CN208546984U - A kind of pre-processing device of Antimonous Oxide from Wasted Antimonic Chloride Catalyst - Google Patents
A kind of pre-processing device of Antimonous Oxide from Wasted Antimonic Chloride Catalyst Download PDFInfo
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- CN208546984U CN208546984U CN201821014977.9U CN201821014977U CN208546984U CN 208546984 U CN208546984 U CN 208546984U CN 201821014977 U CN201821014977 U CN 201821014977U CN 208546984 U CN208546984 U CN 208546984U
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Abstract
The utility model discloses a kind of pre-processing devices of Antimonous Oxide from Wasted Antimonic Chloride Catalyst, mainly solving the technical problems that lacking the problem of carrying out pretreated equipment to Antimonous Oxide from Wasted Antimonic Chloride Catalyst in the prior art, the utility model passes through a kind of pre-processing device of Antimonous Oxide from Wasted Antimonic Chloride Catalyst, including reactor, the reactor connects rectifying column, the rectifying column connects catalyst treatment tank, the catalyst treatment tank connects knockout drum, the knockout drum connection washing unit, the washing unit connects caustic wash unit, the technical solution of the caustic wash unit connection incinerator, preferably solves the problems, such as this, it can be used for the pretreatment of Antimonous Oxide from Wasted Antimonic Chloride Catalyst.
Description
Technical field
The utility model relates to a kind of pre-processing devices of Antimonous Oxide from Wasted Antimonic Chloride Catalyst.
Background technique
In HFC-245fa production technology, it is liquid-phase catalyst fluoride process that technique, which can be used, according to Antimony pentachloride as urging
Agent, catalyst become dead catalyst because of inactivation, and complicated component mainly contains halogenated hydrocarbon, fluorinated hydrocarbons, hydrogen fluoride, chlorination
Hydrogen etc., effect on environment is big, belongs to hazardous waste, properly must dispose or comprehensively utilize.There are many methods and specialized company can at present
To carry out recycling treatment to Antimonous Oxide from Wasted Antimonic Chloride Catalyst.But contain hydrogen fluoride, organic matter in Antimonous Oxide from Wasted Antimonic Chloride Catalyst,
Wherein the corrosivity of hydrogen fluoride is very strong, and organic matter is burned and is unable to direct emission, otherwise can generate serious ring
Border pollution, while there are also moieties facile hydrolysis, and acidic materials can be generated after hydrolysis, it may have corrosivity, so processing pentachloro-
Change that antimony dead catalyst is very high to equipment requirement and incinerator with incinerator etc, however recycles company and not necessarily have
So good equipment handles Antimonous Oxide from Wasted Antimonic Chloride Catalyst, thus Antimonous Oxide from Wasted Antimonic Chloride Catalyst be transferred to recycling company it
It is preceding to be pre-processed.
Utility model content
The technical problems to be solved in the utility model is to lack to locate Antimonous Oxide from Wasted Antimonic Chloride Catalyst in advance in the prior art
The problem of equipment of reason, a kind of pre-processing device of new Antimonous Oxide from Wasted Antimonic Chloride Catalyst is proposed, which has removing pentachloro-
The characteristics of changing the impurity such as organic matter and hydrogen fluoride in antimony dead catalyst.
In order to solve the above-mentioned technical problem, the technical solution adopted in the utility model is as follows: a kind of useless catalysis of Antimony pentachloride
The pre-processing device of agent, including catalyst treatment tank, the catalyst treatment tank connect organic matter processing unit, the catalyst
Process tank connects knockout drum, and the knockout drum connection washing unit, the washing unit connects caustic wash unit, described
Caustic wash unit connects incinerator.
Further, it is preferable that the washing unit includes and the tank connected water scrubber of the gas-liquid separation, the washing
Tower connects caustic wash unit, and the water scrubber connects municipal water feed unit.
It is highly preferred that the municipal administration water feed unit includes the storage tank one for connecting the water scrubber, the storage tank one is connected
Pump one, the one connection cooler one of pump, the cooler one connect water scrubber.
Preferably, the caustic wash unit includes the caustic wash tower connecting with the washing unit, and the caustic wash tower connection is burned
Unit, the caustic wash tower connect lye feed unit.
It is highly preferred that the lye feed unit includes the storage tank two for connecting the caustic wash tower, the connection of storage tank two pump
Two, the two connection cooler two of pump, the cooler two connects caustic wash tower.
Preferably, the organic matter processing unit includes sequentially connected reactor and rectifying column, the rectifying column connection
Organic matter storage tank, the reactor connect feed pipe three, and return pipe is equipped between the rectifier bottoms and the reactor
One, the return pipe is equipped with pump three, and the reactor is connect with the catalyst treatment tank.
Preferably, collet is equipped on the outside of the catalyst treatment tank.
Preferably, the incinerator is incinerator.
Preferably, the catalyst treatment tank top is equipped with two feed pipes one, and catalyst treatment tank side is equipped with
Feed pipe two and discharge nozzle one, the catalyst treatment pot bottom are equipped with two feed pipes two, the catalyst treatment pot bottom
Equipped with discharge nozzle two.
Preferably, return pipe two is additionally provided between the knockout drum and the catalyst treatment tank.
It is catalyzed the utility model has the beneficial effects that: the utility model is given up Antimony pentachloride by organic matter processing unit
Organic matter removing in agent；The utility model passes through rectifying column separating fluorine hydride and organic matter；The utility model passes through catalyst
Process tank handles the Antimonous Oxide from Wasted Antimonic Chloride Catalyst after removal organic matter again, removes hydrogen fluoride；The utility model passes through
Washing unit and caustic wash unit carry out washing and alkali cleaning to the gas for handling generation in catalyst treatment tank；The utility model passes through
Incinerator burns the gas after washing with alkali cleaning.
Detailed description of the invention
Fig. 1 is a kind of structural schematic diagram of the pre-processing device of Antimonous Oxide from Wasted Antimonic Chloride Catalyst of the utility model.
Specific embodiment
The utility model is described in further detail in the following with reference to the drawings and specific embodiments, so that those skilled in the art
The utility model may be better understood and can be practiced, but illustrated embodiment is not as the restriction to the utility model.
Referring to Figure 1, present embodiment discloses a kind of pre-processing devices of Antimonous Oxide from Wasted Antimonic Chloride Catalyst, including at catalyst
Tank 1 is managed, the catalyst treatment tank 1 connects organic matter processing unit, and the organic matter processing unit includes sequentially connected anti-
Device 5 and rectifying column 6 are answered, is connect by pipeline 1 with rectifying column 6 at the top of the reactor 5, the rectifying column 6 connects organic matter
Storage tank 8, the reactor 5 connect feed pipe 3 51, convey the useless catalysis of Antimony pentachloride into reactor 5 by feed pipe 3 51
Organic matter and hydrofluoric acid are isolated by rectifying column 6 after agent and hydrofluoric acid, Antimonous Oxide from Wasted Antimonic Chloride Catalyst and hydrofluoric acid reaction, it is described
Return pipe 1 is equipped between 6 bottom of rectifying column and the reactor 5, the return pipe 61 is equipped with pump 3 62, passes through reflux
Hydrofluoric acid in rectifying column 6 is sent in reactor 5 and continues with by pipe 1, is equipped with control on feed pipe 3 51 and pipeline 1
Valve processed；
The reactor 5 connects catalyst treatment tank 1, is equipped with collet 11 on the outside of the catalyst treatment tank 1, at catalyst
Reason tank 1 is jacket canister, and the catalyst treatment tank 1 connects knockout drum 2, by knockout drum 2 by catalyst treatment tank 1
In the gas that generates of each substance reaction carry out gas-liquid separation, also set between the knockout drum 2 and the catalyst treatment tank 1
There is return pipe 2 21, the return pipe 2 21 is equipped with pump 4 211, knockout drum 2 is isolated by return pipe 2 21
For liquid reflux into catalyst treatment tank 1, the connection of the knockout drum 2 washing unit, the washing unit connects alkali cleaning list
Member, the caustic wash unit connect incinerator 7, and the incinerator 7 is incinerator, by washing unit and caustic wash unit for gas
Gas after liquid separation carries out washing and alkali cleaning, is finally burned in being sent into incinerator；
More feed pipes 1 are equipped at the top of the catalyst treatment tank 1, the feed pipe 1 is equipped with two, wherein one
For sodium hydroxide to be added into catalyst treatment tank 1, another feed pipe 1 is used for toward at catalyst root feed pipe 1
Water is added in reason tank 1, water and sodium hydroxide form lye, and 1 side of catalyst treatment tank is equipped with feed pipe 2 13 and discharging
Pipe 1, feed pipe 2 13 are improved in catalyst treatment tank 1 for being sent into steam into catalyst treatment tank 1 by steam
Temperature, so that hydrofluoric acid in Antimonous Oxide from Wasted Antimonic Chloride Catalyst be evaporated, discharge nozzle 1 is for defeated from catalyst treatment tank 1
Steam generation lime set is sent out, the feed pipe 2 13 for being sent into steam is located at the top of catalyst treatment tank 1, sends out the feed pipe of lime set
2 14 are located at the lower part of catalyst treatment tank 1, and 1 bottom of catalyst treatment tank is equipped with more feed pipes 2 15, the charging
Pipe 2 15 is equipped with two, wherein a feed pipe 2 15 urges useless Antimony pentachloride for being sent into chloroform into catalyst treatment tank 1
Fluorine antimony chloride (SbFxCl in agenty) reaction be replaced into SbCly, another feed pipe 2 15 into catalyst treatment tank 1 for sending
Enter nitrogen, by nitrogen various gases and liquid in catalyst treatment tank 1 is uniformly mixed, the catalyst treatment tank 1
Bottom is equipped with discharge nozzle 2 16, and by discharge nozzle 2 16, by treated, hydrating solution is sent to the further resource of resource reclaim company
It recycles, is equipped with control valve on all discharge nozzles and feed pipe and each pipeline；
The washing unit includes connecting alkali cleaning list with the tank connected water scrubber 31 of the gas-liquid separation, the water scrubber 31
Member, the water scrubber 31 connect municipal water feed unit, and the municipal administration water feed unit includes the storage for connecting the water scrubber 31
Tank 1, the connection of storage tank 1 pump 1, the one 33 connection cooler 1 of pump, the connection of cooler 1 water
Tower 31 is washed, water is stored in storage tank 1, storage tank 1 connects municipal water, and municipal water is after pump 1 and cooler 1 are cooling
It is admitted in water scrubber 31, fully absorbs, returned to after washing gas in storage tank 1 in water scrubber 31；
The caustic wash unit includes the caustic wash tower 41 connecting with the washing unit, and the connection of caustic wash tower 41 is burned single
Member, the caustic wash tower 41 connect lye feed unit, and the lye feed unit includes the storage tank 2 42 for connecting the caustic wash tower,
The connection of storage tank 2 42 pump 2 43, the 2 43 connection cooler 2 44 of pump, the cooler 2 44 connect caustic wash tower 41, storage
Lye is stored in tank 2 42, lye is admitted in caustic wash tower 41 after pump 2 43 and cooler 2 44 are cooling, in caustic wash tower 41
It is middle to absorb, returned in storage tank 2 42 after washing gas；
The processing method of the pre-processing device of Antimonous Oxide from Wasted Antimonic Chloride Catalyst:
Step 1: with the anhydrous hydrofluoric acid for supplementing 2~5 ton/hours in Antimonous Oxide from Wasted Antimonic Chloride Catalyst reactor 5, it will
Temperature control is at 110~160 DEG C in reactor 5, and pressure controls between 0.6~1.4Mpa, and continuous operating time 24~48 is small
When, using hydrogen fluoride and organic matter azeotropic point feature, remove the organic matter in dead catalyst；
Step 2: being separated hydrogen fluoride, organic matter and organic matter using rectifying column 6, the hydrogen fluoride isolated is recycled into
It is continued in reactor 5, the organic matter isolated enters organic matter storage tank；
Step 3: stopping that hydrofluoric acid is supplemented or recycled into reactor 5,5 temperature of reactor is controlled at 110~160 DEG C, is pressed
Power gradually removes remaining hydrogen fluoride in reactor 5 between 0.6~1.4Mpa, until in reactor 5 level stability no longer under
Drop；
Step 4: the useless antimony pentachloride catalyst for being stripped of organic matter is transferred in catalyst treatment tank 1, control catalysis
20~60 DEG C of the temperature of agent process tank 1, pressure 0.1Mpa~0.5Mpa；The hydrogen fluoride gas of generation is through 1 row of catalyst treatment tank
Enter to wash unit and caustic wash unit carries out washing and alkali cleaning processing, continuous operation 48 hours or more, removes the fluorination of the overwhelming majority
Hydrogen, to further remove remaining hydrogen fluoride；
Step 5: chloroform and nitrogen are added into catalyst treatment tank 1, the temperature of catalyst treatment tank 1 is controlled 30
It~40 DEG C, 0.1~0.5Mpa of pressure, is reacted using chloroform and useless antimony pentachloride catalyst, by fluorine in useless antimony pentachloride catalyst
Antimony chloride (SbFxCly) reaction be replaced into SbCly, meanwhile, the fluorine-containing organic gas containing chlorine of generation discharges after washing, alkali cleaning
To incinerator processing, using nitrogen, so that chloroform and dead catalyst are sufficiently mixed；
Step 6: being passed through excessive water into catalyst treatment tank 1, water is no more than 1 volume of catalyst treatment tank
60%, antimony chloride hydrolyzes, and the vapor (containing micro hydrogen fluoride and organic matter) of generation discharges, liquid after washing, lye
Time of repose is not less than 5 hours；Antimony chloride hydrolysis:
SbCl5+H2O→Sb2O5+SbO2Cl+SbOCl3
SbCl5+H2O+NaOH→NaSbO3+NaH2SbO4+NaSb(OH)6
SbCl5+5NaOH→H3SbO4+5NaCl+H2O
SbCl3+H2O→Sb2O3+SbOCl
SbCl3+H2O+NaOH→NaSbO2；
Step 7: being passed through suitable 10~30% sodium hydroxide solution into catalyst treatment tank 1, catalyst treatment is adjusted
PH value in tank 1 makes its pH value not less than 10；
Step 8: being transferred to resource reclaim public affairs after the hydrating solution in catalyst treatment tank 1 after processing is packed
Department carries out further resource reclaim processing.
Embodiment described above is only preferred embodiments for fully illustrating the utility model, the utility model
Protection scope it is without being limited thereto.Those skilled in the art made equivalent substitute or change on the basis of the utility model
It changes, both is within the protection scope of the present invention.The protection scope of the utility model is subject to claims.
Claims (10)
1. a kind of pre-processing device of Antimonous Oxide from Wasted Antimonic Chloride Catalyst, it is characterised in that: including catalyst treatment tank, the catalyst
Process tank connects organic matter processing unit, and the catalyst treatment tank connects knockout drum, and the knockout drum connects water
Unit is washed, the washing unit connects caustic wash unit, and the caustic wash unit connects incinerator.
2. a kind of pre-processing device of Antimonous Oxide from Wasted Antimonic Chloride Catalyst as described in claim 1, which is characterized in that the washing is single
Member includes connecting caustic wash unit, the water scrubber connection municipal administration with the tank connected water scrubber of the gas-liquid separation, the water scrubber
Water feed unit.
3. a kind of pre-processing device of Antimonous Oxide from Wasted Antimonic Chloride Catalyst as claimed in claim 2, which is characterized in that the municipal administration water
Feed unit includes the storage tank one for connecting the water scrubber, the connection of storage tank one pump one, the one connection cooler one of pump, institute
It states cooler one and connects water scrubber.
4. a kind of pre-processing device of Antimonous Oxide from Wasted Antimonic Chloride Catalyst as described in claim 1, which is characterized in that the alkali cleaning list
Member includes the caustic wash tower connecting with the washing unit, and unit is burned in the caustic wash tower connection, and the caustic wash tower connection lye supplies
To unit.
5. a kind of pre-processing device of Antimonous Oxide from Wasted Antimonic Chloride Catalyst as claimed in claim 4, which is characterized in that the lye supplies
It include the storage tank two for connecting the caustic wash tower to unit, the connection of storage tank two pump two, the pump two connects cooler two, described
Cooler two connects caustic wash tower.
6. a kind of pre-processing device of Antimonous Oxide from Wasted Antimonic Chloride Catalyst as described in claim 1, which is characterized in that the organic matter
Processing unit includes sequentially connected reactor and rectifying column, and the rectifying column connects organic matter storage tank, and the reactor connects
Expects pipe three is tapped into, return pipe one is equipped between the rectifier bottoms and the reactor, the return pipe is equipped with pump three, institute
Reactor is stated to connect with the catalyst treatment tank.
7. a kind of pre-processing device of Antimonous Oxide from Wasted Antimonic Chloride Catalyst as described in claim 1, which is characterized in that the catalyst
Collet is equipped on the outside of process tank.
8. a kind of pre-processing device of Antimonous Oxide from Wasted Antimonic Chloride Catalyst as described in claim 1, which is characterized in that the burning dress
It is set to incinerator.
9. a kind of pre-processing device of Antimonous Oxide from Wasted Antimonic Chloride Catalyst as described in claim 1, which is characterized in that the catalyst
Two feed pipes one are equipped at the top of process tank, catalyst treatment tank side is equipped with feed pipe two and discharge nozzle one, described to urge
Agent handles pot bottom and is equipped with two feed pipes two, and the catalyst treatment pot bottom is equipped with discharge nozzle two.
10. a kind of pre-processing device of Antimonous Oxide from Wasted Antimonic Chloride Catalyst as described in claim 1, which is characterized in that the gas-liquid
Return pipe two is additionally provided between knockout drum and the catalyst treatment tank.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201821014977.9U CN208546984U (en) | 2018-06-28 | 2018-06-28 | A kind of pre-processing device of Antimonous Oxide from Wasted Antimonic Chloride Catalyst |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201821014977.9U CN208546984U (en) | 2018-06-28 | 2018-06-28 | A kind of pre-processing device of Antimonous Oxide from Wasted Antimonic Chloride Catalyst |
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| Publication Number | Publication Date |
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| CN208546984U true CN208546984U (en) | 2019-02-26 |
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| CN201821014977.9U Active CN208546984U (en) | 2018-06-28 | 2018-06-28 | A kind of pre-processing device of Antimonous Oxide from Wasted Antimonic Chloride Catalyst |
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