CN107055495A - A kind of acid phosphorus-containing wastewater is used for the method for phosphorus ore de-magging - Google Patents
A kind of acid phosphorus-containing wastewater is used for the method for phosphorus ore de-magging Download PDFInfo
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- CN107055495A CN107055495A CN201710278085.3A CN201710278085A CN107055495A CN 107055495 A CN107055495 A CN 107055495A CN 201710278085 A CN201710278085 A CN 201710278085A CN 107055495 A CN107055495 A CN 107055495A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/01—Treating phosphate ores or other raw phosphate materials to obtain phosphorus or phosphorus compounds
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05B—PHOSPHATIC FERTILISERS
- C05B17/00—Other phosphatic fertilisers, e.g. soft rock phosphates, bone meal
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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Abstract
The invention provides a kind of method that acid phosphorus-containing wastewater is used for phosphorus ore de-magging, this method is, by acid phosphorus-containing wastewater and mid low grade phosphate rock stirring mixing, to be then sent to subsider, natural subsidence adds flocculant flocculating setting, then press filtration, washing, drying, that is, obtain de-magging phosphorus concentrate.The method applied in the present invention realizes the acid phosphorus-containing wastewater zero-emission of Phosphate Fertilizer Nitrate with Frozen Method production technology, saves production cost, magnesia in mid low grade phosphate rock can be down to less than 0.5% by the present invention, is adapted to production N:The requirement of the nitrophosphate fertilizer of P≤2.0, new approach is explored for the acid phosphorus-containing wastewater produced by processing nitrophosphate fertilizer technique.
Description
Technical field
The present invention relates to chemical technology field, being specifically related to a kind of acid phosphorus-containing wastewater is used for the method for phosphorus ore de-magging.
Technical background
In recent years, with production-scale continuous expansion, fertilizer enterprises, which are increasingly becoming, uses water rich and influential family, then becomes blowdown
And heavy polluter, nitrophosphate fertilizer is there is also the emission problem of phosphorus-containing wastewater, therefore, how rational utilization of water resources, the row of reduction
The matter of utmost importance that dirt faces as fertilizer enterprises.
Acid phosphorus-containing wastewater produced by existing nitrophosphate fertilizer technique is washed including the water shutoff of pump machine, equipment flushing water, waste gas
Water etc. is washed, it is at present, external, domestic de- for phosphorus ore without the acid phosphorus-containing wastewater produced by utilizing Phosphate Fertilizer Nitrate with Frozen Method technique
The technique of magnesium, traditional acid phosphorus-containing wastewater processing method is：Calcium hydroxide and ammonia are added in sewage, adjusted to pH=7.5
~8.0, calcium phosphate precipitation is generated, and flocculant flocculating setting is added, then separated and recovered.
Patent CN201410312375.1 discloses the production waste recovery and treatment method containing high ammonia nitrogen and nitrate nitrogen, should
Method is the pretreatment process that heat exchange+precipitation+chemical oxidation+filtering is used for nitrophosphate fertilizer sewage treatment process, gained mistake
Filter production water is directly entered electrodialysis, and concentrated water is stored in concentration liquid case through electrodialysis cell and is pumped up to Nitro Phosphate Unit following
Ring is used, desalination 75% or so after electrodialysis cell desalination of the fresh water through two-stage series connection, then continues desalination by two steps ro.
But the processing method investment cost is high, and the active principle in sewage is not fully utilized.
Production waste and each flooring hydrops in Norway's Hydro Phosphate Fertilizer Nitrate with Frozen Method technique, the production nitrophosphate fertilizer technique
Enter geosyncline through floor drain, dashpot is squeezed into pump, lead to ammonia regulation pH=3~5, then with being pumped to pH control flumes, then logical ammonia tune
PH=4~5 are saved, by potential difference overflow to scale traps premixed device, flocculant is added and is settled, separated and recovered and reuse；This
The peace and quiet water purification installation of increase after technique is improved, realizes that phosphorus-containing wastewater shunting is handled, improves water quality, meet technological requirement, and
Run, drip, leak in strict control production, reduce sewage generating capacity.But the processing method technique is complex, logical ammonia is also needed
The increase production cost such as sewage pH is adjusted, and solid content accumulation also wears out pump shaft, axle sleeve, filler etc..
The content of the invention
The present invention is solves above-mentioned deficiency of the prior art, and there is provided one for progress inventive improvements in existing technology
Kind of acid phosphorus-containing wastewater is used for the method for phosphorus ore de-magging, this method by the acid phosphorus-containing wastewater produced by nitrophosphate fertilizer technique and
Mid low grade phosphate rock stirring mixing, delivers to natural subsidence or flocculating setting, then press filtration, washs, and drying prepares high-quality de-magging phosphorus
Concentrate, the acid phosphorus-containing wastewater produced by the present invention can make in nitrophosphate fertilizer technique is turned waste into wealth, and has saved the life of phosphorus ore de-magging
Cost is produced, meanwhile, obtained de-magging phosphorus concentrate quality is high, can meet the production requirement of low N/P nitrophosphate fertilizers.
The invention provides a kind of acid phosphorus-containing wastewater be used for phosphorus ore de-magging method, by acid phosphorus-containing wastewater and in low product
Position phosphorus ore stirring mixing, is then sent to subsider sedimentation, and then press filtration is washed, and drying obtains de-magging phosphorus concentrate.
Further, it is described to be settled into natural subsidence.
Further, the described addition flocculant that is settled into is settled.
Further, described flocculant is configured to 1~5% for solid flocculant and washing lotion are delivered into flocculating agent formulation groove
Solution.
Further, described solid flocculant is bodied ferric sulfate.
Specifically, invention, which provides a kind of acid phosphorus-containing wastewater, is used for the method for phosphorus ore de-magging, comprise the following steps：
(1) mid low grade phosphate rock and acid phosphorus-containing wastewater are delivered into de-magging groove, is sufficiently stirred for, treats that pH value rises to 2.0~2.5
Afterwards, reaction paste is delivered into subsider；
(2) flocculant or natural subsidence are added into step (1) subsider, 1~3 hour sedimentation time, pressure is then sent to
Filter process；
(3) slurry for settling trench bottom is returned to production system, is washed with water and washed with filter press, press filtration, filtrate is pumped to,
Washing lotion, which returns to flocculating agent formulation groove, to be used to prepare flocculant, and washing is dried up with compressed air again after terminating, and then draws off filter cake,
Drying, that is, obtain de-magging phosphorus concentrate.
It is preferred that, it the described method comprises the following steps：
(1) mid low grade phosphate rock and acid phosphorus-containing wastewater are delivered into de-magging groove, are sufficiently stirred for, will after pH value rises to 2.0
Reaction paste delivers to subsider；
(2) flocculant or natural subsidence are added into step (1) subsider, 2 hours sedimentation times, press filtration work is then sent to
Sequence；
(3) slurry for settling trench bottom is returned to production system, is washed with water and washed with filter press, press filtration, filtrate is pumped to,
Washing lotion, which returns to flocculating agent formulation groove, to be used to prepare flocculant, and washing is dried up with compressed air again after terminating, and then draws off filter cake,
Drying, that is, obtain de-magging phosphorus concentrate.
Further, described acid phosphorus-containing wastewater is produced by existing nitrophosphate fertilizer technique and Wet Processes of Phosphoric Acid
Phosphorus-containing wastewater, including the water shutoff of pump machine, equipment flushing water, waste gas washings.
Further, the mass ratio of described mid low grade phosphate rock and acid phosphorus-containing wastewater is 1:1~3.
Further, the mass ratio of flocculant described above and reaction paste is 0~3:100.
Due to using above-mentioned technical proposal, the present invention has the advantages that：
The present invention is mixed using by acid phosphorus-containing wastewater and mid low grade phosphate rock stirring produced in nitrophosphate fertilizer technique,
Flocculation settling tank is then sent to, flocculant flocculating setting or natural subsidence is added, then after press filtration, washing, drying, drying
De-magging phosphorus concentrate is obtained, is had the characteristics that：
(1) process problem of acid phosphorus-containing wastewater in nitrophosphate fertilizer technique is not only solved using the process, and is subtracted
The consumption of few calcium hydroxide and ammonia, it is cost-effective.
(2) after mid low grade phosphate rock is handled by acid phosphorus-containing wastewater, magnesia can be down to less than 0.5%, so as to drop
Low acid hydrolysis solution, neutralize slip viscosity, adapt to production N：The requirement of the nitrophosphate fertilizer of P≤2.0.
(3) acid phosphorus-containing wastewater is used for mid low grade phosphate rock (P2O527.13%th, CaO 46.19%, MgO 5.20%)
De-magging, the phosphorus ore after acid phosphorus-containing wastewater de-magging contains P2O534.43%th, CaO 46.59%, MgO 0.30%, can meet nitre
The production requirement of sour phosphate fertilizer, and reclaim the phosphorus in acid phosphorus-containing wastewater.
Compared with prior art, the present invention is low during directly the acid phosphorus-containing wastewater produced by Phosphate Fertilizer Nitrate with Frozen Method is used for
Grade phosphorus mine de-magging, the treatment of wastes with processes of wastes against one another is turned waste into wealth；Make full use of H in acid phosphorus-containing wastewater+Ion carrys out decomposing medium and low grade
Middle impurity dolomite, reduces calcium hydroxide and ammonia consumption, cost-effective, realizes Phosphate Fertilizer Nitrate with Frozen Method production technology acidity and contains
Phosphorus sewage zero-discharge, technique is simple, easy to operate, is particularly suitable for industrial production application.
The present invention has also listed part test example, it is intended to illustrate this to preferably illustrate the beneficial effect of innovation and creation
The technique effect of invention, never limits the scope of the present invention.
Technological parameter is studied
Test example 1：Influence of the technological parameter to de-magging phosphorus concentrate
PH value, flocculant concentration, reaction rotating speed, reaction temperature, the mass ratio of mid low grade phosphate rock and acid phosphorus-containing wastewater,
Influence of the mass ratio of flocculant and reaction paste to de-magging phosphorus concentrate：
Under the conditions of ceteris paribus, pH value, flocculant concentration, reaction rotating speed, reaction temperature, middle-low grade phosphorus are investigated
Influence of the mass ratio of the mass ratio of ore deposit and acid phosphorus-containing wastewater, flocculant and reaction paste to de-magging phosphorus concentrate, the results are shown in Table 1
~3：
The different PH of table 1, influence of the flocculant concentration to de-magging phosphorus concentrate
The differential responses rotating speed of table 2, the influence of reaction temperature de-magging phosphorus concentrate
The mass ratio of the mass ratio of the different mid low grade phosphate rocks of table 3 and acid phosphorus-containing wastewater, flocculant and reaction paste is de-
The influence of magnesium phosphorus concentrate
As can be known from the above table, when pH value is less than 2.0, mid low grade phosphate rock and acid phosphorus-containing wastewater neutralization reaction are incomplete,
When pH value is higher than 2.5, has calcium ion and other impurities are separated out, influence de-magging phosphorus concentrate, be unfavorable for de-magging, therefore react most
Good PH is 2~2.5；And reaction temperature, reaction rotating speed are higher, its reaction is more abundant, but when temperature is higher than 50 DEG C, rotating speed is higher than
100r/min, reaction is not further added by slightly reducing on the contrary, therefore 40~50 DEG C of optimal reaction temperature, and optimum response rotating speed is 50~
100r/min；The mass ratio of mid low grade phosphate rock and acid phosphorus-containing wastewater is 1:1~3 is optimal, low, reacts not thoroughly, high then anti-
It should take a turn for the worse；The mass ratio of flocculant and reaction paste is 0~3:100 is optimal.
By to different PH, flocculant concentration, reaction rotating speed, reaction temperature, mid low grade phosphate rock and acid phosphorous dirt
The investigation of the mass ratio of the mass ratio of water, flocculant and reaction paste, draw when PH between 2-2.5, reaction rotating speed be 50~
100r/min, reaction temperature are between 40~50 DEG C, the mass ratio of mid low grade phosphate rock and acid phosphorus-containing wastewater is 1:1~3, wad a quilt with cotton
The mass ratio of solidifying agent and reaction paste is 0~3:100 is optimal, and its content of magnesia is between 0.29~0.48%, five oxidations two
Phosphorus content between 32.94~34.56%, illustrate using this interval pH value, flocculant concentration, reaction rotating speed, reaction temperature,
Each quality of material is than the de-magging phosphorus concentrate quality better of production, acid phosphorus-containing wastewater phosphorous recovery height.
Test example 2：Comparative experimental research
Test group 1：The de-magging phosphorus concentrate prepared according to the process route disclosed in patent CN201510239368.8.
Test group 2：The de-magging phosphorus concentrate prepared according to present invention process route.
De-magging phosphorus concentrate obtained by above-mentioned test group is detected that testing result is shown in Table 4：
Table 4：De-magging phosphorus concentrate assay
| Detection project | Test group 1 | Test group 2 |
| P2O5/ % | 32.56 | 34.34 |
| MgO/% | 0.40 | 0.31 |
As can be seen from the above table, the present invention uses de-magging phosphorus concentrate grade made from technique higher.
Embodiment
The preparation of flocculant：By bodied ferric sulfate 300g and washing lotion 10kg deliver to flocculating agent formulation groove be configured to 3% it is molten
Liquid.
The preparation of the de-magging phosphorus concentrate of embodiment 1
(1) mid low grade phosphate rock 10kg and acidity phosphorus-containing wastewater 10kg are delivered into de-magging groove, is sufficiently stirred for, treats that pH value rises to
After 2.0, reaction paste is delivered into subsider；
(2) by reaction slurry natural subsidence 3 hours in step (1), it is then sent to press filtration process；
(3) slurry for settling trench bottom is returned to production system, is washed with water and washed with filter press, press filtration, filtrate is pumped to,
Washing lotion, which returns to flocculating agent formulation groove, to be used to prepare flocculant, and washing is dried up with compressed air again after terminating, and then draws off filter cake,
Drying, that is, obtain de-magging phosphorus concentrate.
Its testing result contains P2O533.89%th, CaO 45.90%, MgO 0.29%, the filtrate detection inspection of filter press discharge
Survey result and contain P2O50.47%th, CaO 0.56%, MgO 0.72%, meet the production requirement of low N/P nitrophosphate fertilizers.
The preparation of the de-magging phosphorus concentrate of embodiment 2
(1) mid low grade phosphate rock 10kg and acidity phosphorus-containing wastewater 20kg are delivered into de-magging groove, is sufficiently stirred for, treats that pH value rises to
After 2.4, reaction paste is delivered into subsider；
(2) flocculant 0.3kg is added into step (1) flocculation settling tank, flocculating setting time 2 h is then sent to pressure
Filter process；
(3) by the slurry of flocculating setting trench bottom with filter press is pumped to, press filtration, filtrate returns to production system, then uses water
Washing, washing lotion, which returns to flocculating agent formulation groove, to be used to prepare flocculant, and washing is dried up with compressed air, then drawn off again after terminating
Filter cake, drying, that is, obtain de-magging phosphorus concentrate.
Its testing result contains P2O534.43%th, CaO 46.20%, MgO 0.30%, the filtrate detection inspection of filter press discharge
Survey result and contain P2O50.46%th, CaO 0.54%, MgO 0.71%, meet the production requirement of low N/P nitrophosphate fertilizers.
The preparation of the de-magging phosphorus concentrate of embodiment 3
(1) mid low grade phosphate rock 10kg and acidity phosphorus-containing wastewater 30kg are delivered into de-magging groove, is sufficiently stirred for, treats that pH value rises to
After 2.3, reaction paste is delivered into subsider；
(2) 0.8kg flocculants are added into step (1) flocculation settling tank, 1 hour flocculating setting time, be then sent to
Press filtration process；
(3) by the slurry of flocculating setting trench bottom with filter press is pumped to, press filtration, filtrate returns to production system, then uses water
Washing, washing lotion, which returns to flocculating agent formulation groove, to be used to prepare flocculant, and washing is dried up with compressed air, then drawn off again after terminating
Filter cake, drying, that is, obtain de-magging phosphorus concentrate.
Its testing result contains P2O534.26%th, CaO 46.35%, MgO 0.32%, the filtrate detection inspection of filter press discharge
Survey result and contain P2O50.43%th, CaO 0.51%, MgO 0.69%, meet the production requirement of low N/P nitrophosphate fertilizers.
Claims (7)
1. a kind of acid phosphorus-containing wastewater is used for the method for phosphorus ore de-magging, it is characterised in that：Comprise the following steps：
(1) mid low grade phosphate rock and acid phosphorus-containing wastewater are delivered into de-magging groove, are sufficiently stirred for, after pH value rises to 2.0~2.5,
Reaction paste is delivered into subsider；
(2) flocculant or natural subsidence are added into step (1) subsider, 1~3 hour sedimentation time, press filtration work is then sent to
Sequence；
(3) slurry for settling trench bottom is returned to production system, is washed with water and washed with filter press, press filtration, filtrate is pumped to, washing lotion
Returning to flocculating agent formulation groove is used to prepare flocculant, and washing is dried up with compressed air again after terminating, and then draws off filter cake, is dried
It is dry, that is, obtain de-magging phosphorus concentrate.
2. acid phosphorus-containing wastewater according to claim 1 is used for the method for phosphorus ore de-magging, it is characterised in that：Described sedimentation
For one kind in natural subsidence and flocculant sedimentation.
3. acid phosphorus-containing wastewater according to claim 2 is used for the method for phosphorus ore de-magging, it is characterised in that：Described flocculation
Agent is that solid flocculant and washing lotion are delivered into the solution that flocculating agent formulation groove is configured to 1~5%.
4. acid phosphorus-containing wastewater according to claim 3 is used for the method for phosphorus ore de-magging, it is characterised in that：Described solid
Flocculant is bodied ferric sulfate.
5. the method for phosphorus ore de-magging is used for according to any described acid phosphorus-containing wastewaters of claim 1-4, it is characterised in that：It is described
Acid phosphorus-containing wastewater be the waste water that produces in nitrophosphate fertilizer preparation technology, including the water shutoff of pump machine, equipment flushing water, waste gas washing
Water.
6. acid phosphorus-containing wastewater according to claim 1 is used for the method for phosphorus ore de-magging, it is characterised in that：It is low in described
The mass ratio of grade phosphorus mine and acid phosphorus-containing wastewater is 1:1~3.
7. the acid phosphorus-containing wastewater according to claim 1 or 3 is used for the method for phosphorus ore de-magging, it is characterised in that described
The mass ratio of flocculant and reaction paste is 0~3:100.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109455684A (en) * | 2018-12-12 | 2019-03-12 | 贵州芭田生态工程有限公司 | Utilize the method for the thick calcium nitrate preparation phosphorus concentrate of nitrophosphate fertilizer by-product |
| CN109701344A (en) * | 2019-01-04 | 2019-05-03 | 贵州芭田生态工程有限公司 | A kind of recycling of calcined by rotary kiln flue gas, purification method |
| CN113461202A (en) * | 2021-06-24 | 2021-10-01 | 宜都兴发化工有限公司 | Resource treatment method for high phosphorus, high calcium and high magnesium |
| CN115520843A (en) * | 2022-09-30 | 2022-12-27 | 昆明川金诺化工股份有限公司 | Method for improving phosphorus yield of low-magnesium phosphorite produced by chemical magnesium removal of magnesium-containing phosphorite |
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| CN106187327A (en) * | 2016-07-12 | 2016-12-07 | 贵州芭田生态工程有限公司 | Mid low grade phosphate rock prepares method and the compound fertilizer product of high contents of calcium and magnesium compound fertilizer |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109455684A (en) * | 2018-12-12 | 2019-03-12 | 贵州芭田生态工程有限公司 | Utilize the method for the thick calcium nitrate preparation phosphorus concentrate of nitrophosphate fertilizer by-product |
| CN109701344A (en) * | 2019-01-04 | 2019-05-03 | 贵州芭田生态工程有限公司 | A kind of recycling of calcined by rotary kiln flue gas, purification method |
| CN113461202A (en) * | 2021-06-24 | 2021-10-01 | 宜都兴发化工有限公司 | Resource treatment method for high phosphorus, high calcium and high magnesium |
| CN113461202B (en) * | 2021-06-24 | 2023-10-27 | 宜都兴发化工有限公司 | High-phosphorus and high-calcium magnesium recycling treatment method |
| CN115520843A (en) * | 2022-09-30 | 2022-12-27 | 昆明川金诺化工股份有限公司 | Method for improving phosphorus yield of low-magnesium phosphorite produced by chemical magnesium removal of magnesium-containing phosphorite |
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