 CN CN202310534036.7A patent/CN116492937B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0302336A1 (en) * | 1987-08-04 | 1989-02-08 | Ec Erdölchemie Gmbh | Process for splitting alkyl-tert.-alkyl ethers |
| EP0860412A1 (en) * | 1997-02-21 | 1998-08-26 | Institut Francais Du Petrole | Process for the preparation of tertiary olefins by decomposition of tertiary alkyl ethers |
| US6049020A (en) * | 1997-04-02 | 2000-04-11 | Institut Francais Du Petrole | Process for producing an ether and an olefin from a hydrocarbon cut containing at least one tertiary olefin by synthesising then decomposing an ether, comprising a first step for purifying the olefin by fractionation |
| CN101134705A (en) * | 2006-08-29 | 2008-03-05 | 奥克森诺奥勒芬化学股份有限公司 | Process for the decomposition of methyl tertiary-butyl ether |
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