CN105537004A - Preparing method for phosphogypsum flotation collector - Google Patents
Preparing method for phosphogypsum flotation collector Download PDFInfo
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- CN105537004A CN105537004A CN201510930935.4A CN201510930935A CN105537004A CN 105537004 A CN105537004 A CN 105537004A CN 201510930935 A CN201510930935 A CN 201510930935A CN 105537004 A CN105537004 A CN 105537004A
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- Prior art keywords
- ardealite
- flotation collector
- flotation
- hydrogen
- hydrogen peroxide
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D1/00—Flotation
- B03D1/001—Flotation agents
- B03D1/018—Mixtures of inorganic and organic compounds
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D2201/00—Specified effects produced by the flotation agents
- B03D2201/02—Collectors
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- Inorganic Chemistry (AREA)
- Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)
Abstract
The invention discloses a preparing method for a phosphogypsum flotation collector, particularly relates to a method for preparing the phosphogypsum flotation collector by utilizing isooctyl amine as a raw material, and belongs to the technical field of chemical and mineral processing. The flotation collector is formed by synthesizing raw materials of isooctyl amine, acrylonitrile, a catalyst, hydrogen and hydrogen peroxide. The preparing method has the beneficial technical effects that the chemical performance is stable, and water solubility is good; the environment influence is small, viscosity of generated bubbles is low, and the higher acid resistance and unavoidable ion resistance capacity are achieved; the floatation collector can be used for direct flotation of phosphogypsum, the higher selectivity and good collecting are achieved, the flotation time can be obviously shortened, the concentrate grade is improved, and the grade of tailings is reduced.
Description
Technical field
The invention discloses a kind of octodrine that utilizes and prepare the method for ardealite collecting agent for raw material, belong to chemical industry, technical field of mineral processing.
Background technology
Ardealite is with the accessory substance produced during sulfuric acid treating phosphorite in Wet-process phosphoric acid (WPPA) process, and its main component is calcium sulfate, often produces 1 ton of phosphoric acid (in 100%P2O5) and produces 4.8 ~ 5.0 tons of ardealites.Its main component sulphur, calcium and gypsum resource have multiple potential use, again containing phosphorus, fluorine, organic matter, alkali metal, silicon, iron, aluminium, magnesium etc. to environment and the harmful impurity of comprehensive utilization and radionuclide etc.Facilitate phosphoric acid by wet process industrial expansion along with domestic and international to the continuous growth of high-concentration phosphate compound fertilizers demand, the discharge capacity of ardealite is in the trend significantly increased progressively year by year.The whole nation in 2014 is produced discharge capacity per year and has been reached 7,600 ten thousand tons, but the ardealite that the whole nation utilizes for 2014 is only 2,300 ten thousand tons.So far, the accumulative ardealite of stacking in the whole nation, more than 300,000,000 tons, both brought immense pressure to environment, had also become a large bottleneck of restriction high-concentration phosphate compound fertilizers industry sustainable development simultaneously.
Therefore, for obtaining the doulbe-sides' victory of economic benefit and environmental protection, be necessary the paces of the resource Appropriate application accelerating ardealite.Impurity in ardealite becomes the key factor affecting its resource Appropriate application, needs to carry out upgrading removal of impurities by the technological means of flotation to ardealite.Due to slag dam backwater low ph value in production process of phosphoric acid, the characteristic of high metal ion, existing technique of preparing adopts the conventional collecting agent such as kiber alkyl amine or ether amine to carry out flotation, calcium sulphate dihydrate grade in the mineral processing index obtained in mine tailing is higher reaches 30% ~ 50%, have impact on the rate of recovery of sulfate dihydrate, the consumption of collecting agent is also comparatively large simultaneously, increases flotation cost.
The present invention is by the screening to raw material, the exploration of collecting agent synthesis condition, obtain a kind of collecting agent of efficient flotation separation ardealite, collector dosage can be effectively reduced, reduce flotation tailing grade, improve the concentrate calcium sulphate dihydrate rate of recovery, reduce enterprise's production cost, there is good industrial application value.
Summary of the invention
Object of the present invention to the deficiency of ardealite upgrading removal of impurities, by the exploration of collecting agent synthesis condition, provides a kind of collecting agent of efficient flotation separation ardealite for current conventional collecting agent.This collecting agent stable chemical performance, ambient influnence is little, can effectively reduce the consumption of floating agent, reduces flotation tailing grade, improves the flotation operation rate of recovery, reduces enterprise and produces this, have higher industrial application value.
Ardealite flotation collector preparation method of the present invention is achieved by the following technical programs, wherein comprises following technological process:
(1) octodrine, acrylonitrile, hydrogen, hydrogen peroxide raw material is adopted directly to synthesize ardealite flotation collector.
(2) octodrine is warmed to uniform temperature, slowly adds acrylonitrile under agitation, reaction 30 ~ 60min, obtains amine nitrile.
(3) under certain reaction pressure, temperature and mixing speed condition, adding hydrogen and controlling the reaction time is 1 ~ 2h, obtains hydrogenation reaction thing.
(4) in hydrogenation reaction thing, slowly add hydrogen peroxide, be warming up to 60 ~ 75 DEG C, control reaction time 4 ~ 6h, namely obtain ardealite flotation collector.
Uniform temperature described in step 2 is 30 ~ 50 DEG C, and the mass ratio of octodrine and acrylonitrile is 2.23 ~ 2.45.
Pressure described in step 3 is 1.5 ~ 3.5MPa, and temperature is 130 DEG C ~ 170 DEG C, and speed of agitator is 600 ~ 1000R/min, and hydrogen is 2 ~ 5% of amine nitrile inventory.
Hydrogen peroxide mass concentration described in step 4 is 30%, and hydrogen peroxide is 0.1% ~ 10% of hydrogenation feed liquid quality.
Owing to have employed technique scheme, beneficial effect of the present invention is as follows: 1) by the nucleophilic hydrogenation reaction to octodrine and acrylonitrile, can generate the collecting agent having two amidos, can reduce the consumption of collecting agent in the process of flotation phosphate gypsum; 2) by adding hydrogen peroxide reaction, making the amine key in part collecting agent carry out peroxidating, generating peroxidating base, can improve the collecting ability of collecting agent, the bubble viscosity that simultaneously can reduce collecting agent is little, has stronger acid resistance and anti-unavoidable ion ability.
Detailed description of the invention
A kind of ardealite flotation collector preparation method, comprises following characteristics technique:
(1) octodrine, acrylonitrile, hydrogen, hydrogen peroxide raw material is adopted directly to synthesize ardealite flotation collector.
(2) octodrine is warmed to uniform temperature, slowly adds acrylonitrile under agitation, reaction 30 ~ 60min, obtains amine nitrile.
(3) under certain reaction pressure, temperature and mixing speed condition, adding hydrogen and controlling the reaction time is 1 ~ 2h, obtains hydrogenation reaction thing.
(4) in hydrogenation reaction thing, slowly add hydrogen peroxide, be warming up to 60 ~ 75 DEG C, control reaction time 4 ~ 6h, namely obtain ardealite flotation collector.
Uniform temperature described in step 2 is 30 ~ 50 DEG C, and the mass ratio of octodrine and acrylonitrile is 2.23 ~ 2.45.
Pressure described in step 3 is 1.5 ~ 3.5MPa, and temperature is 130 DEG C ~ 170 DEG C, and speed of agitator is 600 ~ 1000R/min, and hydrogen is 2 ~ 5% of amine nitrile inventory.
Hydrogen peroxide concentration described in step 4 is 30%, and hydrogen peroxide is 0.1% ~ 10% of hydrogenation feed liquid quality.
Below by instantiation, technical scheme of the present invention is described in further detail.
Case study on implementation 1.
(1) 100g octodrine is warmed to 35 DEG C, stirs, slowly add acrylonitrile 44.44g, to add after acrylonitrile reaction 40 minutes, stop heating, centrifugal go out amine nitrile.
(2) by centrifugal go out amine nitrile be placed in autoclave, be added to the pressure of 2.0MPa, start stir, mixing speed is 700R/min, after being warming up to 140 DEG C, add hydrogen, hydrogen is 3% of amine nitrile inventory, and keep pressure stability, reaction 1h, cooling discharging.
(3) slip after above-mentioned hydrogenation is got 50g, be warming up to 60 DEG C, slowly add 0.25g hydrogen peroxide, control temperature is 65 DEG C, reacts 4 hours, namely obtains ardealite flotation collector.
Case study on implementation 2.
(1) 100g octodrine is warmed to 45 DEG C, stirs, slowly add acrylonitrile 41.67g, to add after acrylonitrile reaction 50 minutes, stop heating, centrifugal go out amine nitrile.
(2) by centrifugal go out amine nitrile be placed in autoclave, be added to the pressure of 3.0MPa, start stir, mixing speed is 800R/min, after being warming up to 150 DEG C, adds hydrogen, and keeps pressure stability, reaction 1.5h, cooling discharging.
(3) slip after above-mentioned hydrogenation is got 50g, be warming up to 60 DEG C, slowly add 0.5g hydrogen peroxide, control temperature is 70 DEG C, reacts 5 hours, namely obtains ardealite flotation collector.
Case study on implementation 3.
The phosphoric acid plant getting Yunnan Tian'an Chemical Co., Ltd. produces ardealite 200g, and mineral chemical composition is:
| Main component | Calcium sulphate dihydrate (%) | Silica (%) |
| Analysis result | 83.26 | 13.76 |
Adding 600g fresh water (FW) makes ardealite pulp density be 25%, using the flotation collector that the aqueous solution that the ardealite flotation collector of case study on implementation 1 makes 1% is tested as this, experimental procedure is one roughing and primary cleaning, in roughly selecting, the consumption of flotation collector is 180g/t, selected not adding medicine.Gained concentrate chemical composition is:
| Main component | Calcium sulphate dihydrate (%) | Silica (%) |
| Analysis result | 95.28 | 2.87 |
The concentrate rate of recovery is 98.33%.
Case study on implementation 4.
The phosphoric acid plant getting Yunnan Tian'an Chemical Co., Ltd. produces ardealite 200g, and mineral chemical composition is:
| Main component | Calcium sulphate dihydrate (%) | Silica (%) |
| Analysis result | 83.19 | 14.33 |
Adding 600g fresh water (FW) makes ardealite pulp density be 25%, using the flotation collector that the aqueous solution that the ardealite flotation collector of case study on implementation 1 makes 1% is tested as this, experimental procedure is one roughing and primary cleaning, in roughly selecting, the consumption of flotation collector is 160g/t, selected not adding medicine.Gained concentrate chemical composition is:
| Main component | Calcium sulphate dihydrate (%) | Silica (%) |
| Analysis result | 95.65 | 2.56 |
The concentrate rate of recovery is 97.71%.
Percentage in above-mentioned case study on implementation is mass percent.
The above; be only the specific embodiment of the present invention, but protection scope of the present invention is not limited thereto, is anyly familiar with those skilled in the art in the technical scope that the present invention discloses; change can be expected easily or replace, all should be encompassed within protection scope of the present invention.Therefore, protection scope of the present invention should described be as the criterion with the protection domain of claim.
Claims (4)
1. the method prepared of ardealite flotation collector, is characterized in that: comprise following characteristics technique:
(1) octodrine, acrylonitrile, hydrogen, hydrogen peroxide raw material is adopted directly to synthesize ardealite flotation collector;
(2) octodrine is warmed to uniform temperature, slowly adds acrylonitrile under agitation, reaction 30 ~ 60min, obtains amine nitrile;
(3) under certain reaction pressure, temperature and mixing speed condition, adding hydrogen and controlling the reaction time is 1 ~ 2h, obtains hydrogenation reaction thing;
(4) in hydrogenation reaction thing, slowly add hydrogen peroxide, be warming up to 60 ~ 75 DEG C, control reaction time 4 ~ 6h, namely obtain ardealite flotation collector.
2. the method prepared of a kind of ardealite flotation collector according to claim 1, it is characterized in that: the uniform temperature described in step 2 is 30 ~ 50 DEG C, the mass ratio of octodrine and acrylonitrile is 2.23 ~ 2.45.
3. the method prepared of a kind of ardealite flotation collector according to claim 1, it is characterized in that: the pressure described in step 3 is 1.5 ~ 3.5MPa, temperature is 130 DEG C ~ 170 DEG C, and speed of agitator is 600 ~ 1000R/min, and hydrogen is 2% ~ 5% of amine nitrile inventory.
4. the method prepared of a kind of ardealite flotation collector according to claim 1, it is characterized in that: the hydrogen peroxide concentration described in step 4 is 30%, hydrogen peroxide is 0.1% ~ 10% of hydrogenation feed liquid quality.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113695085A (en) * | 2021-06-29 | 2021-11-26 | 郑州大学 | Phosphogypsum desiliconization and decarbonization combined collecting agent and solution preparation method and application thereof |
| CN115672568A (en) * | 2022-12-30 | 2023-02-03 | 矿冶科技集团有限公司 | Method for preparing low-silicon high-grade phosphogypsum by reverse flotation and desiliconization of phosphogypsum waste residues |
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| CN1186455A (en) * | 1995-06-07 | 1998-07-01 | Cytec技术有限公司 | Method of depressing non-sulfide silicate gangue minerals |
| CN101585017A (en) * | 2009-06-05 | 2009-11-25 | 湖南有色金属研究院 | Ore-selecting method of difficultly-selected copper zinc sulphur ore |
| CN102319633A (en) * | 2011-10-09 | 2012-01-18 | 中蓝连海设计研究院 | A kind of method for floating of phosphogypsum slag |
| CN102500469A (en) * | 2011-10-20 | 2012-06-20 | 曲靖师范学院 | Phosphogypsum reverse flotation, desilication and impurity removal process |
| CN103172289A (en) * | 2013-04-08 | 2013-06-26 | 杨连树 | Ardealite block moss mildew inhibitor and preparation method thereof |
| CN103861740A (en) * | 2014-03-25 | 2014-06-18 | 中南大学 | Method for flotation separation of copper sulfide and lead concentrate processed through pre-oxidation |
| CN103894276A (en) * | 2014-03-03 | 2014-07-02 | 武平紫金矿业有限公司 | Grinding separation technology for silver-containing polymetallic ore |
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2015
- 2015-12-15 CN CN201510930935.4A patent/CN105537004B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1186455A (en) * | 1995-06-07 | 1998-07-01 | Cytec技术有限公司 | Method of depressing non-sulfide silicate gangue minerals |
| CN101585017A (en) * | 2009-06-05 | 2009-11-25 | 湖南有色金属研究院 | Ore-selecting method of difficultly-selected copper zinc sulphur ore |
| CN102319633A (en) * | 2011-10-09 | 2012-01-18 | 中蓝连海设计研究院 | A kind of method for floating of phosphogypsum slag |
| CN102500469A (en) * | 2011-10-20 | 2012-06-20 | 曲靖师范学院 | Phosphogypsum reverse flotation, desilication and impurity removal process |
| CN103172289A (en) * | 2013-04-08 | 2013-06-26 | 杨连树 | Ardealite block moss mildew inhibitor and preparation method thereof |
| CN103894276A (en) * | 2014-03-03 | 2014-07-02 | 武平紫金矿业有限公司 | Grinding separation technology for silver-containing polymetallic ore |
| CN103861740A (en) * | 2014-03-25 | 2014-06-18 | 中南大学 | Method for flotation separation of copper sulfide and lead concentrate processed through pre-oxidation |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113695085A (en) * | 2021-06-29 | 2021-11-26 | 郑州大学 | Phosphogypsum desiliconization and decarbonization combined collecting agent and solution preparation method and application thereof |
| CN115672568A (en) * | 2022-12-30 | 2023-02-03 | 矿冶科技集团有限公司 | Method for preparing low-silicon high-grade phosphogypsum by reverse flotation and desiliconization of phosphogypsum waste residues |
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| CN105537004B (en) | 2018-04-06 |
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