CN110436598B - Application of ammonium magnesium phosphate/nano magnesium hydroxide in treatment of heavy metal-containing wastewater - Google Patents
Application of ammonium magnesium phosphate/nano magnesium hydroxide in treatment of heavy metal-containing wastewater Download PDFInfo
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- CN110436598B CN110436598B CN201910728434.6A CN201910728434A CN110436598B CN 110436598 B CN110436598 B CN 110436598B CN 201910728434 A CN201910728434 A CN 201910728434A CN 110436598 B CN110436598 B CN 110436598B
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- magnesium hydroxide
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- magnesium
- ammonia nitrogen
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- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 title claims abstract description 83
- 239000000347 magnesium hydroxide Substances 0.000 title claims abstract description 83
- 229910001862 magnesium hydroxide Inorganic materials 0.000 title claims abstract description 83
- 229910001385 heavy metal Inorganic materials 0.000 title claims abstract description 64
- 239000002351 wastewater Substances 0.000 title claims abstract description 54
- MXZRMHIULZDAKC-UHFFFAOYSA-L ammonium magnesium phosphate Chemical compound [NH4+].[Mg+2].[O-]P([O-])([O-])=O MXZRMHIULZDAKC-UHFFFAOYSA-L 0.000 title claims abstract description 35
- XKMRRTOUMJRJIA-UHFFFAOYSA-N ammonia nh3 Chemical compound N.N XKMRRTOUMJRJIA-UHFFFAOYSA-N 0.000 claims abstract description 47
- 229910052567 struvite Inorganic materials 0.000 claims abstract description 32
- 239000002994 raw material Substances 0.000 claims abstract description 15
- 239000000203 mixture Substances 0.000 claims abstract description 14
- 150000002500 ions Chemical class 0.000 claims abstract description 9
- 238000000227 grinding Methods 0.000 claims description 73
- 239000002002 slurry Substances 0.000 claims description 54
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 43
- 238000002156 mixing Methods 0.000 claims description 39
- 239000002245 particle Substances 0.000 claims description 38
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 30
- 239000007787 solid Substances 0.000 claims description 20
- 239000000706 filtrate Substances 0.000 claims description 17
- 239000004094 surface-active agent Substances 0.000 claims description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 15
- 239000003607 modifier Substances 0.000 claims description 14
- -1 phthalate ester Chemical class 0.000 claims description 13
- 238000002360 preparation method Methods 0.000 claims description 11
- 239000001509 sodium citrate Substances 0.000 claims description 10
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims description 10
- 239000002270 dispersing agent Substances 0.000 claims description 8
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 5
- 235000019333 sodium laurylsulphate Nutrition 0.000 claims description 5
- 235000021355 Stearic acid Nutrition 0.000 claims description 4
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 4
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 4
- 229920002545 silicone oil Polymers 0.000 claims description 4
- 239000008117 stearic acid Substances 0.000 claims description 4
- 239000011148 porous material Substances 0.000 claims description 3
- OABYVIYXWMZFFJ-ZUHYDKSRSA-M sodium glycocholate Chemical compound [Na+].C([C@H]1C[C@H]2O)[C@H](O)CC[C@]1(C)[C@@H]1[C@@H]2[C@@H]2CC[C@H]([C@@H](CCC(=O)NCC([O-])=O)C)[C@@]2(C)[C@@H](O)C1 OABYVIYXWMZFFJ-ZUHYDKSRSA-M 0.000 claims description 3
- 239000002202 Polyethylene glycol Substances 0.000 claims description 2
- 239000004115 Sodium Silicate Substances 0.000 claims description 2
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 2
- 229920001223 polyethylene glycol Polymers 0.000 claims description 2
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 2
- 235000019795 sodium metasilicate Nutrition 0.000 claims description 2
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 2
- 229910052911 sodium silicate Inorganic materials 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 34
- 239000000395 magnesium oxide Substances 0.000 abstract description 23
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 abstract description 23
- 229910052761 rare earth metal Inorganic materials 0.000 abstract description 17
- 150000002910 rare earth metals Chemical class 0.000 abstract description 17
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 abstract description 16
- 239000006185 dispersion Substances 0.000 abstract description 9
- 239000010865 sewage Substances 0.000 abstract description 5
- 239000002699 waste material Substances 0.000 abstract description 3
- 239000001095 magnesium carbonate Substances 0.000 abstract description 2
- 235000014380 magnesium carbonate Nutrition 0.000 abstract description 2
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 abstract description 2
- 229910000021 magnesium carbonate Inorganic materials 0.000 abstract description 2
- 230000001376 precipitating effect Effects 0.000 abstract description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 10
- 238000006243 chemical reaction Methods 0.000 description 8
- 238000003756 stirring Methods 0.000 description 8
- 229910000831 Steel Inorganic materials 0.000 description 7
- 238000002441 X-ray diffraction Methods 0.000 description 7
- 238000004458 analytical method Methods 0.000 description 7
- 238000004455 differential thermal analysis Methods 0.000 description 7
- 239000010959 steel Substances 0.000 description 7
- 239000000126 substance Substances 0.000 description 6
- 238000002411 thermogravimetry Methods 0.000 description 6
- 229910021529 ammonia Inorganic materials 0.000 description 5
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 238000010668 complexation reaction Methods 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- 239000011324 bead Substances 0.000 description 2
- 238000009388 chemical precipitation Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229920000609 methyl cellulose Polymers 0.000 description 2
- 239000001923 methylcellulose Substances 0.000 description 2
- 235000010981 methylcellulose Nutrition 0.000 description 2
- XNGIFLGASWRNHJ-UHFFFAOYSA-L phthalate(2-) Chemical compound [O-]C(=O)C1=CC=CC=C1C([O-])=O XNGIFLGASWRNHJ-UHFFFAOYSA-L 0.000 description 2
- HSFQBFMEWSTNOW-UHFFFAOYSA-N sodium;carbanide Chemical group [CH3-].[Na+] HSFQBFMEWSTNOW-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 238000003915 air pollution Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000006056 electrooxidation reaction Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 235000010755 mineral Nutrition 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 239000002952 polymeric resin Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 229920003002 synthetic resin Polymers 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F5/00—Compounds of magnesium
- C01F5/14—Magnesium hydroxide
-
- 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
- C02F1/58—Treatment of water, waste water, or sewage by removing specified dissolved compounds
- C02F1/586—Treatment of water, waste water, or sewage by removing specified dissolved compounds by removing ammoniacal nitrogen
-
- 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
- C02F1/58—Treatment of water, waste water, or sewage by removing specified dissolved compounds
- C02F1/62—Heavy metal compounds
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
Abstract
The invention provides an application of a magnesium ammonium phosphate/nano magnesium hydroxide mixture in treating heavy metal-containing wastewater. In this application, the magnesium ammonium phosphate: nano magnesium hydroxide: the molar ratio of heavy metals is 1: (2-10): (0.1-0.8). Wherein, the magnesium ammonium phosphate/nano magnesium hydroxide can be converted from low-purity magnesium oxide waste. The method can convert low-purity magnesium oxide waste into nano-grade high-dispersion magnesium hydroxide, can be used as a raw material for precipitating ammonia nitrogen in sewage by a magnesium ammonium phosphate method, realizes resource utilization of low-purity magnesium oxide and low-grade magnesite, and simultaneously can remove heavy metals in heavy metal wastewater and ammonia nitrogen and heavy metal ions in rare earth wastewater.
Description
Technical Field
The invention relates to the technical field of environment-friendly materials, and in particular relates to application of a magnesium ammonium phosphate/nano magnesium hydroxide mixture in treatment of heavy metal-containing wastewater.
Background
The method for removing heavy metal ions in sewage comprises an adsorption removal method, a chemical precipitation method, a polymer resin complexation method and the like. In the aspect of removing heavy metals, researchers have done a great deal of work by adopting a method of removing polymer materials by complexation and removing by adsorption, and the removal has achieved more success. The adsorbing material mainly comprises active carbon and various natural porous minerals. At present, the complexation removal method and the adsorption method have been industrially applied, the treatment effect is good, the removal rate is high, the chemical precipitation method is combined to obtain better comprehensive treatment effect and reduce the cost, but the comprehensive treatment cost is higher, so that the pollution discharge enterprises are difficult to bear.
Ammonia nitrogen is an important item in water quality indexes, and ammonia in water is from domestic sewage and industrial sewage. Ammonia may be emitted by industries that utilize ammonia in the industry. The method for treating ammonia mainly comprises the following steps: nitration-denitrification, physical stripping, magnesium ammonium phosphate and electrochemical oxidation. The physical stripping method has the problem of air pollution and is often used as pretreatment of the nitrification-denitrification method. The rare earth wastewater mainly contains ammonia nitrogen and various heavy metal ions, and the removal of the ammonia nitrogen and the heavy metal ions is the key to the protection of the water quality of the yellow river. Finding a method capable of simultaneously and effectively removing ammonia nitrogen and heavy metal ions in rare earth wastewater is a hotspot of current research.
Disclosure of Invention
The first purpose of the invention is to provide application of a magnesium ammonium phosphate/nano magnesium hydroxide mixture in treating heavy metal-containing wastewater, wherein the weight ratio of the magnesium ammonium phosphate: nano magnesium hydroxide: the molar ratio of heavy metals is 1: (2-10): (0.1-0.8).
Under the proportion, the mixture of the ammonium magnesium phosphate and the nano magnesium hydroxide can effectively remove heavy metals in the wastewater, and the removal rate of the heavy metals is at least more than 80%.
In a preferred embodiment of the invention, the heavy metal is Pb and/or Cd.
In a preferred embodiment of the present invention, the ratio of magnesium ammonium phosphate: nano magnesium hydroxide: the molar ratio of heavy metal ions is 1: (3-6): (0.3-0.5). More preferably, the ratio of magnesium ammonium phosphate: nano magnesium hydroxide: the molar ratio of heavy metal ions is 1: (4-5): (0.3-0.4).
In a preferred embodiment of the invention, the magnesium ammonium phosphate is a porous particle; the diameter of the porous particles is 1 um-1 mm, and the pore diameter is 0.01 um-0.8 um. More preferably, the porous particles have a diameter of 10um to 100um and a pore size of 0.1um to 0.5 um.
In a preferred embodiment of the present invention, the method for preparing the magnesium ammonium phosphate/nano magnesium hydroxide mixture comprises the following steps: adding nano magnesium hydroxide slurry, phosphoric acid and a surfactant into the ammonia nitrogen wastewater, and reacting for 10 min-2 h; the mass ratio of N, nano magnesium hydroxide slurry, phosphoric acid and surfactant in the ammonia nitrogen wastewater is 0.14: 1: (0.5-1.5): (0.01-0.05).
The preparation method also comprises the application of the nano magnesium hydroxide slurry in treating wastewater containing heavy metal and ammonia.
In a preferred embodiment of the present invention, the surfactant is one or more of sodium dodecylbenzene sulfonate, sodium methyl cellulose, sodium dodecyl sulfate, polyethylene glycol, sodium metasilicate, preferably sodium methyl cellulose.
In a preferred embodiment of the invention, the mass ratio of N, nano magnesium hydroxide slurry, phosphoric acid and surfactant in the ammonia nitrogen wastewater is 0.14: 1: (0.6-0.9): (0.015 to 0.03). The reaction time is preferably 30-60 min.
The ammonia nitrogen content in the ammonia nitrogen wastewater can be effectively and rapidly reduced to be below 20mg/L after the reaction, and the aim of reducing the ammonia nitrogen content in the ammonia nitrogen wastewater can be effectively achieved.
In a preferred embodiment of the present invention, the method for preparing nano magnesium hydroxide slurry comprises the following steps:
1) taking light-burned magnesium powder as a raw material, and mixing the light-burned magnesium powder with a dispersing agent and water according to a mass ratio of 1: (0.01-0.04): (4-6) uniformly mixing, controlling the pH value to be not higher than 12, and adding a grinding medium for grinding; the grinding temperature is 70-80 ℃, the grinding time is 150-190 min, the grinding speed is 1200-1500 rpm, and the average particle size of the grinding medium is 0.5-3 mm;
2) adding a surface modifier into the system obtained in the step 1), and fully modifying to obtain the nano magnesium hydroxide slurry; the mass ratio of the surface modifier to the light-burned magnesium powder is (0.03-0.05): 1.
in a preferred embodiment of the present invention, the content of magnesium oxide in the soft-burned magnesium powder is not more than 65%. In the present invention, a light-burned magnesium powder having a magnesium oxide content of 65% is taken as an example. And will not be described in detail below.
In a preferred embodiment of the present invention, the dispersant in step 1) is one or more of sodium citrate, sodium lauryl sulfate and sodium glycocholate, and is preferably sodium citrate.
In a preferred embodiment of the present invention, the mass ratio of the light-burned magnesium powder, the dispersant and the water is 1: (0.02-0.03): (4-5), preferably 1: (0.02-0.03): 4.
in the present invention, it is known in the art that the pH in step 1) is 9 to 12 in order to obtain magnesium hydroxide. In a preferred embodiment of the present invention, in step 1), the pH is controlled to be 10 to 11. The pH of the mixed system can be adjusted to 10-11 by a method commonly used in the art.
In the present invention, the mixed system is usually fed to a stirring mill for milling. In a preferred embodiment of the present invention, the grinding temperature is 75 to 80 ℃, the grinding time is 160 to 180min, and the grinding speed is 1300 to 1400 rpm. More preferably, the grinding temperature is 80 ℃, the grinding time is 180min, and the grinding speed is 1300 rpm.
In a preferred embodiment of the invention, the grinding media have an average particle size of 0.5mm to 3mm, preferably 1mm to 2 mm. The grinding medium may be one or more of steel balls, zirconia balls and glass beads, and is preferably a steel ball.
In a preferred embodiment of the present invention, in step 2), the surface modifier is one or more of silicone oil, stearic acid, and phthalate ester, preferably phthalate ester.
In a preferred embodiment of the invention, in the step 2), the mass ratio of the surface modifier to the light-burned magnesium powder is (0.03-0.05): 1, more preferably, the mass ratio of the surface modifier to the light-burned magnesium powder is (0.03-0.04): 1. among them, the modification of the present invention is a well-mixed modification in the art.
In a preferred embodiment of the present invention, the method for preparing nano magnesium hydroxide slurry comprises the following steps:
1) taking light-burned magnesium powder with the content of magnesium oxide not higher than 65% as a raw material, and mixing the light-burned magnesium powder with sodium citrate serving as a dispersant and water according to a mass ratio of 1: (0.01-0.04): (4-6) uniformly mixing, controlling the pH value to be not higher than 12, and adding a grinding medium for grinding; the grinding temperature is 70-80 ℃, the grinding time is 150-190 min, the grinding speed is 1200-1500 rpm, and the average particle size of the grinding medium is 0.5-3 mm;
2) adding surface modifier phthalate into the system obtained in the step 1), and fully modifying to obtain the nano magnesium hydroxide slurry; the mass ratio of the surface modifier to the light-burned magnesium powder is (0.03-0.05): 1.
the nano magnesium hydroxide slurry obtained by the method is monodisperse and stable slurry, the average particle diameter is 80-200 nm, and at least 90 percent of particles have the particle size smaller than (d)90)300nm in size.
The invention also aims to provide application of the light-burned magnesium powder in treatment of ammonia nitrogen wastewater containing heavy metals, which comprises the following steps:
1) taking light-burned magnesium powder with the content of magnesium oxide not higher than 65% as a raw material, and mixing the light-burned magnesium powder with sodium citrate serving as a dispersant and water according to a mass ratio of 1: (0.01-0.04): (4-6) uniformly mixing, controlling the pH value to be not higher than 12, and adding a grinding medium for grinding; the grinding temperature is 70-80 ℃, the grinding time is 150-190 min, the grinding speed is 1200-1500 rpm, and the average particle size of the grinding medium is 0.5-3 mm;
2) adding surface modifier phthalate into the system obtained in the step 1), and fully modifying to obtain the nano magnesium hydroxide slurry; the mass ratio of the surface modifier to the light-burned magnesium powder is (0.03-0.05): 1;
3) adding nano magnesium hydroxide slurry, phosphoric acid and a surfactant into the heavy metal-containing ammonia nitrogen wastewater, reacting for 10 min-2 h, and filtering to obtain filtrate and solid; the mass ratio of N, nano magnesium hydroxide slurry, phosphoric acid and surfactant in the ammonia nitrogen wastewater is 0.14: 1: (0.5-1.5): (0.01 to 0.05);
4) mixing the solid obtained in the step 3) and the filtrate with magnesium ammonium phosphate: nano magnesium hydroxide: the molar ratio of heavy metals is 1: (2-10): (0.1-0.8) and completely reacting.
The preferable values in the preparation method are referred to in the scheme, and are not described in detail here.
The method can convert low-purity magnesium oxide waste into nano-grade high-dispersion magnesium hydroxide, can be used as a raw material for precipitating ammonia nitrogen in sewage by a magnesium ammonium phosphate method, realizes resource utilization of low-purity magnesium oxide and low-grade magnesite, and simultaneously can remove heavy metals in heavy metal wastewater and ammonia nitrogen and heavy metal ions in rare earth wastewater. Compared with the existing method for treating ammonia nitrogen wastewater, the method provided by the invention does not bring secondary pollution. The application provided by the invention has the heavy metal removal rate of more than 90%.
Detailed Description
The following examples are given to further illustrate the embodiments of the present invention. The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.
Unless otherwise specified, the technical means used in the examples are conventional means well known to those skilled in the art, and the raw materials used are commercially available.
Example 1
The embodiment provides a nano magnesium hydroxide slurry, and the preparation method comprises the following steps:
1) taking light-burned magnesium powder with MgO content of about 65% as a raw material, and mixing the light-burned magnesium powder with sodium citrate and water according to a mass ratio of 1: 0.03: 4, after uniformly mixing, controlling the pH value of the mixed system to be 10, and carrying out superfine grinding in a medium stirring mill; during grinding, the temperature is controlled at 80 ℃, the grinding time is 180min, and the grinding rotating speed is 1300 r/min, wherein the grinding medium is steel balls with the average grain diameter of 1 mm;
2) adding phthalate ester into the system obtained in the step 1), and fully modifying to obtain high-dispersion nano magnesium hydroxide slurry; wherein the mass ratio of the light-burned magnesium powder to the phthalate ester is 1: 0.03.
the nano magnesium hydroxide slurry obtained in this example had an average particle size of 80nm, and at least 90% of the particles had a particle size of less than (d)90) Size of 100 nm. Using chemical composition analysis, X-ray diffraction and thermogravimetric summationThe conversion rate of the magnesium oxide in the nano magnesium hydroxide slurry is 98 percent by differential thermal analysis.
Example 2
The embodiment provides a nano magnesium hydroxide slurry, and the preparation method comprises the following steps:
1) taking light-burned magnesium powder with MgO content of about 65% as a raw material, and mixing the light-burned magnesium powder with sodium citrate and water according to a mass ratio of 1: 0.02: 4, after uniformly mixing, controlling the pH value of the mixed system to be 11, and carrying out superfine grinding in a medium stirring mill; during grinding, the temperature is controlled at 75 ℃, the grinding time is 160min, and the grinding rotating speed is 1300 r/min, wherein the grinding medium is a steel ball with the average grain diameter of 2 mm;
2) adding phthalate ester into the system obtained in the step 1), and fully modifying to obtain high-dispersion nano magnesium hydroxide slurry; wherein the mass ratio of the light-burned magnesium powder to the phthalate ester is 1: 0.04.
the nano magnesium hydroxide slurry obtained in this example has an average particle size of 100nm, and at least 90% of the particles have a particle size of less than (d)90)130nm in size. The conversion rate of the magnesium oxide in the nano magnesium hydroxide slurry is 96 percent by utilizing chemical composition analysis, X-ray diffraction and thermogravimetric and differential thermal analysis.
Example 3
The embodiment provides a nano magnesium hydroxide slurry, and the preparation method comprises the following steps:
1) taking light-burned magnesium powder with MgO content of about 65% as a raw material, and mixing the light-burned magnesium powder with sodium citrate and water according to a mass ratio of 1: 0.02: 5, after uniformly mixing, controlling the pH value of the mixed system to be 11, and carrying out superfine grinding in a medium stirring mill; during grinding, the temperature is controlled at 80 ℃, the grinding time is 180min, and the grinding rotating speed is 1400 revolutions per minute, wherein the grinding medium is a steel ball with the average grain diameter of 2 mm;
2) adding phthalate ester into the system obtained in the step 1), and fully modifying to obtain high-dispersion nano magnesium hydroxide slurry; wherein the mass ratio of the light-burned magnesium powder to the phthalate ester is 1: 0.04.
the nano magnesium hydroxide slurry obtained in this example had an average particle size of 80nm, and at least 90% of the particles had a particle size of less than (d)90)120nm in size. By using chemistryAnd the conversion rate of the magnesium oxide in the nano magnesium hydroxide slurry is 95 percent through composition analysis, X-ray diffraction and thermogravimetric and differential thermal analysis.
Example 4
The embodiment provides a nano magnesium hydroxide slurry, and the preparation method comprises the following steps:
1) taking light-burned magnesium powder with MgO content of about 65% as a raw material, and mixing the light-burned magnesium powder with sodium citrate and water according to a mass ratio of 1: 0.01: 4, after uniformly mixing, controlling the pH value of the mixed system to be 9, and carrying out superfine grinding in a medium stirring mill; during grinding, the temperature is controlled at 70 ℃, the grinding time is 150min, and the grinding rotating speed is 1500 rpm, wherein the grinding medium is steel balls with the average grain diameter of 0.5 mm;
2) adding phthalate ester into the system obtained in the step 1), and fully modifying to obtain high-dispersion nano magnesium hydroxide slurry; wherein the mass ratio of the light-burned magnesium powder to the phthalate ester is 1: 0.03.
the nano magnesium hydroxide slurry obtained in this example had an average particle size of 250nm, and at least 90% of the particles had a particle size of less than (d)90)200nm in size. The conversion rate of the magnesium oxide in the nano magnesium hydroxide slurry is 85 percent by utilizing chemical composition analysis, X-ray diffraction and thermogravimetric and differential thermal analysis.
Example 5
The embodiment provides a nano magnesium hydroxide slurry, and the preparation method comprises the following steps:
1) taking light-burned magnesium powder with MgO content of about 65% as a raw material, and mixing the light-burned magnesium powder with sodium citrate and water according to a mass ratio of 1: 0.04: 6, after uniformly mixing, controlling the pH value of the mixed system to be 12, and carrying out superfine grinding in a medium stirring mill; during grinding, the temperature is controlled at 80 ℃, the grinding time is 190min, and the grinding rotating speed is 1200 r/min, wherein the grinding medium is steel balls with the average grain diameter of 3 mm;
2) adding phthalate ester into the system obtained in the step 1), and fully modifying to obtain high-dispersion nano magnesium hydroxide slurry; wherein the mass ratio of the light-burned magnesium powder to the phthalate ester is 1: 0.05.
the nano magnesium hydroxide slurry obtained in this example has an average particle size of 80nm, and at least 90% of the particles have a particle size of less than(d90)200nm in size. The conversion rate of the magnesium oxide in the nano magnesium hydroxide slurry is 88 percent by utilizing chemical composition analysis, X-ray diffraction and thermogravimetric and differential thermal analysis.
Example 6
The embodiment provides a nano magnesium hydroxide slurry, and the preparation method comprises the following steps:
1) taking light-burned magnesium powder with MgO content of about 65% as a raw material, and mixing the light-burned magnesium powder with sodium dodecyl sulfate and water according to a mass ratio of 1: 0.03: 4, after uniformly mixing, controlling the pH value of the mixed system to be 10, and carrying out superfine grinding in a medium stirring mill; during grinding, the temperature is controlled at 80 ℃, the grinding time is 180min, and the grinding rotating speed is 1300 r/min, wherein the grinding medium is zirconia balls with the average grain diameter of 1 mm;
2) adding stearic acid into the system in the step 1), and fully modifying to obtain high-dispersion nano magnesium hydroxide slurry; wherein the mass ratio of the light-burned magnesium powder to the stearic acid is 1: 0.03.
the nano magnesium hydroxide slurry obtained in this example had an average particle size of 200nm, and at least 90% of the particles had a particle size of less than (d)90) Size of 100 nm. The conversion rate of magnesium oxide in the nano magnesium hydroxide slurry is 75% by utilizing chemical composition analysis, X-ray diffraction and thermogravimetric and differential thermal analysis.
Example 7
The embodiment provides a nano magnesium hydroxide slurry, and the preparation method comprises the following steps:
1) taking light-burned magnesium powder with MgO content of about 65% as a raw material, and mixing the light-burned magnesium powder with sodium glycocholate and water according to a mass ratio of 1: 0.02: 4, after uniformly mixing, controlling the pH value of the mixed system to be 11, and carrying out superfine grinding in a medium stirring mill; during grinding, the temperature is controlled at 70 ℃, the grinding time is 180min, and the grinding rotating speed is 1500 rpm, wherein the grinding medium is glass beads with the average grain diameter of 1.5 mm;
2) adding silicone oil into the system in the step 1), and fully modifying to obtain high-dispersion nano magnesium hydroxide slurry; wherein the mass ratio of the light-burned magnesium powder to the silicone oil is 1: 0.03.
the nano magnesium hydroxide slurry obtained in this exampleHas an average particle diameter of 180nm, at least 90% of the particles having a particle diameter of less than (d)90)200nm in size. The conversion rate of magnesium oxide in the nano magnesium hydroxide slurry is 70% by utilizing chemical composition analysis, X-ray diffraction and thermogravimetric and differential thermal analysis.
Example 8
The embodiment provides a method for removing ammonia nitrogen and heavy metals in rare earth wastewater, which comprises the following steps:
3) adding the nano magnesium hydroxide slurry obtained in the example 1, phosphoric acid and a surfactant into rare earth wastewater, reacting for 30min, and filtering to obtain filtrate and solid; the mass ratio of N, nano magnesium hydroxide slurry, phosphoric acid and surfactant in the ammonia nitrogen wastewater is 0.14: 1: 0.8: 0.02;
4) mixing the solid obtained in the step 3) and the filtrate with magnesium ammonium phosphate: nano magnesium hydroxide: the molar ratio of heavy metals is 1: 5: 0.4, mixing and completely reacting.
The magnesium ammonium phosphate in the solid obtained in the step 3) is porous particles, the diameter is 50um, the aperture is 0.3um, the content of ammonia nitrogen in the wastewater is less than 20mg/L, and the removal rate of heavy metals reaches 98%.
Example 9
The embodiment provides a method for removing ammonia nitrogen and heavy metals in rare earth wastewater, which comprises the following steps:
4) the solid obtained in step 3) of example 8 was mixed with the filtrate in the presence of magnesium ammonium phosphate: nano magnesium hydroxide: the molar ratio of heavy metals is 1: 4: 0.3, mixing and completely reacting.
The content of ammonia nitrogen in the wastewater is less than 20mg/L, and the removal rate of heavy metals reaches 96%.
Example 10
The embodiment provides a method for removing ammonia nitrogen and heavy metals in rare earth wastewater, which comprises the following steps:
4) the solid obtained in step 3) of example 8 was mixed with the filtrate in the presence of magnesium ammonium phosphate: nano magnesium hydroxide: the molar ratio of heavy metals is 1: 3: 0.3, mixing and completely reacting.
The content of ammonia nitrogen in the wastewater is less than 20mg/L, and the removal rate of heavy metals reaches 93 percent.
Example 11
The embodiment provides a method for removing ammonia nitrogen and heavy metals in rare earth wastewater, which comprises the following steps:
4) the solid obtained in step 3) of example 8 was mixed with the filtrate in the presence of magnesium ammonium phosphate: nano magnesium hydroxide: the molar ratio of heavy metals is 1: 6: 0.5, mixing and completely reacting.
The content of ammonia nitrogen in the wastewater is less than 20mg/L, and the removal rate of heavy metals reaches 92%.
Example 12
The embodiment provides a method for removing ammonia nitrogen and heavy metals in rare earth wastewater, which comprises the following steps:
4) the solid obtained in step 3) of example 8 was mixed with the filtrate in the presence of magnesium ammonium phosphate: nano magnesium hydroxide: the molar ratio of heavy metals is 1: 2: 0.1, mixing and completely reacting.
The content of ammonia nitrogen in the wastewater is less than 20mg/L, and the removal rate of heavy metals reaches 90 percent.
Example 13
The embodiment provides a method for removing ammonia nitrogen and heavy metals in rare earth wastewater, which comprises the following steps:
4) the solid obtained in step 3) of example 8 was mixed with the filtrate in the presence of magnesium ammonium phosphate: nano magnesium hydroxide: the molar ratio of heavy metals is 1: 10: 0.8, mixing and completely reacting.
The content of ammonia nitrogen in the wastewater is less than 20mg/L, and the removal rate of heavy metals reaches 89%.
Example 14
The embodiment provides a method for removing ammonia nitrogen and heavy metals in rare earth wastewater, which comprises the following steps:
3) adding the nano magnesium hydroxide slurry obtained in the example 1, phosphoric acid and a surfactant into rare earth wastewater, reacting for 30min, and filtering to obtain filtrate and solid; the mass ratio of N, nano magnesium hydroxide slurry, phosphoric acid and surfactant in the ammonia nitrogen wastewater is 0.14: 1: 0.6: 0.015;
4) mixing the solid obtained in the step 3) and the filtrate with magnesium ammonium phosphate: nano magnesium hydroxide: the molar ratio of heavy metals is 1: 4: 0.4, mixing and completely reacting.
The magnesium ammonium phosphate in the solid obtained in the step 3) is porous particles, the diameter is 100um, the aperture is 0.5um, the content of ammonia nitrogen in the wastewater is less than 30mg/L, and the removal rate of heavy metals reaches 90%.
Example 15
The embodiment provides a method for removing ammonia nitrogen and heavy metals in rare earth wastewater, which comprises the following steps:
3) adding the nano magnesium hydroxide slurry obtained in the example 1, phosphoric acid and a surfactant into rare earth wastewater, reacting for 30min, and filtering to obtain filtrate and solid; the mass ratio of N, nano magnesium hydroxide slurry, phosphoric acid and surfactant in the ammonia nitrogen wastewater is 0.14: 1: 0.9: 0.03;
4) mixing the solid obtained in the step 3) and the filtrate with magnesium ammonium phosphate: nano magnesium hydroxide: the molar ratio of heavy metals is 1: 4: 0.4, mixing and completely reacting.
The magnesium ammonium phosphate in the solid obtained in the step 3) is porous particles, the diameter is 80um, the aperture is 0.2um, the content of ammonia nitrogen in the wastewater is less than 40mg/L, and the removal rate of heavy metals reaches 90%.
Comparative example 1
The comparative example provides a method for removing ammonia nitrogen and heavy metals in rare earth wastewater, which comprises the following steps:
4) the solid obtained in step 3) of example 8 was mixed with the filtrate in the presence of magnesium ammonium phosphate: nano magnesium hydroxide: the molar ratio of heavy metals is 1: 1: 0.3, mixing and completely reacting.
The content of ammonia nitrogen in the wastewater is less than 20mg/L, and the removal rate of heavy metals is 75 percent.
Comparative example 2
The comparative example provides a method for removing ammonia nitrogen and heavy metals in rare earth wastewater, which comprises the following steps:
4) the solid obtained in step 3) of example 8 was mixed with the filtrate in the presence of magnesium ammonium phosphate: nano magnesium hydroxide: the molar ratio of heavy metals is 1: 4: 0.9, mixing and completely reacting.
The content of ammonia nitrogen in the wastewater is less than 20mg/L, and the removal rate of heavy metals is 70%.
Finally, the method of the present invention is only a preferred embodiment and is not intended to limit the scope of the present invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (4)
1. The application of the mixture of magnesium ammonium phosphate and nano magnesium hydroxide in treating heavy metal-containing wastewater is characterized in that,
the magnesium ammonium phosphate: nano magnesium hydroxide: the molar ratio of heavy metal ions is 1: (3-6): (0.3 to 0.5);
the magnesium ammonium phosphate is porous particles; the diameter of the porous particles is 10-100 um, and the pore diameter is 0.1-0.5 um; the heavy metal is Pb and/or Cd;
the preparation method of the magnesium ammonium phosphate/nano magnesium hydroxide mixture comprises the following steps: adding nano magnesium hydroxide slurry, phosphoric acid and a surfactant into the ammonia nitrogen wastewater, and reacting for 10 min-2 h; the mass ratio of N, nano magnesium hydroxide slurry, phosphoric acid and surfactant in the ammonia nitrogen wastewater is 0.14: 1: (0.5-1.5): (0.01 to 0.05);
the surfactant is one or more of sodium dodecyl benzene sulfonate, sodium dodecyl sulfate, polyethylene glycol and sodium metasilicate.
2. The application of claim 1, wherein the preparation method of the nano magnesium hydroxide slurry comprises the following steps:
1) taking light-burned magnesium powder as a raw material, and mixing the light-burned magnesium powder with a dispersing agent and water according to a mass ratio of 1: (0.01-0.04): (4-6) uniformly mixing, controlling the pH value to be not higher than 12, and adding a grinding medium for grinding; the grinding temperature is 70-80 ℃, the grinding time is 150-190 min, the grinding speed is 1200-1500 rpm, and the average particle size of the grinding medium is 0.5-3 mm;
2) adding a surface modifier into the system obtained in the step 1), and fully modifying to obtain the nano magnesium hydroxide slurry; the mass ratio of the surface modifier to the light-burned magnesium powder is (0.03-0.05): 1.
3. the use according to claim 2, wherein the dispersant is one or more of sodium citrate, sodium lauryl sulfate, sodium glycocholate;
and/or the surface modifier is one or more of silicone oil, stearic acid and phthalate ester.
4. The application of the light-burned magnesium powder in the treatment of ammonia nitrogen wastewater containing heavy metals is characterized by comprising the following steps:
1) taking light-burned magnesium powder as a raw material, and mixing the light-burned magnesium powder with a dispersing agent and water according to a mass ratio of 1: (0.01-0.04): (4-6) uniformly mixing, controlling the pH value to be not higher than 12, and adding a grinding medium for grinding; the grinding temperature is 70-80 ℃, the grinding time is 150-190 min, the grinding speed is 1200-1500 rpm, and the average particle size of the grinding medium is 0.5-3 mm;
2) adding a surface modifier into the system obtained in the step 1), and fully modifying to obtain nano magnesium hydroxide slurry; the mass ratio of the surface modifier to the light-burned magnesium powder is (0.03-0.05): 1;
3) adding the nano magnesium hydroxide slurry, phosphoric acid and a surfactant in the step 2) into the heavy metal-containing ammonia nitrogen wastewater, reacting for 10 min-2 h, and filtering to obtain filtrate and solid; the mass ratio of N, nano magnesium hydroxide slurry, phosphoric acid and surfactant in the ammonia nitrogen wastewater is 0.14: 1: (0.5-1.5): (0.01 to 0.05);
4) mixing the solid obtained in the step 3) and the filtrate with magnesium ammonium phosphate: nano magnesium hydroxide: the molar ratio of heavy metals is 1: (2-10): (0.1-0.8) and completely reacting.
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