CN110092385B - Preparation method of magnesium aluminum silicate hydrogel - Google Patents
Preparation method of magnesium aluminum silicate hydrogel Download PDFInfo
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- CN110092385B CN110092385B CN201910256715.6A CN201910256715A CN110092385B CN 110092385 B CN110092385 B CN 110092385B CN 201910256715 A CN201910256715 A CN 201910256715A CN 110092385 B CN110092385 B CN 110092385B
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- SNAAJJQQZSMGQD-UHFFFAOYSA-N aluminum magnesium Chemical compound [Mg].[Al] SNAAJJQQZSMGQD-UHFFFAOYSA-N 0.000 title claims abstract description 55
- 239000000017 hydrogel Substances 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 54
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 42
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 37
- 239000008367 deionised water Substances 0.000 claims abstract description 35
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 35
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000003513 alkali Substances 0.000 claims abstract description 24
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 24
- 239000010703 silicon Substances 0.000 claims abstract description 24
- 238000003756 stirring Methods 0.000 claims abstract description 21
- 239000007864 aqueous solution Substances 0.000 claims abstract description 17
- 238000006243 chemical reaction Methods 0.000 claims abstract description 17
- 239000000843 powder Substances 0.000 claims abstract description 16
- 239000000243 solution Substances 0.000 claims abstract description 15
- 235000019353 potassium silicate Nutrition 0.000 claims abstract description 14
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims abstract description 14
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 claims abstract description 11
- 159000000003 magnesium salts Chemical class 0.000 claims abstract description 11
- 238000002156 mixing Methods 0.000 claims abstract description 11
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 claims abstract description 7
- 238000001816 cooling Methods 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 7
- 238000007873 sieving Methods 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims abstract description 7
- 239000000126 substance Substances 0.000 claims abstract description 6
- 229910052782 aluminium Inorganic materials 0.000 claims description 25
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 24
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 23
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 21
- 239000011777 magnesium Substances 0.000 claims description 21
- 229910052749 magnesium Inorganic materials 0.000 claims description 21
- 239000007788 liquid Substances 0.000 claims description 17
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 14
- 239000012295 chemical reaction liquid Substances 0.000 claims description 14
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims description 12
- 235000017557 sodium bicarbonate Nutrition 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 9
- 239000000377 silicon dioxide Substances 0.000 claims description 7
- 235000012239 silicon dioxide Nutrition 0.000 claims description 6
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical group [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 claims description 4
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical group Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims description 4
- YIXJRHPUWRPCBB-UHFFFAOYSA-N magnesium nitrate Chemical compound [Mg+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O YIXJRHPUWRPCBB-UHFFFAOYSA-N 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
- 229910001629 magnesium chloride Inorganic materials 0.000 claims description 2
- 239000013078 crystal Substances 0.000 abstract description 13
- 230000007547 defect Effects 0.000 abstract description 6
- 230000009286 beneficial effect Effects 0.000 abstract description 4
- 238000000975 co-precipitation Methods 0.000 abstract description 4
- 239000012535 impurity Substances 0.000 abstract description 4
- 230000005496 eutectics Effects 0.000 abstract description 3
- 238000001556 precipitation Methods 0.000 abstract description 3
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 abstract description 2
- 229940091250 magnesium supplement Drugs 0.000 description 18
- 238000010438 heat treatment Methods 0.000 description 8
- 238000001027 hydrothermal synthesis Methods 0.000 description 7
- 229910052604 silicate mineral Inorganic materials 0.000 description 7
- MFUVDXOKPBAHMC-UHFFFAOYSA-N magnesium;dinitrate;hexahydrate Chemical compound O.O.O.O.O.O.[Mg+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MFUVDXOKPBAHMC-UHFFFAOYSA-N 0.000 description 4
- 239000003921 oil Substances 0.000 description 4
- 238000010992 reflux Methods 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 3
- XNDZQQSKSQTQQD-UHFFFAOYSA-N 3-methylcyclohex-2-en-1-ol Chemical compound CC1=CC(O)CCC1 XNDZQQSKSQTQQD-UHFFFAOYSA-N 0.000 description 2
- JGDITNMASUZKPW-UHFFFAOYSA-K aluminium trichloride hexahydrate Chemical compound O.O.O.O.O.O.Cl[Al](Cl)Cl JGDITNMASUZKPW-UHFFFAOYSA-K 0.000 description 2
- 229940009861 aluminum chloride hexahydrate Drugs 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 239000010410 layer Substances 0.000 description 2
- 229940050906 magnesium chloride hexahydrate Drugs 0.000 description 2
- DHRRIBDTHFBPNG-UHFFFAOYSA-L magnesium dichloride hexahydrate Chemical compound O.O.O.O.O.O.[Mg+2].[Cl-].[Cl-] DHRRIBDTHFBPNG-UHFFFAOYSA-L 0.000 description 2
- 239000012429 reaction media Substances 0.000 description 2
- 235000012431 wafers Nutrition 0.000 description 2
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- OBNDGIHQAIXEAO-UHFFFAOYSA-N [O].[Si] Chemical compound [O].[Si] OBNDGIHQAIXEAO-UHFFFAOYSA-N 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 229940063656 aluminum chloride Drugs 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000005341 cation exchange Methods 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 238000002288 cocrystallisation Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000003063 flame retardant Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 229960002337 magnesium chloride Drugs 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 235000010755 mineral Nutrition 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000006254 rheological additive Substances 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 239000002562 thickening agent Substances 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/0052—Preparation of gels
- B01J13/0065—Preparation of gels containing an organic phase
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/0073—Preparation of non-Newtonian sols, e.g. thixotropic solutions
- B01J13/0078—Preparation of non-Newtonian sols, e.g. thixotropic solutions containing inorganic material and water
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/20—Silicates
- C01B33/26—Aluminium-containing silicates, i.e. silico-aluminates
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Silicates, Zeolites, And Molecular Sieves (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
A preparation method of magnesium aluminum silicate hydrogel comprises the following steps: mixing sodium bicarbonate, sodium hydroxide, deionized water and ethylene glycol to prepare an alkali liquor, mixing magnesium salt, aluminum salt and deionized water to prepare a magnesium-aluminum-containing aqueous solution, dripping water glass into the alkali liquor under the conditions of constant temperature of 40-60 ℃ and stirring to obtain a silicon-containing solution, dripping the magnesium-aluminum-containing aqueous solution into the silicon-containing solution to obtain a reaction solution, stirring the obtained reaction solution at constant temperature of 90-140 ℃ for 8-24 hours, cooling to room temperature, centrifuging, washing with water, drying, crushing, sieving to obtain magnesium-aluminum silicate powder, adding the magnesium-aluminum silicate powder into the deionized water, stirring uniformly, and standing to obtain a finished product; the invention takes the glycol aqueous solution as an azeotropic system, enhances heat transfer, protects water from being evaporated, avoids the precipitation of a crystal forming substance in a reaction solution due to supersaturation, can inhibit impurity eutectic and coprecipitation, reduces crystal defects, ensures that the prepared product has fine and uniform grain diameter, and is beneficial to forming hydrogel.
Description
(I) the technical field
The invention relates to a preparation method of magnesium aluminum silicate hydrogel.
(II) background of the invention
A typical layered magnesium aluminum silicate mineral, such as magadiite, has two layers of silicon-oxygen tetrahedral wafers sandwiching a layer of magnesium-oxygen octahedral wafers, each sheet having a negative charge, and some hydrated metal cations adsorbed between the two sheets to balance the negative charge on the sheets. The lamellar magnesium aluminum silicate mineral has small lamellar size, interlayer cation exchange performance and low lamellar charge, is easy to peel off in a water phase to form hydrogel, is easy to modify and can be applied to rheological additives, thickening agents, adsorbents, catalysts, flame retardants and the like.
The layered magnesium aluminum silicate non-metallic mineral is very rare in nature, and has low purity and difficult purification. Therefore, it is usually prepared by artificial synthesis. The artificial synthesis method generally adopts a hydrothermal synthesis method, and the magnesium aluminum silicate mineral is prepared by crystallization of reaction liquid for several hours to several days at a constant temperature of 90-450 ℃ in a laboratory under autogenous water pressure. The hydrothermal synthesis method has simple device, but large energy consumption and high sealing requirement on the reaction kettle. Because the reaction kettle which is kept still is at a high temperature for a long time, liquid water contained in a reaction system in the reaction kettle is changed into water vapor, the water vapor is easy to leak, and the liquid water in a reaction liquid is reduced or even disappears; when the crystallization temperature is higher than 374 ℃, liquid water is almost absent. In the process of synthesizing the magnesium-aluminum silicate mineral by a hydrothermal method, solid-liquid imbalance occurs due to the loss of liquid water in a reaction kettle, so that a crystal forming substance in a reaction liquid is separated out in a supersaturated state, crystal forming ions are limited to enter a unit cell structure, crystal defects are caused, and the formation and growth of pure crystal nuclei of the magnesium-aluminum silicate mineral are not facilitated. The ethylene glycol aqueous solution is used as an azeotropic system to enhance heat transfer, is used for preparing a hydrothermal reaction medium of the magnesium aluminum silicate mineral, can protect water from being evaporated, avoids local supersaturation, can inhibit impurity eutectic and coprecipitation, reduces crystal defects, enables the prepared product to have fine and uniform grain size, and is beneficial to forming hydrogel.
Disclosure of the invention
The invention aims to provide a preparation method of magnesium aluminum silicate hydrogel. By changing the traditional hydrothermal synthesis process and adopting an ethylene glycol aqueous solution as an azeotropic system, the heat transfer is enhanced, and the precipitation of a crystal forming substance in a reaction liquid in a supersaturated state is avoided, so that impurity co-crystallization and co-precipitation are inhibited, the crystal defects are reduced, the prepared product has fine and uniform particle size, and the hydrogel is favorably formed.
The technical scheme of the invention is as follows:
a preparation method of magnesium aluminum silicate hydrogel comprises the following steps:
(1) mixing sodium bicarbonate, sodium hydroxide, deionized water and ethylene glycol to prepare an alkali liquor;
the mass ratio of the sodium bicarbonate to the sodium hydroxide to the deionized water to the ethylene glycol is 1: 1-2: 8-9: 7.5 to 23;
(2) mixing magnesium salt, aluminum salt and deionized water to prepare a magnesium-aluminum containing aqueous solution;
the mass ratio of the magnesium salt to the contained magnesium to the aluminum salt to the deionized water is 1: 0.05-0.075: 22 to 26;
the magnesium salt is, for example, magnesium chloride or magnesium nitrate;
the aluminum salt is, for example, aluminum chloride or aluminum nitrate;
(3) under the conditions of constant temperature of 40-60 ℃ and stirring, firstly dropwise adding water glass into the alkali liquor prepared in the step (1) to obtain a silicon-containing liquid, then dropwise adding the magnesium-aluminum-containing water solution prepared in the step (2) into the silicon-containing liquid to obtain a reaction liquid, stirring the obtained reaction liquid at the constant temperature of 90-140 ℃ for 8-24 hours, then cooling to room temperature (20-30 ℃), centrifuging, washing with water, drying (60-90 ℃ for 6-24 hours), crushing, and sieving (100 meshes) to obtain magnesium-aluminum silicate powder;
the mass ratio of sodium bicarbonate contained in the alkali liquor to silicon dioxide contained in the water glass is 1: 0.32 to 0.33;
the ratio of the amount of the silicon-to-aluminum-containing substance in the reaction solution is 19 to 28.5: 1;
the ratio of the amount of magnesium contained in the reaction solution to the sum of the amounts of aluminum and silicon is 1: 1.31 to 1.35, preferably 1.33;
(4) adding the magnesium aluminum silicate powder obtained in the step (3) into deionized water, uniformly stirring, and standing to obtain magnesium aluminum silicate hydrogel;
the mass ratio of the magnesium aluminum silicate powder to the deionized water is 2-5: 100.
the invention has the beneficial effects that:
the traditional high-temperature hydrothermal synthesis method is easy to cause solid-liquid imbalance, and crystal formation ions are limited to enter a unit cell structure, so that crystal defects are caused. The invention uses the glycol aqueous solution as an azeotropic system to strengthen heat transfer, is used for preparing a hydrothermal reaction medium of the magnesium aluminum silicate mineral, protects water from being evaporated, avoids the precipitation of a crystal forming substance in a reaction liquid in a supersaturated state, can inhibit impurity eutectic and coprecipitation, reduces crystal defects, ensures that the prepared product has fine and uniform grain diameter, and is beneficial to forming hydrogel.
(IV) description of the drawings
FIG. 1: the magnesium aluminum silicate hydrogels prepared in examples 1-4 (from left to right).
(V) detailed description of the preferred embodiments
The technical solution of the present invention is further described below by using specific examples, but the scope of the present invention is not limited thereto.
The water glass used in the examples was purchased from Aldrich, with a mass fraction of silica of 27% and a mass fraction of sodium hydroxide of 14%.
Example 1
The preparation method of the magnesium aluminum silicate hydrogel of the embodiment comprises the following steps:
(1) mixing 10.78g of sodium bicarbonate, 11.43g of sodium hydroxide, 89g of deionized water and 85g of ethylene glycol according to the mass ratio of 1: 1.06: 8.3: 7.9 of sodium bicarbonate to sodium hydroxide to deionized water to prepare alkali liquor.
(2) Mixing 9.23g of magnesium chloride hexahydrate, 1.13g of aluminum nitrate nonahydrate and 27g of deionized water according to the mass ratio of magnesium in magnesium salt to aluminum in aluminum salt to deionized water of 1: 0.075: 25 to prepare an aqueous solution containing magnesium and aluminum.
(3) Heating the alkali liquor by using an oil bath, configuring a heating reflux condensing device, keeping the temperature at 40 ℃, dropwise adding 12.79g of water glass into the alkali liquor under the stirring condition according to the mass ratio of sodium bicarbonate contained in the alkali liquor to silicon dioxide contained in the water glass of 1: 0.320. According to the molar ratio of silicon to aluminum of 19: 1, and the ratio of the mole number of magnesium to the sum of the mole numbers of aluminum and silicon is 1: 1.33, and then dropwise adding an aqueous solution containing magnesium and aluminum into the silicon-containing liquid to obtain a reaction liquid.
(4) Keeping the reaction solution at the constant temperature of 90 ℃, stirring for reaction for 8 hours, then cooling to room temperature, centrifuging, washing with water, drying (60 ℃, 24 hours), crushing, and sieving (100 meshes) to obtain the magnesium-aluminum silicate powder. Adding the magnesium aluminum silicate powder into deionized water according to the mass fraction of 5%, uniformly stirring, and standing to obtain magnesium aluminum silicate hydrogel.
In the figure, (a) is a magnesium aluminum silicate hydrogel prepared in example 1.
Example 2
The preparation method of the magnesium aluminum silicate hydrogel of the embodiment comprises the following steps:
(1) mixing 10.78g of sodium bicarbonate, 12.89g of sodium hydroxide, 89g of deionized water and 109g of ethylene glycol according to the mass ratio of 1: 1.20: 8.3: 10.1 of sodium bicarbonate to sodium hydroxide to deionized water to prepare alkali liquor.
(2) According to the mass ratio of magnesium in magnesium salt to aluminum in aluminum salt to deionized water of 1: 0.067: 23, 11.64g of magnesium nitrate hexahydrate, 0.65g of aluminum chloride hexahydrate and 25g of deionized water are mixed to prepare an aqueous solution containing magnesium and aluminum.
(3) Heating the alkali liquor by using an oil bath, configuring a heating reflux condensing device, keeping the temperature at 45 ℃, dropwise adding 12.87g of water glass into the alkali liquor to obtain a silicon-containing liquid under the stirring condition according to the mass ratio of sodium bicarbonate contained in the alkali liquor to silicon dioxide contained in the water glass of 1: 0.322. According to the molar ratio of silicon to aluminum of 21.5: 1, and the ratio of the mole number of magnesium to the sum of the mole numbers of aluminum and silicon is 1: 1.33, and then dropwise adding an aqueous solution containing magnesium and aluminum into the silicon-containing liquid to obtain a reaction liquid.
(4) And keeping the temperature of the reaction liquid at 100 ℃, stirring and reacting for 10 hours, then cooling to room temperature, centrifuging, washing with water, drying (70 ℃, 20 hours), crushing, and sieving (100 meshes) to obtain the magnesium-aluminum silicate powder. Adding the magnesium aluminum silicate powder into deionized water according to the mass fraction of 4%, uniformly stirring, and standing to obtain magnesium aluminum silicate hydrogel.
In the figure, (b) is a magnesium aluminum silicate hydrogel prepared in example 2.
Example 3
The preparation method of the magnesium aluminum silicate hydrogel of the embodiment comprises the following steps:
(1) mixing 9.49g of sodium bicarbonate, 13.46g of sodium hydroxide, 82g of deionized water and 130g of ethylene glycol according to the mass ratio of 1: 1.42: 8.6: 13.7 of sodium bicarbonate to sodium hydroxide to deionized water to prepare alkali liquor.
(2) According to the mass ratio of magnesium in magnesium salt to aluminum in aluminum salt to deionized water of 1: 0.059: 23, 8.12g of magnesium chloride hexahydrate, 0.51g of aluminum chloride hexahydrate and 22g of deionized water are mixed to prepare the aqueous solution containing magnesium and aluminum.
(3) Heating the alkali liquor by using an oil bath, configuring a heating reflux condensing device, keeping the temperature at 50 ℃, dropwise adding 11.38g of water glass into the alkali liquor under the stirring condition according to the mass ratio of sodium bicarbonate contained in the alkali liquor to silicon dioxide contained in the water glass of 1: 0.324 to obtain silicon-containing liquid. According to the molar ratio of silicon to aluminum of 24.2: 1, and the ratio of the mole number of magnesium to the sum of the mole numbers of aluminum and silicon is 1: 1.33, and then dropwise adding an aqueous solution containing magnesium and aluminum into the silicon-containing liquid to obtain a reaction liquid.
(4) And keeping the temperature of the reaction solution at 110 ℃, stirring for reacting for 18h, then cooling to room temperature, centrifuging, washing with water, drying (80 ℃, 12h), crushing, and sieving (100 meshes) to obtain the magnesium-aluminum silicate powder. Adding the magnesium aluminum silicate powder into deionized water according to the mass fraction of 3%, uniformly stirring, and standing to obtain magnesium aluminum silicate hydrogel.
In the figure, (c) is a magnesium aluminum silicate hydrogel prepared in example 3.
Example 4
The preparation method of the magnesium aluminum silicate hydrogel of the embodiment comprises the following steps:
(1) mixing 7.91g of sodium bicarbonate, 15.66g of sodium hydroxide, 69g of deionized water and 182g of ethylene glycol according to the mass ratio of 1: 1.98: 8.7: 23.0 of sodium bicarbonate to sodium hydroxide to deionized water to prepare alkali liquor.
(2) 8.53g of magnesium nitrate hexahydrate, 0.57g of aluminum nitrate nonahydrate and 19g of deionized water are mixed according to the mass ratio of magnesium in the magnesium salt to aluminum in the aluminum salt to deionized water of 1: 0.051: 24 to prepare an aqueous solution containing magnesium and aluminum.
(3) Heating the alkali liquor by using an oil bath, configuring a heating reflux condensing device, keeping the temperature at 60 ℃, dropwise adding 9.54g of water glass into the alkali liquor under the stirring condition according to the mass ratio of sodium bicarbonate contained in the alkali liquor to silicon dioxide contained in the water glass of 1: 0.326 to obtain silicon-containing liquid. According to the molar ratio of silicon to aluminum of 28: 1, and the ratio of the mole number of magnesium to the sum of the mole numbers of aluminum and silicon is 1: 1.33, and then dropwise adding an aqueous solution containing magnesium and aluminum into the silicon-containing liquid to obtain a reaction liquid.
(4) Keeping the temperature of the reaction solution constant at 120 ℃, stirring and reacting for 24h, then cooling to room temperature, centrifuging, washing with water, drying (90 ℃, 8h), crushing, and sieving (100 meshes) to obtain the magnesium aluminum silicate powder. Adding the magnesium aluminum silicate powder into deionized water according to the mass fraction of 2%, uniformly stirring, and standing to obtain the magnesium aluminum silicate hydrogel.
In the figure, (d) is a magnesium aluminum silicate hydrogel prepared in example 4.
Claims (5)
1. A preparation method of magnesium aluminum silicate hydrogel is characterized by comprising the following steps:
(1) mixing sodium bicarbonate, sodium hydroxide, deionized water and ethylene glycol to prepare an alkali liquor;
the mass ratio of the sodium bicarbonate to the sodium hydroxide to the deionized water to the ethylene glycol is 1: 1-2: 8-9: 7.5 to 23;
(2) mixing magnesium salt, aluminum salt and deionized water to prepare a magnesium-aluminum containing aqueous solution;
the mass ratio of the magnesium salt to the contained magnesium to the aluminum salt to the deionized water is 1: 0.05-0.075: 22 to 26;
(3) under the conditions of constant temperature of 40-60 ℃ and stirring, firstly dropwise adding water glass into the alkali liquor prepared in the step (1) to obtain a silicon-containing liquid, then dropwise adding the magnesium-aluminum-containing aqueous solution prepared in the step (2) into the silicon-containing liquid to obtain a reaction liquid, stirring the obtained reaction liquid at the constant temperature of 90-140 ℃ for 8-24 hours, then cooling to room temperature, centrifuging, washing with water, drying, crushing and sieving to obtain magnesium-aluminum silicate powder;
the mass ratio of sodium bicarbonate contained in the alkali liquor to silicon dioxide contained in the water glass is 1: 0.32 to 0.33;
the ratio of the amount of the silicon-to-aluminum-containing substance in the reaction solution is 19 to 28.5: 1;
the ratio of the amount of magnesium to the sum of the amounts of aluminum and silicon contained in the reaction solution is 1: 1.31 to 1.35;
(4) and (4) adding the magnesium aluminum silicate powder obtained in the step (3) into deionized water, uniformly stirring, and standing to obtain the magnesium aluminum silicate hydrogel.
2. The method of claim 1, wherein in step (2), the magnesium salt is magnesium chloride or magnesium nitrate.
3. The method of producing a magnesium aluminum silicate hydrogel according to claim 1, wherein in the step (2), the aluminum salt is aluminum chloride or aluminum nitrate.
4. The method of producing a magnesium aluminum silicate hydrogel according to claim 1, wherein in the step (3), the ratio of the amount of magnesium contained in said reaction solution to the sum of the amounts of aluminum and silicon is 1: 1.33.
5. the method for preparing magnesium aluminum silicate hydrogel according to claim 1, wherein in the step (4), the mass ratio of magnesium aluminum silicate powder to deionized water is 2-5: 100.
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