CN113247960A - Production method of nano composite solid polymeric ferric sulfate - Google Patents
Production method of nano composite solid polymeric ferric sulfate Download PDFInfo
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- CN113247960A CN113247960A CN202110497214.4A CN202110497214A CN113247960A CN 113247960 A CN113247960 A CN 113247960A CN 202110497214 A CN202110497214 A CN 202110497214A CN 113247960 A CN113247960 A CN 113247960A
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- ferric sulfate
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- ammonium
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- 239000007787 solid Substances 0.000 title claims abstract description 40
- 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 title claims abstract description 36
- 229910000360 iron(III) sulfate Inorganic materials 0.000 title claims abstract description 36
- 239000002114 nanocomposite Substances 0.000 title claims abstract description 27
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 36
- 238000006243 chemical reaction Methods 0.000 claims description 19
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 18
- 239000000243 solution Substances 0.000 claims description 16
- 239000000203 mixture Substances 0.000 claims description 13
- 239000002070 nanowire Substances 0.000 claims description 13
- LLZRNZOLAXHGLL-UHFFFAOYSA-J titanic acid Chemical compound O[Ti](O)(O)O LLZRNZOLAXHGLL-UHFFFAOYSA-J 0.000 claims description 13
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 12
- 239000011259 mixed solution Substances 0.000 claims description 12
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 10
- 239000000843 powder Substances 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 9
- 229910021641 deionized water Inorganic materials 0.000 claims description 9
- 229910001220 stainless steel Inorganic materials 0.000 claims description 9
- 239000010935 stainless steel Substances 0.000 claims description 9
- 239000004408 titanium dioxide Substances 0.000 claims description 9
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 8
- 239000011790 ferrous sulphate Substances 0.000 claims description 8
- 235000003891 ferrous sulphate Nutrition 0.000 claims description 8
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims description 8
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 7
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims description 6
- 239000001099 ammonium carbonate Substances 0.000 claims description 6
- 150000003863 ammonium salts Chemical class 0.000 claims description 6
- -1 polytetrafluoroethylene Polymers 0.000 claims description 6
- 238000007605 air drying Methods 0.000 claims description 5
- 238000004140 cleaning Methods 0.000 claims description 5
- 238000009833 condensation Methods 0.000 claims description 5
- 230000005494 condensation Effects 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 230000007935 neutral effect Effects 0.000 claims description 5
- 230000003472 neutralizing effect Effects 0.000 claims description 5
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 5
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 5
- 239000002002 slurry Substances 0.000 claims description 5
- 238000000967 suction filtration Methods 0.000 claims description 5
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 claims description 4
- 235000012538 ammonium bicarbonate Nutrition 0.000 claims description 4
- 235000019270 ammonium chloride Nutrition 0.000 claims description 4
- PAWQVTBBRAZDMG-UHFFFAOYSA-N 2-(3-bromo-2-fluorophenyl)acetic acid Chemical compound OC(=O)CC1=CC=CC(Br)=C1F PAWQVTBBRAZDMG-UHFFFAOYSA-N 0.000 claims description 3
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 claims description 3
- 229910052921 ammonium sulfate Inorganic materials 0.000 claims description 3
- 235000011130 ammonium sulphate Nutrition 0.000 claims description 3
- 239000004254 Ammonium phosphate Substances 0.000 claims description 2
- 235000012501 ammonium carbonate Nutrition 0.000 claims description 2
- 229910000148 ammonium phosphate Inorganic materials 0.000 claims description 2
- 235000019289 ammonium phosphates Nutrition 0.000 claims description 2
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 claims description 2
- ODZPKZBBUMBTMG-UHFFFAOYSA-N sodium amide Chemical compound [NH2-].[Na+] ODZPKZBBUMBTMG-UHFFFAOYSA-N 0.000 claims description 2
- 238000005507 spraying Methods 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 abstract description 4
- 230000018044 dehydration Effects 0.000 abstract description 3
- 238000006297 dehydration reaction Methods 0.000 abstract description 3
- 239000010865 sewage Substances 0.000 abstract description 3
- 239000002781 deodorant agent Substances 0.000 abstract description 2
- 239000003651 drinking water Substances 0.000 abstract description 2
- 235000020188 drinking water Nutrition 0.000 abstract description 2
- 238000001035 drying Methods 0.000 abstract description 2
- 230000002194 synthesizing effect Effects 0.000 abstract description 2
- 238000000034 method Methods 0.000 description 12
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 7
- 238000005303 weighing Methods 0.000 description 6
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 description 5
- 239000007788 liquid Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- CDCCFXKFZODWRW-UHFFFAOYSA-N sodium azane azanide Chemical compound N.[NH2-].[Na+] CDCCFXKFZODWRW-UHFFFAOYSA-N 0.000 description 3
- GROMGGTZECPEKN-UHFFFAOYSA-N sodium metatitanate Chemical compound [Na+].[Na+].[O-][Ti](=O)O[Ti](=O)O[Ti]([O-])=O GROMGGTZECPEKN-UHFFFAOYSA-N 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- HKDXPUPTIQCIPH-UHFFFAOYSA-L [O--].[O--].[O--].O[Ti+3].O[Ti+3] Chemical compound [O--].[O--].[O--].O[Ti+3].O[Ti+3] HKDXPUPTIQCIPH-UHFFFAOYSA-L 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 238000005189 flocculation Methods 0.000 description 2
- 230000016615 flocculation Effects 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000012808 vapor phase Substances 0.000 description 2
- FPFSGDXIBUDDKZ-UHFFFAOYSA-N 3-decyl-2-hydroxycyclopent-2-en-1-one Chemical compound CCCCCCCCCCC1=C(O)C(=O)CC1 FPFSGDXIBUDDKZ-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical group [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 150000004703 alkoxides Chemical class 0.000 description 1
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000013043 chemical agent Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000001877 deodorizing effect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 239000008394 flocculating agent Substances 0.000 description 1
- 230000005484 gravity Effects 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
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 235000012149 noodles Nutrition 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000010532 solid phase synthesis reaction Methods 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000001694 spray drying Methods 0.000 description 1
- 229910021653 sulphate ion Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- 238000003911 water pollution Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/14—Sulfates
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a production method of nano composite solid polymeric ferric sulfate, belonging to the technical field of preparation of solid polymeric ferric sulfate. The production method is a short-flow production process for directly synthesizing the nano composite polymeric ferric sulfate in one step without drying and dehydration at room temperature, the produced nano composite solid polymeric ferric sulfate meets the requirements in the national standard (GB 14591-2006 water treatment agent polymeric ferric sulfate), has wide application, and can purify sewage and drinking water and be used as a high-efficiency deodorant.
Description
Technical Field
The invention belongs to the technical field of preparation of solid polymeric ferric sulfate, and particularly relates to a production method of nano composite solid polymeric ferric sulfate.
Background
Chemical treatment is a very important unit in the treatment of feed water and sewage, where a flocculant is a chemical agent that can be used to not effectively separate fine suspended particles that cause water pollution. The main varieties of flocculants are still iron and aluminum salts at present. The inorganic polymeric flocculant polymeric ferric sulfate is developed from the beginning of the 80 th years in China. Since the 80 s, the market of nano titanium dioxide is opened, and the nano titanium dioxide has wide application prospects in the aspects of catalysis and environmental protection.
The nano titanium dioxide has excellent antibacterial performance, has good adsorption effect on heavy metals, and is an adsorbent with excellent performance. The liquid polymeric ferric sulfate is inconvenient to store and difficult to transport, and the popularization and application of the liquid polymeric ferric sulfate are greatly restricted, so the research and development of the solid polymeric ferric sulfate become the focus of attention of people. The solid polyferric sulfate has the advantages of high hydrolysis speed, large flocculation specific gravity, rapid sedimentation, wide applicable pH range and the like, and has wide raw material sources, low price and low production cost, thereby having strong competitiveness.
At present, the preparation methods of the nano titanium dioxide are many, and the preparation methods can be divided into the following steps according to the original state of the substances: the solid phase method, which relies on mixing between solid particles to promote the reaction, is not suitable for preparing fine particles; the liquid phase method is that chloride or alkoxide of titanium is firstly hydrolyzed to generate titanium hydroxide (or hydroxyl titanium oxide), and then the titanium hydroxide (or hydroxyl titanium oxide) is obtained by calcination; the vapor phase method is a method in which a sample which is previously treated into a vapor phase is condensed and nucleated in an atmosphere of liquid nitrogen to prepare nano titanium dioxide powder, but the method is not suitable for preparing a semiconductor oxide with a high boiling point. There are two routes for the solidification of polymeric ferric sulphate: firstly, liquid is generated firstly, and then solid is obtained by adopting spray drying or reduced pressure concentration, and the method has complex production equipment and large energy consumption; secondly, the dehydration oxidation method related to patent document CN1105342A has the disadvantages of low basicity of the obtained product, complicated process conditions and poor flocculation effect.
Disclosure of Invention
The invention solves the technical problem of providing a production method of nano composite solid polymeric ferric sulfate with simple process and low cost, the method is a short-flow production process for directly synthesizing the nano composite polymeric ferric sulfate in one step without drying and dehydration at room temperature, and the product obtained by the production process meets the national standard and can meet the requirements in industrial use.
The invention adopts the following technical scheme for solving the technical problems, and the production method of the nano composite solid polymeric ferric sulfate is characterized by comprising the following specific steps:
step S1: dissolving sodium hydroxide solid in deionized water, adding titanium dioxide powder, placing the mixture on a magnetic stirrer, stirring and mixing the mixture at normal temperature, placing the uniformly stirred mixed solution in a stainless steel reaction kettle with a polytetrafluoroethylene lining, placing the stainless steel reaction kettle in an electric air drying box, setting the temperature to be 160-200 ℃, reacting for 20-30 hours, naturally cooling to room temperature, taking out a product, repeatedly cleaning the product with deionized water until the residual mass is unchanged, performing suction filtration, and neutralizing the product with a hydrochloric acid solution to be neutral to obtain the titanic acid nanowire;
step S2: mixing industrial-grade ferrous sulfate (FeSO)4·7H2O) and the titanic acid nanowire obtained in the step S1 are placed in an acid-proof reaction kettle, the titanic acid nanowire is heated to 300-400 ℃ and is electrically stirred to be slurry, then concentrated sulfuric acid solution and hydrogen peroxide solution are added in a spraying mode, the mixture is fully stirred and reacts for 1-3 hours after the addition, then industrial ammonium salt is added, all products are transferred to a condensation tank after the mixture is uniformly stirred, the mixture is cooled and stands for 24-48 hours, and finally the nano composite solid polymeric ferric sulfate is obtained, wherein the nano composite solid polymeric ferric sulfate meets the requirements of the national standard-GB 14591-2006 water treatment agent polymeric ferric sulfate.
Further, in step S1, the feeding mass ratio of the sodium hydroxide solid to the titanium dioxide powder is 9: 1.
Further limiting, in the step S2, the feeding mass ratio of the ferrous sulfate industrial acid, the titanic acid nanowire, the concentrated sulfuric acid, the hydrogen peroxide and the industrial-grade ammonium salt is 100:20: 5-15: 15-25: 1-5, wherein the mass concentration of the concentrated sulfuric acid solution is 98%, and the mass concentration of the hydrogen peroxide solution is 50%.
Further, in step S2, the industrial-grade ammonium salt is a mixture of sodium amide and one or more of ammonium bicarbonate, ammonium chloride, ammonium carbonate, ammonium sulfate, ammonium phosphate and ammonium nitrate.
According to the method for producing the nano composite solid polyferric sulfate, ammonium ions with strong water locking capacity, sulfate radicals and ferric ions form ferric ammonium sulfate, and twelve water molecules are combined to form a crystal of one molecule, so that the flowing state polyferric sulfate can be directly changed into the nano composite solid polyferric sulfate without being dried. The nano composite solid ferric sulfate product compounded by the titanic acid nano wire and the industrial ferrous sulfate has wider treatment range, and particularly has better effects of treating organic wastewater and deodorizing.
Compared with the prior art, the invention has the following advantages: the method has the advantages of low cost, low energy consumption, simple operation process, simple equipment and the like, and the produced nano composite solid polyferric sulfate meets the requirements of national standard (GB 14591-2006 water treatment agent polyferric sulfate) and has wide application, thereby not only purifying sewage and drinking water, but also being used as an efficient deodorant.
Detailed Description
The present invention is described in further detail below with reference to examples, but it should not be construed that the scope of the above subject matter of the present invention is limited to the following examples, and that all the technologies realized based on the above subject matter of the present invention belong to the scope of the present invention.
Example 1
Weighing 36g of sodium hydroxide solid, dissolving the sodium hydroxide solid in 500mL of deionized water, weighing 4g of titanium dioxide powder, adding the titanium dioxide powder into a sodium hydroxide solution, placing the mixed solution on a magnetic stirrer, stirring the mixed solution at normal temperature for 1h, placing the uniformly stirred mixed solution into 6 stainless steel reaction kettles with 100mL of polytetrafluoroethylene linings on average, placing the stainless steel reaction kettles in an electric air drying box, setting the temperature to be 180 ℃, reacting for 24h, naturally cooling the mixed solution to room temperature, taking out a product, repeatedly cleaning the product with deionized water until the residual mass is unchanged, performing suction filtration, and neutralizing the product with a hydrochloric acid solution to be neutral to obtain the titanic acid nanowire; 10kg of industrial ferrous sulfate (FeSO) is weighed4·7H2O) and 2kg of the sodium titanate rice noodle prepared by the method are put into an acid-proof reaction kettle, heated to 300-400 ℃, electrically stirred to be slurry, and then 1kg of concentrated sulfuric acid solution with the mass concentration of 98 percent and 2kg of concentrated sulfuric acid solution with the mass concentration of 2kg are respectively sprayed into the reaction kettleAnd (3) fully stirring and reacting 50% hydrogen peroxide solution for 2 hours after the hydrogen peroxide solution is added, adding 0.0125kg of industrial ammonium salt sodium amide, 0.025kg of ammonium bicarbonate and 0.163kg of ammonium chloride, uniformly stirring, then completely transferring the products to a condensation tank, cooling and standing for 48 hours to obtain the nano composite solid polymeric ferric sulfate, wherein the nano composite solid polymeric ferric sulfate meets the requirements of the national standard-GB 14591-2006 water treatment agent polymeric ferric sulfate.
Example 2
Weighing 36g of sodium hydroxide solid, dissolving the sodium hydroxide solid in 500mL of deionized water, weighing 4g of titanium dioxide powder, adding the titanium dioxide powder into a sodium hydroxide solution, placing the mixed solution on a magnetic stirrer, stirring the mixed solution at normal temperature for 1h, placing the uniformly stirred mixed solution into 6 stainless steel reaction kettles with 100mL of polytetrafluoroethylene linings on average, placing the stainless steel reaction kettles in an electric air drying box, setting the temperature to be 180 ℃, reacting for 24h, naturally cooling the mixed solution to room temperature, taking out a product, repeatedly cleaning the product with deionized water until the residual mass is unchanged, performing suction filtration, and neutralizing the product with a hydrochloric acid solution to be neutral to obtain the titanic acid nanowire; 20kg of industrial ferrous sulfate (FeSO) was weighed4·7H2O) and 4kg of the prepared sodium titanate nanowire are placed in an acid-proof reaction kettle, the temperature is heated to 300-400 ℃, the mixture is electrically stirred to be slurry, then 2kg of concentrated sulfuric acid solution with the mass concentration of 98% and 4.2kg of hydrogen peroxide solution with the mass concentration of 50% are respectively sprayed into the reaction kettle, the mixture is fully stirred and reacted for 4 hours after the addition, 0.025kg of industrial ammonium salt sodium amide, 0.200 kg of ammonium bicarbonate and 0.926 kg of ammonium chloride are added, the product is completely transferred to a condensation tank after the uniform stirring, and the product is cooled and kept stand for 36 hours to obtain the nano composite solid polymeric ferric sulfate, wherein the nano composite solid polymeric ferric sulfate meets the requirements of the national standard-GB 14591-2006 polymeric ferric sulfate as a water treatment agent.
Example 3
Weighing 36g of sodium hydroxide solid, dissolving in 500mL of deionized water, weighing 4g of titanium dioxide powder, adding into the sodium hydroxide solution, placing the mixed solution on a magnetic stirrer, stirring at normal temperature for 1h, placing the uniformly stirred mixed solution into 6 stainless steel reaction kettles with 100mL of polytetrafluoroethylene lining on average, placing in an electric drum air drying box, setting the temperature to 180 ℃, reacting for 24h, naturally cooling to room temperature, taking out the product, and repeatedly cleaning with deionized waterUntil the residual mass is unchanged, carrying out suction filtration, and then neutralizing the obtained product to be neutral by using a hydrochloric acid solution to obtain the titanic acid nanowire; 5kg of industrial ferrous sulfate (FeSO) was weighed4·7H2O) and 1kg of the prepared sodium titanate nanowire are put into an acid-resistant reaction kettle, heated to 300-400 ℃, and stirred electrically to be slurry, then 0.543kg of 98% concentrated sulfuric acid solution and 1.081kg of 50% hydrogen peroxide solution are sprayed into the reaction kettle, after the addition, the reaction kettle is stirred fully for 2 hours, 0.008kg of industrial ammonium salt sodium amide, 0.016kg of ammonium nitrate and 0.012kg of ammonium sulfate are added, after the uniform stirring, the product is moved to a condensation tank, and then cooled and stood for 24 hours, so that the nano composite solid polymeric ferric sulfate is obtained, and the nano composite solid polymeric ferric sulfate meets the requirements of the national standard-GB 14591-2006 polymeric ferric sulfate as a water treatment agent.
While there have been shown and described what are at present considered the fundamental principles of the invention, its essential features and advantages, the invention further resides in various changes and modifications which fall within the scope of the invention as claimed.
Claims (4)
1. A production method of nano composite solid polymeric ferric sulfate is characterized by comprising the following specific steps:
step S1: dissolving sodium hydroxide solid in deionized water, adding titanium dioxide powder, placing the mixture on a magnetic stirrer, stirring and mixing the mixture at normal temperature, placing the uniformly stirred mixed solution in a stainless steel reaction kettle with a polytetrafluoroethylene lining, placing the stainless steel reaction kettle in an electric air drying box, setting the temperature to be 160-200 ℃, reacting for 20-30 hours, naturally cooling to room temperature, taking out a product, repeatedly cleaning the product with deionized water until the residual mass is unchanged, performing suction filtration, and neutralizing the product with a hydrochloric acid solution to be neutral to obtain the titanic acid nanowire;
step S2: mixing industrial-grade ferrous sulfate (FeSO)4·7H2O) and the titanic acid nanowire obtained in the step S1 are placed in an acid-proof reaction kettle, the mixture is heated to 300-400 ℃ and is electrically stirred to be slurry, then concentrated sulfuric acid solution and hydrogen peroxide solution are added in a spraying mode, the mixture is fully stirred and reacts for 1-3 hours after the addition, then industrial ammonium salt is added, and after the uniform stirring, the product is completely transferred to a condensation poolAnd cooling and standing for 24-48 h to finally obtain the nano composite solid polymeric ferric sulfate, wherein the nano composite solid polymeric ferric sulfate meets the requirements of the national standard-GB 14591-2006 water treatment agent polymeric ferric sulfate.
2. The method for producing the nanocomposite solid polymeric ferric sulfate according to claim 1, wherein: in step S1, the feeding mass ratio of the sodium hydroxide solid to the titanium dioxide powder is 9: 1.
3. The method for producing the nanocomposite solid polymeric ferric sulfate according to claim 1, wherein: in the step S2, the feeding mass ratio of the industrial ferrous sulfate, the titanic acid nanowire, the concentrated sulfuric acid, the hydrogen peroxide and the industrial ammonium salt is 100:20: 5-15: 15-25: 1-5, wherein the mass concentration of the concentrated sulfuric acid solution is 98%, and the mass concentration of the hydrogen peroxide solution is 50%.
4. The method for producing the nanocomposite solid polymeric ferric sulfate according to claim 1, wherein: in step S2, the industrial grade ammonium salt is a mixture of sodium amide and one or more of ammonium bicarbonate, ammonium chloride, ammonium carbonate, ammonium sulfate, ammonium phosphate and ammonium nitrate.
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