CN102516036A - Process method for preparing methyl tert-butyl ether by differential reaction rectification and equipment for same - Google Patents
Process method for preparing methyl tert-butyl ether by differential reaction rectification and equipment for same Download PDFInfo
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- CN102516036A CN102516036A CN2011104158631A CN201110415863A CN102516036A CN 102516036 A CN102516036 A CN 102516036A CN 2011104158631 A CN2011104158631 A CN 2011104158631A CN 201110415863 A CN201110415863 A CN 201110415863A CN 102516036 A CN102516036 A CN 102516036A
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Abstract
The invention relates to a process method for preparing methyl tert-butyl ether by differential reaction rectification and equipment for the same, wherein isobutene and methanol are used raw materials for preparing methyl tert-butyl ether. The process method comprises the following steps of: feeding isobutene and methanol in a fixed-bed reactor (1) in a certain mixing ratio to perform pre-reaction; feeding the raw materials after the pre-reaction in a catalytic reaction rectification tower (2); primarily separating the methyl tert-butyl ether generated in the pre-reaction from the unreacted raw materials under the action of a tower internal part (6) at a lower rectification section; further concentrating the generated methyl tert-butyl ether under the action of a tower internal part (5) at a stripping section; and finally obtaining a methyl tert-butyl ether qualified product at the bottom of the tower, and feeding the unreacted raw materials primarily separated by the tower internal part (6) at a lower rectification section in a differential catalytic reaction rectification tower plate (7) to continue to react.
Description
Technical field
The present invention relates to a kind of process method and equipment thereof for preparing MTBE, particularly a kind of differential reactive distillation prepares the process method and the equipment thereof of MTBE.
Background technology
MTBE (MTBE) is a kind of high-octane rating (RON 115) gasoline dope, and chemical oxygen level is much lower than methyl alcohol, is beneficial to warming up and fuel economy, and vaporization heat is low, and is favourable to cold start-up, is usually used in the blending of white gasoline and low lead oil.MTBE also can be cracked into iso-butylene again, as the raw material of rubber and other Chemicals.Top-quality MTBE can be a medicine intermediate as medicine.
In the prior art, MTBE is to be raw material with methyl alcohol and iso-butylene, and is synthetic by an acidic catalyst, and wherein catalyzer is with the most use in industry is resin catalyst.The catalyzer of synthesize methyl tert-butyl ether has hydrofluoric acid, sulfuric acid, styrene type cation exchange resin, solid acid, molecular sieve etc.The reaction of MTBE is a selectivity addition reaction, and the tertiary carbon atom in the alkene forms carbonium ion in the presence of an acidic catalyst, combines to form ether again with alcohol.Its reaction is a reversible exothermic reaction.
MTBE synthetic equipment mainly contains two kinds of fixed-bed reactor and reactive distillation equipment.
Fixed-bed reactor are claimed packed bed reactor again, are filled with solid catalyst or solid reactant in order to realize a kind of reactor drum of heterogeneous reaction process.Solid catalyst is piled into the bed of certain altitude (or thickness).The bed transfixion, fluid reacts through bed.The advantage of fixed-bed reactor is: 1. back-mixing is little, and fluid can effectively contact with catalyzer, can be than highly selective when reacting with the series connection side reaction.2. the catalyzer mechanical loss is little.3. simple in structure.The shortcoming of fixed-bed reactor is: it is poor 1. to conduct heat, when the exothermic heat of reaction amount is very big, even temperature runaway (temperature of reaction is out of hand, sharply rises, and surpasses allowed band) also possibly appear in shell and tube reactor.2. catalyzer can not be changed in the operating process, and catalyzer needs the reaction of frequent regeneration generally should not use, and often replaces fluidized-bed reactor or moving-burden bed reactor.
Reactive distillation is exactly a process of when reacting, isolating product with rectificating method.In the Chemical Manufacture, react and separate two kinds of operations and in two types of independent equipment, carry out respectively usually.Reactive distillation equipment, product or intermediate product that reaction is generated in time separate, and improve the yield of product, and reaction heat simultaneously capable of using again supplies product separation, reaches purpose of energy saving.Its advantage is: 1. destroyed the reversible reaction balance, increased the selectivity and the transformation efficiency of reaction, speed of response has been improved, thereby improved throughput.2. rectifying can utilize reaction heat, has saved energy.3. the synthetic equipment of reactor drum and rectifying tower is reduced investment outlay.4. to some difficult isolating system, can obtain purer product.
Chinese patent CN1170609C discloses a kind of reaction distillation equipment, and it has overcome, and big shortcoming falls in catalyzed reaction distillation tower pressure in the prior art, has increased operational stability, and need not catalyzer be carried out complicated packing, is convenient to loading and unloading.The catalyst loading of this catalytic distillation tower is on the plate of conversion zone; Be provided with air-lift tube on the tower tray; Loading catalyst in the freeboard between the air-lift tube; Liquid phase reacting material passes beds, and under catalyst action, reacts, and reacted liquid phase material carries out heat, matter transmission at steam lifting tube top and vapor-phase material.But because the loadings of catalyzer is bigger; So the riser aspect ratio is higher; Bed resistance is bigger; And the mass transfer original paper of gas speed and riser in riser top depends on height and the density of liquid and the viscosity of riser, so the tower pressure drop is still very high, cause easily that liquid can not in time get into problems such as catalyzed reaction inefficiency such as catalyzer on liquid flooding or the column plate of column plate.
Summary of the invention
The object of the present invention is to provide a kind of differential reactive distillation to prepare the process method and the equipment thereof of MTBE, prepare the catalyzed reaction efficient in the process to improve MTBE.
The invention provides the process method that a kind of differential reactive distillation prepares MTBE; Adopt iso-butylene and methyl alcohol as the feedstock production MTBE; Iso-butylene and methyl alcohol at first get into fixed-bed reactor with certain blending ratio and carry out pre-reaction; Get into catalytic rectifying tower through the raw material after the pre-reaction, under the effect of rectifying hypomere column internals, MTBE that in pre-reaction, generates and unreacted raw material obtain initial gross separation; The MTBE that generates is further carried dense under the effect of stripping section column internals, at the bottom of tower, obtains the MTBE specification product at last; Get into differential catalytic rectifying tower plate through the unreacted raw material after the initial gross separation of rectifying hypomere column internals and proceed reaction; On the last layer column plate of differential catalytic rectifying tower plate, replenish methanol feeding; Unreacted raw material got into rectifying epimere column internals and removes the MTBE component of carrying secretly after reaction finished, and obtained unreacted raw material at cat head at last; Catalyzed reaction and mass transfer sepn process on said differential catalytic rectifying tower plate do; The liquid that the last layer column plate flows down is getting into catalytic unit under the effect of mass transfer liquid distribution plate; Get into the inner gas that rises with the lower floor column plate of mass transfer unit at a liquid part that last catalytic unit reacted liquid Vomitory from the column plate through liquid-inlet and carry out the mass transfer sepn process, continuing to get into upward from the liquid of the last injection channel ejection of mass transfer unit, catalytic unit reacts; Another part that last catalytic unit reacted needs the liquid of overflow to pass through following catalytic unit and upflow tube flows to down on the mass transfer liquid distribution plate of one deck column plate.
Further preferred, the working pressure of catalytic rectifying tower is 0.3-2.0MPa; The service temperature of catalytic rectifying tower is 10-180 ℃; The operating reflux ratio of catalytic rectifying tower is 0.5-3.0.
Further preferred, methyl alcohol and iso-butylene mol ratio are 1: 1-1.5: 1.
The present invention also provides a kind of differential reactive distillation to prepare the equipment of MTBE; Comprise fixed-bed reactor, catalytic rectifying tower, reboiler and condensing surface, said catalytic rectifying tower comprises tower body, stripping section column internals, rectifying hypomere column internals, differential catalytic rectifying tower plate and rectifying epimere column internals; Said differential catalytic rectifying tower plate comprises plane differential column plate, mass transfer unit and catalytic unit; Said catalytic unit comprises liquid Vomitory on catalytic unit, the column plate, following catalytic unit and upflow tube, and said mass transfer unit comprises the mass transfer liquid distribution plate, goes up injection channel, cartouche and liquid-inlet.
Further preferred stripping section column internals is filler internals or column plate internals; Rectifying hypomere column internals is filler internals or column plate internals; Rectifying epimere column internals is filler internals or column plate internals.
The advantage of this invention is: pre-reaction has removed the objectionable impurities in the reaction raw materials, avoids the poisoning of catalyst on the differential catalyzed reaction column plate; On the last layer column plate of differential catalytic rectifying tower plate, replenish methanol feeding, can make the isobutene reaction in the raw material complete, improve reaction conversion ratio; Column plate has been realized micronized, and catalytic unit and mass transfer unit are staggered, and has avoided catalyzed reaction and has separated the mass transfer process subregion and carry out, and has improved reaction conversion ratio and separation efficiency; This tower upflow tube has been saved the column plate sectional area in catalytic unit, improved the column plate area utilization, and bigger catalyst loading space can be provided; The mass transfer liquid distribution plate of mass transfer unit has played the effect of quickening mass transfer and cloth liquid, has improved speed of reaction.
Description of drawings
Fig. 1 is the production technique figure that the differential reactive distillation of a preferred embodiment according to the invention prepares MTBE; Fig. 2 is the mass transfer unit and the interior plane of arrangement figure of catalytic unit tower of the equipment of a preferred embodiment according to the invention; Fig. 3 is the mass transfer unit and the interior vertical planning drawing of arranging of catalytic unit tower of the equipment of a preferred embodiment according to the invention.
Wherein, 1 fixed-bed reactor; 2 catalytic rectifying towers; 3 reboilers; 4 tower bodies; 5 stripping section column internalss; 6 rectifying hypomere column internalss; 7 differential catalytic rectifying tower plates; 8 rectifying epimere column internalss; 9 condensing surfaces; Catalytic unit on 10; Liquid Vomitory on 11 column plates; 12 plane differential column plates; 13 times catalytic units; 14 upflow tubes; 15 mass transfer liquid distribution plates; Injection channel on 16; 17 cartouches; 18 liquid-inlets; 19 mass transfer units; 20 catalytic units.
Embodiment
Shown in Fig. 1-3; A kind of differential reactive distillation prepares the process method of MTBE; Adopt iso-butylene and methyl alcohol as the feedstock production MTBE, iso-butylene and methyl alcohol at first get into fixed-bed reactor 1 with certain blending ratio and carry out pre-reaction, get into catalytic rectifying tower 2 through the raw material after the pre-reaction; Under the effect of rectifying hypomere column internals 6; MTBE that in pre-reaction, generates and unreacted raw material obtain initial gross separation, and the MTBE of generation is further carried dense under the effect of stripping section column internals 5, at the bottom of tower, obtain the MTBE specification product at last; Get into differential catalytic rectifying tower plate 7 through the unreacted raw material after 6 initial gross separations of rectifying hypomere column internals and proceed reaction; On the last layer column plate of differential catalytic rectifying tower plate 7, replenish methanol feeding; Unreacted raw material got into rectifying epimere column internals 8 and removes the MTBE component of carrying secretly after reaction finished, and obtained unreacted raw material at cat head at last; It is characterized in that; Catalyzed reaction and mass transfer sepn process on said differential catalytic rectifying tower plate 7 do; The liquid that the last layer column plate flows down is getting into catalytic unit 10 under the effect of mass transfer liquid distribution plate 15; Get into the inner gases that rise with the lower floor column plate of mass transfer units 19 at a liquid part that last catalytic unit 10 reacted liquid Vomitory 11 from the column plate through liquid-inlet 18 and carry out the mass transfer sepn process, continuing to get into upward from the liquid of last injection channel 16 ejections of mass transfer unit 19, catalytic unit 10 reacts; Another part that last catalytic unit 10 reacted needs the liquid of overflow through catalytic unit 13 and upflow tube 14 flow to down on the mass transfer liquid distribution plate 15 of one deck column plate down.
Shown in Fig. 1-3; A kind of differential reactive distillation prepares the equipment of MTBE; Comprise fixed-bed reactor 1, catalytic rectifying tower 2, reboiler 3 and condensing surface 9; It is characterized in that said catalytic rectifying tower 2 comprises tower body 4, stripping section column internals 5, rectifying hypomere column internals 6, differential catalytic rectifying tower plate 7 and rectifying epimere column internals 8; Said differential catalytic rectifying tower plate 7 comprises plane differential column plate 12, mass transfer unit 19 and catalytic unit 20; Said catalytic unit 20 comprises liquid Vomitory 11 on catalytic unit 10, the column plate, following catalytic unit 13 and upflow tube 14, and said mass transfer unit 19 comprises mass transfer liquid distribution plate 15, goes up injection channel 16, cartouche 17 and liquid-inlet 18.Said stripping section column internals 5 is filler internals or column plate internals; Said rectifying hypomere column internals 6 is filler internals or column plate internals; Said rectifying epimere column internals 8 is filler internals or column plate internals.
Embodiment 1: use aforesaid device and process method to prepare MTBE, wherein:
Methyl alcohol and iso-butylene ratio: 1.1: 1;
Fixed bed reaction transformation efficiency: 90%;
Catalytic rectifying tower working pressure: 0.3MPa;
Service temperature: 10～70 ℃;
Catalytic rectifying tower structural shape (from top to bottom): the efficient structured packing of the 3m+efficient structured packing of 30 layers of efficient structured packing+5m of differential catalytic rectifying tower plate+3m;
Cat head iso-butylene content (mole %): 0.1%;
MTBE purity at the bottom of the tower (mole %): 98%;
Isobutene conversion: 99%.
Embodiment 2: use aforesaid device and process method to prepare MTBE, wherein:
Methyl alcohol and iso-butylene ratio: 1.1: 1;
Fixed bed reaction transformation efficiency: 90%;
Catalytic rectifying tower working pressure: 2.0MPa;
Service temperature: 50～180 ℃;
Catalytic rectifying tower structural shape (from top to bottom): 18 layers of valve tray+30 layer differential catalytic rectifying tower plate+18 layers of valve tray+30 layer valve tray;
Cat head iso-butylene content (mole %): 0.1%;
MTBE purity at the bottom of the tower (mole %): 98.5%;
Isobutene conversion: 99.3%.
Embodiment 3: use aforesaid device and process method to prepare MTBE, wherein:
Methyl alcohol and iso-butylene ratio: 1.1: 1;
Fixed bed reaction transformation efficiency: 90%;
Catalytic rectifying tower working pressure: 0.8MPa;
Service temperature: 40～130 ℃;
Catalytic rectifying tower structural shape (from top to bottom): the efficient structured packing of the 3m+efficient structured packing of 30 layers of differential catalytic rectifying tower plate+3m+30 layers of valve tray;
Cat head iso-butylene content (mole %): 0.1%;
MTBE purity at the bottom of the tower (mole %): 98.5%;
Isobutene conversion: 99.5%.
Claims (9)
1. a differential reactive distillation prepares the process method of MTBE; Adopt iso-butylene and methyl alcohol as the feedstock production MTBE; Iso-butylene and methyl alcohol at first get into fixed-bed reactor (1) with certain blending ratio and carry out pre-reaction; Get into catalytic rectifying tower (2) through the raw material after the pre-reaction, under the effect of rectifying hypomere column internals (6), MTBE that in pre-reaction, generates and unreacted raw material obtain initial gross separation; The MTBE that generates is further carried dense under the effect of stripping section column internals (5), at the bottom of tower, obtains the MTBE specification product at last; Get into differential catalytic rectifying tower plate (7) through the unreacted raw material after rectifying hypomere column internals (6) initial gross separation and proceed reaction; On the last layer column plate of differential catalytic rectifying tower plate (7), replenish methanol feeding; Unreacted raw material got into rectifying epimere column internals (8) and removes the MTBE component of carrying secretly after reaction finished, and obtained unreacted raw material at cat head at last; It is characterized in that; Catalyzed reaction and mass transfer sepn process on said differential catalytic rectifying tower plate (7) do; The liquid that the last layer column plate flows down gets into catalytic unit (10) under the effect of mass transfer liquid distribution plate (15); Get into the inner gas that rises with the lower floor column plate of mass transfer unit (19) at a liquid part that last catalytic unit (10) reacted liquid Vomitory (11) from the column plate through liquid-inlet (18) and carry out the mass transfer sepn process, continuing to get into upward from the liquid of last injection channel (16) ejection of mass transfer unit (19), catalytic unit (10) reacts; Another part that last catalytic unit (10) reacted needs the liquid of overflow to pass through following catalytic unit (13) and upflow tube (14) flows to down on the mass transfer liquid distribution plate (15) of one deck column plate.
2. differential reactive distillation according to claim 1 prepares the process method of MTBE, it is characterized in that, the working pressure of catalytic rectifying tower (2) is 0.3-2.0MPa.
3. differential reactive distillation according to claim 1 prepares the process method of MTBE, it is characterized in that, the service temperature of catalytic rectifying tower (2) is 10-180 ℃.
4. differential reactive distillation according to claim 1 prepares the process method of MTBE, it is characterized in that, the operating reflux ratio of catalytic rectifying tower (2) is 0.5-3.0.
5. prepare the process method of MTBE according to the arbitrary described differential reactive distillation of claim 1-4, it is characterized in that methyl alcohol and iso-butylene mol ratio are 1: 1-1.5: 1.
6. a differential reactive distillation prepares the equipment of MTBE; Comprise fixed-bed reactor (1), catalytic rectifying tower (2), reboiler (3) and condensing surface (9); It is characterized in that said catalytic rectifying tower (2) comprises tower body (4), stripping section column internals (5), rectifying hypomere column internals (6), differential catalytic rectifying tower plate (7) and rectifying epimere column internals (8); Said differential catalytic rectifying tower plate (7) comprises plane differential column plate (12), mass transfer unit (19) and catalytic unit (20); Said catalytic unit (20) comprises liquid Vomitory (11) on catalytic unit (10), the column plate, following catalytic unit (13) and upflow tube (14), and said mass transfer unit (19) comprises mass transfer liquid distribution plate (15), goes up injection channel (16), cartouche (17) and liquid-inlet (18).
7. differential reactive distillation according to claim 6 prepares the equipment of MTBE, it is characterized in that, said stripping section column internals (5) is filler internals or column plate internals.
8. differential reactive distillation according to claim 6 prepares the equipment of MTBE, it is characterized in that, said rectifying hypomere column internals (6) is filler internals or column plate internals.
9. differential reactive distillation according to claim 6 prepares the equipment of MTBE, it is characterized in that, said rectifying epimere column internals (8) is filler internals or column plate internals.
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| CN 201110415863 CN102516036B (en) | 2011-12-14 | 2011-12-14 | Process method for preparing methyl tert-butyl ether by differential reaction rectification and equipment for same |
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| CN 201110415863 CN102516036B (en) | 2011-12-14 | 2011-12-14 | Process method for preparing methyl tert-butyl ether by differential reaction rectification and equipment for same |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103253676A (en) * | 2013-05-10 | 2013-08-21 | 河北工业大学 | Preparation method of trichlorosilane |
| CN103739485A (en) * | 2013-10-29 | 2014-04-23 | 河北美邦工程科技有限公司 | Production method of cyclohexyl acetate and used reaction rectifying tower |
| CN103773494A (en) * | 2013-12-24 | 2014-05-07 | 天津市昊永化工科技有限公司 | Production process and equipment of hydrogen circulation differential catalyst distillation and desulfuration |
| CN106565516A (en) * | 2016-11-14 | 2017-04-19 | 成都惠恩精细化工有限责任公司 | Long-chain alkyl formamide, preparation method thereof, and formylation rectification device |
| CN109173310A (en) * | 2018-08-29 | 2019-01-11 | 张家港市科华化工装备制造有限公司 | Dimethoxym ethane rectifying column |
| CN112316856A (en) * | 2020-09-01 | 2021-02-05 | 河北工业大学 | Equipment and method for producing ethylbenzene by catalytic reaction distillation with concentrated ethylene as raw material |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103253676A (en) * | 2013-05-10 | 2013-08-21 | 河北工业大学 | Preparation method of trichlorosilane |
| CN103253676B (en) * | 2013-05-10 | 2015-04-08 | 河北工业大学 | Preparation method of trichlorosilane |
| CN103739485A (en) * | 2013-10-29 | 2014-04-23 | 河北美邦工程科技有限公司 | Production method of cyclohexyl acetate and used reaction rectifying tower |
| CN103739485B (en) * | 2013-10-29 | 2015-07-22 | 河北美邦工程科技有限公司 | Production method of cyclohexyl acetate and used reaction rectifying tower |
| CN103773494A (en) * | 2013-12-24 | 2014-05-07 | 天津市昊永化工科技有限公司 | Production process and equipment of hydrogen circulation differential catalyst distillation and desulfuration |
| CN103773494B (en) * | 2013-12-24 | 2016-01-20 | 天津市昊永化工工程有限公司 | The production technique of hydrogen circulation differential catalytic distillation desulfurization and equipment |
| CN106565516A (en) * | 2016-11-14 | 2017-04-19 | 成都惠恩精细化工有限责任公司 | Long-chain alkyl formamide, preparation method thereof, and formylation rectification device |
| CN106565516B (en) * | 2016-11-14 | 2019-08-13 | 成都惠恩精细化工有限责任公司 | A kind of chain alkyl formamide, preparation method and formylated rectifier unit |
| CN109173310A (en) * | 2018-08-29 | 2019-01-11 | 张家港市科华化工装备制造有限公司 | Dimethoxym ethane rectifying column |
| CN112316856A (en) * | 2020-09-01 | 2021-02-05 | 河北工业大学 | Equipment and method for producing ethylbenzene by catalytic reaction distillation with concentrated ethylene as raw material |
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