CN106316758B - The separation method of preparing propylene by methanol transformation reaction product - Google Patents
The separation method of preparing propylene by methanol transformation reaction product Download PDFInfo
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Abstract
The invention discloses a kind of separation methods of preparing propylene by methanol transformation reaction product：The gas-phase feed and liquid phase feeding that MTP reaction products are preprocessed, reaction product separator is isolated enter dethanizer and are handled, and polymerization-grade propylene is obtained after the processing of the technique with deethanizer reflux tank deck top still deethanization.The product quality and the rate of recovery of propylene can be effectively ensured in this method, while dethanizer being made to be not required to operate at low temperature, fractionating system obvious energy conservation.
Description
Technical field
The invention belongs to coal chemical industry or gas chemical industry fields, and in particular to a kind of preparing propylene by methanol transformation reaction product
Separation method improves the rate of recovery of propylene, reduces energy consumption, simple flow.
Background technology
The development in short supply that will restrict China's oil chemical engineering industry of petroleum resources, preparing olefin by conversion of methanol technology open
The new technology route that basic organic chemical industry raw material is produced by coal or natural gas, realizes coal chemical industry or gas chemical industry to oil
The effective way of work infiltration and development.
Into over 10 years, patent quotient develops the isolation technics of preparing olefin by conversion of methanol, is concentrated mainly on methanol and converts alkene processed
Processes production polymer grade ethylene and propylene product, MTO reaction products and the methanol such as hydrocarbon (MTO) reaction product is refined, compresses, detaches
Preparing propylene transformed (MTP) distribution of reaction products has similarity, but has particularity, cannot directly detach MTO reaction products
Flow is detached for MTP reaction products.Currently, the separation process of MTP reaction products mainly has：MTP points of Lurgi companies exploitation
From flow, CN1203033C, CN101381270B, CN102304009B etc..
Lurgi companies MTP separation process, after cooling, chilling, crude propylene gas after compression, passes through for reactor outlet logistics
Front-end deethanization, depropanization, debutanization, de- hexane and propylene recovery, ethylene recovery, isolate polymerization-grade propylene, polymer grade ethylene,
Fuel gas, liquefied gas, C4-C6 hydro carbons, gasoline etc., this method use deep cooling process for separating, step by step each component in separating mixture,
Separation process length, high energy consumption.DME (dimethyl ether) removes flow and uses absorption process technique, while absorbing DME, also absorbs propylene,
Increase loss, liquid-liquid extraction units need to be increased, the methanol content easily caused in ethylene, propylene product is unqualified, moisture is introduced low
Warm system.
CN1203033C discloses a kind of method preparing propylene with methanol, and this method propose reaction product separation process
Blank scheme, reaction product is preprocessed (including chilling etc.), detaches gas, hydrocarbon liquid phase and water in separator, takes off second before menstruation
Alkane tower, de- third tower, propylene recovery, part hydrocarbon Returning reactor entrance increase propene yield.This method, which discloses, to be not enough.
CN101381270B discloses a kind of separation method of MTO/MTP reaction mixtures, and this approach includes the following steps：
(1) reactor outlet gas is sent into depropanization prefractionator by pretreated hydrocarbon lime set, the depropanization prefractionator
Overhead product includes light gas, three or more fraction of carbon two, carbon three and carbon, and tower kettle product is four or more fraction of carbon four and carbon；
(2) the reaction was continued or is routed directly to through handling Returning reactor for depropanization prefractionator tower reactor product carbon four and four or more fraction of carbon
Debutanizing tower carries out the cutting of four C5 fraction of carbon, and overhead product enters depropanizing tower progress carbon after continuing compression and imurity-removal
The cutting of three carbon four；(3) depropanizing tower tower reactor is four or more fraction of carbon four and carbon, and through handling Returning reactor, the reaction was continued or straight
Pick the cutting that four C5 fraction of carbon is carried out toward debutanizing tower.This method essentially discloses as reaction exit gas by pretreatment
Hydrocarbon lime set afterwards adds depropanization prefractionator, improves the rate of recovery of the products such as ethylene, propylene, depropanization prefractionation tower reactor product
The reaction was continued through handling Returning reactor for carbon four and four or more fraction of carbon, and carbon containing six or more hydro carbons in the logistics has not reaction
The influence of profit.
CN102304009B discloses a kind of MTP reaction mixture gas separation method and system, by pre- chilling tower and chilling tower
The chilled water (chw) of tower reactor is pocessed respectively；II sections of obtained gas hydrocarbon are compressed through washing and entering III sections of compression, compression three after alkali cleaning
The liquid hydrocarbon for the gas hydrocarbon and not carbon containing six or more heavy hydrocarbon that section obtains is sent after dry, liquid hydrocarbon coacervation and drying to depropanization through gas hydrocarbon respectively
Tower；The intersegmental lime set of compression is detached compressing the intersegmental condensate stripper that is equipped with, light hydrocarbon component returns to II sections of outlets of compression, heavy hydrocarbon component
It send to debutanizing tower refinement treatment；Depropanizing tower is located between IV sections of III sections of compression and compression, and uses conventional rectification；Piptonychia
Alkane column overhead sets differential condensation device, recycles itself cold and reduces ethylene loss rate.This method introduces pre- chilling flow, with
Lurgi companies MTP separation process compares, and separation process is longer, energy consumption higher.
Invention content
The problems such as in order to solve current MTP reaction products separation process complexity, high energy consumption, impacted propylene recovery rate, this
Invention provides a kind of separation method of preparing propylene by methanol transformation reaction product.
The separation method of preparing propylene by methanol transformation reaction product provided by the invention mainly includes the following steps：
1) MTP reaction products after pretreatment, into reaction product separator, gas are separated into reaction product separator
Phase product, liquid product and process water；Gas-phase product carries out initial gas-liquid separation, initial gas-liquid separation after one section of compression is cooling
After obtain first gas-phase product and first lime set, first gas-phase product carries out secondary gas-liquid separation after two sections of compressions are cooling, two
Secondary gas-phase product and secondary lime set are obtained after secondary gas-liquid separation, secondary gas-phase product carries out gas three times after three sections of compressions are cooling
Liquid detaches, and obtains gas-phase product three times and three times lime set after gas-liquid separation three times, three times gas-phase product conduct after four sections of compressions
Gas-phase feed enters tower from the middle and upper part of dethanizer；Liquid product, first lime set, secondary lime set and conduct after lime set mixing three times
Liquid phase feeding enters tower from dethanizer middle and lower part；Process water is divided into two-way, is used as reaction system moisturizing to return to reaction member all the way,
Another way is sent to methanol distillation column；
2) enter the gas-phase feed of dethanizer and liquid phase feeding is fractionated into tower and is separated into dethanizer top gas and C3+
Fraction；Dethanizer top gas is condensed through deethanization tower top condenser portion, into deethanizer reflux tank, in deethanizer reflux
Gas-liquid separation is carried out in tank, and deethanization tower top, the gas phase isolated all are returned to as reflux after the liquid phase isolated is boosted
It is fractionated into deethanizer reflux tank deck still, the liquid phase isolated through deethanizer reflux tank deck still returns back
Tank is flowed, the gas phase isolated carries out gas-liquid separation after further condensation is cooling, into dethanizer deep cooling tank, through dethanizer
What deep cooling tank was isolated is further processed rich in ethylene pneumatic transmission to corresponding units, is used as back after the liquid phase isolated is boosted
Stream all returns to deethanizer reflux tank deck and is fractionated capital；C3+ fractions are from dethanizer bottom from force feed to depropanizing tower；
3) the C3+ fractions for entering depropanizing tower are fractionated into tower and are separated into C3 fractions and C4+ fractions, and C4+ fractions are from de-
Propane bottom of tower is sent to dehexanizing column and carries out subsequent processing, and C3 fractions are sent from depropanization tower top to propylene rectification tower；
4) the C3 fractions for entering propylene rectification tower are fractionated into obtain polymerization-grade propylene in tower.
Depropanizing tower, propylene rectification tower and dehexanizing column use routine operation, and those skilled in the art can be according to specific feelings
Condition selects operating condition；Propylene rectification tower uses heat pump flowsheet or old process, tower top to obtain polymerization-grade propylene product, bottom of tower production
Object propane fraction is as byproduct carrying device；Dehexanizer overhead product is C4~C6 fractions, and a part is under flow control
Returning to reaction member, the reaction was continued, and to prevent butane, pentane and/or hexane from building up, the control of another part pressure is lower to send out dress
It sets, bottom product is C7+ fractions, carrying device under being controlled under bottom of tower liquid level and the tandem of flow.
The pretreatment includes fixed bed depickling and heat exchange etc..
The technique water flow to methanol distillation column of sending is the water generated in preparing propylene by methanol transformation reaction process
The 100~110% of flow.
The pressure of the gas-phase feed into dethanizer is 2.5~3.5MPa (g).
The operating pressure of the dethanizer is 2.5~3.5MPa (g), the tower top operation temperature of dethanizer is 45~
55 DEG C, the bottom of tower operation temperature of dethanizer is 95~125 DEG C, and deethanizer reflux tank operation temperature is 38~42 DEG C；It is described
Deethanizer reflux tank deck still theoretical cam curve be 5~15 pieces, isolated through deethanizer reflux tank deck still
Gas phase -30~-15 DEG C are further cooled under the action of propylene or propane make the refrigeration system of refrigerant.
The present invention has the advantages that compared with prior art：
1) only to impurity such as the process water separating methanols that is generated in preparing propylene by methanol transformation reaction process, ensure that purified water is up to standard
Discharge, while recycling methanol.
2) method of the present invention is used, still, deethanizer reflux tank deck are set in deethanizer reflux tank deck
Gas enters reflux tank deck still fractionation, and the gas phase isolated is cooled down through further condensation, reduces the temperature of still top gas,
So that dethanizer deep cooling tank is reduced rich in propylene loss in ethylene gas, improves the rate of recovery of propylene.
3) de- using band deethanizer reflux tank deck top still under the premise of ensureing propylene product quality and the rate of recovery
Ethane technique so that low-grade heat source and low-temperature receiver can be used in dethanizer, and dethanizer is not required to operate at low temperature, fractionating system
Obvious energy conservation.
4) to gas-phase product three times and liquid product, first lime set, secondary lime set and the mixed liquor of lime set is distinguished three times
It is dry, i.e., to logistics pressure is higher, under the lower operating condition of temperature it is dry, advantageously ensure that the water content of logistics in 5ppm
Below.
Present invention will be described in further detail below with reference to the accompanying drawings and specific embodiments, but is not intended to limit the present invention
Protection domain.
Description of the drawings
Fig. 1 is a kind of separation method flow diagram of preparing propylene by methanol transformation reaction product of the present invention.
In figure：1-MTP reaction products, 2- pretreatment systems, 3- reaction product separators, 4- return to water pump, 5- reaction systems
System moisturizing, 6- process water booster pumps, one section of 7- compressors, 8- one section outlet coolers, the first liquid separation tanks of 9-, 10- compressors two
Section, 11- second stage exit coolers, bis- liquid separation tanks of 12-, three sections of 13- compressors, tri- sections of outlet coolers of 14-, 15- divide three times
Flow container, 16- gas-phase product drying systems, four sections of 17- compressors, 18- liquid product coalescers, 19- liquid product drying systems,
20- dethanizers, 21- deethanization overhead condensers, 22- deethanizer reflux tanks, 23- deethanizer reflux pump, 24- deethanizations
Tower reflux tank deck still, 25- deethanization tower top refrigerators, 26- deethanization tower top refrigeration systems, 27- dethanizer deep cooling tanks,
28- is rich in ethylene gas, 29- dethanizer force (forcing) pumps, 30- depropanizing towers, 31- propylene rectification towers, 32- polymerization-grade propylenes, 33- third
Alkane fraction, 34- dehexanizers, 35-C4~C6 fractions, 36-C7+ fractions, 37- methanol distillation columns, 38- crude carbinols, 39- purifications
Water.
Specific implementation mode
As shown in Figure 1, entering reaction product separator 3 after the pretreatment of 1 preprocessed system 2 of MTP reaction products, reacting
Gas-phase product, liquid product and process water are separated into product separator 3, gas-phase product is sent to compression unit, through compressor one
Section 7 is compressed to 0.15~0.25MPa (g), and temperature is 60~70 DEG C, is cooled to 38~42 DEG C into one section outlet cooler 8, warp
First 9 gas-liquid separation of liquid separation tank obtains first gas-phase product and first lime set, and first gas-phase product is through two section of 10 compression of compressor
To 0.5~0.80MPa (g), temperature is 80~95 DEG C, 38~42 DEG C is cooled into second stage exit cooler 11, through secondary point
12 gas-liquid separation of flow container, obtains secondary gas-phase product and secondary lime set, and secondary gas-phase product is compressed to 1.0 for three section 13 through compressor
~1.5MPa (g), temperature are 80~90 DEG C, 38~42 DEG C are cooled into three sections of outlet coolers 14, through liquid separation tank 15 three times
Gas-liquid separation obtains gas-phase product three times and three times lime set, and gas-phase product enters gas-phase product drying system 16 three times, through drying
Gas phase water content be less than 5ppm, it is dry after gas phase send to compressor and be compressed to for four section 17 to 2.5~3.5MPa (g), temperature
It is sent into tower from 20 middle and upper part of dethanizer as gas-phase feed after being 65~80 DEG C；It is liquid product and a lime set, secondary solidifying
After liquid and three times lime set mixing, after liquid product coalescer 18 and liquid product drying system 19 are dried as liquid phase feeding from
20 middle and lower part of dethanizer is sent into tower；Process water is divided into two-way, is used as reaction system moisturizing 5 through returning to the boosting of water pump 4 all the way
Reaction member is returned to, another way is sent through the boosting of process water booster pump 6 to methanol distillation column 37, the crude carbinol 38 of Methanol Recovery tower top
Returning to reaction member, the reaction was continued, 39 carrying device of purified water of Methanol Recovery bottom of tower.
Gas-phase feed and liquid phase feeding into dethanizer 20 are fractionated into tower and are separated into dethanizer top gas and C3+
Fraction；Dethanizer top gas is cooled to 38~42 DEG C through 21 partial condensation of deethanization overhead condenser, into deethanizer reflux
Tank 22, carries out gas-liquid separation in the deethanizer reflux tank 22, the liquid phase isolated after 23 boosting of deethanizer reflux pump
Deethanization tower top is all returned to as reflux under liquid level and flow serials control, the gas phase isolated enters deethanizer reflux tank
Top still 24 is fractionated, and the liquid phase isolated through deethanizer reflux tank deck still 24 returns to deethanizer reflux tank
22, the gas phase isolated is under the action of deethanization tower top refrigeration system 26 as refrigerant of propylene or propane through dethanizer
After top refrigerator 25 is further cooled to -30~-15 DEG C, gas-liquid separation is carried out into dethanizer deep cooling tank 27, through de-
What ethane tower deep cooling tank 27 was isolated return to reaction member rich in the part of ethylene gas 28 under flow control, and the reaction was continued, is anti-
Only methane is built up, and another part is used as fuel gas carrying device, the liquid phase isolated rich in ethylene gas under pressure control
Dethanizer is all returned to after the boosting of dethanizer force (forcing) pump 29 as reflux under tank bottom liquid level and flow serials control to return
It flows tank deck and is fractionated capital；C3+ fractions are from dethanizer bottom from force feed to depropanizing tower 30.
C3+ fractions into depropanizing tower 30 are fractionated into tower and are separated into C3 fractions and C4+ fractions；C4+ fractions are from de-
Propane bottom of tower is sent to dehexanizer 34, is fractionated to obtain overhead product to be C4~C6 fractions 35 through dehexanizer, a part is in flow
The reaction was continued for the lower return reaction member of control, and to prevent butane, pentane and/or hexane from building up, another part is controlled in pressure
Lower carrying device, bottom product are C7+ fractions 36, carrying device under being controlled under bottom of tower liquid level and the tandem of flow；C3 fractions
It is sent from depropanization tower top to propylene rectification tower 31.
C3 fractions into propylene rectification tower 31 are fractionated into obtain overhead product polymerization-grade propylene 32, tower bottom product in tower
Propane fraction 33 is used as byproduct carrying device.
In the method for the present invention, the C3+ fractions refer to C3~C9 fractions, and C4+ fractions refer to C4~C9 fractions, and C7+ evaporates
It refers to C7~C9 fractions to divide.
Claims (7)
1. a kind of separation method of preparing propylene by methanol transformation reaction product, it is characterised in that mainly include the following steps：
1) MTP reaction products after pretreatment, into reaction product separator, are separated into gas phase production in reaction product separator
Object, liquid product and process water；Gas-phase product carries out initial gas-liquid separation after one section of compression is cooling, after initial gas-liquid separation
To first gas-phase product and first lime set, first gas-phase product carries out secondary gas-liquid separation, secondary gas after two sections of compressions are cooling
Secondary gas-phase product and secondary lime set are obtained after liquid separation, secondary gas-phase product carries out gas-liquid point three times after three sections of compressions are cooling
From, gas-phase product three times and three times lime set are obtained after gas-liquid separation three times, three times gas-phase product through four sections compression after be used as gas phase
Charging enters tower from the middle and upper part of dethanizer；Liquid product, first lime set, secondary lime set and three times lime set mixing after be used as liquid phase
Charging enters tower from dethanizer middle and lower part；Process water is divided into two-way, and reaction system moisturizing is used as to return to reaction member all the way, another
It send to methanol distillation column on road；
2) enter the gas-phase feed of dethanizer and liquid phase feeding is fractionated into tower and is separated into dethanizer top gas and C3+ evaporates
Point；Dethanizer top gas is condensed through deethanization tower top condenser portion, into deethanizer reflux tank, in deethanizer reflux tank
Interior carry out gas-liquid separation all returns to deethanization tower tops after the liquid phase isolated is boosted as reflux, the gas phase isolated into
Enter deethanizer reflux tank deck still to be fractionated, the liquid phase isolated through deethanizer reflux tank deck still returns to reflux
Tank, the gas phase isolated carry out gas-liquid separation after further condensation is cooling, into dethanizer deep cooling tank, through dethanizer depth
What cold tank was isolated is further processed rich in ethylene pneumatic transmission to corresponding units, as reflux after the liquid phase isolated is boosted
It all returns to deethanizer reflux tank deck and is fractionated capital；C3+ fractions are from dethanizer bottom from force feed to depropanizing tower；
3) the C3+ fractions for entering depropanizing tower are fractionated into tower and are separated into C3 fractions and C4+ fractions, and C4+ fractions are from depropanization
Bottom of tower is sent to dehexanizing column and carries out subsequent processing, and C3 fractions are sent from depropanization tower top to propylene rectification tower；
4) the C3 fractions for entering propylene rectification tower are fractionated into obtain polymerization-grade propylene in tower.
2. according to the method described in claim 1, it is characterized in that：Described gas-phase feed and liquid phase into dethanizer into
Expect to need the drying process for passing through drying system respectively before entering dethanizer.
3. according to the method described in claim 1, it is characterized in that：The technique water flow to methanol distillation column of sending is first
The 100~110% of the flow of the water generated in the preparing propylene transformed reaction process of alcohol.
4. according to the method described in claim 1, it is characterized in that：The pressure of the gas-phase feed into dethanizer is
2.5~3.5MPa.
5. according to the method described in claim 1, it is characterized in that：The operating pressure of the dethanizer be 2.5~
The tower top operation temperature of 3.5MPa, dethanizer are 45~55 DEG C, and the bottom of tower operation temperature of dethanizer is 95~125 DEG C, is taken off
Ethane tower return tank operation temperature is 38~42 DEG C；The theoretical cam curve of the deethanizer reflux tank deck still be 5~
15 pieces, the gas phase isolated through deethanizer reflux tank deck still is further cooled to -30~-15 DEG C.
6. according to the method described in claim 1, it is characterized in that：The cooling refrigerant used of further condensation is third
Alkene or propane.
7. according to the method described in claim 1, it is characterized in that：The pretreatment includes fixed bed depickling and heat exchange.
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| CN102746083A (en) * | 2011-04-22 | 2012-10-24 | 中国石油化工股份有限公司 | Technology for separating low carbon olefin gases |
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