CN105271123B - A kind of method and its device recycling iodine in phosphorus production the first grade cooling tower cooling water - Google Patents
A kind of method and its device recycling iodine in phosphorus production the first grade cooling tower cooling water Download PDFInfo
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- CN105271123B CN105271123B CN201510602809.6A CN201510602809A CN105271123B CN 105271123 B CN105271123 B CN 105271123B CN 201510602809 A CN201510602809 A CN 201510602809A CN 105271123 B CN105271123 B CN 105271123B
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Abstract
The present invention relates to iodine recovery technology in phosphorus production,The method and device of iodine in especially a kind of recycling phosphorus production the first grade cooling tower cooling water,Sedimentation Air Exposure is carried out by the way that the cooling water in the grade cooling tower during phosphorus production to be sent into sedimentation aeration tank,In its supernatant to be overflowed to sedimentation deblending slot by overflow manner,By way of sulphurizing salt is added,So that the impurity in supernatant obtains precipitation and removes,And make iodide ion,Iodine all remains in the solution,And also so that phosphorus production is not affected,During carrying out sedimentation Air Exposure in settling aeration tank,It is separated with iodine,Subsequent oxidation is carried out again,Desorption,It absorbs,Analyse iodine,Filtration drying step,So that the iodine being dissolved in solution is recycled,Thereby reduce the discharge capacity and treating capacity of cooling water in phosphorus production system,And it is handled by the cyclic absorption on absorption tower,So that the rate of recovery of iodine is improved,Reduce cost.
Description
Technical field
The present invention relates to iodine recovery technology fields in phosphorus production, especially a kind of the first grade cooling tower of recycling phosphorus production
The method and its device of iodine in cooling water.
Background technology
It is carried in phosphoric acid by wet process there are mainly two types of iodine methods, first, certain oxidant is added in phosphoric acid by wet process, it may be possible to chlorine
Gas, potassium permanganate, potassium chlorate or hydrogen peroxide are mixed with the one or more of of strong oxidizers such as vanadic anhydrides, by iodine by dissociating
The I of state-It is oxidized to iodine molecule, the extractants such as carbon tetrachloride are then added, is sufficiently stirred and iodine molecule is extracted into organic phase, point
From organic phase and acid solution phase, under certain temperature and pressure evaporating carbon tetrachloride by vacuum distillation mode obtains thick iodine；Second is that
Certain oxidant is added in phosphoric acid by wet process, it may be possible to chlorine, potassium permanganate, potassium chlorate or hydrogen peroxide and vanadic anhydride etc.
One or more of mixing of strong oxidizer, by iodine by the I of free state-It is oxidized to iodine molecule, blasts air or nitrogen by phosphoric acid
In iodine molecule blowout, the iodine steam in air-flow introduces behind absorption tower with dissolved with SO2Or Na2SO3A kind of iodine solution absorb.
Iodide solution is flowed out with a certain concentration from bottom of tower, and chlorine, potassium permanganate, potassium chlorate or hydrogen peroxide and five oxygen are added in solution
Change the one or more of the strong oxidizers such as two vanadium, standing makes iodine be precipitated, filters to obtain thick iodine.
There is the above-mentioned prior art to can be seen that the method that it is mainly used as extractive distillation method and gas blowout reduction
Method, and blowing out method first is proposed by Japanese Yi Xi chemical industrial companies, is recycled due to the superiority of its technique, and then in iodine
It neutralizes and is widely used in production, main method is that clear bittern water is acidified to PH=2~3, is passed through chlorine
Enter stripping tower after mixing, be allowed to gasify with air draught by the iodine that chlorine displaces, the iodine steam in air-flow, which introduces, to be inhaled
It is absorbed with a kind of iodine solution dissolved with sulfur dioxide after receiving tower.Iodide solution is flowed out simultaneously with the concentration of 50~100g/L from bottom of tower
Iodide solution recycling is kept, then solution is passed through chlorine treatment in the reactor of glass again makes iodine be precipitated, then iodine
Suspended matter filters, and filtrate returns in iodide system.Iodine is as filter cake melt refining in concentrated sulfuric acid.Obtain thick iodine.
But nevertheless, technique of extracting iodine in the prior art is not met by iodine, there are each sides in living environment
Situation among face and various substances, the generality in turn resulting in the technique of iodine recycling is also relatively weak, for this purpose, there is researcher
For the method for extracting iodine in the phosphorus factory recirculated water containing iodine, the Publication No. CN101318624A of patent, which employs from Huang
In phosphorus factory waste water containing iodine, the technique of iodine is extracted using blowout method, but since the impurity component in Yellow Phosphorus Wastewater is complex, contain
There are many impurity for influencing elemental iodine precipitation, such as rare metal, heavy metal all easily to form complex compound, Jin Erzao with elemental iodine
It is difficult to be precipitated at elemental iodine, reduces the rate of recovery of iodine and the treating capacity of the waste water containing iodine, for this reason, it may be necessary to be carried out to Yellow Phosphorous Plant waste water
Pretreatment, the cost for causing Yellow Phosphorous Plant wastewater treatment is higher, and energy consumption is big.
Meanwhile this researcher is by retrieving and consulting the relevant prior art, not it has been found that there is relevant technical literature in Huang
The processing scheme of iodine is extracted in phosphorus production process to a grade cooling tower cooling water.
Invention content
In order to solve the above technical problems existing in the prior art, the present invention provides a kind of recycling phosphorus production first order
The method and its device of iodine in cooling tower cooling water.
It is achieved particular by following technical scheme：
A method of iodine in recycling phosphorus production the first grade cooling tower cooling water, the cooling water that a grade cooling tower is come out
Progress settler overflow in sedimentation aeration tank is sent into come out, after settling the supernatant in aeration tank and overflowing in sedimentation deblending slot,
Aqueous slkali is added thereto again and adjusts pH value to 9-12, and is stirred for uniformly, then sulphurizing salt is added thereto to excess, stands
1-2h is used filter to be filtered processing, obtains the stillness of night, will be sent into oxidation trough the stillness of night, and composite oxidant progress is added
Oxidation processes, then carried out in desorber after desorption processing, feeding absorption tower is absorbed using reducing agent, then is carried out analysis iodine
Tower carries out analysis iodine, filtration drying, packaging, obtains thick iodine finished product.
The sulphurizing salt is one kind or several in vulcanized sodium, potassium sulfide, ammonium sulfide, phosphorus pentasulfide or phosphorus trisulfide
The mixing of kind.
The aqueous slkali is one or several kinds of mixed liquors in sodium hydroxide, calcium hydroxide, ammonium hydroxide.
The composite oxidant is chlorine, potassium permanganate, potassium chlorate or hydrogen peroxide and one kind in vanadic anhydride
Or several mixing.
The reducing agent is one or two kinds of mixed aqueous solutions in sulfurous acid, sodium nitrite.
The addition of the composite oxidant is every liter of stillness of night 20-50g to be added.
The addition of the reducing agent is so that the flow velocity for the liquid that absorbing tower underflow comes out is 2-6m3/ h, reduction
Agent is cyclic absorption in absorption tower, until it is a concentration of more than or equal to after 600ppm containing iodine, feeding analysis iodine column is analysed
Iodine.
A kind of device recycling iodine in phosphorus production the first grade cooling tower cooling water, is connected by Yellow phosphorus furnace 1, with Yellow phosphorus furnace 1
Sedimentation aeration tank 3, oxidation trough 4, the desorber 5 being connected with oxidation trough 4 and the desorption of logical cooling tower 2, the connection of cooling tower 2
Air separation plant 6 that tower 5 is connected, absorption tower 7, the detector 8 being connected with absorption tower 7, detector 8, which pass through, detects absorption tower 7
In iodin-containing liquid concentration, in a concentration of iodin-containing liquid more than or equal to 600ppm, outlet a；It is less than a concentration of
When the iodin-containing liquid of 600ppm, outlet b；Outlet a with analysis iodine column 9 be connected, analysis iodine column 9 be connected with Filter dryer 10 and
At wherein being disposed with sedimentation deblending slot 11, filter 12 between sedimentation aeration tank 3 and oxidation trough 4.
The device is additionally provided with shurry pump between oxidation trough 4 and desorber 5.
Compared with prior art, technique effect of the invention is embodied in：
Sedimentation exposure is carried out by the way that the cooling water in the grade cooling tower during phosphorus production to be sent into sedimentation aeration tank
Gas disposal, in its supernatant to be overflowed to sedimentation deblending slot by overflow manner, by way of sulphurizing salt is added so that on
Impurity in clear liquid obtains precipitation and removes, and iodide ion, iodine are all remained in the solution, and also so that yellow phosphorus
Production is not affected, and during carrying out sedimentation Air Exposure in settling aeration tank, is separated with iodine, then will
It carries out subsequent oxidation, desorption, absorbs, analysis iodine, filtration drying step so that the iodine being dissolved in solution is returned
It receives, thereby reduces the discharge capacity and treating capacity of cooling water in phosphorus production system, and at the cyclic absorption for passing through absorption tower
Reason so that the rate of recovery of iodine is improved, and reduces cost.
Also, the present invention is passed through by setting sedimentation deblending slot and filter between oxidation trough and sedimentation aeration tank
Addition sulphurizing salt in deblending slot is settled again and carries out removal of impurities processing so that the impurity content for the cooling water that cooling tower comes out is dropped
It is low, and then the eduction rate of iodine is improved, the rate of recovery of iodine is improved, waste liquid circulation amount is reduced, reduces waste liquid circulation energy, is saved
To the cost of the iodine recycling of the cooling water of a grade cooling tower about during phosphorus production.
Meanwhile the present invention also chooses to the cooling water of a grade cooling tower recycle and iodinate so that the iodine in mother liquor contains
Amount is higher, while reducing the volume waste liquid discharging amount of phosphorus production, also improves the rate of recovery of iodine, reduce the recycling of iodine at
This so that the concentrate time during cooling water carries out recycling iodine shortens, and shortens the return period of recycling iodine, reduces into
This.
Description of the drawings
Fig. 1 be the present invention recycling phosphorus production the first grade cooling tower cooling water in iodine method process flow chart.
Fig. 2 is the schematic diagram for recycling the device of iodine in phosphorus production the first grade cooling tower cooling water.
The 3- sedimentation aeration tank 4- oxidation trough 5- desorber 6- air separation plant 7- absorption tower 8- detections of 1- Yellow phosphorus furnace 2- cooling towers
Device 9- analysis iodine column 10- Filter dryers 11- settles deblending slot 12- filters.
A- meets the iodin-containing liquid outlet that iodine concentration is greater than or equal to 600ppm；B- meets iodine concentration and contains iodine less than 600ppm
Liquid outlet.
Specific implementation mode
It is limited technical scheme of the present invention is further, but is required with specific embodiment below in conjunction with the accompanying drawings
The range of protection describes made by being not only limited to.
Embodiment 1
As shown in Figure 1, a kind of method recycling iodine in phosphorus production the first grade cooling tower cooling water, a grade cooling tower is gone out
The cooling water come is sent into progress settler overflow in sedimentation aeration tank and is come out, and the supernatant in aeration tank to be settled overflows to sedimentation and removes
After in miscellaneous slot, then aqueous slkali is added thereto and adjusts pH value to 9, and be stirred for uniformly, then sulphurizing salt is added thereto to mistake
Amount stands 1h, is used filter to be filtered processing, obtain the stillness of night, will be sent into oxidation trough the stillness of night, and composite oxidant is added
Oxidation processes are carried out, then are carried out in desorber after desorption processing, feeding absorption tower is absorbed using reducing agent, then is carried out
Analysis iodine column carries out analysis iodine, filtration drying, packaging, obtains thick iodine finished product.The sulphurizing salt is vulcanized sodium.The aqueous slkali is hydrogen
Sodium oxide molybdena.The composite oxidant is that hydrogen peroxide is mixed with vanadic anhydride.The reducing agent is the aqueous solution of sulfurous acid.
The addition of the composite oxidant is every liter of stillness of night 20g to be added.The addition of the reducing agent is so that absorbing tower
The flow velocity for the liquid that underflow comes out is 2m3/ h, reducing agent is cyclic absorption in absorption tower, until its a concentration of containing iodine is more than
Or carry out analysis iodine equal to analysis iodine column after 600ppm, is sent into.
Embodiment 2
As shown in Figure 1, a kind of method recycling iodine in phosphorus production the first grade cooling tower cooling water, a grade cooling tower is gone out
The cooling water come is sent into progress settler overflow in sedimentation aeration tank and is come out, and the supernatant in aeration tank to be settled overflows to sedimentation and removes
After in miscellaneous slot, then aqueous slkali is added thereto and adjusts pH value to 12, and be stirred for uniformly, then sulphurizing salt is added thereto to mistake
Amount stands 2h, is used filter to be filtered processing, obtain the stillness of night, will be sent into oxidation trough the stillness of night, and composite oxidant is added
Oxidation processes are carried out, then are carried out in desorber after desorption processing, feeding absorption tower is absorbed using reducing agent, then is carried out
Analysis iodine column carries out analysis iodine, filtration drying, packaging, obtains thick iodine finished product.The sulphurizing salt is vulcanized sodium, potassium sulfide, ammonium sulfide.Institute
The aqueous slkali stated is the mixed liquor of sodium hydroxide, calcium hydroxide, ammonium hydroxide.The composite oxidant is chlorine, hydrogen peroxide and five
V 2 O mixes.The reducing agent is sulfurous acid, sodium nitrite mixed aqueous solutions.The addition of the composite oxidant
50g is added for every liter of stillness of night in amount.The addition of the reducing agent is so that the flow velocity for the liquid that absorbing tower underflow comes out is
6m3/ h, reducing agent are cyclic absorption in absorption tower, until it is a concentration of more than or equal to after 600ppm containing iodine, are sent into analysis
Iodine column carries out analysis iodine.
Embodiment 3
As shown in Figure 1, a kind of method recycling iodine in phosphorus production the first grade cooling tower cooling water, a grade cooling tower is gone out
The cooling water come is sent into progress settler overflow in sedimentation aeration tank and is come out, and the supernatant in aeration tank to be settled overflows to sedimentation and removes
After in miscellaneous slot, then aqueous slkali is added thereto and adjusts pH value to 11, and be stirred for uniformly, then sulphurizing salt is added thereto to mistake
Amount stands 1.5h, is used filter to be filtered processing, obtain the stillness of night, will be sent into oxidation trough the stillness of night, and combined oxidation is added
Agent carries out oxidation processes, then after being carried out in desorber desorption processing, is sent into absorption tower using reducing agent absorption, then by its into
Row analysis iodine column carries out analysis iodine, filtration drying, packaging, obtains thick iodine finished product.The sulphurizing salt be vulcanized sodium, potassium sulfide, ammonium sulfide,
The mixing of phosphorus pentasulfide, phosphorus trisulfide.The aqueous slkali is the mixed liquor of calcium hydroxide, ammonium hydroxide.The composite oxygen
Agent is that potassium chlorate is mixed with vanadic anhydride.The reducing agent is the aqueous solution of sodium nitrite.The composite oxidant
Addition be every liter of stillness of night 40g to be added.The addition of the reducing agent is so that the liquid that absorbing tower underflow comes out
Flow velocity is 5m3/ h, reducing agent in absorption tower be cyclic absorption, until its containing iodine it is a concentration of be greater than or equal to 600ppm after,
It is sent into analysis iodine column and carries out analysis iodine.
Embodiment 4
As shown in Fig. 2, a kind of device recycling iodine in phosphorus production the first grade cooling tower cooling water, by Yellow phosphorus furnace 1 and Huang
Sedimentation aeration tank 3 that cooling tower 2 that phosphorus stove 1 is connected, cooling tower 2 are connected to, oxidation trough 4, the desorber being connected with oxidation trough 4
5, the air separation plant 6 that is connected with desorber 5, absorption tower 7, the detector 8 being connected with absorption tower 7, detector 8 pass through detection
The concentration of iodin-containing liquid in absorption tower 7, in a concentration of iodin-containing liquid more than or equal to 600ppm, outlet a；A concentration of
When iodin-containing liquid less than 600ppm, outlet b；Outlet a is connected with analysis iodine column 9, and analysis iodine column 9 is connected with Filter dryer 10
It is logical to form, wherein being disposed with sedimentation deblending slot 11, filter 12 between sedimentation aeration tank 3 and oxidation trough 4.
Embodiment 5
As shown in Fig. 2, on the basis of embodiment 4, the device is also set up between oxidation trough 4 and desorber 5
There is shurry pump.
Embodiment 6
As depicted in figs. 1 and 2, the side of iodine is recycled using the device of iodine in recycling phosphorus production the first grade cooling tower cooling water
Method after the gas generated in producing Yellow phosphorus furnace carries out cooling by cooling tower 2, is chosen cooling in a grade cooling tower of cooling tower
Cooling water out, by the cooling water be sent into sedimentation aeration tank 3 in, by be passed through gas fill stirring after, then by its it is static sink
Drop processing so that the supernatant in sedimentation aeration tank 3 is entered by way of overflow in sedimentation deblending slot 11, then is added thereto
Enter aqueous slkali and adjust pH value to 9, and be stirred for uniformly, then sulphurizing salt is added thereto to excess, stands 1h, used
Filter 12 is filtered processing, obtains the stillness of night, will be sent into oxidation trough 4 stillness of night, and composite oxidant is added and carries out oxidation processes, then will
It is carried out in desorber 5 after desorption processing, and feeding absorption tower 7 is absorbed using reducing agent, then is carried out analysis iodine column 9 and analysed
Iodine, Filter dryer 10 are filtered dry, packaging, obtain thick iodine finished product.The sulphurizing salt is phosphorus pentasulfide, trisulfides two
The mixing of phosphorus.The aqueous slkali is the mixed liquor of sodium hydroxide, ammonium hydroxide.The composite oxidant is potassium permanganate, chloric acid
Potassium is mixed with vanadic anhydride.The reducing agent is the aqueous solution of sulfurous acid.The addition of the composite oxidant is every
Rise stillness of night addition 30g.The addition of the reducing agent is so that the flow velocity for the liquid that absorbing tower underflow comes out is 5m3/ h,
Reducing agent in absorption tower be cyclic absorption, until its containing iodine it is a concentration of be greater than or equal to 600ppm after, be sent into analysis iodine column into
Row analysis iodine.
Claims (7)
1. a kind of method of iodine in recycling phosphorus production the first grade cooling tower cooling water, which is characterized in that go out a grade cooling tower
The cooling water come is sent into progress settler overflow in sedimentation aeration tank and is come out, and the supernatant in aeration tank to be settled overflows to sedimentation and removes
After in miscellaneous slot, then aqueous slkali is added thereto and adjusts pH value to 9-12, and be stirred for uniformly, then sulfide is added extremely thereto
It is excessive, 1-2h is stood, is used filter to be filtered processing, obtains clear liquid, clear liquid is sent into oxidation trough, and composite oxygen is added
Agent carries out oxidation processes, then after being carried out in desorber desorption processing, is sent into absorption tower using reducing agent absorption, then by its
It carries out analysis iodine column and carries out analysis iodine, filtration drying, packaging, obtain thick iodine finished product；The sulfide is vulcanized sodium, potassium sulfide, vulcanization
The mixing of one or more of ammonium, phosphorus pentasulfide or phosphorus trisulfide；
The device of iodine in recycling phosphorus production the first grade cooling tower cooling water that the above method uses, by Yellow phosphorus furnace (1) and yellow phosphorus
Cooling tower (2) that stove (1) is connected, oxidation trough (4), is connected with oxidation trough (4) at the sedimentation aeration tank (3) of cooling tower (2) connection
Logical desorber (5), the air separation plant (6) being connected with desorber (5), absorption tower (7), the inspection being connected with absorption tower (7)
Device (8), detector (8) are surveyed by the concentration of the iodin-containing liquid in detection absorption tower (7), is greater than or equal to 600ppm's a concentration of
When iodin-containing liquid, outlet a；In a concentration of iodin-containing liquid less than 600ppm, outlet b, outlet b are into absorption tower
(7) in；Outlet a is connected with analysis iodine column (9), and analysis iodine column (9) is connected with Filter dryer (10), wherein being exposed in sedimentation
Sedimentation deblending slot (11), filter (12) are disposed between air drain (3) and oxidation trough (4).
2. the method for recycling iodine in phosphorus production the first grade cooling tower cooling water as described in claim 1, which is characterized in that institute
The aqueous slkali stated is one or several kinds of mixed liquors in sodium hydroxide, calcium hydroxide, ammonium hydroxide.
3. the method for recycling iodine in phosphorus production the first grade cooling tower cooling water as described in claim 1, which is characterized in that institute
The composite oxidant stated is that one or more are mixed with vanadic anhydride in chlorine, potassium permanganate, potassium chlorate or hydrogen peroxide.
4. the method for recycling iodine in phosphorus production the first grade cooling tower cooling water as described in claim 1, which is characterized in that institute
The reducing agent stated is one or two kinds of mixed aqueous solutions in sulfurous acid, sodium nitrite.
5. the method for iodine, feature exist in recycling phosphorus production the first grade cooling tower cooling water as described in claim 1 or 3
In the addition of the composite oxidant is that 20-50g is added in every liter of clear liquid.
6. the method for iodine, feature exist in recycling phosphorus production the first grade cooling tower cooling water as described in claim 1 or 4
In the addition of the reducing agent is so that the flow velocity for the liquid that absorbing tower underflow comes out is 2-6m3/ h, reducing agent are being inhaled
It is cyclic absorption to receive in tower, until it is a concentration of more than or equal to after 600ppm containing iodine, feeding analysis iodine column carries out analysis iodine.
7. the method for recycling iodine in phosphorus production the first grade cooling tower cooling water as described in claim 1, which is characterized in that institute
The device stated is additionally provided with shurry pump between oxidation trough (4) and desorber (5).
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510602809.6A CN105271123B (en) | 2015-09-21 | 2015-09-21 | A kind of method and its device recycling iodine in phosphorus production the first grade cooling tower cooling water |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510602809.6A CN105271123B (en) | 2015-09-21 | 2015-09-21 | A kind of method and its device recycling iodine in phosphorus production the first grade cooling tower cooling water |
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| CN105271123A CN105271123A (en) | 2016-01-27 |
| CN105271123B true CN105271123B (en) | 2018-09-14 |
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Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3857704A (en) * | 1971-03-05 | 1974-12-31 | Bp Chem Int Ltd | Mercury recovery process |
| CN1284723C (en) * | 2003-09-10 | 2006-11-15 | 陈肖虎 | Method for extracting iodine from rejected material generated during production of phosphor product from iodine-containing phosphorus ore |
| CN101318624B (en) * | 2008-06-26 | 2010-09-15 | 贵州大学 | Method for extracting iodine from iodine containing circulation water of yellow phosphorus factory |
| CN101318625B (en) * | 2008-07-10 | 2010-06-09 | 贵州大学 | Method for recycling iodine from diluted phosphoric acid for phosphoric acid manufacture with wet-process |
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Effective date of registration: 20190228 Address after: 550300 Xinguanshan, Shuangliu Town, Kaiyang County, Guiyang City, Guizhou Province Patentee after: Guizhou new Tianxin Chemical Co., Ltd. Address before: 550022 28 Floor, Block C, Jinyang Century Jinyuan Shopping Center, Guiyang City, Guizhou Province Patentee before: GUIZHOU XIN XIN CHEMICAL GROUP CO., LTD. |