CN105217574A - A kind ofly reclaim the method for iodine and the cooling tower of device and employing in phosphorus production first step cooling tower water coolant - Google Patents
A kind ofly reclaim the method for iodine and the cooling tower of device and employing in phosphorus production first step cooling tower water coolant Download PDFInfo
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- CN105217574A CN105217574A CN201510602870.0A CN201510602870A CN105217574A CN 105217574 A CN105217574 A CN 105217574A CN 201510602870 A CN201510602870 A CN 201510602870A CN 105217574 A CN105217574 A CN 105217574A
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Abstract
The present invention relates to phosphorus production iodine recovery technology, especially a kind ofly the method for iodine and the cooling tower of device and employing in phosphorus production first step cooling tower water coolant is reclaimed, by the first step cooling tower water coolant of phosphorus production is sent in sedimentation aerator tank, overflow to after in oxidation trough, after adding oxidizing one-tenth iodate more wherein, resolve again, reductive agent absorbs, and then the rate of recovery of iodine is improved, and in conjunction with the improvement of the structure to cooling, and then the liquid making the cooling tower first step cool out can obtain preferential entering settlement treatment in subsider, and then shorten the internal circulating load of solution of cyclic absorption, reduce energy consumption, also shorten the cycle to iodine recycling simultaneously, reduce cost recovery, and directly the first step cooling tower of high density liquid is out carried out priority reclamation, and then the rate of recovery of iodine is improved, concentrate step when avoiding the recovery to the iodine in phosphorus production process, reduce cost.
Description
Technical field
The present invention relates to phosphorus production iodine recovery technology field, especially a kind ofly reclaim the method for iodine and the cooling tower of device and employing in phosphorus production first step cooling tower water coolant.
Background technology
In the recovery process of iodine, method that is the most typical and that use the earliest is blowout method, this method is taken the lead in putting forward by Japanese Yi Xi chemical industrial company, its concrete technical process is that the bittern water of clarification is acidified to pH=2 ~ 3, stripping tower is entered after passing into chlorine mixing, made it gasification by the iodine air draught that chlorine displaces, absorb with a kind of iodine solution being dissolved with sulfurous gas after the iodine steam in air-flow introduces absorption tower.Iodide solution to go out from tower bottom flow with the concentration of 50 ~ 100g/L and keeps iodide solution recirculation, and pass into chlorine treatment in the reactor of then solution glass again and iodine is separated out, then the suspended substance of iodine is filtered, filtrate turns back in iodide system and goes.Iodine is as filter cake melt refining in concentrated sulfuric acid.Obtain thick iodine.After this method produces, along with the development of Wet Processes of Phosphoric Acid, this method doubly introduces in the iodine recovery process in Wet-process Phosphoric Acid Production process, it is in phosphoric acid by wet process, add certain oxygenant that its concrete working method comprises two kinds: one, may be chlorine, potassium permanganate, Potcrate or hydrogen peroxide mixes, by the I of iodine by free state with one or more of the strong oxidizers such as Vanadium Pentoxide in FLAKES
-be oxidized to iodine molecule, then add the extraction agents such as tetracol phenixin, fully stir and iodine molecule is extracted in organic phase, be separated organic phase and acid solution phase, under certain temperature and pressure, evaporate tetracol phenixin by underpressure distillation mode obtain thick iodine; Two is in phosphoric acid by wet process, add certain oxygenant, and may be chlorine, potassium permanganate, Potcrate or hydrogen peroxide mixes, by the I of iodine by free state with one or more of the strong oxidizers such as Vanadium Pentoxide in FLAKES
-be oxidized to iodine molecule, blast air or nitrogen by the iodine molecule blowout in phosphoric acid, the iodine steam in air-flow is introduced behind absorption tower with being dissolved with SO
2or Na
2sO
3a kind of iodine solution absorb.Iodide solution goes out from tower bottom flow with finite concentration, adds chlorine, potassium permanganate, Potcrate or the strong oxidizer such as hydrogen peroxide and Vanadium Pentoxide in FLAKES one or more in solution, leaves standstill and iodine is separated out, and filters to obtain thick iodine.
But, for in phosphorus production process, it is only in China, all need the Rock Phosphate (72Min BPL) consuming up to a million tons every year, and in these Rock Phosphate (72Min BPL), be difficult to the iodine element that also exists avoided, and in currently available technology, although there is publication number to be that " from containing the method extracting iodine iodine circulation water of yellow phosphorus factory " of CN101318624A adopts blowout method to extract the technique of iodine, but because Yellow Phosphorus Wastewater is a complicated system, wherein affect elemental iodine extraction factor containing multiple, as yttrium, heavy metal elements etc. all very easily form complex compound with elemental iodine, make blowout efficiency very low, and then after making the waste water that must produce phosphorus production carry out pre-treatment, the extraction of iodine can be carried out, do not have the report that can extract the Technology document of iodine from phosphorus production process, the waste gas produced in phosphorus production process is discharged, this not only causes the waste of resource, but also bring serious pollution to environment.
Summary of the invention
In order to solve the above-mentioned technical problem existed in prior art, the invention provides and a kind ofly reclaim the method for iodine and the cooling tower of device and employing in phosphorus production first step cooling tower water coolant.
Be achieved particular by following technical scheme:
Reclaim a method for iodine in phosphorus production first step cooling tower water coolant, a grade cooling tower water coolant proceeded to settlement treatment in subsider, then the mode of its supernatant liquor by overflow is overflowed in oxidation trough, and add oxygenant in oxidation trough,
and adopt agitator stir process 2-3h,again liquid Pulp pump is squeezed into and resolve in groove, and from air separation plant, pass into air carry out dissection process, and the gas containing iodine is entered absorption tower, carry out cyclic absorption by reductive agent, until the concentration of iodine in solution reach>=600ppm after, then carried out analysing iodinate, obtain iodine, and iodine is put into drying plant and carry out drying, packaging, can obtain the thick iodine of finished product.
Described oxygenant is one or several of chlorine, clorox, hydrogen peroxide, potassium permanganate, Potassium Iodate or Potcrate.
Described reductive agent is the aqueous solution of a kind of or two kinds of mixing in sulfurous acid, Sodium Nitrite.
The add-on of described oxygenant is that every rising foam flow liquid adds 10-30g oxygenant.
The add-on of described reductive agent is to make at the bottom of absorbing tower flow rate of liquid out be 1-5m
3/ min.
A kind of device reclaiming iodine in phosphorus production first step cooling tower water coolant, containing Yellow phosphorus furnace, Yellow phosphorus furnace is communicated with cooling tower, cooling tower and sedimentation aerator tank, sedimentation aerator tank is connected with oxidation trough by overflow manner, oxidation trough is communicated with desorption tower, desorption tower is communicated with air separation plant, desorption tower is connected with absorption tower, absorption tower is connected with detector, detector is connected with iodin-containing liquid outlet, iodin-containing liquid outlet is divided into and meets iodine concentration and be more than or equal to the iodin-containing liquid outlet a of 600ppm and meet the iodin-containing liquid outlet b that iodine concentration is less than 600ppm, iodin-containing liquid outlet a with analyse iodine column and be connected, iodin-containing liquid outlet b is connected with absorption tower, analyse iodine column to be connected with Filter dryer.
A kind of cooling tower reclaiming iodine employing in phosphorus production first step cooling tower water coolant, by a grade cooling tower, two grade cooling towers, N grade cooling tower and the settling bowl coupled together bottom a grade cooling tower, bottom two grade cooling towers, bottom N grade cooling tower is formed, the baffle plate wherein extended bottom settling bowl between a grade cooling tower and two grade cooling towers.
Described settling bowl is made up of the nearly mouth layer bottom cooling tower, the mud layer bottom settling bowl, the supernatant layer between mud layer and nearly mouth layer.
Described settling bowl, is provided with overflow port at the intersection of supernatant layer and nearly mouth layer.
Described overflow port is arranged on the two ends, left and right of settling bowl.
Described baffle plate extends to the bottom near settling bowl.
The distance that described baffle plate extends near the bottom of settling bowl is 2-4cm.
Described overflow port is arranged on one, the settling bowl left side, to be arranged on the right of settling bowl one.
Compared with prior art, technique effect of the present invention is embodied in:
By the first step cooling tower water coolant of phosphorus production is sent in sedimentation aerator tank, overflow to after in oxidation trough, after adding oxidizing one-tenth iodate more wherein, resolve again, reductive agent absorbs, and then the rate of recovery of iodine is improved, and in conjunction with the improvement of the structure to cooling, and then the liquid making the cooling tower first step cool out can obtain preferential entering settlement treatment in subsider, and then shorten the internal circulating load of solution of cyclic absorption, reduce energy consumption, also shorten the cycle to iodine recycling simultaneously, reduce cost recovery, and directly the first step cooling tower of high density liquid is out carried out priority reclamation, and then the rate of recovery of iodine is improved, concentrate step when avoiding the recovery to the iodine in phosphorus production process, reduce cost.
Further, process and the technique of the recovery iodine in the present invention can not have any impact to the technique of phosphorus production, also reduce the quantity discharged of follow-up waste gas, reduce environmental pollution rate.
Accompanying drawing explanation
Fig. 1 is the process flow sheet of the method for iodine in recovery phosphorus production first step cooling tower water coolant of the present invention.
Fig. 2 is the device schematic diagram of iodine in recovery phosphorus production first step cooling tower water coolant of the present invention.
1-Yellow phosphorus furnace 2-cooling tower 3-sedimentation aerator tank 4-oxidation trough 5-desorption tower 6-air separation plant 7-absorption tower 8-detector 9-analyses iodine column 10-Filter dryer.
A-meets the iodin-containing liquid outlet that iodine concentration is more than or equal to 600ppm; B-meets the iodin-containing liquid outlet that iodine concentration is less than 600ppm.
Fig. 3 is the cooling tower result schematic diagram that in recovery phosphorus production first step cooling tower water coolant of the present invention, iodine adopts.
11-mono-grade cooling tower 12-bis-grade cooling tower 13-N grade cooling tower 14-overflow port 15-settling bowl 16-mud layer 17-supernatant layer 18-baffle plate.
Embodiment
Below in conjunction with accompanying drawing and concrete embodiment, further restriction is done to technical scheme of the present invention, but claimed scope is not only confined to done description.
Embodiment 1
As shown in Figure 1, a kind of method reclaiming iodine in phosphorus production first step cooling tower water coolant, proceeds to settlement treatment in subsider by a grade cooling tower water coolant, then the mode of its supernatant liquor by overflow is overflowed in oxidation trough, and add oxygenant in oxidation trough,
and adopt agitator stir process 2.5h,again liquid Pulp pump is squeezed into and resolve in groove, and from air separation plant, pass into air carry out dissection process, and the gas containing iodine is entered absorption tower, carry out cyclic absorption by reductive agent, until the concentration of iodine in solution reach>=600ppm after, then carried out analysing iodinate, obtain iodine, and iodine is put into drying plant and carry out drying, packaging, can obtain the thick iodine of finished product.Described oxygenant is chlorine.Described reductive agent is sulfurous aqueous acid.The add-on of described oxygenant is that every rising foam flow liquid adds 20g oxygenant.The add-on of described reductive agent is to make at the bottom of absorbing tower flow rate of liquid out be 3m
3/ min.
Embodiment 2
As shown in Figure 1, a kind of method reclaiming iodine in phosphorus production first step cooling tower water coolant, proceeds to settlement treatment in subsider by a grade cooling tower water coolant, then the mode of its supernatant liquor by overflow is overflowed in oxidation trough, and add oxygenant in oxidation trough,
and adopt agitator stir process 2h,again liquid Pulp pump is squeezed into and resolve in groove, and from air separation plant, pass into air carry out dissection process, and the gas containing iodine is entered absorption tower, carry out cyclic absorption by reductive agent, until the concentration of iodine in solution reach>=600ppm after, then carried out analysing iodinate, obtain iodine, and iodine is put into drying plant and carry out drying, packaging, can obtain the thick iodine of finished product.Described oxygenant is chlorine, clorox compound.Described reductive agent is, the aqueous solution of Sodium Nitrite.The add-on of described oxygenant is that every rising foam flow liquid adds 10g oxygenant.The add-on of described reductive agent is to make at the bottom of absorbing tower flow rate of liquid out be 1m
3/ min.
Embodiment 3
As shown in Figure 1, a kind of method reclaiming iodine in phosphorus production first step cooling tower water coolant, proceeds to settlement treatment in subsider by a grade cooling tower water coolant, then the mode of its supernatant liquor by overflow is overflowed in oxidation trough, and add oxygenant in oxidation trough,
and adopt agitator stir process 3h,again liquid Pulp pump is squeezed into and resolve in groove, and from air separation plant, pass into air carry out dissection process, and the gas containing iodine is entered absorption tower, carry out cyclic absorption by reductive agent, until the concentration of iodine in solution reach>=600ppm after, then carried out analysing iodinate, obtain iodine, and iodine is put into drying plant and carry out drying, packaging, can obtain the thick iodine of finished product.Described oxygenant is chlorine, clorox, hydrogen peroxide.Described reductive agent is the aqueous solution of sulfurous acid, Sodium Nitrite.The add-on of described oxygenant is that every rising foam flow liquid adds 30g oxygenant.The add-on of described reductive agent is to make at the bottom of absorbing tower flow rate of liquid out be 5m
3/ min.
Embodiment 4
As shown in Figure 2, a kind of device reclaiming iodine in phosphorus production first step cooling tower water coolant, containing Yellow phosphorus furnace 1, Yellow phosphorus furnace 1 is communicated with cooling tower 2, cooling tower 2 and sedimentation aerator tank 3, sedimentation aerator tank 3 is connected with oxidation trough 4 by overflow manner, oxidation trough 4 is communicated with desorption tower 5, desorption tower 5 is communicated with air separation plant 6, desorption tower 5 is connected with absorption tower 7, absorption tower 7 is connected with detector 8, detector 8 is connected with iodin-containing liquid outlet, iodin-containing liquid outlet is divided into and meets iodine concentration and be more than or equal to the iodin-containing liquid outlet a of 600ppm and meet the iodin-containing liquid outlet b that iodine concentration is less than 600ppm, iodin-containing liquid outlet a with analyse iodine column 9 and be connected, iodin-containing liquid outlet b is connected with absorption tower 7, analyse iodine column 9 to be connected with Filter dryer 10.
Embodiment 5
As depicted in figs. 1 and 2, the device reclaiming iodine in phosphorus production first step cooling tower water coolant is adopted to carry out reclaiming the method for iodine in phosphorus production first step cooling tower water coolant, tail gas out from Yellow phosphorus furnace 1 is passed in cooling tower 2 and carries out multistage cooling, and the one-level cooling fluid in cooling tower 2 is proceeded in sedimentation aerator tank 3, and gas stirring process is passed in sedimentation aerator tank, again by its settlement treatment, its supernatant liquor is made to overflow in oxidation trough 4, and oxygenant is added in oxidation trough, and stir process 4h, again liquid Pulp pump is squeezed in desorption tower 5, and from air separation plant 6, pass into air carry out dissection process, and the gas containing iodine is entered absorption tower 7, cyclic absorption is carried out by reductive agent, sent into again in detector 8 and carried out check processing, after the concentration of the iodin-containing liquid after cyclic absorption is wherein greater than or equal to 600ppm, sent into analyse in iodine column 9 and carry out analysing iodinate, sent into again in Filter dryer 10 and carried out filtration treatment, obtain thick elemental iodine, packaging, product can be obtained, concentration as the iodin-containing liquid after the cyclic absorption of detection is less than 600ppm's, then returned to absorption tower and carry out cyclic absorption process.The oxygenant added in above-mentioned is chlorine, clorox, hydrogen peroxide, potassium permanganate, and add-on is that every rising foam flow liquid adds 15g; Above-mentioned adds the aqueous solution that reductive agent is Sodium Nitrite, and add-on is to make at the bottom of absorbing tower flow rate of liquid out be 4m
3/ min.
Embodiment 6
As shown in Figure 3, a kind of cooling tower reclaiming iodine employing in phosphorus production first step cooling tower water coolant, by grade cooling tower 11, two grade cooling tower 12, N grade cooling tower 13 and by bottom a grade cooling tower 11, bottom two grade cooling towers 12, the settling bowl 15 that couples together bottom N grade cooling tower 13 forms, the baffle plate 18 wherein extended bottom settling bowl 15 between a grade cooling tower 11 and two grade cooling towers 12.And then make to enter settling bowl from the liquid after the absorption of absorption tower top spray, can according to the difference containing iodine concentration in absorption liquid in settling bowl, separate containing the higher solution of iodine concentration and lower the carrying out of Biodine, namely be exactly the first order absorption in absorption tower and secondary absorbed absorb to N level the absorption liquid obtained and be separated, and then improve when recycling the iodine in absorption liquid, the iodine content in mother liquor can be made higher, and then improve the rate of recovery of iodine, reduce cost recovery; And also make the iodin-containing liquid that in absorption tower, concentration is lower can obtain cyclic absorption timely, shorten the cycle that iodine reclaims, reduce energy consumption.Described settling bowl 15 is made up of the nearly mouth layer bottom cooling tower, the mud layer 16 bottom settling bowl 15, the supernatant layer 17 between mud layer 16 and nearly mouth layer.Described settling bowl 15, is provided with overflow port 14 in supernatant layer 17 and the intersection of nearly mouth layer.Described overflow port 14 is arranged on the two ends, left and right of settling bowl 15.Described baffle plate extends to the bottom near settling bowl.The distance that described baffle plate extends near the bottom of settling bowl is 2-4cm.Described overflow port is arranged on one, the settling bowl left side, to be arranged on the right of settling bowl one.
Embodiment 7
As Fig. 1, Fig. 2, shown in Fig. 3, its device reclaiming iodine in phosphorus production first step cooling tower water coolant carries out the method reclaiming iodine in phosphorus production first step cooling tower water coolant, by arranging a baffle plate in the settling bowl of the bottom of cooling tower, baffle plate extends to the bottom of settling bowl, there is the gap of about 3cm bottom settling bowl, again its recovery method according to above-described embodiment 5 is recycled, and then the rate of recovery of iodine is improved, the cost recovery of iodine obtains reduction, shorten the cycle index of the recirculated water in iodine recovery process, reduce recovery energy consumption.
Claims (10)
1. one kind is reclaimed the method for iodine in phosphorus production first step cooling tower water coolant, it is characterized in that, one grade cooling tower water coolant is proceeded to settlement treatment in subsider, again its supernatant liquor is overflowed in oxidation trough by the mode of overflow, and oxygenant is added in oxidation trough, and adopt agitator stir process 2-3h, again liquid Pulp pump is squeezed into and resolve in groove, and from air separation plant, pass into air carry out dissection process, and the gas containing iodine is entered absorption tower, cyclic absorption is carried out by reductive agent, until the concentration of iodine in solution reach >=600ppm after, carried out analysing iodinate again, obtain iodine, and iodine is put into drying plant and carry out drying, packaging, the thick iodine of finished product can be obtained.
2. the as claimed in claim 1 method reclaiming iodine in phosphorus production first step cooling tower water coolant, is characterized in that, described oxygenant is one or several of chlorine, clorox, hydrogen peroxide, potassium permanganate, Potassium Iodate or Potcrate.
3. the method reclaiming iodine in phosphorus production first step cooling tower water coolant as claimed in claim 1, is characterized in that, described reductive agent is the aqueous solution of a kind of or two kinds of mixing in sulfurous acid, Sodium Nitrite.
4. the method reclaiming iodine in phosphorus production first step cooling tower water coolant as claimed in claim 1, it is characterized in that, the add-on of described oxygenant is that every rising foam flow liquid adds 10-30g oxygenant.
5. the as claimed in claim 1 method reclaiming iodine in phosphorus production first step cooling tower water coolant, is characterized in that, the add-on of described reductive agent is to make at the bottom of absorbing tower flow rate of liquid out be 1-5m
3/ min.
6. one kind is reclaimed the device of iodine in phosphorus production first step cooling tower water coolant, it is characterized in that, containing Yellow phosphorus furnace (1), Yellow phosphorus furnace (1) is communicated with cooling tower (2), cooling tower (2) and sedimentation aerator tank (3), sedimentation aerator tank (3) is connected with oxidation trough (4) by overflow manner, oxidation trough (4) is communicated with desorption tower (5), desorption tower (5) is communicated with air separation plant (6), desorption tower (5) is connected with absorption tower (7), absorption tower (7) is connected with detector (8), detector (8) is connected with iodin-containing liquid outlet, iodin-containing liquid outlet is divided into and meets iodine concentration and be more than or equal to iodin-containing liquid outlet (a) of 600ppm and meet iodin-containing liquid outlet (b) that iodine concentration is less than 600ppm, iodin-containing liquid outlet (a) with analyse iodine column (9) and be connected, iodin-containing liquid outlet (b) is connected with absorption tower (7), analyse iodine column (9) to be connected with Filter dryer (10).
7. one kind is reclaimed the cooling tower that in phosphorus production first step cooling tower water coolant, iodine adopts, it is characterized in that, by a grade cooling tower (11), two grade cooling towers (12), N grade cooling tower (13) and a grade cooling tower (11) bottom, two grade cooling towers (12) bottom, the settling bowl (15) that couples together of N grade cooling tower (13) bottom forms, the baffle plate (18) of wherein extension bottom settling bowl (15) between a grade cooling tower (11) and two grade cooling towers (12).
8. the cooling tower reclaiming iodine employing in phosphorus production first step cooling tower water coolant as claimed in claim 7, it is characterized in that, described settling bowl (15) is made up of the mud layer (16) of the nearly mouth layer bottom cooling tower, settling bowl (15) bottom, the supernatant layer (17) between mud layer (16) and nearly mouth layer.
9. the cooling tower reclaiming iodine employing in phosphorus production first step cooling tower water coolant as claimed in claim 8, it is characterized in that, described settling bowl (15), is provided with overflow port (14) in supernatant layer (17) and the intersection of nearly mouth layer.
10. the cooling tower reclaiming iodine employing in phosphorus production first step cooling tower water coolant as claimed in claim 9, it is characterized in that, described overflow port (14) is arranged on the two ends, left and right of settling bowl (15).
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510602870.0A CN105217574A (en) | 2015-09-21 | 2015-09-21 | A kind ofly reclaim the method for iodine and the cooling tower of device and employing in phosphorus production first step cooling tower water coolant |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510602870.0A CN105217574A (en) | 2015-09-21 | 2015-09-21 | A kind ofly reclaim the method for iodine and the cooling tower of device and employing in phosphorus production first step cooling tower water coolant |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3857704A (en) * | 1971-03-05 | 1974-12-31 | Bp Chem Int Ltd | Mercury recovery process |
| CN1676461A (en) * | 2003-09-10 | 2005-10-05 | 陈肖虎 | Method for extracting iodine from rejected material generated during production of phosphor product from iodine-containing phosphorus ore |
| CN102730642A (en) * | 2012-06-29 | 2012-10-17 | 贵州开磷（集团）有限责任公司 | Gas-liquid mixed extraction iodine recovery technology |
-
2015
- 2015-09-21 CN CN201510602870.0A patent/CN105217574A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3857704A (en) * | 1971-03-05 | 1974-12-31 | Bp Chem Int Ltd | Mercury recovery process |
| CN1676461A (en) * | 2003-09-10 | 2005-10-05 | 陈肖虎 | Method for extracting iodine from rejected material generated during production of phosphor product from iodine-containing phosphorus ore |
| CN102730642A (en) * | 2012-06-29 | 2012-10-17 | 贵州开磷（集团）有限责任公司 | Gas-liquid mixed extraction iodine recovery technology |
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