CN208166890U - Interval catalytic reaction rectification prepares the device of dibutyl phthalate - Google Patents
Interval catalytic reaction rectification prepares the device of dibutyl phthalate Download PDFInfo
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- CN208166890U CN208166890U CN201820491916.5U CN201820491916U CN208166890U CN 208166890 U CN208166890 U CN 208166890U CN 201820491916 U CN201820491916 U CN 201820491916U CN 208166890 U CN208166890 U CN 208166890U
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Abstract
The utility model relates to the devices that a kind of interval catalytic reaction rectification prepares dibutyl phthalate, including reactive distillation column (C1), the first tower reactor (T1), the second tower reactor (T2), circulating pump (P1), condenser (E1), phase separation tank (D)；The middle and upper part reactive distillation column (C1), middle part, lower part are respectively equipped with gas-liquid distributor, catalyst sulfonate resin is filled in gas-liquid distributor, the first tower reactor (T1) and the second tower reactor (T2) middle part, lower part are equipped with the bed of loading catalyst resin；In reactive distillation column (C1), tower top is provided with gaseous phase outlet, and reactive distillation column (C1) tower body is from top to bottom respectively arranged with butanol refluxing opening, tower reactor fluid inlet, two tower lower part gas phase imports, tower bottom extraction mouth；Liquid phase entrance is provided at the top of phase separation tank (D), top is equipped with butanol bypass outlet, and bottom is equipped with water phase and produces mouth.Method described in the utility model solves prior art seriously corroded, and side reaction is more, the more problem of waste water, and the utility model simple process is controllable, the more low advantage of wastewater through organic matter content.
Description
Technical field
The utility model belongs to the technical field of catalytic reaction rectification, and in particular to a kind of interval catalytic reaction rectification preparation
The device of dibutyl phthalate.
Background technique
Dibutyl phthalate (DBP) is a kind of good plasticizer, is current most widely used plasticizer, accounts for about
The 75% of whole plasticizer yield has very strong solvability for various kinds of resin, is mainly used for the processing of polyvinyl chloride, makes
Product softness is good；For cellulose nitrate coating, there are good emollescence and excellent stability, resistance to deflection, glues
Property, waterproofness；Also act as the plasticizer of vinyl acetate, alkyd resin, ethyl cellulose and neoprene.
Currently, domestic common synthetic method is esterified under effect of sulfuric acid by phthalic anhydride and n-butanol,
Although sulfuric acid is inexpensive, technical maturity, product yield are higher, easily cause side reaction, seriously corroded, there are three-waste pollutions and product
The disadvantages of quality is difficult to control.The master operation of DBP production has esterification, neutralizes washing, dealcoholysis, filtering, wastewater treatment, recycles alcohol
Processing etc..Generating process generates waste water and brings water and neutralization, washing water into from chemical reaction generation water, raw materials for production.Waste water
Composition is more complicated, inside there is DBP, phthalic acid, two octanoic acid of adjacent benzene, sodium sulphate, free H2SO4, the pungent vinegar of adjacent benzene list, only son's vinegar
Equal chemical analysis give up impurities in water based on organic matter.
It is more more and more urgent to the cleaning generation demand of dibutyl phthalate with the raising that Environmental Protection in China requires, it needs
The problem of being directed to traditional batch production process, a kind of DBP production technology of efficient environmental protection is developed, improves product
Yield and conversion ratio reduce waste water yield, are all extremely important for society and enterprise.
Utility model content
The utility model develops a kind of environmental protection, product yield for the more problem of the more sewage yield of side reaction
The device that dibutyl phthalate is prepared with the interval catalytic reaction rectification of high conversion rate carries out traditional esterifications reaction process
It improves.
The utility model solves technical solution used by above-mentioned technical problem：
A kind of interval catalytic reaction rectification prepares the device of dibutyl phthalate, including reactive distillation column (C1),
One tower reactor (T1), the second tower reactor (T2), circulating pump (P1), condenser (E1), phase separation tank (D)；The middle and upper part reactive distillation column (C1),
Middle part, lower part are respectively equipped with gas-liquid distributor, and catalyst sulfonate resin, the first tower reactor (T1) and are filled in gas-liquid distributor
Two tower reactors (T2) middle part, lower part are equipped with the bed of loading catalyst resin；
In reactive distillation column (C1), tower top is provided with gaseous phase outlet, and reactive distillation column (C1) tower body is from top to bottom set respectively
It is equipped with butanol refluxing opening, tower reactor fluid inlet, two tower lower part gas phase imports, tower bottom extraction mouth；
Liquid phase entrance is provided at the top of phase separation tank (D), top is equipped with butanol bypass outlet, and bottom is equipped with water phase and produces mouth；
Gaseous phase outlet is set at the top of the first tower reactor (T1) and the second tower reactor (T2), and fluid inlet, bottom setting is arranged in top
Liquid-phase outlet；
The outlet of reactive distillation column (C1) top gaseous phase is connect with condenser (E1), condenser (E1) outlet connection phase separation tank
(D) liquid phase entrance, phase separation tank (D) upper outlet are connect with the top reactive distillation column (C1) butanol refluxing opening, reactive distillation column
(C1) gas phase entrance in lower part is connect with the first tower reactor (T1) and the second tower reactor (T2) gaseous phase outlet respectively, reactive distillation column (C1)
Bottom liquid phases outlet connect respectively with the fluid inlet of the first tower reactor (T1) and the top the second tower reactor (T2), the first tower reactor (T1) and
The outlet of second tower reactor (T2) bottom liquid phases is connect with reflux pump (P1) entrance, in reflux pump (P1) outlet and reactive distillation column (C1)
The connection of portion's tower reactor fluid inlet.
The advantages of the utility model and good effect are as follows：
The utility model is to replace sulfuric acid as catalyst using sulfonate resin, and reactive distillation column replaces stirred autoclave,
The side reaction in reaction process is reduced, reaction and dehydration is integrated with, avoids neutralization water-washing process, reduced wastewater flow rate.
Method described in the utility model solves prior art seriously corroded, and side reaction is more, the more problem of waste water,
And the utility model simple process is controllable, the more low advantage of wastewater through organic matter content.
Detailed description of the invention
Fig. 1 is the process flow that the utility model interval catalytic reaction rectification prepares dibutyl phthalate.
C1- reactive distillation column, E1- condenser, T1- tower reactor, T2- tower reactor, D- phase separation tank, P1- circulating pump, Z1- valve,
Z2- valve, Z3- valve, Z4- valve；
Liquid explanation in pipeline：1- condensate liquid, 2- reflux butanol, 3- produce water phase, 4- tower reactor liquid phase, 5- tower reactor gas
Phase, 6- tower reactor gas phase, 7- reactive distillation column tower bottom liquid phase, 8- reactive distillation column tower bottom liquid phase, 9- tower reactor liquid phase, 10- tower bottoms
Phase.
Specific embodiment
Technical solutions of the utility model are described in detail below, specific embodiment described herein is only to explain
The utility model, but the protection scope of the utility model is not limited to the embodiment.
A kind of interval catalytic reaction rectification prepares the device of dibutyl phthalate, including reactive distillation column C1, first
Tower reactor T1, the second tower reactor T2, circulating pump P1, condenser E1, phase separation tank D, valve Z1, valve Z2, valve Z3, valve Z4；Reaction
Upper, middle and lower is respectively equipped with the gas-liquid distributor for being filled with catalyst sulfonate resin, the first tower reactor T1 and the second tower reactor in rectifying column C1
The middle and lower part T2 is equipped with the bed of loading catalyst resin；
In reactive distillation column C1, tower top is provided with gaseous phase outlet, from top to bottom, is respectively arranged with butanol refluxing opening, tower reactor
Fluid inlet, the gas phase import of tower lower part, tower bottom produce mouth；Liquid phase entrance is provided at the top of phase separation tank D, top is flowed back equipped with butanol
Outlet, bottom are equipped with water phase and produce mouth；Gaseous phase outlet is set at the top of the first tower reactor T1 and T2, and fluid inlet, bottom is arranged in top
Liquid-phase outlet is set；The outlet of reactive distillation column C1 top gaseous phase is connect with condenser E1, the outlet condenser E1 connection phase separation tank D liquid
Phase entrance, phase separation tank D upper outlet are connect with the top reactive distillation column C1 butanol refluxing opening, and the lower part reactive distillation column C1 gas phase enters
Mouth is connect with the first tower reactor T1 and T2 gaseous phase outlet, the outlet of reactive distillation column C1 bottom liquid phases and the first top tower reactor T1 and T2
Fluid inlet connection, the outlet of the first tower reactor T1 and T2 bottom liquid phases are connect with reflux pump P1 entrance, and reflux pump P1 is exported and reacted
The top rectifying column C1 tower bottoms phase import connection.
The method that above-mentioned apparatus uses, includes the following steps：
Valve Z1 and Z4 are closed, and valve Z2 and Z3 are opened, the phthalic anhydride and butanol (mass ratio 1 in the first tower reactor T1:1.4) add
Heat carries out esterification to 140 DEG C in catalyst bed；The reacted rectifying column lower part gas phase of gas phase of first tower reactor T1 gasification
Import enters in synthesis under normal pressure rectifying column C1, and liquid phase enters the top reactive distillation column C1 tower reactor by circulating pump P1 in the first tower reactor T1
Fluid inlet, phthalic anhydride and butanol mixture carry out esterification in the catalyst bed of distributor；The moisture and butanol of generation
It forms azeotropic mixture and enters split-phase in phase separation tank D after overhead condenser E1 is cooling, the butanol after split-phase is back to reactive distillation column
In C1, continue to react, water phase is produced from the bottom phase separation tank D；Reactive distillation column C1 bottom product is into the second tower reactor T2's
Fluid inlet, the temperature of the second tower reactor T2 is controlled at 140 DEG C, so that mixture continues in the catalyst bed of the second tower reactor T2
It is reacted, whole process is until the feed liquid in the first tower reactor T1 fully enters in reactive distillation column.Later close valve Z2 and
Z3 opens valve Z1 and Z4, and the feed liquid in the second tower reactor T2 carries out above-mentioned reaction process as reaction raw materials, so circulation behaviour
Make, until the reaction is complete.
Using the preparation embodiment 1 of above-mentioned apparatus
Valve Z1 and Z4 are closed, and valve Z2 and Z3 are opened, the phthalic anhydride and butanol in the first tower reactor T1, mass ratio 1:1.4,
It is heated to 140 DEG C in tower reactor, and carries out esterification in catalyst bed；The reacted rectifying of gas phase of first tower reactor T1 gasification
The gas phase import of tower lower part enters in reactive distillation column C1, and liquid phase enters reactive distillation column C1 by circulating pump P1 in the first tower reactor T1
Top tower bottoms phase import, reactive distillation column rectifying tower packing be screen waviness structured packing, atmospheric operation, number of theoretical plate 12,
Phthalic anhydride and butanol mixture carry out esterification in the catalyst bed of distributor；The moisture and butanol of generation form azeotropic mixture
(feature is water content 16%, butanol amount 83%) enters split-phase in phase separation tank D, the fourth after split-phase after overhead condenser E1 is cooling
In alcohol reflux to reactive distillation column C1, continue to react, water phase is produced from the bottom phase separation tank D；Is produced from the bottom reactive distillation column C1
Object enters the fluid inlet of the second tower reactor T2, and the temperature of the second tower reactor T2 is controlled at 140 DEG C, so that mixture continues in the second tower
It is reacted in the catalyst bed of kettle T2, whole process is until the feed liquid in the first tower reactor T1 fully enters reactive distillation column
In.Valve Z2 and Z3 are closed later, opens valve Z1 and Z4, and the feed liquid in the second tower reactor T2 carries out above-mentioned as reaction raw materials
Reaction process, such circulate operation, equipment continuous operation 2h, until the reaction is complete, finally obtained product purity are 99.7%.
Using the preparation embodiment 2 of above-mentioned apparatus
Valve Z1 and Z4 are closed, and valve Z2 and Z3 are opened, the phthalic anhydride and butanol in the first tower reactor T1, mass ratio 1:1.4,
It is heated to 150 DEG C in tower reactor, and carries out esterification in catalyst bed；The reacted rectifying of gas phase of first tower reactor T1 gasification
The gas phase import of tower lower part enters in reactive distillation column C1, and liquid phase enters reactive distillation column C1 by circulating pump P1 in the first tower reactor T1
Top tower bottoms phase import, reactive distillation column rectifying tower packing be screen waviness structured packing, atmospheric operation, number of theoretical plate 12,
Phthalic anhydride and butanol mixture carry out esterification in the catalyst bed of distributor；The moisture and butanol of generation form azeotropic mixture
(feature is water content 16%, butanol amount 83%) enters split-phase in phase separation tank D, the fourth after split-phase after overhead condenser E1 is cooling
In alcohol reflux to reactive distillation column C1, continue to react, water phase is produced from the bottom phase separation tank D；Is produced from the bottom reactive distillation column C1
Object enters the fluid inlet of the second tower reactor T2, and the temperature of the second tower reactor T2 is controlled at 150 DEG C, so that mixture continues in the second tower
It is reacted in the catalyst bed of kettle T2, whole process is until the feed liquid in the first tower reactor T1 fully enters reactive distillation column
In.Valve Z2 and Z3 are closed later, opens valve Z1 and Z4, and the feed liquid in the second tower reactor T2 carries out above-mentioned as reaction raw materials
Reaction process, such circulate operation, equipment continuous operation 2h, until the reaction is complete, finally obtained product purity are 99.8%.
Claims (3)
1. the device that a kind of interval catalytic reaction rectification prepares dibutyl phthalate, it is characterised in that：Including reactive distillation
Tower (C1), the first tower reactor (T1), the second tower reactor (T2), circulating pump (P1), condenser (E1), phase separation tank (D)；Reactive distillation column
(C1) middle and upper part, middle part, lower part are respectively equipped with gas-liquid distributor, are filled with catalyst sulfonate resin in gas-liquid distributor, and first
Tower reactor (T1) and the second tower reactor (T2) middle part, lower part are equipped with the bed of loading catalyst resin；
In reactive distillation column (C1), tower top is provided with gaseous phase outlet, and reactive distillation column (C1) tower body is from top to bottom respectively arranged with
Butanol refluxing opening, tower reactor fluid inlet, two tower lower part gas phase imports, tower bottom produce mouth；
Liquid phase entrance is provided at the top of phase separation tank (D), top is equipped with butanol bypass outlet, and bottom is equipped with water phase and produces mouth；
Gaseous phase outlet is set at the top of the first tower reactor (T1) and the second tower reactor (T2), and fluid inlet is arranged in top, and liquid phase is arranged in bottom
Outlet；
The outlet of reactive distillation column (C1) top gaseous phase is connect with condenser (E1), condenser (E1) outlet connection phase separation tank (D) liquid
Phase entrance, phase separation tank (D) upper outlet are connect with the top reactive distillation column (C1) butanol refluxing opening, the lower part reactive distillation column (C1)
Gas phase entrance is connect with the first tower reactor (T1) and the second tower reactor (T2) gaseous phase outlet respectively, and reactive distillation column (C1) bottom liquid phases go out
Mouth is connect with the fluid inlet of the first tower reactor (T1) and the top the second tower reactor (T2) respectively, the first tower reactor (T1) and the second tower reactor
(T2) bottom liquid phases outlet is connect with reflux pump (P1) entrance, reflux pump (P1) outlet and the top reactive distillation column (C1) tower bottoms
Phase import connection.
2. interval catalytic reaction rectification according to claim 1 prepares the device of dibutyl phthalate, feature exists
In：The lower part reactive distillation column (C1) gas phase entrance respectively with the first tower reactor (T1) and the second tower reactor (T2) gaseous phase outlet connecting pipe
On valve is installed.
3. interval catalytic reaction rectification according to claim 1 prepares the device of dibutyl phthalate, feature exists
In：Valve is installed in first tower reactor (T1) and the outlet of the second tower reactor (T2) bottom liquid phases and reflux pump (P1) entrance connecting pipe
Door.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201820491916.5U CN208166890U (en) | 2018-04-09 | 2018-04-09 | Interval catalytic reaction rectification prepares the device of dibutyl phthalate |
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|---|---|---|---|
| CN201820491916.5U CN208166890U (en) | 2018-04-09 | 2018-04-09 | Interval catalytic reaction rectification prepares the device of dibutyl phthalate |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108456139A (en) * | 2018-04-09 | 2018-08-28 | 石家庄白龙化工股份有限公司 | A kind of interval catalytic reaction rectification prepares the device and method of dibutyl phthalate |
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2018
- 2018-04-09 CN CN201820491916.5U patent/CN208166890U/en active Active
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108456139A (en) * | 2018-04-09 | 2018-08-28 | 石家庄白龙化工股份有限公司 | A kind of interval catalytic reaction rectification prepares the device and method of dibutyl phthalate |
| CN108456139B (en) * | 2018-04-09 | 2024-01-30 | 石家庄白龙化工股份有限公司 | Device and method for preparing dibutyl phthalate by batch catalytic reaction rectification |
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