CN105194899A - Variable-diameter rectifying device and method for separating methylbenzene-isobutylbenzene mixture - Google Patents
Variable-diameter rectifying device and method for separating methylbenzene-isobutylbenzene mixture Download PDFInfo
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- CN105194899A CN105194899A CN201510677224.0A CN201510677224A CN105194899A CN 105194899 A CN105194899 A CN 105194899A CN 201510677224 A CN201510677224 A CN 201510677224A CN 105194899 A CN105194899 A CN 105194899A
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- tower
- isobutylbenzene
- rectifying
- reducing
- methylbenzene
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- 239000000203 mixture Substances 0.000 title claims abstract description 34
- 238000000034 method Methods 0.000 title claims abstract description 23
- ODBZLWQDWXYVFQ-UHFFFAOYSA-N 2-methylpropylbenzene toluene Chemical compound CC1=CC=CC=C1.CC(C)CC1=CC=CC=C1 ODBZLWQDWXYVFQ-UHFFFAOYSA-N 0.000 title claims abstract description 15
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims abstract description 105
- KXUHSQYYJYAXGZ-UHFFFAOYSA-N isobutylbenzene Chemical compound CC(C)CC1=CC=CC=C1 KXUHSQYYJYAXGZ-UHFFFAOYSA-N 0.000 claims abstract description 42
- 238000000926 separation method Methods 0.000 claims abstract description 18
- 239000007788 liquid Substances 0.000 claims abstract description 11
- 238000010992 reflux Methods 0.000 claims description 10
- 239000012071 phase Substances 0.000 claims description 7
- 238000000605 extraction Methods 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 6
- 239000007791 liquid phase Substances 0.000 claims description 4
- 238000004821 distillation Methods 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims description 2
- 239000002994 raw material Substances 0.000 abstract description 3
- 238000000746 purification Methods 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- 238000009833 condensation Methods 0.000 description 9
- 230000005494 condensation Effects 0.000 description 9
- 238000004519 manufacturing process Methods 0.000 description 6
- 238000003786 synthesis reaction Methods 0.000 description 5
- 230000015572 biosynthetic process Effects 0.000 description 4
- 238000009835 boiling Methods 0.000 description 3
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 3
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 3
- 238000005804 alkylation reaction Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- HEFNNWSXXWATRW-UHFFFAOYSA-N Ibuprofen Chemical compound CC(C)CC1=CC=C(C(C)C(O)=O)C=C1 HEFNNWSXXWATRW-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000000498 cooling water Substances 0.000 description 1
- 229930007927 cymene Natural products 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- HFPZCAJZSCWRBC-UHFFFAOYSA-N p-cymene Chemical compound CC(C)C1=CC=C(C)C=C1 HFPZCAJZSCWRBC-UHFFFAOYSA-N 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 238000009834 vaporization Methods 0.000 description 1
- 230000008016 vaporization Effects 0.000 description 1
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to a variable-diameter rectifying device and a method for separating a methylbenzene-isobutylbenzene mixture and belongs to the field of chemical separation and purification. A variable-diameter tower body adopts a plate tower mechanism, is divided into upper and lower sections with different tower diameters according to the highest gas flow velocity, the upper section is a rectifying section, two round downcomers are arranged between tower plates inside the upper section, the lower section is a stripping section, two arch downcomers are arranged between tower plates inside the lower section, and the tower diameter of the rectifying section is smaller than that of the stripping section. After a methylbenzene-isobutylbenzene raw material liquid is separated by the variable-diameter rectifying device, methylbenzene with the concentration of 99.9% (in terms of the mass fraction) is obtained at the tower top, and isobutylbenzene with the concentration of 99% (in terms of the mass fraction) is obtained at the tower bottom. The device and the method have the advantages that single-tower operation is flexible, the equipment cost is saved due to different tower diameters, and the cost is substantially reduced; the two arranged downcomers can easily and effectively control all kinds of disturbance during rectifying separation.
Description
[technical field]
The present invention relates to being separated of a kind of toluene and isobutylbenzene mixture, particularly a kind of reducing rectifying separator and use the method for this device separation of methylbenzene and isobutylbenzene mixture, belong to chemical separating purification art.
[background technology]
Isobutylbenzene is mainly used in organic synthesis, is the primary raw material producing brufen.The alkylation process that the primary synthetic methods of isobutylbenzene is is raw material with toluene and propylene, there is phenyl ring alkylated reaction in the presence of acidic and generate cymene in toluene and propylene, then side chain alkylation reaction occurs under base catalyst exists and generates isobutylbenzene.Consider the relative toluene expensive of propylene price and difficult recycling, therefore the ingredient proportion of general toluene is excessive.There is part side reaction in building-up process, containing impurity in product, be wherein mainly the mixture of isobutylbenzene and toluene.
Between isobutyl Benzene and Toluene, this does not form azeotropic, still-process can realize being separated in principle, but there is the problems such as steam consumption is large, cooling water amount is large, automatization level is low, manpower consumption is many, adopt continuous rectification separating technology to be separated the synthesis liquid that isobutylbenzene synthesis procedure produces so general.
Rectifying column tower diameter mainly determines according to the empty tower gas velocity of gas phase, when the gas phase load of full tower each several part is more or less the same, can realize the separation of mixture with isometrical rectifying column.But when the upper and lower gas phase load of feed plate differs greatly, as cold liquid charging, common rectifying column equipment cost is higher, can adopt reducing tower, strengthen the operability of tower, reduce cost of equipment.
Patent (104258687A) proposes a kind of toluene recovery device, and comprise some absorption towers, steam generator, some condensers, separator box and air accumulator, its recovery utilization rate reaches 99%.This device can obtain the toluene of higher degree, but equipment relative complex, complex steps.
[summary of the invention]
[technical problem that will solve]
The object of this invention is to provide the reducing rectifier unit of a kind of separation of methylbenzene-isobutylbenzene mixture.
Another object of the present invention is to provide a kind of method using described device separation of methylbenzene-isobutylbenzene mixture.
The present invention overcomes the deficiencies in the prior art, proposes reducing rectifier unit and the method for a kind of separation of methylbenzene-isobutylbenzene mixture.To give vent to anger the larger situation of liquid phase load difference for feedboard, adopt the method for reducing rectifying to realize effective separation of mixture.
The present invention is achieved through the following technical solutions: the reducing rectifier unit of a kind of separation of methylbenzene-isobutylbenzene mixture, tower body adopts plate column mechanism, be divided into two sections, epimere is rectifying section, between inner column plate, two circular downeomers are set, hypomere is stripping section, and arrange two chord downcomers between inner column plate, rectifying section tower diameter is less than stripping section tower diameter;
The method of this reducing rectifier unit separation of methylbenzene-isobutylbenzene mixture is adopted to comprise the steps:
(1) material liquid of toluene and isobutylbenzene mixture is from the charging of reducing tower reducing;
(2) feeding temperature is 20-50 DEG C, and material liquid high-purity toluene product after reducing tower is separated presses certain reflux ratio extraction from tower top after condenser condenses, then utilizes as the feedstock circulation of synthesis isobutylbenzene after condenser system condensation;
(3) highly purified isobutylbenzene product enters in tower through tower reactor reboiler heating rear section gas phase and continues to be separated, and liquid phase is as product extraction.
According to another preferred embodiment of the present invention, it is characterized in that: the operating pressure of reducing tower is 1atm; Reflux ratio is 0.1-0.5; The rectifying section number of plates is 8-16 block, tower diameter 200-400mm; The stripping section number of plates is 12-18 block, tower diameter 300-600mm.
According to another preferred embodiment of the present invention, it is characterized in that: tower top temperature 110-121 DEG C after rectifying, obtain the high-purity toluene that mass fraction is 99.9%; Bottom temperature 177-180 DEG C, obtains the isobutylbenzene that mass fraction is 99%.
The reducing rectifier unit of the present invention's a kind of separation of methylbenzene-isobutylbenzene mixture and the specific descriptions of method as follows:
Toluene and isobutylbenzene material liquid are from the charging of reducing tower reducing, and that laminate of charging is called feed plate, is rectifying section, (comprises feed plate) and be called stripping section below feed plate above feed plate; Feeding temperature is 20-50 DEG C.Cold liquid charging, for material liquid is heated to temperature on plate, will inevitably some be fewer than the vapor volume of stripping section, therefore rectifying section tower diameter is less than stripping section tower diameter; Liquid mixture carries out repeatedly components vaporize, simultaneously again the steam repeatedly partial condensation produced, because the boiling point of isobutyl Benzene and Toluene is different, when its at a certain temperature components vaporize time, toluene boiling point is relatively low is easy to vaporization, therefore toluene concentration is higher in gas phase, and in liquid phase, due to isobutylbenzene boiling point relatively high event isobutylbenzene concentration, comparatively gas phase is high; Final toluene from overhead extraction, after condenser system condensation as synthesis isobutylbenzene feedstock circulation utilize, isobutylbenzene as final products from tower reactor extraction.
The invention has the advantages that, compared with traditional rectifying column, adopt reducing tower distillation separation of methylbenzene-isobutylbenzene mixture, single tower flexible operation, be separated and obtain high-purity isobutyl Benzene and Toluene; Reducing tower adopts different tower diameters according to gas flow rate, saves cost of equipment, considerably reduces cost; Device adopts two downspouts, and the various disturbances be easy to occurring in rectifying separation process control.
[accompanying drawing explanation]
Fig. 1 is the flow chart utilizing the rectifying of reducing tower to be separated isobutylbenzene-toluene, and Fig. 2 is tower partial, detailed view, wherein:
T-reducing tower; D-condenser; C-condenser system; R-reboiler; A-rectifying section; B-circular downeomer; E-stripping section; F-chord downcomer.
The each logistics of numeral.
[detailed description of the invention]
Below in conjunction with specific embodiment, the present invention will be further described.
Embodiment 1: produce the mixture of 5t containing isobutyl Benzene and Toluene in isobutylbenzene production process, inlet amount is 1t/h, completes process in 5 hours.Feeding temperature is 25 DEG C, and reflux ratio is 0.25, rectifying section 10 blocks of column plates, and tower diameter is 200mm, and stripping section 13 blocks of column plates, tower diameter is 350mm.Mixture is separated through reducing rectifying, obtains the toluene that concentration is 99.9% (mass fraction), obtain the isobutylbenzene that concentration is 99% (mass fraction) at the bottom of tower after overhead condensation.
Embodiment 2: produce the mixture of 5t containing isobutyl Benzene and Toluene in isobutylbenzene production process, inlet amount is 1t/h, completes process in 5 hours.Feeding temperature is 40 DEG C, and reflux ratio is 0.2, rectifying section 9 blocks of column plates, and tower diameter is 200mm, and stripping section 11 blocks of column plates, tower diameter is 330mm.Mixture is separated through reducing rectifying, obtains the toluene that concentration is 99.9% (mass fraction), obtain the isobutylbenzene that concentration is 99% (mass fraction) at the bottom of tower after overhead condensation.
Embodiment 3: produce the mixture of 10t containing isobutyl Benzene and Toluene in isobutylbenzene production process, inlet amount is 2t/h, completes process in 5 hours.Feeding temperature is 25 DEG C, and reflux ratio is 0.3, rectifying section 12 blocks of column plates, and tower diameter is 300mm, and stripping section 13 blocks of column plates, tower diameter is 500mm.Mixture is separated through reducing rectifying, obtains the toluene that concentration is 99.9% (mass fraction), obtain the isobutylbenzene that concentration is 99% (mass fraction) at the bottom of tower after overhead condensation.
Embodiment 4: produce the mixture of 10t containing isobutyl Benzene and Toluene in isobutylbenzene production process, inlet amount is 2t/h, completes process in 5 hours.Feeding temperature is 40 DEG C, and reflux ratio is 0.4, rectifying section 13 blocks of column plates, and tower diameter is 300mm, and stripping section 14 blocks of column plates, tower diameter is 500mm.Mixture is separated through reducing rectifying, obtains the toluene that concentration is 99.9% (mass fraction), obtain the isobutylbenzene that concentration is 99% (mass fraction) at the bottom of tower after overhead condensation.
Embodiment 5: produce the mixture of 30t containing isobutyl Benzene and Toluene in isobutylbenzene production process, inlet amount is 3t/h, completes process in 10 hours.Feeding temperature is 25 DEG C, and reflux ratio is 0.42, rectifying section 15 blocks of column plates, and tower diameter is 350mm, and stripping section 17 blocks of column plates, tower diameter is 600mm.Mixture is separated through reducing rectifying, obtains the toluene that concentration is 99.9% (mass fraction), obtain the isobutylbenzene that concentration is 99% (mass fraction) at the bottom of tower after overhead condensation.
Embodiment 6: produce the mixture of 30t containing isobutyl Benzene and Toluene in isobutylbenzene production process, inlet amount is 3t/h, completes process in 10 hours.Feeding temperature is 40 DEG C, and reflux ratio is 0.38, rectifying section 14 blocks of column plates, and tower diameter is 400mm, and stripping section 16 blocks of column plates, tower diameter is 550mm.Mixture is separated through reducing rectifying, obtains the toluene that concentration is 99.9% (mass fraction), obtain the isobutylbenzene that concentration is 99% (mass fraction) at the bottom of tower after overhead condensation.
Claims (3)
1. the reducing rectifier unit of separation of methylbenzene-isobutylbenzene mixture and method, it is characterized in that: equipment therefor is reducing rectifying column, tower body adopts plate column mechanism, be divided into two sections, epimere is rectifying section, arranges two circular downeomers between inner column plate, and hypomere is stripping section, arrange two chord downcomers between inner column plate, rectifying section tower diameter is less than stripping section tower diameter;
The method of this distillation separation of methylbenzene and isobutylbenzene mixture comprises the steps:
(1) toluene and isobutylbenzene mixture material liquid are from the charging of reducing tower reducing:
(2) feeding temperature is 20-50 DEG C, and material liquid high-purity toluene product after reducing tower is separated presses certain reflux ratio extraction from tower top after condenser condenses;
(3) highly purified isobutylbenzene product enters in tower through tower reactor reboiler heating rear section gas phase and continues to be separated, and liquid phase is as product extraction.
2. the reducing rectifier unit of a kind of separation of methylbenzene-isobutylbenzene mixture according to claim 1 and method, is characterized in that: reducing tower operating pressure is 1atm; Reflux ratio is 0.1-0.5; The rectifying section number of plates is 8-16 block, tower diameter 200-400mm; The stripping section number of plates is 12-18 block, tower diameter 300-600mm.
3. the reducing rectifier unit of a kind of separation of methylbenzene-isobutylbenzene mixture according to claim 1 and method, is characterized in that: tower top temperature 110-121 DEG C after rectifying, obtain the high-purity toluene that mass fraction is 99.9; Bottom temperature 177-180 DEG C, obtains the isobutylbenzene that mass fraction is 99%.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510677224.0A CN105194899A (en) | 2015-10-16 | 2015-10-16 | Variable-diameter rectifying device and method for separating methylbenzene-isobutylbenzene mixture |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108211405A (en) * | 2016-12-21 | 2018-06-29 | 中国石油化工股份有限公司 | Alkylated reaction device and alkylated reaction separation method |
| CN111167146A (en) * | 2019-12-26 | 2020-05-19 | 重庆市中润化学有限公司 | NMP waste liquid is retrieved with dehydration tower |
| CN111265902A (en) * | 2020-03-09 | 2020-06-12 | 内蒙古兰格生物科技有限公司 | Continuous rectification device |
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2015
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108211405A (en) * | 2016-12-21 | 2018-06-29 | 中国石油化工股份有限公司 | Alkylated reaction device and alkylated reaction separation method |
| CN108211405B (en) * | 2016-12-21 | 2024-03-12 | 中国石油化工股份有限公司 | Alkylation reaction device and alkylation reaction separation method |
| CN111167146A (en) * | 2019-12-26 | 2020-05-19 | 重庆市中润化学有限公司 | NMP waste liquid is retrieved with dehydration tower |
| CN111265902A (en) * | 2020-03-09 | 2020-06-12 | 内蒙古兰格生物科技有限公司 | Continuous rectification device |
| CN111265902B (en) * | 2020-03-09 | 2023-04-21 | 内蒙古兰格生物科技有限公司 | Continuous rectifying device |
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Application publication date: 20151230 |