CN109954588B - Sesquioxide inhibitor and preparation method and application thereof - Google Patents
Sesquioxide inhibitor and preparation method and application thereof Download PDFInfo
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- CN109954588B CN109954588B CN201711404492.0A CN201711404492A CN109954588B CN 109954588 B CN109954588 B CN 109954588B CN 201711404492 A CN201711404492 A CN 201711404492A CN 109954588 B CN109954588 B CN 109954588B
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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
- B03D2201/06—Depressants
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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
- B03D2203/00—Specified materials treated by the flotation agents; specified applications
- B03D2203/02—Ores
- B03D2203/04—Non-sulfide ores
- B03D2203/06—Phosphate ores
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Abstract
The invention relates to a sesquioxide inhibitor which is prepared from the following raw materials in parts by mass: 100 parts of sodium lignosulfonate; 100-200 parts of water; 1-3 parts of ammonium persulfate; 12-20 parts of acrylic acid; 25-35 parts of aminopropyltriethoxysilane. The invention also discloses a preparation method of the sesquioxide inhibitor, which comprises the following steps: reacting sodium lignosulfonate and an acrylic acid monomer under the action of an initiator ammonium persulfate at a certain temperature to obtain a material A, performing hydrolysis reaction on aminopropyltriethoxysilane at a certain temperature in a strong alkali solution to obtain a material B, mixing and stirring the material A and the material B uniformly, and drying to obtain the inhibitor. The inhibitor has good selective inhibition effect on sesquioxide in phosphorite, can effectively reduce the content of aluminum oxide and ferric oxide in the phosphorite, improves the quality of phosphate concentrate, and reduces the production cost in the subsequent acid making process.
Description
Technical Field
The invention belongs to the field of phosphorite beneficiation, and particularly relates to an sesquioxide inhibitor in phosphorite and a preparation method thereof.
Background
China is a big agricultural country and needs a large amount of chemical fertilizers and other phosphorus chemical products. Phosphate rock is used as a main raw material of phosphate fertilizer, and at present, no substance can replace the phosphate rock in the world. However, with the rapid development of phosphorus chemical industry, the exploitation amount of phosphorite is increased rapidly, high-grade phosphorite in China is exhausted gradually, the components in the phosphorite become complex, and the impurity content is higher and higher, especially the content of iron oxide and aluminum oxide. Iron and aluminum impurities can seriously affect the quality of phosphoric acid and the quality of further purification processing and high-end products. When sesquioxide R is present in the phosphate concentrate2O3When the content of (B) exceeds 3wt%, the productivity of the fertilizer is greatly reduced. To reduce R2O3The solubility of the phosphoric acid is required to be pre-sintered and then treated by nitric acid, so that the production cost of the wet-process phosphoric acid is greatly increased.
Sesquioxide iron oxide and aluminium oxide mainly come from the slime in the phosphorite, and the slime accessible is reselected and is desliming the mode and remove most, but collophanite weathering degree is high, and the slime content is big, and to collophanite at present, there is not suitable equipment to carry out desliming grading, can cause the direct loss of a large amount of phosphorus minerals like this. The reduction of the sesquioxide content in the phosphorite by the flotation method is a more effective scheme and mainly comprises direct flotation and reverse flotation. Chinese patent publication No. CN102179308B discloses a beneficiation method for removing iron and aluminum sesquioxide from collophanite, which uses a cationic collector to perform reverse flotation of sesquioxide under acidic conditions. Chinese patent publication No. CN102716806B discloses a method for removing magnesium oxide, iron oxide and aluminum oxide sesquioxide from middle-low grade phosphorite simultaneously by a double reverse flotation process, wherein sesquioxide is removed under acidic conditions by using a step method and using cations as collecting agents. The sesquioxide is removed by reverse flotation with the cationic collecting agent, the separation efficiency is high, the using amount of the collecting agent is small, but the cationic collecting agent is greatly influenced by slime, the foam is sticky, the trough is easy to run, and the method cannot be applied to the industry at present.
The direct flotation of phosphate rock is a mature process, which uses water glass as an inhibitor to remove silicate gangue under alkaline conditions. However, the inhibitor water glass has weak inhibiting effect on the sesquioxide and has low separation efficiency on the sesquioxide. At present, research on removing the sesquioxide mainly focuses on the aspects of the process and the collecting agent, and research on the sesquioxide inhibitor is not reported.
Disclosure of Invention
The invention aims to provide a novel high-efficiency sesquioxide inhibitor which is used for positive flotation of phosphorite, inhibiting sesquioxide gangue and realizing effective separation of the phosphorite and the sesquioxide.
Another object of the present invention is to provide a process for the preparation of said inhibitors.
It is a further object of the present invention to provide the use of said inhibitors.
The object of the present invention is achieved by the following means. The invention relates to a sesquioxide inhibitor which is characterized by being prepared from the following raw materials in parts by mass:
100 parts of sodium lignosulfonate;
100-200 parts of water;
1-3 parts of ammonium persulfate;
12-20 parts of acrylic acid;
25-35 parts of aminopropyltriethoxysilane.
The sesquioxide inhibitor provided by the invention has a further preferable technical scheme that the sesquioxide inhibitor is prepared from the following raw materials in parts by mass:
100 parts of sodium lignosulfonate;
150 parts of water;
2 parts of ammonium persulfate;
16 parts of acrylic acid;
30 parts of aminopropyltriethoxysilane.
The invention also discloses a preparation method of the sesquioxide inhibitor, which is characterized in that the raw materials are prepared according to the mass ratio, and the preparation method comprises the following steps:
(1) adding sodium lignosulfonate and water into a reaction kettle, stirring and dissolving, adding an initiator ammonium persulfate, raising the temperature of a reaction system to 60-90 ℃, adding acrylic acid, and carrying out heat preservation stirring reaction for 3-5 hours to obtain a material A;
(2) dissolving aminopropyltriethoxysilane in a strong alkali solution in another reaction kettle, and stirring for hydrolysis reaction for 2-4 hours at the temperature of 40-70 ℃ to obtain a material B;
(3) and mixing the material A and the material B, uniformly stirring at 80-100 ℃, and drying to obtain the inhibitor.
The preparation method of the sesquioxide inhibitor provided by the invention has the further preferable technical scheme that: the temperature of the reaction system in the step (1) is 80 ℃, and the reaction time is 4 hours. The strong alkali solution in the step (2) is a sodium hydroxide solution, a strong potassium oxide solution or a sodium carbonate solution. The concentration of the strong alkali solution in the step (2) is 1-3 mol/L, and 2mol/L is further preferable. The reaction temperature in the step (2) was 55 ℃ and the reaction time was 3 hours.
The sesquioxide inhibitor can be used as sesquioxide R in phosphorite flotation2O3The separation of phosphorite and sesquioxide is realized. When the inhibitor is used, the dosage of the inhibitor is preferably 200-2000 g/t, and the inhibitor is prepared into a solution to be directly added into a phosphorite direct flotation operation flow when the inhibitor is used.
Compared with the prior art, the invention has the beneficial effects that:
(1) the inhibitor raw material and the preparation method thereof are simple, and the raw material source is wide.
(2) The inhibitor has good selective inhibition effect on sesquioxide, is convenient to use and has low dosage.
(3) The sesquioxide inhibitor is used in the phosphorite positive flotation, so that the sesquioxide in the phosphorite can be removed in the flotation process, and the quality of the phosphate concentrate is effectively improved.
(4) The reduction of the contents of iron and aluminum in the phosphate concentrate can simplify the subsequent wet acid making process and reduce the production cost.
(5) The sesquioxide inhibitor provided by the invention has the advantages of high separation efficiency and simplicity in operation, and can effectively reduce the content of sesquioxide through positive flotation, and the industrial production is easy to realize.
Detailed Description
The invention is further illustrated by, but is not limited to, the following examples. All parts and percentages in the examples are by mass unless otherwise specified.
Example 1, a sesquioxide inhibitor is prepared from the following raw materials in parts by mass:
100 parts of sodium lignosulfonate;
100 parts of water;
1 part of ammonium persulfate;
12 parts of acrylic acid;
25 parts of aminopropyltriethoxysilane.
The preparation method comprises the following steps:
(1) adding sodium lignosulfonate and water into a reaction kettle, stirring and dissolving, adding an initiator ammonium persulfate, raising the temperature of a reaction system to 60 ℃, adding acrylic acid, keeping the temperature, stirring and reacting for 3 hours to obtain a material A;
(2) dissolving aminopropyltriethoxysilane in 1mol/L strong potassium oxide solution in another reaction kettle, and stirring at 40 deg.C for hydrolysis reaction for 2 hr to obtain material B;
(3) and mixing the material A and the material B, uniformly stirring at 80 ℃, and drying to obtain the inhibitor.
The sesquioxide inhibitor is used as sesquioxide R in phosphorite flotation2O3The flotation inhibitor and the application of the flotation inhibitor to the separation of phosphorite and sesquioxide. The dosage of the inhibitor is 200 g/t, and the inhibitor is prepared into solution to be directly added into the direct flotation operation flow of phosphorite when in use.
Embodiment 2, a sesquioxide inhibitor is prepared by the following raw materials by mass:
100 parts of sodium lignosulfonate;
200 parts of water;
3 parts of ammonium persulfate;
20 parts of acrylic acid;
and 35 parts of aminopropyltriethoxysilane.
The preparation method comprises the following steps:
(1) adding sodium lignosulfonate and water into a reaction kettle, stirring and dissolving, adding an initiator ammonium persulfate, raising the temperature of a reaction system to 90 ℃, adding acrylic acid, keeping the temperature, stirring and reacting for 5 hours to obtain a material A;
(2) dissolving aminopropyltriethoxysilane in 1.5mol/L sodium hydroxide solution in another reaction kettle, and stirring at 70 deg.C for hydrolysis reaction for 4 hr to obtain material B;
(3) and mixing the material A and the material B, uniformly stirring at 100 ℃, and drying to obtain the inhibitor.
The sesquioxide inhibitor is used as sesquioxide R in phosphorite flotation2O3The flotation inhibitor and the application of the flotation inhibitor to the separation of phosphorite and sesquioxide. The dosage of the inhibitor is 2000 g/t, and the inhibitor is prepared into solution to be directly added into the direct flotation operation flow of phosphorite when in use.
Embodiment 3, a sesquioxide inhibitor is prepared by the following raw materials by mass:
100 parts of sodium lignosulfonate;
120 parts of water;
1.5 parts of ammonium persulfate;
18 parts of acrylic acid;
28 parts of aminopropyltriethoxysilane.
The preparation method comprises the following steps:
(1) adding sodium lignosulfonate and water into a reaction kettle, stirring and dissolving, adding an initiator ammonium persulfate, raising the temperature of a reaction system to 70 ℃, adding acrylic acid, keeping the temperature, stirring and reacting for 3.5 hours to obtain a material A;
(2) dissolving aminopropyltriethoxysilane in 3mol/L sodium carbonate solution in another reaction kettle, and stirring at 60 deg.C for hydrolysis reaction for 2.5 hr to obtain material B;
(3) and mixing the material A and the material B, uniformly stirring at 98 ℃, and drying to obtain the inhibitor.
The sesquioxide inhibitor is used as sesquioxide R in phosphorite flotation2O3The flotation inhibitor and the application of the flotation inhibitor to the separation of phosphorite and sesquioxide. The dosage of the inhibitor is 1500 g/t, and the inhibitor is prepared into solution to be directly added into the direct flotation operation flow of phosphorite when in use.
Example 4, a sesquioxide inhibitor is prepared from the following raw materials in parts by mass:
100 parts of sodium lignosulfonate;
150 parts of water;
2 parts of ammonium persulfate;
16 parts of acrylic acid;
30 parts of aminopropyltriethoxysilane.
The preparation method comprises the following steps:
(1) adding sodium lignosulfonate and water into a reaction kettle, stirring and dissolving, adding an initiator ammonium persulfate, raising the temperature of a reaction system to 80 ℃, adding acrylic acid, keeping the temperature, stirring and reacting for 4 hours to obtain a material A;
(2) dissolving aminopropyltriethoxysilane in 2mol/L sodium hydroxide solution, strong potassium oxide solution or sodium carbonate solution in another reaction kettle, and performing hydrolysis reaction for 3 hours under stirring at 55 ℃ to obtain a material B;
(3) and mixing the material A and the material B, uniformly stirring at 80-100 ℃, and drying to obtain the inhibitor.
The sesquioxide inhibitor is used as sesquioxide R in phosphorite flotation2O3The flotation inhibitor and the application of the flotation inhibitor to the separation of phosphorite and sesquioxide. The dosage of the inhibitor is 1000 g/t, and the inhibitor is prepared into solution to be directly added into the direct flotation operation flow of phosphorite when in use.
Example 5: comparative experiment
Preparation of mono-and sesquioxide inhibitors
Adding 100 parts of sodium lignosulphonate and 150 parts of water into a reaction kettle, stirring and dissolving, adding 2 parts of initiator ammonium persulfate, raising the temperature of a reaction system to 80 ℃, adding 16 parts of acrylic acid, keeping the temperature at 80 ℃, stirring and reacting for 4 hours to obtain a material A; dissolving 30 parts of aminopropyltriethoxysilane in 2mol/L sodium hydroxide solution in another reaction kettle, heating the reaction system to 55 ℃, and carrying out hydrolysis reaction for 3 hours under stirring at the temperature to obtain a material B; and mixing the material A and the material B, uniformly stirring at 80-100 ℃, and drying to obtain the sesquioxide inhibitor.
Second, experiment 1: flotation test of certain collophanite in Guizhou: p in raw ore2O5Grade of 23.52%, Fe2O32.38% of Al2O3The content was 4.68%. The flotation test is a double-reverse flow, an ore mill is used for milling an ore sample to be 60 percent of-0.074 mm, and water is addedAnd (3) pulp mixing is carried out until the concentration of the pulp is 40%, 4Kg/t phosphoric acid, 0.8Kg/t sodium carbonate and 5Kg/t water glass are added for pulp mixing for 2 minutes, 1.8Kg/t fatty acid soap collecting agent is added for pulp mixing for 2 minutes, and foam flotation is carried out for 5-8 minutes.
Third, experiment 2: flotation test of certain collophanite in Guizhou: p in raw ore2O5Grade of 24.22%, Fe2O32.38% of Al2O3The content was 4.68%. The flotation test is a single positive flotation process, an ore mill is used for grinding an ore sample to 85% of-0.074 mm, water is added for size mixing until the concentration of ore pulp is 40%, 3kg/t of sodium carbonate and 5kg/t of water glass are added for size mixing for 2 minutes, 0.6kg/t of sesquioxide inhibitor is added for size mixing for 2 minutes, 1.8kg/t of fatty acid soap collecting agent is added for size mixing for 2 minutes, and foam flotation is carried out for 5-8 minutes.
Fourth, results of comparative experiments 1 and 2: experiment 1, no synthetic inhibitor is added, experiment 2, 0.6kg/t of sesquioxide inhibitor is added, other flotation conditions are the same, and the flotation result of certain collophanite in Guizhou is shown in Table 1.
TABLE 1 flotation results for a certain collophanite in Guizhou
As can be seen from Table 1, the sesquioxide R in the phosphate concentrate without the use of the inhibitor according to the invention2O3（Fe2O3+ Al2O3) Content of (b) 4.37%, after inhibition with the present invention, sesquioxide R in phosphate concentrate2O3The content of (B) was 2.95%. When the sesquioxide inhibitor is used, high-quality phosphate concentrate can be obtained, the grade of the phosphate concentrate is improved, and sesquioxide R in the phosphate concentrate is improved2O3The content of (a) is effectively low.
Fifth, experiment 3: flotation test of some collophanite in Sichuan: p in raw ore2O5Grade of 27.83%, Fe2O32.36% of Al2O3The content was found to be 3.49%. The flotation test is a single positive flotation process, an ore mill is used for grinding an ore sample to-0.074 mm accounting for 82 percent, water is added for size mixing until the concentration of ore pulp is 40 percent, and 2kg/t of sodium carbonate and 6kg/t of sodium carbonate are addedAnd (3) mixing the water glass for 2 minutes in kg/t, adding a fatty acid soap collecting agent for 1.3kg/t, mixing for 2 minutes, and performing foam flotation for 5-8 minutes.
Sixthly, experiment 4: flotation test of some collophanite in Sichuan: p in raw ore2O5Grade of 27.83%, Fe2O32.36% of Al2O3The content was found to be 3.49%. The flotation test is a single positive flotation process, an ore mill is used for grinding an ore sample to be-0.074 mm accounting for 82%, water is added for size mixing until the concentration of ore pulp is 40%, 2kg/t of sodium carbonate and 6kg/t of water glass are added for size mixing for 2 minutes, 0.5kg/t of sesquioxide inhibitor is added for size mixing for 2 minutes, 1.3kg/t of fatty acid soap collecting agent is added for size mixing for 2 minutes, and foam flotation is carried out for 5-8 minutes.
Seventhly, results of comparative experiments 3 and 4: experiment 3 does not double the half-oxide inhibitor, experiment 4 adds 0.5kg/t of the half-oxide inhibitor, other flotation conditions are the same, and the flotation results of Sichuan gum phosphorus are shown in Table 2.
TABLE 2 flotation results of certain Sichuan collophanite
The comparative experiment of the embodiment shows that the sesquioxide inhibitor prepared by the invention has a remarkable inhibiting effect in phosphorite flotation.
Claims (10)
1. The sesquioxide inhibitor is characterized by being prepared from the following raw materials in parts by mass:
100 parts of sodium lignosulfonate;
100-200 parts of water;
1-3 parts of ammonium persulfate;
12-20 parts of acrylic acid;
25-35 parts of aminopropyltriethoxysilane.
2. The sesquioxide inhibitor according to claim 1, characterized in that the inhibitor is prepared from the following raw materials in parts by mass:
100 parts of sodium lignosulfonate;
150 parts of water;
2 parts of ammonium persulfate;
16 parts of acrylic acid;
30 parts of aminopropyltriethoxysilane.
3. The preparation method of the sesquioxide inhibitor according to claim 1 or 2, characterized in that raw materials are prepared according to the mass ratio, and the preparation method comprises the following steps:
(1) adding sodium lignosulfonate and water into a reaction kettle, stirring and dissolving, adding an initiator ammonium persulfate, raising the temperature of a reaction system to 60-90 ℃, adding acrylic acid, and carrying out heat preservation stirring reaction for 3-5 hours to obtain a material A;
(2) dissolving aminopropyltriethoxysilane in a strong alkali solution in another reaction kettle, and stirring for hydrolysis reaction for 2-4 hours at the temperature of 40-70 ℃ to obtain a material B;
(3) and mixing the material A and the material B, uniformly stirring at 80-100 ℃, and drying to obtain the inhibitor.
4. The method of claim 3, wherein the inhibitor is selected from the group consisting of: the temperature of the reaction system in the step (1) is 80 ℃, and the reaction time is 4 hours.
5. The method of claim 3, wherein the inhibitor is selected from the group consisting of: the strong alkali solution in the step (2) is a sodium hydroxide solution, a strong potassium oxide solution or a sodium carbonate solution.
6. The method of claim 3 or 5, wherein the step of preparing the sesquioxide inhibitor comprises: the concentration of the strong alkali solution in the step (2) is 1-3 mol/L.
7. The method of claim 6, wherein the inhibitor is selected from the group consisting of: the concentration of the strong alkali solution in the step (2) is 2 mol/L.
8. The method of claim 3, wherein the reaction temperature in step (2) is 55 ℃ and the reaction time is 3 hours.
9. An sesquioxide inhibitor as defined in claim 1 or 2 or as defined in any one of claims 3 to 8 as sesquioxide R in phosphorite flotation2O3The flotation inhibitor and the application of the flotation inhibitor to the separation of phosphorite and sesquioxide.
10. Use according to claim 9, characterized in that: the dosage of the inhibitor is 200-2000 g/t, and the inhibitor is prepared into a solution to be directly added into the direct flotation operation flow of phosphorite when in use.
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| US4229287A (en) * | 1978-12-04 | 1980-10-21 | Engelhard Minerals & Chemicals Corporation | Tin flotation |
| CN101234366A (en) * | 2007-07-31 | 2008-08-06 | 中南大学 | Reverse flotation iron increase and silicon removing method for refractory limonite |
| CN101791592B (en) * | 2010-02-07 | 2012-12-19 | 紫金矿业集团股份有限公司 | Positive flotation method of low grade refractory phosphate ores |
| CN102029226B (en) * | 2010-12-13 | 2013-03-20 | 中国海洋石油总公司 | Collophanite flotation collector and application thereof |
| CN103588935B (en) * | 2013-11-14 | 2016-03-02 | 湖北工业大学 | Take acrylic acid wastewater as the method that modified lignosulfonate water reducing agent prepared by raw material |
| CN103657870B (en) * | 2013-12-03 | 2016-02-10 | 安徽朝山新材料股份有限公司 | A kind of auriferous pyrite capture reagent for gold and preparation method thereof |
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