CN216236033U - Device for recovering bromine from bromination waste acid - Google Patents
Device for recovering bromine from bromination waste acid Download PDFInfo
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- CN216236033U CN216236033U CN202122829542.8U CN202122829542U CN216236033U CN 216236033 U CN216236033 U CN 216236033U CN 202122829542 U CN202122829542 U CN 202122829542U CN 216236033 U CN216236033 U CN 216236033U
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- bromine
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- waste acid
- bromination
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Abstract
The utility model relates to a device for recovering bromine from bromination reaction waste acid, which comprises a bromination reaction waste acid storage tank and an oxidant storage tank, wherein the bromination reaction waste acid storage tank and the oxidant storage tank are respectively connected with a waste acid metering tank and an oxidant metering tank, the waste acid metering tank and the oxidant metering tank are both connected with a microchannel reactor, an osmotic membrane is arranged in the microchannel reactor, and the microchannel reactor is sequentially connected with a gas-liquid separator, a liquid-liquid separator, a dryer and a bromine refined product storage tank. The device for recovering bromine from the bromination reaction waste acid converts various bromine-containing substances into bromine in one step, improves the comprehensive utilization rate of bromine atoms, has short reaction time, stable reaction process, high production efficiency and high safety, and can realize continuous production.
Description
Technical Field
The utility model belongs to the technical field of bromine recovery, and particularly relates to a device for recovering bromine from bromination reaction waste acid.
Background
Bromine or bromine-containing compounds are used for bromination reaction, and the method is widely applied to industries such as medicines, pesticides and flame retardants. In the process of producing decabromodiphenylethane by using bromine, the utilization rate of bromine atoms is only 50%, the other half of the bromine atoms exist in the tail gas absorption liquid in the form of HBr, and a large amount of bromine which cannot be separated by simple phase separation exists in the tail gas absorption liquid due to the volatility of the bromine. In addition, in the process of producing brominated polystyrene products by using bromine, a reducing agent is used for removing free bromine and hydrogen bromide in the products in the post-treatment process to generate a large amount of bromine-containing wastewater with the bromine content of 20-45%.
In the above bromine-containing wastewater, bromine is recovered from the bromine-containing wastewater by a distillation tower in the conventional method, and bromine atoms in the bromine-containing wastewater are recovered from high-concentration hydrobromic acid by a chlorine gas replacement method, but chlorine gas is used as a recovery reagent, wherein the chlorine gas is a highly toxic substance and is a national restricted substance.
CN201610967913.X discloses a method for separating bromine and hydrobromic acid by three-tower rectification, wherein the concentration of bromine recovered is more than 99%, the rectification method has high energy consumption, and the obtained high-purity hydrobromic acid still needs to be converted into bromine for reuse.
Disclosure of Invention
The utility model aims to provide a device for recovering bromine from bromination reaction waste acid, which converts various bromine-containing substances into bromine in one step, improves the comprehensive utilization rate of bromine atoms, has short reaction time, stable reaction process, high production efficiency and high safety, and can realize continuous production.
The technical scheme adopted by the utility model for solving the problems is as follows: a device for recovering bromine from bromination reaction waste acid comprises a bromination reaction waste acid storage tank and an oxidant storage tank, wherein the bromination reaction waste acid storage tank and the oxidant storage tank are respectively connected with a waste acid metering tank and an oxidant metering tank, the waste acid metering tank and the oxidant metering tank are both connected with a microchannel reactor, an osmotic membrane is arranged in the microchannel reactor, and the microchannel reactor is sequentially connected with a gas-liquid separator, a liquid-liquid separator, a dryer and a bromine refined product storage tank.
Preferably, an air floatation oil remover and a filter are connected between the bromination reaction waste acid storage tank and the waste acid metering tank.
Preferably, the liquid-liquid separator and the dryer are both connected with a waste water storage tank.
Preferably, the permeable membrane is a NaA molecular sieve membrane with pore size less than 0.42 nm.
Preferably, the microchannel structure in the microchannel reactor is one of a straight-flow channel, a flat channel with a rectangular cross section and a pulse variable diameter rectangular flat pipeline.
Compared with the prior art, the utility model has the advantages that:
(1) the utility model utilizes the microchannel reactor to recover bromine from the bromination waste acid, and carries out filtration and air flotation oil removal before recovery, so that impurities are effectively removed, the consumption of an oxidant is reduced, and the method is energy-saving and environment-friendly.
(2) The utility model adopts the microchannel reactor, and the waste acid metering tank and the oxidant metering tank are both connected with the microchannel reactor, so that the reaction materials can be instantly and uniformly mixed, the mass transfer and heat transfer efficiency is extremely high, the reaction period is greatly shortened, the oxidation reaction risk is reduced, the utilization rate of raw materials is improved, and the yield and the purity of the product are improved.
(3) The microchannel reactor is provided with the permeable membrane, so that part of water molecules can be removed during reaction, the reaction liquid tends to be saturated, and the reduction of the yield of the product caused by the disproportionation reaction of the generated bromine in water is avoided or reduced.
(4) The microchannel reactor is sequentially connected with the gas-liquid separator and the liquid-liquid separator, namely, the reaction liquid is sequentially subjected to gas-liquid separation to discharge non-condensable gas, and then the liquid phase is subjected to phase separation, so that the microchannel reactor is safer and more environment-friendly, avoids the new three wastes problem caused by introducing an extracting agent in the traditional aftertreatment, and is more suitable for industrial production.
Drawings
FIG. 1 is a schematic structural diagram of a device for recovering bromine from waste acid from bromination in the embodiment of the utility model.
Wherein, 1 is a bromination reaction waste acid storage tank, 2 is an oxidant storage tank, 3 is a waste acid metering tank, 4 is an oxidant metering tank, 5 is a microchannel reactor, 6 is a gas-liquid separator, 7 is a liquid-liquid separator, 8 is a dryer, 9 is a bromine refined product storage tank, 10 is an air flotation oil remover, 11 is a filter, and 12 is a waste water storage tank.
Detailed Description
The utility model is described in further detail below with reference to the accompanying examples.
As shown in fig. 1, the structure of the device for recovering bromine from waste acid of bromination reaction in the example is schematic.
The utility model provides a retrieve device of bromine in follow bromo reaction spent acid, includes bromo reaction spent acid storage tank 1, filter 11, air supporting degreaser 10 that connect gradually, air supporting degreaser 10 connects spent acid metering tank 3, and the device of retrieving bromine still includes oxidant storage tank 2, oxidant metering tank 4 is connected to oxidant storage tank 2, spent acid metering tank 3, oxidant metering tank 4 all are connected with microchannel reactor 5, be equipped with the osmotic membrane in microchannel reactor 5 (microchannel structure is straight-flow type passageway, and the heating medium is the conduction oil), the osmotic membrane is the NaA molecular sieve membrane that the aperture is less than 0.42nm, microchannel reactor 5 connects gradually vapour and liquid separator 6, liquid-liquid separator 7, desicator 8, bromine essence storage tank 9, liquid-liquid separator 7, desicator 8 all connects waste water storage tank 12.
The operation of this embodiment is described in detail below with reference to the accompanying drawings:
filtering bromine-containing waste acid in a bromine reaction waste acid storage tank 1 by a filter 11 to remove floccules or mechanical impurities in the bromine-containing waste acid, and removing oil from the filtered bromine-containing waste acid by air floatation by an air floatation oil remover 10 to remove oil substances in the bromine-containing waste acid; bromine-containing waste acid subjected to air floatation and oil removal and oxidant compressed air in an oxidant storage tank 2 respectively pass through a waste acid metering tank 3 and an oxidant metering tank 4 and then enter a microchannel reactor 5 for reaction, part of water molecules are discharged through a molecular sieve membrane with the aperture smaller than 0.42nmNaA on the wall of the microchannel in the reaction process, so that a reaction liquid tends to be saturated, the reduction of the product yield caused by the disproportionation reaction of the generated bromine in water is avoided or reduced, the microchannel reaction liquid is sequentially subjected to gas-liquid separation through a gas-liquid separator 6 to discharge non-condensable gas, then is subjected to phase separation through a liquid-liquid separator 7 to obtain a bromine crude product and waste water, the bromine crude product is dried through a dryer 8 to obtain bromine refined product and waste water, the bromine refined product is placed in a bromine refined product storage tank 9, and the waste water enters a waste water storage tank 12 for three-waste treatment.
In addition to the above embodiments, the present invention also includes other embodiments, and any technical solutions formed by equivalent transformation or equivalent replacement should fall within the scope of the claims of the present invention.
Claims (5)
1. A device for recovering bromine from bromination reaction waste acid is characterized in that: including bromo reaction spent acid storage tank (1), oxidant storage tank (2), spent acid metering tank (3), oxidant metering tank (4) are connected respectively to bromo reaction spent acid storage tank (1), oxidant storage tank (2), spent acid metering tank (3), oxidant metering tank (4) all are connected with microchannel reactor (5), be equipped with the osmotic membrane in microchannel reactor (5), microchannel reactor (5) connect gradually vapour and liquid separator (6), liquid-liquid separator (7), desicator (8), bromine essence storage tank (9).
2. The apparatus for recovering bromine from spent acid from bromination as claimed in claim 1, wherein: and an air floatation oil remover (10) and a filter (11) are also connected between the bromination reaction waste acid storage tank (1) and the waste acid metering tank (3).
3. The apparatus for recovering bromine from spent acid from bromination as claimed in claim 1, wherein: the liquid-liquid separator (7) and the dryer (8) are both connected with a waste water storage tank (12).
4. The apparatus for recovering bromine from spent acid from bromination as claimed in claim 1, wherein: the permeable membrane is a NaA molecular sieve membrane with the pore diameter less than 0.42 nm.
5. The apparatus for recovering bromine from spent acid from bromination as claimed in claim 1, wherein: the micro-channel structure in the micro-channel reactor is one of a direct-current channel, a flat channel with a rectangular cross section and a pulse variable-diameter rectangular flat pipeline.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202122829542.8U CN216236033U (en) | 2021-11-18 | 2021-11-18 | Device for recovering bromine from bromination waste acid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202122829542.8U CN216236033U (en) | 2021-11-18 | 2021-11-18 | Device for recovering bromine from bromination waste acid |
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| Publication Number | Publication Date |
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| CN216236033U true CN216236033U (en) | 2022-04-08 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN202122829542.8U Active CN216236033U (en) | 2021-11-18 | 2021-11-18 | Device for recovering bromine from bromination waste acid |
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2021
- 2021-11-18 CN CN202122829542.8U patent/CN216236033U/en active Active
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