CN1053386C - Separating mixed dimethyl benzene with catalytic rectifying method - Google Patents
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Abstract
The present invention relates to a method for separating an organic mixture. The method is theoretically based on thermodynamics, phase balance and dynamic laws for separating material. The present invention is characterized in that in the whole rectification process, a catalyst is continuously added from the lower half part of a rectification tower so that ingredients of which the boiling points are approximate and even have a difference of 0.75 DEG C can be effectively separated. When the catalyst rectification method is used for separating xylene, four single products can be obtained, required conditions are moderate, and required equipment is simple; besides, the catalyst can be circularly used. The present invention has the advantages of low energy consumption, low material consumption, high product yield and high quality, and has good economic benefits in industrial production.
Description
The present invention relates to a kind of separation method of organic mixture, the separation method of the organic mixture that particularly the component boiling point is close very much, molecular configuration is very similar.
Traditional distillation theory is based on the macroscopic property of separation mixture and vapour, liquid equilibrium rule, the various components of not considering system are transferred to the factor of dynamics aspect of the speed speed degree of vapour phase from liquid phase, so can not fully reflect and illustrate the actual rule of the mass transfer separation process of distillation, the method that distillating method of setting up under this theoretical premise such as rectification method, extractive distillation method and azeotropic distillation etc. separate organic mixture all can not realize the separation fully to the system that the component boiling point is close very much, molecular configuration is similar.
Be close very much for boiling point, very difficult organic mixture that separates such as mixed xylenes etc., existing separation method all can not be accomplished just can all separate out the product that obtains each one-component to each component in the mixture with a kind of method separately, and the supporting use of the separation method that can only adopt two or more just can achieve the goal, separation as mixed xylenes, especially wherein right-dimethylbenzene with-the separating of dimethylbenzene, at present adopt " rectification methods+cryogenic crystallization partition method " more, or " complexometric extraction partition method+rectification method ", or " adsorption method of separation+rectification method ", though these methods have separating effect preferably, but yield in unit time is not high, and exist equipment needed thereby many and complicated, the technology more complicated, long flow path, productivity ratio is low, energy consumption, material consumption is very high, thereby the high shortcoming of production cost.
The purpose of this invention is to provide a kind of method of separating organic mixture, the very approaching organic mixture of energy separation component boiling point, and efficient high yield, low energy consumption, low material consumption.
During with the rectification method separating mixture, the liquid-vaqor interface of system is very big in the rectifying column, vapour in the distillation process, the mass transfer of liquid two-phase carries out in liquid-vaqor interface, the quality of the effect of separation mixture, the vapour phase that not only depends on system, the macroscopic property of liquid phase and the rule of stream-liquid phase balance, but also the surface nature that depends on liquid and various components break away from speed speed different of vapour phase from liquid surface, therefore, can use to increase the relative volatility that desire is separated the purpose component, the special extract rectification method that can make the faster disengaging liquid surface of purpose component again and transfer to vapour phase realizes the separation of the system that boiling point is close very much, this special rectificating method is to adopt a kind of special solvent to achieve the above object, this special solvent separates the purpose component with desire have bigger seemingly affinity and bigger surface-active, can increase desire and separate the relative volatility of purpose component, the purpose component is shifted to vapour phase from liquid phase quickly than other component.Therefore, above-mentioned special extract rectification method is named as benzene with catalytic rectifying method, and used special solvent claims to urge agent.
Benzene with catalytic rectifying method is achieved in that in whole rectifying process, continuously outside the rectifying column Lower Half, add a kind of urgency agent, and urging the volume ratio of agent and other components in the control distillate is 1: (0.5～3), the urgency agent that is added must be dissolved each other with separated mixture, and its boiling point separates low 10～100 ℃ of purpose component than desire.
When separated mixture is a mixed xylenes, the component that comprises be ethylbenzene, right-dimethylbenzene ,-dimethylbenzene and ortho-xylene, component boiling point be close very much, the boiling-point difference of ethylbenzene and right-dimethylbenzene is 2.2 ℃, right-dimethylbenzene and-boiling-point difference of dimethylbenzene is 0.75 ℃, between-boiling-point difference of dimethylbenzene and ortho-xylene is 5.3 ℃, can adopt the tert-butyl alcohol, carbon tetrachloride, ethanol, methyl alcohol, isopropyl alcohol, sec-butyl alcohol, chloroform, triethylamine, butanone, ethyl acetate or n-butanol to do to urge agent to realize the separation of mixed xylenes, obtain four lists-product.
At first isolate ortho-xylene,, can allow other three components become distillate, and tower bottoms is ortho-xylene as a highest component of mixture mid-boiling point.
After isolating ortho-xylene, ethylbenzene, right-dimethylbenzene and-can isolate the minimum ethylbenzene of boiling point earlier in the dimethylbenzene, ethylbenzene in distillate, tower bottoms be right-dimethylbenzene and-dimethylbenzene.
At last with right-dimethylbenzene with-dimethylbenzene separates, right-dimethylbenzene in distillate, tower bottoms be between-dimethylbenzene.
In each separation process, urge agent to become one of composition of distillate, therefore urge agent constantly to replenish to rectifying column, and owing to urge the boiling point of agent all lower than the boiling point of any component in the mixture, be easy to from distillate, separate, do not influence the purity of other component in the distillate, therefore, in the distillation process of main distillation column, can make and urge agent can be recycled simultaneously with the urgency agent of urging in the agent recovery tower separation distillate.
Adopt one of above-mentioned urgency agent, urging the volume ratio of agent and other component (C8 aromatic hydrocarbons) in the control distillate is 1: (0.5～3), and the full separation process of mixed xylenes is as follows:
The purpose component is an ortho-xylene, theoretical cam curve is 30～75, reflux ratio is 3～8, tower top pressure is 500～760mmHg, tower still temperature is 130～148 ℃, tower top temperature is 110～130 ℃, distillate for urge agent, ethylbenzene, right-dimethylbenzene and-dimethylbenzene, tower bottoms is the ortho-xylene product.
The purpose component is an ethylbenzene, separated mixture be ethylbenzene, right-dimethylbenzene and-dimethylbenzene, in the theoretical number of plates is 80～150, and reflux ratio is 5～12, and tower top pressure is 500～760mmHg, tower still temperature is 125～148 ℃, tower top pressure is 100～126 ℃, and distillate is for urging agent and ethylbenzene, tower bottoms be right-dimethylbenzene and-dimethylbenzene, distillate gets ethylbenzene product after isolating and urging agent.
Right-dimethylbenzene with-the separating of dimethylbenzene, adopt the rectifying column of 200～300 blocks of theoretical trays, reflux ratio is 10～20, divides following two steps to carry out:
1. theoretical cam curve is 100～150, and reflux ratio is 10～20, and tower top pressure is 500～760mmHg, and tower still temperature is 130～148 ℃, and tower top temperature is 100～120 ℃, and distillate is for urging agent and the thick product of right-dimethylbenzene, tower bottoms be between-the dimethylbenzene product;
2. after the distillate in inciting somebody to action is 1. isolated and is urged agent, in the theoretical number of plates is 100～150, reflux ratio is 10～20, tower top pressure is 500～760mmHg, and tower still temperature is 130～148 ℃, and tower top temperature is to separate right-dimethylbenzene under 100～120 ℃ of conditions, distillate is for urging agent and right-dimethylbenzene, isolate urge agent after, must right-dimethylbenzene product, tower bottoms as the 1. the raw material in step pump into the 1. the rectifying column in the step use.
The 1., 2. the step can carry out simultaneously, rectifying column with two 100～150 theoretical plates, the 1. the distillate in step deliver to simultaneously and urge the agent recovery tower to urge agent to separate, the thick product of right-dimethylbenzene that obtains enters the 2. rectifying column in step, the gained tower bottoms pumps into the 1. rectifying column in step again.
The separation of mixed xylenes, urging agent preferably is carbon tetrachloride or ethanol.
Urge the volume ratio of agent and other components can be chosen in 1 in the distillate: the scope of (0.8～1.5) preferably is controlled at 1: (0.9～1.1).
Method of the present invention, a kind of thermodynamics that is based upon system has been proposed, balance each other and the kinetic property basis on new distillation theory, can reflect and illustrate the actual rule of the mass transfer separation process of distillation fully, putting the benzene with catalytic rectifying method of design before this, second all constantly add to urge the method for agent from rectifying column with unprecedented, purpose component relative volatility was increased, make other component of purpose ratio of component break away from vapour phase from the liquid phase surface faster and more again, therefore, can make the component molecular configuration similar, the boiling point organic mixture that only differs from 0.7 ℃ even that is close also can effectively be separated very, and required mild condition, equipment is simple, only needing to carry out suitable transformation with conventional distillation equipment by the theory and technology requirement of benzene with catalytic rectifying method gets final product, urge agent to recycle, this method low energy consumption, low material consumption, the products obtained therefrom high-quality, the yield height is applied on the industrial production, and economic benefit is considerable.
As adopt ethylbenzene and ortho-xylene in the separating mixed dimethyl benzene with catalytic rectifying method, with the rectification method that adopts both at home and abroad at present relatively, separating resulting is listed in table 1.
Table 1 separates the comparison of ethylbenzene and two components of ortho-xylene from mixed xylenes
| To minute ethylbenzene from | Separation method | The number of theoretical plate of tower | Reflux ratio | Product purity (%) | Recovery rate (%) |
| Rectifying (method of at present domestic and international usefulness) | 300～350 (Maoming station-services 120) | 25～50 (Ba Ling station-services 70) | (99.7 Maoming factory 97) | (Maoming factory 60) | |
| Benzene with catalytic rectifying (the inventive method) | 80～120 | 8～12 | 99 | ＞95 | |
| To two fens first of benzene neighbour from | Rectifying (method of at present domestic and international usefulness) | 100～150 | 5～8 | 95.3 | |
| Benzene with catalytic rectifying (the inventive method) | 35～70 | 5～8 | 96～99 | ＞95 |
From table 1 data on rectifying column number of theoretical plate one hurdle more as can be known, the height that benzene with catalytic rectifying method separates the required rectifying column of ethylbenzene from mixed xylenes only be rectification method the required tower of separation height 1/4～1/3; From the data on reflux ratio one hurdle more as can be known, the productivity ratio (output/hour) that benzene with catalytic rectifying method is produced ethylbenzene is up to 3～4 times of rectification method, the urgency agent part of deduction in the distillate, and the ethylbenzene product to distillate, its productivity ratio are about 2 times of productivity ratio of rectification method.Can estimate that from this comparison of two energy consumption that benzene with catalytic rectifying method is isolated ethylbenzene from mixed xylenes approximately only is about 30% of rectification method, obviously, energy consumption has greatly reduced.
For right-dimethylbenzene with-the separating of diformazan, because both boiling points only differ from 0.75 ℃, separate with common 4 rectification methods or other single separation method, be difficult to obtain single product, and separation condition is very harsh, and separate with benzene with catalytic rectifying method, adopt carbon tetrachloride for urging agent, the result is as shown in table 2.Table 2
| The system that separates | Name of product | The rectifying column number of theoretical plate | Reflux ratio | Product purity (%) | Recovery rate (%) |
| Mixed xylenes | Ethylbenzene | 70 | 8～12 | 97 | 94 |
| To, meta-xylene mixture " right-31% ;-69% " " is right-93% ,-7% " | Paraxylene | 140 175 35 | 8～12 8～12 5～8 | 94 96 96 | 96 98 |
| Between, ortho-xylene mixture " between-67%, adjacent-33% " | Meta-xylene | 35 | 5～8 | 99.6 | 95 |
| Ortho-xylene | 99.9 | 91 |
By the data of table 2 as seen, with benzene with catalytic rectifying method can reach right-dimethylbenzene with-the separating fully of dimethylbenzene, can infer also that from the data of table 2 with the rectifying column that 150 theoretical plates are arranged be from mixed xylenes separation and Extraction ethylbenzene in reflux ratio under 8～12 the condition; With two rectifying column compartment, paraxylene under the condition of reflux ratio 8～12 that 150 theoretical plates are respectively arranged; Under reflux ratio 5～8 conditions, separate ortho-xylene with the rectifying column that 75 theoretical plates are arranged; The purity of resulting four kinds of products all may reach 99～99.5%, and recovery rate all may reach 99%, that is might reach the index of high-quality, high yield.
The present invention is further illustrated below in conjunction with equipment and embodiment:
Fig. 1 is the equipment and the schematic flow sheet thereof of benzene with catalytic rectifying method separation mixture:
Benzene with catalytic rectifying equipment comprises rectifying column (1), condenser (2), diversion cans (3), urge agent recovery tower (4), urge agent feed storage tank (5), raw material feed storage tank (6), distillate discharging storage tank (7) and tower bottoms discharging storage tank (8), there is material inlet at the middle part of rectifying column, Lower Half has the agent of urgency charging aperture, the bottom of the tower tower bottoms discharging storage tank (8G) of ining succession, the top links to each other with condenser (2G), the other end of condenser connects diversion cans (3G), diversion cans must connect vavuum pump, to realize decompression distillation, a shunting of diversion cans flows to the rectifying column top, another shunting flows to distillate discharging storage tank (7), equally, urge agent recovery tower bottom to connect tower bottoms discharging storage tank (8H), the top links to each other with condenser (2H), the other end of condenser connects diversion cans (3H), diversion cans connects vavuum pump, one flows to the recovery tower top, another shunting flows to urges agent feed storage tank (5G) benzene with catalytic rectifying method quick-reading flow sheets as follows, the raw material that is contained in the raw material feed storage tank adds from the middle part of rectifying column, urge agent to urge agent feed storage tank (5G) from urging agent raw material feed storage tank (5Y) to flow into, enter rectifying column from the rectifying column Lower Half, what rectifying column was evaporated comprises that the mist of urging agent and separation component is after condenser (2G) condensation, through diversion cans (3G), part in the distillate flows back to rectifying column after preheating, a part flows into distillate discharging storage tank (7), enter again and urge agent recovery tower (4) to urge separating of agent and other component, the gas that recovery tower evaporates is through condenser (2H), diversion cans (3H), a part flows back to urges the agent recovery tower, and a part flows into urgency agent feed storage tank (5G) and recycles.The tower bottoms of rectifying column flows to tower bottoms discharging storage tank (8G), equally, urge the tower bottoms of agent recovery tower to flow to tower bottoms discharging storage tank (8H), as tower bottoms is one-component, can be used as product collects, as tower bottoms is non-one-component, can pump into raw material feed storage tank (6) again and further separate.
The separation condition of the separating mixed dimethyl benzene with catalytic rectifying method of embodiment 1--30 and separating resulting are listed in table 3 and table 4 respectively, " second " representative " ethylbenzene " in the table, " to " representative " right-dimethylbenzene ", " " representative "-dimethylbenzene ", " neighbour " representative " ortho-xylene ", agent is urged in " S " representative, C8 aromatic hydrocarbons is represented the component in the mixed xylenes, be other components except urging agent in the distillate, " A " is the tert-butyl alcohol, " B " is carbon tetrachloride, " C " is ethanol, " D " is methyl alcohol, " E " is isopropyl alcohol, " F " is sec-butyl alcohol, " G " is chloroform, " H " is triethylamine, " K " is butanone, " M " is ethyl acetate, " J " is n-butanol.
Table 3
| Embodiment | Raw material | The purpose component | Theoretical cam curve | Reflux ratio | Pressure (mmHg) | The still temperature (℃) | The top temperature (℃) | S | |
| Quantity (ml) | Form | ||||||||
| 1 | 185 | 25% pair, 75% | Right | 40 | 5～8 | 512 | 125 | 110 | B |
| 2 | 185 | 25% pair, 75% | Right | 40 | 5～8 | 514 | 126 | 110 | C |
| 3 | 500 | 19.5% second, 17.3% pair 59.0%, 22.2% neighbour | Second | 35 | 8～12 | 580 | 132 | 108 | B |
| 4 | 1000 | 77% second, 12.4% pair 10.6% | Second | 35 | 8～12 | 580 | 129 | 104 | B |
| 5 | 1000 | 19.5% second, 17.3% pair, 59.0%, 22.2 neighbours | Adjacent | 35 | 5～8 | 545 | 135 | 118 | B |
| 6 | 407 | 1.5% second, 30% pair, 68.5% | Right | 35 | 8～12 | 583 | 134 | 106 | B |
| 7 | 557 | 1.3% second, 55.5% pair, 43.2% | Right | 35 | 8～12 | 575 | 132 | 106 | B |
| 8 | 504 | 0.6% second, 75.8% pair 23.6% | Right | 35 | 8～12 | 587 | 132 | 108 | B |
| 9 | 505 | 0.2% second, 88.3% pair 11.5% | Right | 35 | 8～12 | 582 | 132 | 108 | B |
Continuous table 3
| 10 | 501 | 0.2% second, 93.8% pair, 6.0% | Right | 35 | 8～12 | 576 | 133 | 105 | B |
| 11 | 400 | 27.0% pair, 73% | Right | 35 | 5～8 | 573 | 133 | 108 | B |
| 12 | 505 | 76.3% pair, 23.7% | Right | 35 | 5～8 | 573 | 133 | 116 | B |
| 13 | 505 | 92.9% pair, 7.1% | Right | 35 | 5～8 | 573 | 133 | 116 | B |
| 14 | 394 | 66.7%, 33.3% neighbour | Between | 35 | 5～8 | 573 | 136～ 140 | 116 | B |
| 15 | 394 | 66.7%, 33.3% neighbour | Adjacent | 35 | 5～8 | 573 | 136～ 140 | 116 | B |
| 16 | 500 | 19.5% second, 21.0% pair, 39.3%, 20.2% neighbour | Second | 35 | 5～8 | 573 | 136～ 140 | 114 | C |
| 17 | 1000 | 74.9% second, 15.4% pair, 9.6%, 0.2% neighbour | Second | 35 | 5～8 | 573 | 136～ 140 | 114 | C |
| 18 | 500 | 66.7%, 33.39 neighbours | Between | 35 | 5～8 | 573 | 136～ 140 | 116 | C |
| 19 | 500 | 66.7%, 33.3% neighbour | Adjacent | 35 | 5～8 | 573 | 136～ 140 | 116 | C |
| 20 | 403 | 28.3% pair, 71.7% | Right | 35 | 5～8 | 573 | 135 | 116 | C |
Continuous table 3
| 21 | 402 | 42.7% pair, 51.3% | Right | 35 | 5～8 | 573 | 135 | 116 | C |
| 22 | 547 | 54.7% pair, 45.3% | Right | 35 | 5～8 | 573 | 135 | 116 | C |
| 23 | 140 | 2.3% second, 23.3% pair 46.5%, 27.8% neighbour | Right | 22 | 5～8 | 455 | 125 | 118 | D |
| 24 | 140 | The same | Right | 22 | 5～8 | 450 | 125 | 116 | E |
| 25 | 140 | The same | Right | 22 | 5～8 | 450 | 125 | 115 | F |
| 26 | 140 | The same | Right | 22 | 5～8 | 450 | 125 | 114 | G |
| 27 | 180 | 15.3% second, 22.8% pair, 55.5%, 6.4% neighbour | Right | 22 | 5～8 | 710 | 139 | 118 | H |
| 28 | 200 | The same | Right | 22 | 5～8 | 710 | 138 | 120 | K |
| 29 | 177 | The same | Right | 22 | 5～8 | 706 | 139 | 132 | M |
| 30 | 155 | The same | Right | 22 | 5～8 | 706 | 137 | 122 | J |
Table 4
| Embodiment | Distillate | Recovery rate (%) | Purity (%) | |
| S: C8 aromatic hydrocarbons (volume ratio) | C8 hydrocarbon amount (ml) | |||
| 1 | 1∶1 | 45 | 46.7 | |
| 2 | 1∶1 | 49 | 45.8 | |
| 3 | 1∶1 | 104 | 76.2 | 73.6 |
| 4 | 1∶1 | 748 | 94.3 | 97.0 |
| 5 | 1∶1 | 220 | 95.1 | 96.0 |
| 6 | 1∶1 | 155 | 68.8 | 54.0 |
| 7 | 1∶1 | 320 | 78.6 | 76.3 |
| 8 | 1∶1 | 314 | 69.7 | 84.8 |
| 9 | 1∶1 | 328 | 69.1 | 94.0 |
| 10 | 1∶1 | 468 | 96.0 | 96.4 |
| 11 | 1.5∶1 | 158 | 74.6 | 51.0 |
| 12 | 0.8∶1 | 400 | 90.1 | 88.0 |
| 13 | 0.8∶1 | 472 | 97.9 | 96.1 |
| 14 | 1.1∶1 | 254 | 95.1 | 99.6 |
| 15 | 1.1∶1 | 254 | 91.4 | 100 |
| 16 | 1.1∶1 | 109 | 81.0 | 72.5 |
Continuous table 4
| 17 | 1.1∶1 | 755 | 97.0 | 96.1 |
| 18 | 1.2∶1 | 317 | 94.8 | 99.6 |
| 19 | 1.2∶1 | 317 | 94.2 | 99.6 |
| 20 | 1.1∶1 | 157 | 56.8 | 41.6 |
| 21 | 1.5∶1 | 237 | 77.8 | 56.7 |
| 22 | 1.1∶1 | 309 | 68.7 | 66.5 |
| 23 | 1∶5 | 39 | 37.9 | 31.7 |
| 24 | 1∶5 | 40 | 40.1 | 32.7 |
| 25 | 1∶4 | 34 | 37.2 | 35.7 |
| 26 | 1∶4 | 36 | 39.7 | 36.0 |
| 27 | 1∶3 | 55.5 | 36.4 | 26.9 |
| 28 | 1∶3 | 66 | 37.8 | 26.1 |
| 29 | 1∶3 | 61 | 38.7 | 25.9 |
| 30 | 1∶1 | 52 | 43.0 | 29.2 |
Claims (7)
1, a kind ofly from mixed xylenes, efficiently isolate the neighbour, between, separation method---the benzene with catalytic rectifying of paraxylene and four kinds of high purity products of ethylbenzene, in whole rectifying separation process, needing it is characterized in that in destilling tower, adding a kind of urgency agent that can dissolve each other with separated mixture, the boiling point of urgency agent hangs down 10～100 ℃ than the boiling point of each component in the mixture that gives separation, urging agent is that Lower Half by destilling tower continuously joins in the separated mixture in the destilling tower and goes, and to be controlled at and to urge the volume ratio of agent and component be 1 to constituent content in the distillate: (0.5～3); The urgency agent comprises: the tert-butyl alcohol, carbon tetrachloride, ethanol, methyl alcohol, isopropyl alcohol, sec-butyl alcohol, chloroform, triethylamine, butanone or ethyl acetate; The benzene with catalytic rectifying separating mixed dimethyl divided for three steps carried out: the first step, isolate the ortho-xylene product and discharge from mixed xylenes by the tower still, distillate be ethylbenzene, right-dimethylbenzene ,-dimethylbenzene and urge the mixture of agent; Second step, from ethylbenzene, right-dimethylbenzene ,-dimethylbenzene and urge the mixture of agent and isolate ethylbenzene product, reclaim and urge agent; Tower bottoms be right-dimethylbenzene ,-xylene mixture; The 3rd step, from right-dimethylbenzene and-isolate the xylene mixture right-dimethylbenzene product and-the dimethylbenzene product, reclaim and urge agent, the urgency agent of reclaiming is recycled.
2, benzene with catalytic rectifying method as claimed in claim 1, the rectifying condition that it is characterized in that isolating from mixed xylenes ortho-xylene is as follows: theoretical cam curve is 30～75, reflux ratio is 3～8, tower top pressure is 500～760mmHg, tower still temperature is 130～148 ℃, tower top temperature is 110～130 ℃, distillate be ethylbenzene, right-dimethylbenzene ,-dimethylbenzene and urge agent, tower bottoms is the ortho-xylene product.
3, benzene with catalytic rectifying method as claimed in claim 1, it is characterized in that from contain ethylbenzene, right-dimethylbenzene and-the rectifying condition of isolating ethylbenzene the mixture of three kinds of components of dimethylbenzene is as follows: theoretical cam curve is 80～150, reflux ratio is 5～12, tower top pressure is 500～760mmHg, tower still temperature is 125～148 ℃, tower top temperature is 100～126 ℃, and distillate is for urging agent and ethylbenzene product, and tower bottoms is the mixture of right-dimethylbenzene and meta-xylene.
4, benzene with catalytic rectifying method as claimed in claim 1, it is characterized in that-dimethylbenzene right from containing and-mixture of two kinds of components of dimethylbenzene isolate right-dimethylbenzene and-the rectifying condition of two kinds of products of dimethylbenzene is as follows, total theoretical cam curve is 200～300, divides following two steps to carry out:
1.-dimethylbenzene right from containing and-mixture of two kinds of components of dimethylbenzene isolate between-dimethylbenzene: theoretical cam curve is 100～150, reflux ratio is 10～20, tower top pressure is 500～760mmHg, tower still temperature is 130～148 ℃, tower top temperature is 100～120 ℃, distillate is for urging agent and the thick product of right-dimethylbenzene, tower bottoms be between-the dimethylbenzene product;
2. from the thick product of right-dimethylbenzene, isolate right-diformazan benzin product, theoretical cam curve is 100～150, reflux ratio is 10～20, tower top pressure is 500～760mmHg, tower still temperature is 130～148 ℃, tower top temperature is 100～120 ℃, distillate is for urging agent and right-diformazan benzin product, the volume ratio of controlling both is 1: (0.5～3), by distillate recovery urgency agent wherein, and correspondingly obtain right-diformazan benzin product, tower bottoms as the 1. the raw material in step pump into the 1. the rectifying column in the step use.
5, benzene with catalytic rectifying method as claimed in claim 1 is characterized in that said urgency agent preferred tertiary butanols, carbon tetrachloride or ethanol.
6, the equipment that benzene with catalytic rectifying method as claimed in claim 1 is used, comprise rectifying column (1), condenser (2), diversion cans (3), raw material feed storage tank (6), distillate discharging storage tank (7), tower bottoms discharging storage tank (8), it is characterized in that equipment also comprises urgency agent feed storage tank (5), raw material adds from the middle part of rectifying column, urge agent to add from the Lower Half of rectifying column, what be evaporated in the rectifying column comprises that the mist of urging agent and other component is through condenser (2G), the distillate of diversion cans (3G) back gained, a part flows back to rectifying column after preheating, a part flows into distillate discharging storage tank.
7, benzene with catalytic rectifying equipment as claimed in claim 5, it is characterized in that said equipment also comprises urgency agent recovery tower (4), after said distillate flows into distillate discharging storage tank (7), enter and urge the agent recovery tower to urge separating of agent and other component, add gas that recovery tower is evaporated behind condenser (2H), diversion cans (3H), gained urges an agent part to flow back to recovery tower, and a part flows into urges agent feed storage tank (5G) to recycle.
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| CN94101274A CN1053386C (en) | 1994-01-28 | 1994-01-28 | Separating mixed dimethyl benzene with catalytic rectifying method |
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| CN102464556B (en) * | 2010-11-05 | 2014-01-08 | 中国石油化工股份有限公司 | Method for separating pseudocumene from C9 aromatic hydrocarbon |
| CN105016948B (en) * | 2014-04-16 | 2016-09-28 | 中国石化扬子石油化工有限公司 | A kind of separation ethylbenzene and method of o-Dimethylbenzene from dimethylbenzene |
| CN105732257B (en) * | 2016-03-28 | 2018-01-05 | 南京师范大学 | A kind of separation method of mixed xylenes |
| CN107324967A (en) * | 2016-04-28 | 2017-11-07 | 上海华谊工程有限公司 | A kind of technique of the separating paraxylene from mixed xylenes |
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|---|---|---|---|---|
| US4299668A (en) * | 1981-02-23 | 1981-11-10 | International Synthetic Rubber Co., Ltd. | Separation of ethylbenzene from para- and meta-xylenes by extractive distillation |
| RU2052490C1 (en) * | 1993-08-24 | 1996-01-20 | Брускин Юрий Александрович | Method of synthesis of lower olefins and benzene |
-
1994
- 1994-01-28 CN CN94101274A patent/CN1053386C/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4299668A (en) * | 1981-02-23 | 1981-11-10 | International Synthetic Rubber Co., Ltd. | Separation of ethylbenzene from para- and meta-xylenes by extractive distillation |
| RU2052490C1 (en) * | 1993-08-24 | 1996-01-20 | Брускин Юрий Александрович | Method of synthesis of lower olefins and benzene |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1105898A (en) | 1995-08-02 |
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