CN102372556A - Water diversion method for preparing ethylbenzene from ethanol and benzene - Google Patents
Water diversion method for preparing ethylbenzene from ethanol and benzene Download PDFInfo
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- CN102372556A CN102372556A CN2010102602021A CN201010260202A CN102372556A CN 102372556 A CN102372556 A CN 102372556A CN 2010102602021 A CN2010102602021 A CN 2010102602021A CN 201010260202 A CN201010260202 A CN 201010260202A CN 102372556 A CN102372556 A CN 102372556A
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Abstract
The invention relates to a water diversion method for preparing ethylbenzene from ethanol and benzene and mainly solves the problems of the past ethanol method ethylbenzene production process that the water separation effect of the reaction product is poor and the life of the catalyst is short because of too much water in circulating benzene returning to the reactor. The technical scheme adopted in the invention is as follows: water-containing benzene enters a benzene-water separator to pass through a pre-separation internal member, a steady flow internal member, a demulsification internal member and a benzene phase accumulation internal member which are arranged in the benzene-water separator, benzene and water are separated, wherein the aqueous phase flows from an aqueous phase outlet pipe and the benzene phase overflows through a baffle plate and flows out of a benzene phase outlet pipe. By adopting the technical scheme, the problems can be better solved and the method can be used in the ethanol method industrial production of ethylbenzene.
Description
Technical field
The present invention relates to a kind of ethanol and benzene synthesizing ethyl benzene dividing method for water.
Background technology
Ethylbenzene is important chemical material; Be to produce the indispensable critical materials of vinylbenzene, the purpose that most of ethylbenzene manufacturers produce ethylbenzene is that the styrene device that is used for oneself is produced vinylbenzene, and vinylbenzene is important basic Organic Chemicals; Be mainly used in polymeric material field and produce PS and multipolymer thereof; Like ABS, AS, styrene-butadiene rubber(SBR) and unsaturated polyester thereof, in addition, vinylbenzene also is widely used in pharmacy, coating, pigment and the textile industry as the organic reaction midbody.
Traditional ethylbenzene synthesis technique carries out alkylated reaction with ethene and benzene as raw material usually and obtains ethylbenzene; And riseing day by day and exhaustion day by day along with crude oil price; The ethylene raw cost also constantly increases thereupon, and more and more producers adopt ethanol and one step of benzene to send out technology and make ethylbenzene.
The Ethanol Method process for preparing ethylbenzene is a raw material with ethanol and benzene; Both get into alkylation reactor simultaneously, and the alkylated reaction of ethanol dehydration reaction and ethene and benzene is accomplished in a reactor drum simultaneously, and the required heat of ethanol dehydration is by the heat release supply of alkylated reaction; The ethene that ethanol dehydration generates and benzene high temperature, in calm the anger and carry out alkylation under the condition mutually; About 400 ℃ of temperature of reaction, pressure＜2.0MPaG, reactor drum have used and have satisfied the sieve catalyst that ethanol dehydration and ethylene alkylation carry out particular requirement simultaneously; The selectivity of ethanol dehydration and transformation efficiency are very high, and ethene also can reach the identical level of ethylene process with the transformation efficiency of benzene alkylation.Compare traditional ethanol system ethene that dewaters step by step, make derived product by ethene again, the technology that ethanol dehydration is carried out in the side reaction of ethanol dehydration relatively separately is few; Technical process is simple, reduced investment, and process cost is low; Have remarkable advantages, about ethanol and benzene synthesizing ethyl benzene Technology, concrete document has Chinese patent ZL200410020397.7, CN200710025134.9, CN200910055981.9; But do not specifically describe benzene water sepn effect in the document; Test discovery through the inventor, carry out the benzene water sepn, moisture reaching more than 1.5% in the benzene with its technology.
Owing in the reactor drum ethanol dehydration reaction has taken place, unavoidably there is more water to exist in the reaction product, ethanol and benzene synthesizing ethyl benzene technology adopt the ZSM-5 sieve catalyst usually; High concentration water's existence can have a strong impact on the life-span of this sieve catalyst; Though the water resistance of sieve catalyst is compared traditional ethylene process process for preparing ethylbenzene also in continuous progress now, generally only be 1/3～1/2 of ethylene process the work-ing life of Ethanol Method sieve catalyst; The present common benzene of ethanol legal system ethylbenzene reaction process excessive in a large number (benzene and ethanol mol ratio 4～7); The benzene of reaction product after rectifying separation need be as the recycle benzene Returning reactor, and the separation of reaction product water only is in the benzene separation column condenser, to accomplish, and reaction product divides water not thorough; Cause the water-content in the recycle benzene higher; If water cut reaches more than 1.0% in the benzene, high-content water can obviously make the sieve catalyst regeneration period foreshorten to 3～5 months by former about 6 months behind the entering reactor drum, and foreshortened to 8～10 month by former about 12 months work-ing life; Therefore, the water-content that improve benzene water sepn efficient, reduces in the recycle benzene is very important to prolonging catalyzer work-ing life.
Summary of the invention
Technical problem to be solved by this invention is moisture short problems of catalyst life that cause in the recycle benzene of water sepn weak effect, Returning reactor in the ethanol legal system ethylbenzene production technique reaction product in the past more.A kind of new ethanol and benzene synthesizing ethyl benzene dividing method for water are provided, and this method has that branch water is effective, and water-content is low in the recycle benzene, the advantage that can prolong sieve catalyst regeneration period and work-ing life.
For solving the problems of the technologies described above, the technical scheme that the present invention adopts is following: a kind of ethanol and benzene synthesizing ethyl benzene dividing method for water, and the benzene of moisture 5%～20% (weight) gets into the benzene water separator through inlet pipe; Pre-separation inner member, current stabilization inner member through being provided with in the benzene water separator successively, the breakdown of emulsion inner member is with after benzene is assembled inner member mutually, and benzene water obtains separation; Make that water cut is lower than 0.1% in the benzene, benzol content is lower than 0.5% in the water, and the pre-separation inner member is a structure of container; Have effusive for liquid aperture above, the current stabilization inner member is filler or the vertical waved plate of placing, and the breakdown of emulsion inner member is a metal sheet; Have the aperture that flows through for liquid above; Benzene is assembled horizontal wave card or the wire cloth of inner member for placing along the container circumference mutually, and baffle plate is a metal sheet, is positioned at behind the water outlet pipe before the benzene phase outlet pipe;
In the technique scheme; Moisture benzene gets into the pre-separation inner member through the inlet pipe that stretches into internal tank, and the pre-separation inner member is a structure of container, is distributed with aperture on the inner member; The aperture is 5 millimeters～50 millimeters; It is inner that moisture benzene flow out to get into the benzene water separator through aperture, and the liquid flow velocity that portals is 0.01 meter per second～1.0 meter per seconds, preferred 0.05 meter per second～0.3 meter per second; Be provided with the current stabilization inner member in the benzene water separator, inner member is filler or the vertical waved plate of placing, and waved plate thickness is 0.1 meter～1 meter; Be provided with the breakdown of emulsion inner member in the benzene water separator; Inner member is a metal sheet, and last perforate directly is 10 millimeters～40 millimeters a aperture, and the liquid flow velocity that portals is 0.01 meter per second～0.2 meter per second; Be provided with benzene in the benzene water separator and assemble inner member mutually; Inner member is horizontal wave card or the wire cloth of placing along the container circumference, and waved plate thickness is 0.2 meter～3 meters, and wire cloth thickness is 0.05 meter～1 meter; Water outlet back, benzene are provided with baffle plate before exporting mutually in the benzene water separator, and height of baffle plate is 40%～90% of a container height; Benzene water separator service temperature is 10 ℃～80 ℃, and preferred 20～60 ℃, working pressure is 0.5MPaG～2.0MPaG, preferred 0.8MPaG～1.2MPaG.
The present invention is through adopting the ethanol legal system ethylbenzene reaction product water separation scheme like Fig. 1, and the reaction product that mainly contains benzene, ethylbenzene, diethylbenzene and water gets into the benzene knockout tower, and the separation of benzene column overhead obtains benzene and water; The tower still obtains ethylbenzene and diethylbenzene; Overhead stream is after condenser condenses arrives the breakdown of emulsion temperature (10～80 ℃), and moisture benzene gets into the benzene water separator to be separated, and moisture benzene material gets into the pre-separation inner member through inlet pipe; The pre-separation inner member is positioned at the bottom of benzene water separator; Have aperture above, material makes flow in the process that is penetrated by aperture in pre-separation inner member aperture gets into container; Except that overcoming fluid resistance, also to overcome gravity acting; The underlying of the inner member of pre-separation simultaneously makes the water feed liquor of material below the benzene water termination, and when phlegma passes through water, thereby the coalescence chance that the stirring shearing action between the liquid group has increased between the water droplet has been strengthened benzene water pre-separation effect; Material gets into the current stabilization inner member after pre-separation, the current stabilization inner member is the vertical waved plate of placing, and helps flow and is evenly distributed, and even fluid distribution helps benzene water gravity separation.Phlegma behind the current stabilization inner member through the top breakdown of emulsion inner member that is covered with aperture; The main effect of breakdown of emulsion inner member is the emulsion of broken aqueous phase; Wherein little benzene is dripped separate, special when temperature is higher, benzene is prone to the formation emulsion with water mutually.Behind the breakdown of emulsion inner member, the material of initial gross separation gets into benzene and assembles inner member mutually, and it is that the ripple of horizontal positioned is less that benzene is assembled inner member mutually; Plate group equivalent diameter is little, can be in the larger process amount, and the less residence time keeps laminar flow regime down; Flow is " it " font and flows in the waved plate group, flow to flow area constantly to change, and drips mutual collision and has created chance for benzene drops in the surperficial gathering of waved plate and benzene; Benzene drops in buoyance lift in the gathering, in buoyance lift, assembles, and has improved benzene water sepn efficient; Benzene phase benzene after the separation exports discharge through the baffle plate overflow by benzene mutually, and water is discharged by the water outlet.
With 200,000 tons of/year ethanol and benzene one-step synthesis ethylbenzene device is example; The main weight of reaction product consists of: benzene 71%, ethylbenzene 16%, diethylbenzene 1.6%; Water 11%; After adopting ethanol of the present invention and benzene synthesizing ethyl benzene dividing method for water, water cut drops to 0.08% by original 1.5% in the recycle benzene, and ethanol and benzene synthesizing ethyl benzene used ZSM-5 sieve catalyst regeneration period of reaction extended to 6 months by original 3 months; Extended to 12 month by original 8 months work-ing life, obtained better technical effect.
Description of drawings
Fig. 1 is for adopting the ethanol and the benzene synthesizing ethyl benzene dividing method for water synoptic diagram of technical scheme of the present invention.
Among Fig. 1, I is a shell of tank, and II is an internal tank, and 1 is the benzene knockout tower, and 2 is condensing surface, and 3 is inlet pipe, and 4 is preseparator, and 5 is the current stabilization inner member, and 6 is the breakdown of emulsion inner member, and 7 assemble inner member mutually for benzene, and 8 is baffle plate, and 9 is the water outlet, and 10 be that benzene phase benzene exports.
Reaction product 101 is after benzene knockout tower 1 separates; Tower still logistics 102 is mainly ethylbenzene and many ethylbenzene, and overhead gas stream 103 is mainly benzene and water, through condensing surface 2 condensations after inlet pipe 3 gets into pre-separation inner members 4; The aperture that on the pre-separation inner member, has gets in the container; Assemble inner member 7 mutually through current stabilization inner member 5, breakdown of emulsion inner member 6, benzene successively then, the benzene phase 106 after the separation exports 10 through baffle plate 8 overflows mutually by benzene and discharges, and water 105 is discharged by water outlet 9.
Through embodiment the present invention is done further elaboration below.
Embodiment
[embodiment 1]
Certain 200,000 tons of/year ethanol and benzene synthesizing ethyl benzene device, its reaction product water separating method adopts the technology of Fig. 1, adopts the ZSM-5 sieve catalyst, and the main weight of reaction product consists of: benzene 73%; Ethylbenzene 14.5%, diethylbenzene 1.5%, water 10%, reaction product is after benzene column overhead condenser condenses to 60 ℃; Get into the benzene water separator and carry out the benzene water sepn, the benzene water separator is a horizontal container, 150 cubic metres of volumes, long 10 meters; 4.2 meters of diameters, charging phlegma flow is 300 cubic metres, and wherein water accounts for 5.7% (weight), and benzene accounts for 93.3% (weight); 500 millimeters of feed tube diameter, 40 millimeters in pre-distributor perforate aperture, hole count 500, the current stabilization inner member adopts vertically arranged waved plate; 500 millimeters of thickness, the breakdown of emulsion inner member adopts a metal sheet, on open 25 millimeters apertures, hole count 1000; Benzene is assembled inner member mutually and is adopted the horizontal positioned waved plate, and 2 meters of thickness, benzene export 400 millimeters of calibers mutually, 100 millimeters of water outlet calibers; Height of baffle plate is 80% of a container height, and service temperature is 60 ℃, and pressure is 1.0MPaG.
3,000,000 yuan of this device benzene water separator facility investments, liquid residence time 30 minutes, moisture 0.1% (weight) in analysis cycle benzene, aqueous phase contains benzene 0.3%, and the alkylation ZSM-5 sieve catalyst regeneration period is 6 months, and the life-span is 12 months.
[embodiment 2]
Certain 200,000 tons of/year ethanol and benzene synthesizing ethyl benzene device, its reaction product water separating method adopts the technology of Fig. 1.Benzene water separator inlet amount, composition and device structure are with embodiment 1, and different is 20 millimeters in pre-distributor perforate aperture, hole count 1600.
3,000,000 yuan of this device benzene water separator facility investments, liquid residence time 30 minutes, moisture 0.08% (weight) in analysis cycle benzene, aqueous phase contains benzene 0.4%, and the alkylation ZSM-5 sieve catalyst regeneration period is 6.5 months, and the life-span is 13 months.
[embodiment 3]
Certain 200,000 tons of/year ethanol and benzene synthesizing ethyl benzene device, its reaction product water separating method adopts the technology of Fig. 1.Benzene water separator inlet amount, composition and device structure are with embodiment 1, and different is that the current stabilization inner member adopts filling-material structure.
3,100,000 yuan of this device benzene water separator facility investments, liquid residence time 30 minutes, moisture 0.07% (weight) in analysis cycle benzene, aqueous phase contains benzene 0.5%, and the alkylation ZSM-5 sieve catalyst regeneration period is 7 months, and the life-span is 14 months.
[embodiment 4]
Certain 200,000 tons of/year ethanol and benzene synthesizing ethyl benzene device, its reaction product water separating method adopts the technology of Fig. 1.Benzene water separator inlet amount, composition and device structure are with embodiment 1, and different is that benzene is assembled inner member employing wire cloth mutually.
2,800,000 yuan of this device benzene water separator facility investments, liquid residence time 30 minutes, moisture 0.08% (weight) in analysis cycle benzene, aqueous phase contains benzene 0.5%, and the alkylation ZSM-5 sieve catalyst regeneration period is 6 months, and the life-span is 12 months.
[embodiment 5]
Certain 200,000 tons of/year ethanol and benzene synthesizing ethyl benzene device, its reaction product water separating method adopts the technology of Fig. 1.Benzene water separator inlet amount, composition and device structure are with embodiment 1, and different is that height of baffle plate is 50% of a container height.
3,000,000 yuan of this device benzene water separator facility investments, liquid residence time 30 minutes, moisture 0.09% (weight) in analysis cycle benzene, aqueous phase contains benzene 0.4%, and the alkylation ZSM-5 sieve catalyst regeneration period is 5.5 months, and the life-span is 11 months.
[embodiment 6]
Certain 200,000 tons of/year ethanol and benzene synthesizing ethyl benzene device, its reaction product water separating method adopts the technology of Fig. 1.Benzene water separator inlet amount, composition and device structure are with embodiment 1, and different is that service temperature is 40 ℃.
3,000,000 yuan of this device benzene water separator facility investments, liquid residence time 30 minutes, moisture 0.1% (weight) in analysis cycle benzene, aqueous phase contains benzene 0.5%, and the alkylation ZSM-5 sieve catalyst regeneration period is 5 months, and the life-span is 10 months.
[comparative example 1]
Certain 200,000 tons of/year ethanol and benzene synthesizing ethyl benzene device, its reaction product benzene water sepn operational condition is identical with embodiment 1, does not have in different the is benzene water separator to presort cloth inner member, current stabilization inner member, breakdown of emulsion inner member and benzene and assemble inner member mutually.The benzene water separator is a horizontal container, 250 cubic metres of volumes, long 14 meters, 4.6 meters of diameters; 500 millimeters of feed tube diameter, 400 millimeters of benzene phase benzene outlet calibers, 100 millimeters of water outlet calibers; Height of baffle plate is 80% of a container height, and service temperature is 60 ℃, and pressure is 1.0MPaG.
4,000,000 yuan of this device benzene water separator facility investments, liquid residence time 50 minutes, moisture 2.0% (weight) in analysis cycle benzene, aqueous phase contains benzene 1.6%, and the alkylation ZSM-5 sieve catalyst regeneration period is 5 months, and the life-span is 10 months.
[comparative example 2]
Certain 200,000 tons of/year ethanol and benzene synthesizing ethyl benzene device, its reaction product benzene water sepn operates in the overhead condenser carries out, and other conditions are identical with embodiment 1.
Moisture 1.8% (weight) in this device recycle benzene, aqueous phase contains benzene 1.5%, and the alkylation ZSM-5 sieve catalyst regeneration period is 4 months, and the life-span is 8 months.
[comparative example 3]
Certain 200,000 tons of/year ethanol and benzene synthesizing ethyl benzene device, its reaction product benzene water sepn operational condition is identical with comparative example 1, and different is that benzene water separator service temperature is 120 ℃.
Moisture 1.5% (weight) in this device recycle benzene, aqueous phase contains benzene 1.2%, and the alkylation ZSM-5 sieve catalyst regeneration period is 4.5 months, and the life-span is 9 months.
Claims (9)
1. ethanol and benzene synthesizing ethyl benzene dividing method for water, the benzene of moisture 5%～20% (weight) gets into the benzene water separator through inlet pipe, successively pre-separation inner member, the current stabilization inner member through being provided with in the benzene water separator; The breakdown of emulsion inner member is with after benzene is assembled inner member mutually, and benzene water obtains separating, and makes that water cut is lower than 0.1% in the benzene; Benzol content is lower than 0.5% in the water, and the pre-separation inner member is a structure of container, has effusive for liquid aperture above; The current stabilization inner member is filler or the vertical waved plate of placing; The breakdown of emulsion inner member is a metal sheet, has the aperture that flows through for liquid above, and benzene is assembled horizontal wave card or the wire cloth of inner member for placing along the container circumference mutually; Baffle plate is a metal sheet, is positioned at behind the water outlet pipe before the benzene phase outlet pipe;
2. ethanol according to claim 1 and benzene synthesizing ethyl benzene dividing method for water; It is characterized in that moisture benzene gets into the pre-separation inner member through the inlet pipe that stretches into internal tank; The pre-separation inner member is a structure of container, is distributed with aperture on the inner member, and the aperture is 5 millimeters～50 millimeters; It is inner that moisture benzene flow out to get into the benzene water separator through aperture, and the liquid flow velocity that portals is 0.01 meter per second～1.0 meter per seconds.
3. ethanol according to claim 2 and benzene synthesizing ethyl benzene dividing method for water is characterized in that moisture benzene is 0.05 meter per second～0.3 meter per second through the aperture flow velocity that portals.
4. ethanol according to claim 1 and benzene synthesizing ethyl benzene dividing method for water is characterized in that being provided with in the benzene water separator current stabilization inner member, and inner member is filler or the vertical waved plate of placing, and waved plate thickness is 0.1 meter～1 meter.
5. ethanol according to claim 1 and benzene synthesizing ethyl benzene dividing method for water; It is characterized in that being provided with in the benzene water separator breakdown of emulsion inner member; Inner member is a metal sheet, and last perforate directly is 10 millimeters～40 millimeters a aperture, and the liquid flow velocity that portals is 0.01 meter per second～0.2 meter per second.
6. ethanol according to claim 1 and benzene synthesizing ethyl benzene dividing method for water; It is characterized in that being provided with in the benzene water separator benzene and assemble inner member mutually; Inner member is horizontal wave card or the wire cloth of placing along the container circumference; Waved plate thickness is 0.2 meter～3 meters, and wire cloth thickness is 0.05 meter～1 meter.
7. ethanol according to claim 1 and benzene synthesizing ethyl benzene dividing method for water is characterized in that water outlet back, benzene are provided with baffle plate before exporting mutually in the benzene water separator, and height of baffle plate is 40%～90% of a container height.
8. ethanol according to claim 1 and benzene synthesizing ethyl benzene dividing method for water is characterized in that benzene water separator service temperature is 10 ℃～80 ℃, and working pressure is 0.5MPaG～2.0MPaG.
9. ethanol according to claim 8 and benzene synthesizing ethyl benzene dividing method for water is characterized in that benzene water separator service temperature is 20 ℃～60 ℃, and working pressure is 0.8MPaG～1.2MPaG.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102372581A (en) * | 2010-08-23 | 2012-03-14 | 中国石油化工股份有限公司 | Water distribution method of reaction product in preparation of ethylbenzene by ethanol method |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2449779Y (en) * | 2000-10-08 | 2001-09-26 | 鲁礼民 | Incompatible media separating apparatus |
| CN201240883Y (en) * | 2008-05-08 | 2009-05-20 | 孟繁欣 | Oil-water separating apparatus |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2449779Y (en) * | 2000-10-08 | 2001-09-26 | 鲁礼民 | Incompatible media separating apparatus |
| CN201240883Y (en) * | 2008-05-08 | 2009-05-20 | 孟繁欣 | Oil-water separating apparatus |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102372581A (en) * | 2010-08-23 | 2012-03-14 | 中国石油化工股份有限公司 | Water distribution method of reaction product in preparation of ethylbenzene by ethanol method |
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