CN112645370A - Method for preparing magnesium-based flame retardant by using magnesium-containing wastewater - Google Patents
Method for preparing magnesium-based flame retardant by using magnesium-containing wastewater Download PDFInfo
- Publication number
- CN112645370A CN112645370A CN202011325644.XA CN202011325644A CN112645370A CN 112645370 A CN112645370 A CN 112645370A CN 202011325644 A CN202011325644 A CN 202011325644A CN 112645370 A CN112645370 A CN 112645370A
- Authority
- CN
- China
- Prior art keywords
- magnesium
- aluminum
- flame retardant
- based flame
- preparing
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000011777 magnesium Substances 0.000 title claims abstract description 69
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 title claims abstract description 62
- 229910052749 magnesium Inorganic materials 0.000 title claims abstract description 62
- 239000002351 wastewater Substances 0.000 title claims abstract description 48
- 239000003063 flame retardant Substances 0.000 title claims abstract description 34
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 title claims abstract description 33
- 238000000034 method Methods 0.000 title claims abstract description 27
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 30
- 239000011259 mixed solution Substances 0.000 claims abstract description 22
- SNAAJJQQZSMGQD-UHFFFAOYSA-N aluminum magnesium Chemical compound [Mg].[Al] SNAAJJQQZSMGQD-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000000243 solution Substances 0.000 claims abstract description 17
- CDBYLPFSWZWCQE-UHFFFAOYSA-L sodium carbonate Substances [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 16
- 238000001914 filtration Methods 0.000 claims abstract description 14
- 239000002002 slurry Substances 0.000 claims abstract description 12
- 238000003756 stirring Methods 0.000 claims abstract description 11
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 10
- 239000002131 composite material Substances 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims abstract description 10
- 239000000126 substance Substances 0.000 claims abstract description 10
- JLVVSXFLKOJNIY-UHFFFAOYSA-N Magnesium ion Chemical compound [Mg+2] JLVVSXFLKOJNIY-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000006243 chemical reaction Methods 0.000 claims abstract description 9
- 229910001425 magnesium ion Inorganic materials 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 8
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 8
- 238000005406 washing Methods 0.000 claims abstract description 8
- 150000003839 salts Chemical class 0.000 claims abstract description 7
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 claims abstract description 6
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 6
- 150000001875 compounds Chemical class 0.000 claims abstract description 5
- -1 aluminum ion Chemical class 0.000 claims abstract description 4
- 229910052751 metal Inorganic materials 0.000 claims abstract description 3
- 239000002184 metal Substances 0.000 claims abstract description 3
- 238000002425 crystallisation Methods 0.000 claims description 9
- 230000008025 crystallization Effects 0.000 claims description 9
- 239000000706 filtrate Substances 0.000 claims description 6
- 239000003513 alkali Substances 0.000 claims description 4
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims description 4
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims description 4
- VXAUWWUXCIMFIM-UHFFFAOYSA-M aluminum;oxygen(2-);hydroxide Chemical compound [OH-].[O-2].[Al+3] VXAUWWUXCIMFIM-UHFFFAOYSA-M 0.000 claims description 4
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 claims description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 2
- 239000012670 alkaline solution Substances 0.000 claims description 2
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 claims description 2
- ANBBXQWFNXMHLD-UHFFFAOYSA-N aluminum;sodium;oxygen(2-) Chemical compound [O-2].[O-2].[Na+].[Al+3] ANBBXQWFNXMHLD-UHFFFAOYSA-N 0.000 claims description 2
- 238000000975 co-precipitation Methods 0.000 claims description 2
- 229910001388 sodium aluminate Inorganic materials 0.000 claims description 2
- 239000002994 raw material Substances 0.000 claims 1
- 230000007613 environmental effect Effects 0.000 abstract 1
- 159000000003 magnesium salts Chemical class 0.000 description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 description 6
- 239000000047 product Substances 0.000 description 6
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 description 4
- JGDITNMASUZKPW-UHFFFAOYSA-K aluminium trichloride hexahydrate Chemical compound O.O.O.O.O.O.Cl[Al](Cl)Cl JGDITNMASUZKPW-UHFFFAOYSA-K 0.000 description 3
- 229940009861 aluminum chloride hexahydrate Drugs 0.000 description 3
- 229910001629 magnesium chloride Inorganic materials 0.000 description 3
- 238000001556 precipitation Methods 0.000 description 3
- 238000003747 Grignard reaction Methods 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 229910052943 magnesium sulfate Inorganic materials 0.000 description 2
- 235000019341 magnesium sulphate Nutrition 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000002689 soil Substances 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- XNDZQQSKSQTQQD-UHFFFAOYSA-N 3-methylcyclohex-2-en-1-ol Chemical compound CC1=CC(O)CCC1 XNDZQQSKSQTQQD-UHFFFAOYSA-N 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000008044 alkali metal hydroxides Chemical class 0.000 description 1
- 229940063656 aluminum chloride Drugs 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000012065 filter cake Substances 0.000 description 1
- 230000026030 halogenation Effects 0.000 description 1
- 238000005658 halogenation reaction Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 description 1
- 239000001095 magnesium carbonate Substances 0.000 description 1
- 229910000021 magnesium carbonate Inorganic materials 0.000 description 1
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 description 1
- 239000000347 magnesium hydroxide Substances 0.000 description 1
- 229910001862 magnesium hydroxide Inorganic materials 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 229920000098 polyolefin Polymers 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 235000013599 spices Nutrition 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- 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
- C01F7/00—Compounds of aluminium
- C01F7/78—Compounds containing aluminium and two or more other elements, with the exception of oxygen and hydrogen
- C01F7/784—Layered double hydroxide, e.g. comprising nitrate, sulfate or carbonate ions as intercalating anions
- C01F7/785—Hydrotalcite
-
- 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
- C01F7/00—Compounds of aluminium
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K21/00—Fireproofing materials
- C09K21/02—Inorganic materials
Abstract
The invention discloses a method for preparing a magnesium-based flame retardant by using magnesium-containing wastewater, which comprises the following steps: (1) adding an aluminum-containing compound into the Grignard magnesium-containing wastewater, fully stirring and reacting for 0.5-3 h, reducing the acidity of the wastewater solution to make the pH value reach 3-4, and filtering insoluble substances to be used for the next batch of reaction; (2) then adding soluble aluminum salt according to a certain proportion to make the amount of the aluminum ion substance be 1/4-1/2 of the amount of the magnesium ion substance, stirring and dissolving to obtain a mixed solution A of magnesium aluminum metal salt; (3) preparing an alkaline mixed solution B from sodium hydroxide and sodium carbonate according to a certain proportion; (4) and (3) quickly mixing and coprecipitating the two solutions A and B to prepare magnesium-aluminum composite hydroxide slurry, crystallizing for 3-36 hours at the temperature of 60-100 ℃, and performing centrifugal filtration, washing and drying to obtain the magnesium-based flame retardant. The invention fully utilizes the magnesium resource in the Grignard magnesium-containing wastewater, and the obtained magnesium-based flame retardant has wide application, has the advantages of environmental friendliness, comprehensive utilization of resources and the like, and has good industrialization prospect.
Description
Technical Field
The invention belongs to the field of waste water resource utilization, particularly relates to comprehensive utilization of magnesium resources in magnesium-containing waste water, and particularly provides a method for preparing a magnesium-based flame retardant by utilizing the magnesium-containing waste water.
Background
The Grignard reaction is widely applied to the synthesis of products with high added value, such as medicines, spices, special organic silicon monomers and the like. Can form a large amount of magnesium waste water in the Grignard reaction process, the waste water has strong acid nature, emptys everywhere and can cause environmental pollution, emptys in a large number and can influence soil acidity and alkalinity, changes soil property, and quality of water also can change greatly. The wastewater has high salt content, dissolves partial organic matters, has high COD content, low biodegradability and great treatment difficulty. The magnesium salt content in the waste water is about 20-30%, and the direct discharge causes serious environmental pollution and waste of magnesium resources.
At present, few research reports aiming at resource utilization of magnesium ions in Grignard wastewater are limited to concentration to obtain magnesium salts or precipitation separation by adding alkali. CN200410073583 discloses recovering magnesium ions by generating magnesium sulfate, in the recovery process, a large amount of wastewater needs to be concentrated first, then concentrated sulfuric acid is added to generate magnesium sulfate, high energy consumption is needed, and the concentrated sulfuric acid causes severe corrosion to equipment. CN101130485 discloses recovering magnesium ions by generating magnesium chloride, which is a water-soluble salt, the wastewater needs to be completely evaporated to dryness, the energy consumption is high, and meanwhile, the obtained magnesium chloride often contains organic impurities, and the use of the magnesium chloride is limited due to low purity. CN101665258 discloses a process for recovering magnesium salts from grignard waste water, firstly adjusting the pH value of the waste water with alkali metal hydroxide, then adding carbonate for precipitation to obtain basic magnesium carbonate, thereby avoiding the problem of difficult solid-liquid separation of colloidal magnesium hydroxide precipitate formed by direct precipitation.
From the research results reported in the prior art, the method focuses on how to precipitate or evaporate magnesium ions to obtain a crude magnesium salt product, does not fully consider the final use and product value of the obtained product, and has little practical significance. If magnesium ions in the Grignard waste water are prepared into the magnesium-aluminum composite hydroxide, the magnesium-aluminum composite hydroxide has wide application, particularly has good characteristics on flame retardance of polyolefin, and has huge market prospect along with non-halogenation application and popularization of the flame retardant.
Aiming at the technical problems in the prior art, the invention provides a method for efficiently utilizing magnesium resources in Grignard waste water, which converts magnesium salts in the Grignard waste water into a magnesium-based flame retardant with wide application, has the advantages of low alkali consumption, low cost and high product added value, reduces the salt concentration in the waste water and improves the biodegradability while obtaining the magnesium-based flame retardant, and can be simply and conveniently treated to reach the emission standard.
Disclosure of Invention
The invention aims to provide a method for efficiently utilizing magnesium resources in magnesium-containing wastewater, and a method for converting magnesium salts in Grignard wastewater into magnesium-based flame retardants.
The technical scheme adopted by the invention is as follows: a method for preparing a magnesium-based flame retardant by using magnesium-containing wastewater comprises the following steps:
(l) Adding an aluminum-containing compound into the magnesium-containing wastewater, fully stirring and reacting for 0.5-3 h, reducing the acidity of the wastewater solution to make the pH value reach 3-4, and filtering insoluble substances to be used for the next batch of reaction;
(2) adding soluble aluminum salt into the filtrate obtained in the step (1) according to a certain proportion to enable the amount of aluminum ions to be 1/4-1/2 of the amount of magnesium ions, and stirring and dissolving to obtain a mixed solution A of magnesium-aluminum double metal salt;
(3) preparing an alkaline mixed solution B from sodium hydroxide and sodium carbonate according to a certain proportion;
(4) and (3) quickly mixing and coprecipitating the two solutions A and B to prepare magnesium-aluminum composite hydroxide slurry, crystallizing for a certain time at a certain temperature, and performing centrifugal filtration, washing and drying to obtain the magnesium-based flame retardant.
The aluminum-containing compound is preferably one or two of pseudo-boehmite, aluminum hydroxide and aluminum trioxide.
The soluble aluminum salt is preferably one or two of aluminum chloride, aluminum nitrate, aluminum sulfate and sodium aluminate.
Mg in the solution A2+With Al3+Preferably in a molar ratio of 2:1 to 4: 1.
The mass ratio of sodium carbonate to sodium hydroxide in the alkaline solution B is preferably 0:1 to 1: 1.
The slurry crystallization temperature is preferably 60 to 100 ℃.
The crystallization time of the slurry is preferably 3-36 h.
Compared with the prior art, the invention has the following advantages:
the magnesium salt in the magnesium-containing wastewater can be converted into the widely applied magnesium-based flame retardant by adopting a coprecipitation method, the method has the advantages of low alkali consumption, simple process, low treatment cost and high product added value, the magnesium-based flame retardant is obtained, the salt concentration in the wastewater is reduced, the biodegradability is improved, and the magnesium-based flame retardant can be simply and conveniently treated to reach the emission standard.
Detailed Description
The present invention is described in further detail below with reference to specific examples, but the scope of the present invention is not limited thereto.
Mg in magnesium-containing wastewater used in examples2+Is present in an amount of about 3.0mol/L and has a pH of about-0.48.
Example 1
A method for preparing a magnesium-based flame retardant by using magnesium-containing wastewater comprises the following steps:
(1) adding 15.6g of aluminum hydroxide into 200ml of magnesium-containing wastewater, fully stirring and reacting for 3 hours, reducing the acidity of the wastewater solution to enable the pH value to reach 3-4, and filtering out 3.9g of insoluble substances to be applied to the next batch of reaction;
(2) adding 12.07 parts of the filtrate obtained in the step (1)g aluminum chloride hexahydrate to obtain a mixed solution A, and adding Mg in the mixed solution A2+With Al3+In a molar ratio of 3: 1;
(3) adding 58.3 g of sodium carbonate and 22g of sodium hydroxide into 200ml of water to prepare an alkaline mixed solution B;
(4) and (3) quickly mixing and coprecipitating the two solutions A and B to prepare magnesium-aluminum composite hydroxide slurry, then keeping the crystallization at 65 ℃ for 24 hours, centrifugally filtering, washing and drying to obtain 60.2g of magnesium-based flame retardant with the magnesium-aluminum ratio of 3.
Example 2
A method for preparing a magnesium-based flame retardant by using magnesium-containing wastewater comprises the following steps:
(1) adding 15.6g of pseudo-boehmite into 200ml of magnesium-containing wastewater, fully stirring for reaction for 3 h, reducing the acidity of the wastewater solution to enable the pH value to reach 3-4, and filtering out 1.56g of insoluble substances to be applied to the next batch of reaction;
(2) 45.01g of aluminum nitrate nonahydrate was added to the filtrate obtained in step (1) to obtain a mixed solution A, and Mg was added to the mixed solution A2+With Al3+In a molar ratio of 2: 1;
(3) adding 15.9 g of sodium carbonate and 36g of sodium hydroxide into 200ml of water to prepare an alkaline mixed solution B;
(4) and (3) quickly mixing and coprecipitating the two solutions A and B to prepare magnesium-aluminum composite hydroxide slurry, then keeping the crystallization at 65 ℃ for 24 hours, centrifugally filtering, washing and drying to obtain 83.7g of the magnesium-based flame retardant with the magnesium-aluminum ratio of 3.
Example 3
A method for preparing a magnesium-based flame retardant by using magnesium-containing wastewater comprises the following steps:
(1) adding 7.65g of aluminum oxide into 200ml of Grignard wastewater, fully stirring for reaction for 3 h, reducing the acidity of the wastewater solution to enable the pH value to reach 3-4, and filtering out 3.05g of insoluble substances for the next batch of reaction;
(2) adding 14.48g of aluminum chloride hexahydrate into the filtrate obtained in the step (1) to obtain a mixed solution A, and adding Mg into the mixed solution A2+With Al3+In a molar ratio of 4: 1;
(3) adding 30.9 g of sodium carbonate and 30g of sodium hydroxide into 200ml of water to prepare an alkaline mixed solution B;
(4) and (3) quickly mixing and coprecipitating the two solutions A and B to prepare magnesium-aluminum composite hydroxide slurry, then keeping the crystallization at the temperature of 80 ℃ for 16 hours, and centrifugally filtering, washing and drying to obtain 50.4g of magnesium-based flame retardant with the magnesium-aluminum ratio of 4.
Example 4
A method for preparing a magnesium-based flame retardant by using magnesium-containing wastewater comprises the following steps:
(1) adding 62.4g of aluminum hydroxide into 1L of magnesium-containing wastewater, fully stirring and reacting for 3 hours, and reducing the acidity of the wastewater solution to enable the pH value to reach 3-4;
(2) adding 74.36g of aluminum chloride hexahydrate into the filtrate obtained in the step (1) to obtain a mixed solution A, and enabling Mg in the mixed solution A to be contained2+With Al3+In a molar ratio of 3: 1;
(3) adding 128g of sodium hydroxide into 1L of water to prepare a mixed solution B;
(4) and (3) quickly mixing and coprecipitating the two solutions A and B to prepare magnesium-aluminum composite hydroxide slurry, then keeping the crystallization at 90 ℃ for 12 hours, centrifugally filtering, washing and drying to obtain 410.8g of the magnesium-based flame retardant with the magnesium-aluminum ratio of 3.
Example 5
A method for preparing a magnesium-based flame retardant by using magnesium-containing wastewater comprises the following steps:
(1) adding 4.68Kg of pseudoboehmite and 1.23Kg of sodium metaaluminate into 100L of Grignard wastewater, stirring and dissolving uniformly to obtain a mixed solution A, wherein Mg in the mixed solution A is2+With Al3+In a molar ratio of 4: 1;
(2) adding 23.2Kg of sodium hydroxide into 100L of water to prepare a mixed solution B for later use;
(3) and (3) quickly mixing and coprecipitating the two solutions A and B to prepare magnesium-aluminum composite hydroxide slurry, keeping the temperature of 100 ℃ for crystallization for 6 hours, filtering the reaction solution, washing a filter cake to be alkalescent or neutral by pure water, and drying to obtain 10.2Kg of magnesium-based flame retardant with the magnesium-aluminum ratio of 4.
Claims (7)
1. A method for preparing a magnesium-based flame retardant by using magnesium-containing wastewater is characterized by comprising the following steps: the method comprises the following steps of taking Grignard magnesium-containing wastewater as a raw material, adding an aluminum source, and then carrying out coprecipitation by using alkali to prepare the magnesium-based flame retardant:
(l) Adding an aluminum-containing compound into the magnesium-containing wastewater, fully stirring and reacting for 0.5-3 h, reducing the acidity of the wastewater solution to make the pH value reach 3-4, and filtering insoluble substances to be used for the next batch of reaction;
(2) adding soluble aluminum salt into the filtrate obtained in the step (1) according to a certain proportion to enable the amount of aluminum ions to be 1/4-1/2 of the amount of magnesium ions, and stirring and dissolving to obtain a mixed solution A of magnesium-aluminum double metal salt;
(3) preparing an alkaline mixed solution B from sodium hydroxide and sodium carbonate according to a certain proportion;
(4) and (3) quickly mixing and coprecipitating the two solutions A and B to prepare magnesium-aluminum composite hydroxide slurry, crystallizing for a certain time at a certain temperature, and performing centrifugal filtration, washing and drying to obtain the magnesium-based flame retardant.
2. The method of preparing a magnesium-based flame retardant according to claim 1, wherein: in the step (1), the aluminum-containing compound is one or two of pseudo-boehmite, aluminum hydroxide and aluminum trioxide.
3. The method of preparing a magnesium-based flame retardant according to claim 1, wherein: in the step (2), the soluble aluminum salt is one or two of aluminum chloride, aluminum nitrate, aluminum sulfate and sodium aluminate.
4. The method of preparing a magnesium-based flame retardant according to claim 1, wherein: in the step (2), the adding amount of the soluble aluminum salt is 1/4-1/2 of the amount of the substance of the aluminum ion in the mixed solution as the substance of the magnesium ion.
5. The method of preparing a magnesium-based flame retardant according to claim 1, wherein: in the step (2), the mass ratio of sodium carbonate to sodium hydroxide in the prepared alkaline solution is 0:1-2: 1.
6. The method of preparing a magnesium-based flame retardant according to claim 1, wherein: in the step (3), the crystallization temperature of the obtained slurry is 60-100 ℃.
7. The method of preparing a magnesium-based flame retardant according to claim 1, wherein: in the step (3), the crystallization time of the obtained slurry is 3-36 h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011325644.XA CN112645370A (en) | 2020-11-24 | 2020-11-24 | Method for preparing magnesium-based flame retardant by using magnesium-containing wastewater |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011325644.XA CN112645370A (en) | 2020-11-24 | 2020-11-24 | Method for preparing magnesium-based flame retardant by using magnesium-containing wastewater |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN112645370A true CN112645370A (en) | 2021-04-13 |
Family
ID=75350069
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202011325644.XA Pending CN112645370A (en) | 2020-11-24 | 2020-11-24 | Method for preparing magnesium-based flame retardant by using magnesium-containing wastewater |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112645370A (en) |
-
2020
- 2020-11-24 CN CN202011325644.XA patent/CN112645370A/en active Pending
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN111847416B (en) | Method for preparing hydrated iron phosphate from ferrous sulfate serving as titanium dioxide byproduct | |
| WO2016184055A1 (en) | Process method for extracting magnesium and lithium from brine and coproducing hydrotalcite | |
| CN110699756B (en) | Method for preparing alpha-type gypsum whisker by using ammonia-soda waste liquid | |
| CN111689508B (en) | Method for treating tetrachloro sodium aluminate solid slag | |
| CN106745106B (en) | A method of nanometric magnesium hydroxide is prepared by phosphorus ore de-magging waste liquid | |
| WO2021143809A1 (en) | Method for extracting lithium from lithium-containing low-magnesium brine | |
| WO2018041272A1 (en) | Method for preparing industrial grade lithium carbonate from crude lithium fluoride, and a lithium carbonate product | |
| CN112978805A (en) | Comprehensive recovery method of titanium, iron and sulfate radicals in titanium white waste acid | |
| CN1335262A (en) | Lithium carbonate preparing process from salt lake bittern with high Mg/Li ratio | |
| CN111137909B (en) | Method for stepwise recovering lithium and magnesium in salt lake brine | |
| CN102776367B (en) | Method for demagging ground phosphorite and preparing MgHPO4.3H2O | |
| CN103290239A (en) | Method for extracting vanadium from production flow of aluminum oxide | |
| CN112645370A (en) | Method for preparing magnesium-based flame retardant by using magnesium-containing wastewater | |
| CN105271341A (en) | Method for preparing potassium alum by utilization of activated clay production waste water | |
| CN105293796A (en) | Method for co-production of sodalumite and gypsum through activated clay production mother liquid | |
| CN112028094A (en) | Method for preparing magnesium hydroxide and calcium chloride by treating desulfurization wastewater of coal-fired power plant | |
| CN1425612A (en) | Process for preparing active aluminium oxide | |
| CN112573550A (en) | Method for preparing magnesium-based flame retardant by utilizing Grignard wastewater | |
| CN101780978A (en) | Method for recycling sodium molybdate solution from molybdenum contained silica slag | |
| CN1673083A (en) | Technological process of preparing potassium nitrate and magnesium chloride | |
| CN105384184A (en) | Method for preparing alum from mother solution produced by activated clay | |
| CN109095484A (en) | A method of utilizing desulfurization wastewater preparing magnesium hydroxide | |
| US11180369B2 (en) | Renewable magnesium removing agent and its use in preparation of low-magnesium lithium-rich brine | |
| CN113651344A (en) | Method for purifying magnesium chloride by using salt lake brine | |
| CN1103321C (en) | Clean production process of ammonium chromate crystal |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20210413 |