CN108585146B - Preparation method of titanium-containing composite ferric polysulfate flocculant - Google Patents
Preparation method of titanium-containing composite ferric polysulfate flocculant Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 44
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 38
- 239000010936 titanium Substances 0.000 title claims abstract description 38
- 229910052719 titanium Inorganic materials 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title abstract description 6
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 69
- 238000000034 method Methods 0.000 claims abstract description 40
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 28
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 27
- SURQXAFEQWPFPV-UHFFFAOYSA-L iron(2+) sulfate heptahydrate Chemical compound O.O.O.O.O.O.O.[Fe+2].[O-]S([O-])(=O)=O SURQXAFEQWPFPV-UHFFFAOYSA-L 0.000 claims abstract description 21
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 16
- 230000003647 oxidation Effects 0.000 claims abstract description 14
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 14
- 230000002378 acidificating effect Effects 0.000 claims abstract description 13
- XTEGARKTQYYJKE-UHFFFAOYSA-M Chlorate Chemical compound [O-]Cl(=O)=O XTEGARKTQYYJKE-UHFFFAOYSA-M 0.000 claims abstract description 8
- IOVCWXUNBOPUCH-UHFFFAOYSA-M Nitrite anion Chemical compound [O-]N=O IOVCWXUNBOPUCH-UHFFFAOYSA-M 0.000 claims abstract description 5
- 238000006555 catalytic reaction Methods 0.000 claims abstract description 5
- 239000000243 solution Substances 0.000 claims description 51
- 235000010215 titanium dioxide Nutrition 0.000 claims description 36
- 239000002253 acid Substances 0.000 claims description 23
- 239000002699 waste material Substances 0.000 claims description 23
- 238000006243 chemical reaction Methods 0.000 claims description 18
- 238000003756 stirring Methods 0.000 claims description 14
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 12
- 239000001301 oxygen Substances 0.000 claims description 12
- 229910052760 oxygen Inorganic materials 0.000 claims description 12
- 230000001590 oxidative effect Effects 0.000 claims description 10
- 239000007800 oxidant agent Substances 0.000 claims description 9
- 238000004519 manufacturing process Methods 0.000 claims description 7
- 238000007865 diluting Methods 0.000 claims description 6
- 238000004090 dissolution Methods 0.000 claims description 6
- LPXPTNMVRIOKMN-UHFFFAOYSA-M sodium nitrite Chemical compound [Na+].[O-]N=O LPXPTNMVRIOKMN-UHFFFAOYSA-M 0.000 claims description 6
- BZSXEZOLBIJVQK-UHFFFAOYSA-N 2-methylsulfonylbenzoic acid Chemical compound CS(=O)(=O)C1=CC=CC=C1C(O)=O BZSXEZOLBIJVQK-UHFFFAOYSA-N 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 3
- 235000010288 sodium nitrite Nutrition 0.000 claims description 3
- 239000007864 aqueous solution Substances 0.000 claims description 2
- 239000013078 crystal Substances 0.000 claims description 2
- RUTXIHLAWFEWGM-UHFFFAOYSA-H iron(3+) sulfate Chemical compound [Fe+3].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O RUTXIHLAWFEWGM-UHFFFAOYSA-H 0.000 abstract description 29
- 229910000360 iron(III) sulfate Inorganic materials 0.000 abstract description 29
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 22
- 230000000694 effects Effects 0.000 abstract description 11
- 238000005189 flocculation Methods 0.000 abstract description 5
- 230000016615 flocculation Effects 0.000 abstract description 5
- 238000000746 purification Methods 0.000 abstract description 4
- 238000007146 photocatalysis Methods 0.000 abstract description 3
- 230000001699 photocatalysis Effects 0.000 abstract description 3
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 abstract description 3
- 239000003929 acidic solution Substances 0.000 abstract 1
- 239000008394 flocculating agent Substances 0.000 description 10
- 239000007788 liquid Substances 0.000 description 8
- 239000000701 coagulant Substances 0.000 description 4
- 239000011790 ferrous sulphate Substances 0.000 description 4
- 235000003891 ferrous sulphate Nutrition 0.000 description 4
- 229910000359 iron(II) sulfate Inorganic materials 0.000 description 4
- QJZYHAIUNVAGQP-UHFFFAOYSA-N 3-nitrobicyclo[2.2.1]hept-5-ene-2,3-dicarboxylic acid Chemical compound C1C2C=CC1C(C(=O)O)C2(C(O)=O)[N+]([O-])=O QJZYHAIUNVAGQP-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000004021 humic acid Substances 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- 230000015271 coagulation Effects 0.000 description 2
- 238000005345 coagulation Methods 0.000 description 2
- 239000003651 drinking water Substances 0.000 description 2
- 235000020188 drinking water Nutrition 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000005086 pumping Methods 0.000 description 2
- 239000010865 sewage Substances 0.000 description 2
- 239000006228 supernatant Substances 0.000 description 2
- 229910000349 titanium oxysulfate Inorganic materials 0.000 description 2
- 239000005995 Aluminium silicate Substances 0.000 description 1
- 241000195493 Cryptophyta Species 0.000 description 1
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 229940037003 alum Drugs 0.000 description 1
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 235000012211 aluminium silicate Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 238000005202 decontamination Methods 0.000 description 1
- 230000003588 decontaminative effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000001877 deodorizing effect Effects 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 1
- VLTRZXGMWDSKGL-UHFFFAOYSA-M perchlorate Inorganic materials [O-]Cl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-M 0.000 description 1
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- 239000011550 stock solution Substances 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/5236—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents
- C02F1/5245—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents using basic salts, e.g. of aluminium and iron
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Separation Of Suspended Particles By Flocculating Agents (AREA)
Abstract
A method for preparing a titanium-containing composite ferric polysulfate flocculant relates to the field of preparation of ferric polysulfate, and comprises the following steps: firstly, preparing sol containing nano titanium dioxide. And adding sulfuric acid into the titanium dioxide sol to obtain the acidic nano titanium dioxide sol. And secondly, preparing the composite polymeric ferric sulfate flocculant. Dissolving ferrous sulfate heptahydrate by using an acidic solution containing nano titanium oxide. The composite polymeric ferric sulfate is prepared by adopting a chlorate oxidation method, a hydrogen peroxide oxidation method or a nitrite catalysis method. The prepared composite polymeric ferric sulfate contains nano titanium dioxide, has photocatalysis effect besides flocculation effect, and has excellent purification effect on micro-polluted, low-temperature and low-turbidity raw water with low COD.
Description
Technical Field
The present invention relates to the field of polymeric ferric sulfate preparation.
Background
Inorganic polymeric coagulants and flocculants are widely used in the treatment of drinking water and sewage. Because the residual aluminum has direct biological toxicity, the ferric salt coagulant gradually replaces the application of the aluminum salt coagulant in water treatment. The polyferric sulfate flocculant belongs to a novel, high-quality and high-efficiency ferric salt inorganic polymeric flocculant, and has the advantages of excellent coagulation performance, dense alum floc and high settling velocity; has obvious effects of removing turbidity, decoloring, deoiling, dehydrating, degerming, deodorizing, removing algae, removing COD, BOD and heavy metal ions in water and the like. However, the existing ferric salt flocculating agent has to be improved in the effects of purifying micro-polluted, low-temperature and low-turbidity raw water and low COD. Aiming at the problems, the invention provides a flocculating agent containing titanium polymeric ferric sulfate for efficiently purifying drinking water and sewage and a preparation method thereof.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a preparation method of a titanium-containing composite ferric polysulfate flocculant, and the prepared composite ferric polysulfate contains nano titanium dioxide, has photocatalysis in addition to flocculation, and has excellent purification effect on raw water with micro pollution, low temperature, low turbidity and low COD.
In order to solve the technical problem, the invention is solved by the following technical scheme: a method for preparing a titanium-containing composite ferric polysulfate flocculant comprises the following steps: step A: obtaining titanium ore acidolysis solution, titanium white waste acid and ferrous sulfate heptahydrate by a sulfuric acid method titanium dioxide production process; and B: diluting the titanium ore acidolysis solution to 5g/L to 25g/L in terms of the mass of titanium dioxide; and C: placing the diluted titanium ore acidolysis solution into an aqueous solution at the temperature of between 40 and 100 ℃ and stirring for at least 1 hour to form titanium dioxide sol; step D: adding titanium dioxide waste acid into the titanium dioxide sol to obtain acidic nano titanium dioxide sol; step E: dissolving ferrous sulfate heptahydrate in acidic nano titanium dioxide sol at 40-100 deg.C for at least 1 hr; step F: and (3) obtaining a dissolved solution after the acid mixing and dissolving reaction of the ferrous sulfate heptahydrate and the acidic nano titanium dioxide sol is finished, and preparing the composite polymeric ferric sulfate from the dissolved solution by a chlorate oxidation method, a hydrogen peroxide oxidation method or a nitrite catalysis method.
In the above technical solution, preferably, in the step F, when a hydrogen peroxide oxidation method is adopted, the dissolving solution is added with hydrogen peroxide as an oxidant and oxygen is introduced, and the reaction is carried out at 80 ℃ for 10 hours to obtain the composite polymeric ferric sulfate.
In the above technical solution, preferably, in the step F, when a perchlorate oxidation method is adopted, the dissolved solution is added with sodium chlorate as an oxidant and high-pressure oxygen is introduced, and the reaction is carried out at 90 ℃ for 2 hours to obtain the composite polymeric ferric sulfate.
In the above technical scheme, preferably, in the step F, when a nitrite catalysis method is adopted, the solution is added with sodium nitrite and high-pressure oxygen is introduced, and the reaction is carried out at 90 ℃ and 0.2MPa for 4 hours to obtain the composite polymeric ferric sulfate.
In the technical scheme, preferably, the nano titanium dioxide accounts for 0.1-1% of the composite polymeric ferric sulfate in percentage by mass.
In the above technical solution, preferably, the titanium dioxide in the titanium ore acidolysis solution is anatase type titanium dioxide seed crystal.
In the above technical scheme, preferably, in the step C, the concentration of the titanium dioxide in the titanium dioxide sol is 0.5g/L to 5g/L based on the mass of the titanium dioxide.
In the technical scheme, the pH value of the dissolving solution is preferably 1-5.
The composite flocculant prepared by the invention has high purification efficiency on low-COD raw water; the flocculant only produces flocculent precipitate when purifying water, and the method of filtering, floating, settling and the like is used for separating impurities in water, so that the decontamination capability of small molecules and low-concentration organic matters is poor. And the nano titanium oxide is adsorbed on the ferric sulfate flocculating agent and is easy to separate from water. Meanwhile, the titanium white waste acid and the ferrous sulfate in a sulfuric acid method titanium dioxide factory are used, so that the recycling of the titanium white waste by-products is improved, the polymeric ferric sulfate flocculating agent with the same ferrous content is produced, the amount of the oxidant used in the invention is reduced, and the raw material cost is reduced. The titanium-containing composite polyferric flocculant produced by the invention has high stability, and can be used for directly producing polymeric ferric sulfate by using the waste and secondary ferrous sulfate of titanium white, because the waste and secondary ferrous sulfate contains a small amount of unhydrolyzed titanyl sulfate, titanium in the high-concentration flocculant can be hydrolyzed when the flocculant is used at a high pH value, so that the turbidity of treated water is increased. The nano titanium oxide contained in the process of oxidizing the ferrous sulfate promotes the hydrolysis of the titanyl sulfate, and improves the stability of the flocculant in the use process.
Compared with the prior art, the invention has the beneficial effects that: the prepared composite polymeric ferric sulfate contains nano titanium dioxide, has photocatalysis effect besides flocculation effect, and has excellent purification effect on micro-polluted, low-temperature and low-turbidity raw water with low COD.
Detailed Description
The present invention will be described in further detail with reference to specific embodiments.
Embodiment 1, a method for preparing a titanium-containing composite ferric polysulfate flocculant, which obtains titanium ore acidolysis solution, titanium white waste acid and ferrous sulfate heptahydrate through a sulfuric acid method titanium dioxide production process. Preparing sol containing nano titanium dioxide: diluting the titanium ore acidolysis solution with the concentration of 220g/L to 10g/L, slowly adding 1L of the diluted titanium ore acidolysis solution into 1L of water with the temperature of 50 ℃, and stirring for 5h to ensure that the solution becomes turbid. Adding 0.1L of 15% waste acid solution, and stirring uniformly for later use. The waste acid is sulfuric acid.
Preparing a composite polymeric ferric sulfate flocculating agent: 200g of ferrous sulfate heptahydrate is added into the acidic nano titanium dioxide sol for dissolution. The dissolving temperature is 40 ℃, and the dissolving time is 1 h. Adding oxidant hydrogen peroxide for oxidation, introducing oxygen, and reacting at 80 ℃ for 10h to obtain the composite polymeric ferric sulfate liquid. The nano titanium dioxide in the composite polymeric ferric sulfate accounts for 0.5 percent.
Embodiment 2, a method for preparing a titanium-containing composite ferric polysulfate flocculant, which obtains titanium ore acidolysis solution, titanium white waste acid and ferrous sulfate heptahydrate through a sulfuric acid method titanium dioxide production process. Preparing nano titanium dioxide sol: adding water to 0.1m3 titanium ore acidolysis solution with the concentration of 200g/L for dilution to 20g/L to obtain 1m3 titanium ore acidolysis solution; heating a reaction kettle containing water of 1m3 to 60 ℃, slowly adding the titanium ore acidolysis solution into the reaction kettle, stirring for 2 hours, adding 15% waste acid solution of 0.1m3 when the solution becomes turbid, and uniformly stirring to obtain the acidic titanium dioxide sol. The waste acid is sulfuric acid.
Preparing a composite polymeric ferric sulfate flocculating agent: adding 0.2t of ferrous sulfate heptahydrate into the acidic nano titanium dioxide sol for dissolving. The dissolving temperature is 60 ℃, and the dissolving time is 2 h. After the acid mixing and dissolving reaction reaches the end point, keeping the stirring speed at 45r/min, pumping the mixed and dissolved material into a circulating reaction tower by using a material pumping pump, wherein the circulating reaction tower is a tower which keeps circulation, adding 0.1 ton of sodium nitrite dissolved by water, opening a high-pressure oxygen switch, introducing high-pressure oxygen for reaction, wherein the reaction temperature is 90 ℃ at the beginning of the reaction, the reaction time is 4 hours, and the reaction pressure is 0.2MPa, and obtaining the composite polymeric ferric sulfate liquid after the reaction is finished. The nano titanium dioxide in the composite polymeric ferric sulfate accounts for 0.7 percent.
Embodiment 3, a method for preparing a titanium-containing composite ferric polysulfate flocculant, which obtains titanium ore acidolysis solution, titanium white waste acid and ferrous sulfate heptahydrate through a sulfuric acid method titanium dioxide production process. Preparing sol containing nano titanium dioxide: diluting the titanium ore acidolysis solution with the concentration of 100g/L to 5g/L, slowly adding 1L of the diluted titanium ore acidolysis solution into 1L of water with the temperature of 90 ℃, and stirring for 1h to ensure that the solution becomes turbid. Adding 0.2L of 10% waste acid solution, and stirring uniformly for later use. The waste acid is sulfuric acid.
Preparing a composite polymeric ferric sulfate flocculating agent: 300g of ferrous sulfate heptahydrate is added into the acidic nano titanium dioxide sol for dissolution. The dissolving temperature is 70 ℃, and the dissolving time is 1 h. Adding an oxidant sodium chlorate for oxidation, introducing high-pressure oxygen, and reacting for 2 hours at 90 ℃ to obtain the composite polymeric ferric sulfate liquid. The nano titanium dioxide in the composite polymeric ferric sulfate accounts for 0.4 percent.
Embodiment 4, a method for preparing a titanium-containing composite ferric polysulfate flocculant, which obtains titanium ore acidolysis solution, titanium white waste acid and ferrous sulfate heptahydrate through a sulfuric acid method titanium dioxide production process. Preparing sol containing nano titanium dioxide: diluting the titanium ore acidolysis solution with the concentration of 100g/L to 25g/L, slowly adding 1L of the diluted titanium ore acidolysis solution into 1L of water with the temperature of 100 ℃, and stirring for 5h to ensure that the solution becomes turbid. Adding 0.2L of 10% waste acid solution, and stirring uniformly for later use. The waste acid is sulfuric acid.
Preparing a composite polymeric ferric sulfate flocculating agent: 300g of ferrous sulfate heptahydrate is added into the acidic nano titanium dioxide sol for dissolution. The dissolving temperature is 100 ℃, and the dissolving time is 3 h. Adding an oxidant sodium chlorate for oxidation, introducing high-pressure oxygen, and reacting for 2 hours at 90 ℃ to obtain the composite polymeric ferric sulfate liquid. The nano titanium dioxide in the composite polymeric ferric sulfate accounts for 0.4 percent.
Embodiment 5, a method for preparing a titanium-containing composite ferric polysulfate flocculant, which obtains titanium ore acidolysis solution, titanium white waste acid and ferrous sulfate heptahydrate through a sulfuric acid method titanium dioxide production process. Preparing sol containing nano titanium dioxide: diluting the titanium ore acidolysis solution with the concentration of 100g/L to 5g/L, slowly adding 1L of the diluted titanium ore acidolysis solution into 1L of water with the temperature of 400 ℃, and stirring for 7h to ensure that the solution becomes turbid. Adding 0.2L of 10% waste acid solution, and stirring uniformly for later use. The waste acid is sulfuric acid.
Preparing a composite polymeric ferric sulfate flocculating agent: 300g of ferrous sulfate heptahydrate is added into the acidic nano titanium dioxide sol for dissolution. The dissolving temperature is 40 ℃, and the dissolving time is 6 h. Adding an oxidant sodium chlorate for oxidation, introducing high-pressure oxygen, and reacting for 2 hours at 90 ℃ to obtain the composite polymeric ferric sulfate liquid. The nano titanium dioxide in the composite polymeric ferric sulfate accounts for 0.4 percent.
And (3) testing the flocculation effect: the experimental water sample is prepared from kaolin and humic acid, wherein 1 g of humic acid is dissolved in 0.01 mol/L sodium hydroxide solution to obtain a humic acid stock solution, and the water quality indexes of the prepared simulated water sample are 13 NTU (turbidity), 8 in p H and 10 mg/L of TOC. In the coagulation experiment, 500 m L water sample is placed on a magnetic stirrer, coagulant is added under the condition of rapid stirring, after 2 min, the mixture is stirred at a low speed for 15 min, then the mixture is settled for 20 min, supernatant liquid is taken 2 cm below the liquid level, the turbidity of the supernatant liquid is measured by a turbidity meter, and the TOC content analysis is measured by a TOC-V analyzer. The data results in table 1 show that the composite flocculant provided by the present invention has excellent flocculation effect.
Table 1.
Claims (7)
1. A method for preparing a titanium-containing composite ferric polysulfate flocculant is characterized by comprising the following steps:
step A: obtaining titanium ore acidolysis solution, titanium white waste acid and ferrous sulfate heptahydrate by a sulfuric acid method titanium dioxide production process;
and B: diluting the titanium ore acidolysis solution to 5g/L to 25g/L in terms of the mass of titanium dioxide;
and C: placing the diluted titanium ore acidolysis solution into an aqueous solution at the temperature of between 40 and 100 ℃ and stirring for at least 1 hour to form titanium dioxide sol, wherein the titanium dioxide in the titanium ore acidolysis solution is anatase titanium dioxide seed crystal;
step D: adding titanium dioxide waste acid into the titanium dioxide sol to obtain acidic nano titanium dioxide sol;
step E: dissolving ferrous sulfate heptahydrate in acidic nano titanium dioxide sol at 40-100 deg.C for at least 1 hr;
step F: and (3) obtaining a dissolved solution after the acid mixing and dissolving reaction of the ferrous sulfate heptahydrate and the acidic nano titanium dioxide sol is finished, and preparing the composite ferric polysulfate from the dissolved solution by a chlorate oxidation method, a hydrogen peroxide oxidation method or a nitrite catalysis method.
2. The method according to claim 1, wherein in step F, when the hydrogen peroxide oxidation method is adopted, the solution is added with hydrogen peroxide as an oxidant, and oxygen is introduced, and the reaction is carried out at 80 ℃ for 10 hours to obtain the composite ferric polysulfate.
3. The method according to claim 1, wherein in the step F, when the chlorate oxidation method is adopted, the oxidant sodium chlorate is added into the solution, and high-pressure oxygen is introduced into the solution, and the reaction is carried out at 90 ℃ for 2 hours to obtain the composite ferric polysulfate.
4. The method according to claim 1, wherein in step F, when a nitrite catalysis method is adopted, sodium nitrite is added to the dissolution solution, and high pressure oxygen is introduced, and the reaction is carried out at 90 ℃ and 0.2MPa for 4 hours to obtain the composite ferric polysulfate.
5. The method according to any one of claims 1 to 4, wherein the nano titanium dioxide accounts for 0.1% to 1% by mass of the composite ferric polysulfate.
6. The method according to claim 1, wherein in step C, the concentration of titanium dioxide in the titanium dioxide sol is 0.5g/L to 5g/L, based on the mass of titanium dioxide.
7. The method according to any one of claims 1 to 4, wherein the pH of the dissolution solution is between 1 and 5.
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| EP3705182A4 (en) * | 2019-01-22 | 2021-01-27 | Chengdu Qianlijin Technological Innovation Co. Ltd | Method for producing self-fitting nano-catalyst sewage treatment agent |
| CN112174279B (en) * | 2020-11-13 | 2022-08-02 | 陕西科技大学 | Polymeric aluminosilicate inorganic flocculant and preparation method and application thereof |
| CN113247960A (en) * | 2021-05-07 | 2021-08-13 | 河南师范大学 | Production method of nano composite solid polymeric ferric sulfate |
| CN114604947A (en) * | 2022-03-21 | 2022-06-10 | 衡阳市建衡实业有限公司 | Titanium-containing composite ferric polysulfate flocculant and preparation method and application thereof |
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| CN100484880C (en) * | 2005-09-22 | 2009-05-06 | 中国科学院理化技术研究所 | Low temperature crystallized nano titanium dioxide powder and sol synthesizing method |
| CN101049961B (en) * | 2007-05-18 | 2011-04-06 | 广东省生态环境与土壤研究所 | Method for preparing sol of high active Nano titanium dioxide |
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Denomination of invention: Preparation Method of a Titanium Containing Composite Polyferric Sulfate Flocculant Effective date of registration: 20231025 Granted publication date: 20201211 Pledgee: Industrial and Commercial Bank of China Limited Ningbo Zhenhai sub branch Pledgor: NINGBO XINFU TITANIUM DIOXIDE Co.,Ltd. Registration number: Y2023330002472 |
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