CN117800374A - Method for synthesizing magnesium-aluminum hydrotalcite - Google Patents
Method for synthesizing magnesium-aluminum hydrotalcite Download PDFInfo
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- GDVKFRBCXAPAQJ-UHFFFAOYSA-A dialuminum;hexamagnesium;carbonate;hexadecahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Al+3].[Al+3].[O-]C([O-])=O GDVKFRBCXAPAQJ-UHFFFAOYSA-A 0.000 title claims abstract description 60
- 229960001545 hydrotalcite Drugs 0.000 title claims abstract description 60
- 229910001701 hydrotalcite Inorganic materials 0.000 title claims abstract description 60
- SNAAJJQQZSMGQD-UHFFFAOYSA-N aluminum magnesium Chemical compound [Mg].[Al] SNAAJJQQZSMGQD-UHFFFAOYSA-N 0.000 title claims abstract description 55
- 238000000034 method Methods 0.000 title claims abstract description 39
- 230000002194 synthesizing effect Effects 0.000 title claims abstract description 28
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 69
- 238000000227 grinding Methods 0.000 claims abstract description 60
- 238000006243 chemical reaction Methods 0.000 claims abstract description 55
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 48
- 239000000395 magnesium oxide Substances 0.000 claims abstract description 28
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims abstract description 28
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims abstract description 28
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims abstract description 25
- QWDJLDTYWNBUKE-UHFFFAOYSA-L magnesium bicarbonate Chemical compound [Mg+2].OC([O-])=O.OC([O-])=O QWDJLDTYWNBUKE-UHFFFAOYSA-L 0.000 claims abstract description 25
- 239000002370 magnesium bicarbonate Substances 0.000 claims abstract description 25
- 229910000022 magnesium bicarbonate Inorganic materials 0.000 claims abstract description 25
- 235000014824 magnesium bicarbonate Nutrition 0.000 claims abstract description 25
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000010438 heat treatment Methods 0.000 claims abstract description 21
- 239000007864 aqueous solution Substances 0.000 claims abstract description 19
- 238000002156 mixing Methods 0.000 claims abstract description 19
- 238000001035 drying Methods 0.000 claims abstract description 10
- 238000005406 washing Methods 0.000 claims abstract description 4
- 238000001914 filtration Methods 0.000 claims abstract description 3
- 238000001238 wet grinding Methods 0.000 claims abstract description 3
- 239000000243 solution Substances 0.000 claims description 10
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims description 3
- 239000002245 particle Substances 0.000 abstract description 15
- 239000012535 impurity Substances 0.000 abstract description 5
- 238000004321 preservation Methods 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 18
- 230000015572 biosynthetic process Effects 0.000 description 16
- 238000003786 synthesis reaction Methods 0.000 description 16
- 238000009736 wetting Methods 0.000 description 16
- 239000000047 product Substances 0.000 description 9
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 6
- 239000006227 byproduct Substances 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 3
- 239000001569 carbon dioxide Substances 0.000 description 3
- 229910002092 carbon dioxide Inorganic materials 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 238000002425 crystallisation Methods 0.000 description 3
- 230000008025 crystallization Effects 0.000 description 3
- 238000010899 nucleation Methods 0.000 description 3
- 230000006911 nucleation Effects 0.000 description 3
- 238000001308 synthesis method Methods 0.000 description 3
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 2
- 238000000975 co-precipitation Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 238000005342 ion exchange Methods 0.000 description 2
- 238000005498 polishing Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- 230000006750 UV protection Effects 0.000 description 1
- YMDYLBWLYFQCEJ-UHFFFAOYSA-I [Mg+2].[Al+3].OC([O-])=O.OC([O-])=O.OC([O-])=O.OC([O-])=O.OC([O-])=O Chemical compound [Mg+2].[Al+3].OC([O-])=O.OC([O-])=O.OC([O-])=O.OC([O-])=O.OC([O-])=O YMDYLBWLYFQCEJ-UHFFFAOYSA-I 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- UJOHNXQDVUADCG-UHFFFAOYSA-L aluminum;magnesium;carbonate Chemical group [Mg+2].[Al+3].[O-]C([O-])=O UJOHNXQDVUADCG-UHFFFAOYSA-L 0.000 description 1
- 125000000129 anionic group Chemical group 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 238000005461 lubrication Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000005060 rubber Substances 0.000 description 1
Abstract
The invention discloses a method for synthesizing magnesium aluminum hydrotalcite, which comprises the following steps: (1) Mixing magnesium oxide, magnesium bicarbonate, aluminum hydroxide and sodium hydroxide, and then adding an ethanol aqueous solution for wet grinding; (2) grinding while gradually heating, and then carrying out heat preservation reaction; (3) And (3) after the reaction is finished, recovering to normal temperature, filtering, washing with water and drying to obtain the magnesium aluminum hydrotalcite. The magnesium aluminum hydrotalcite obtained by the invention has high crystallinity, smaller particle size, good particle size dispersibility, high purity, no impurity and high yield.
Description
Technical Field
The invention relates to a method for synthesizing magnesium aluminum hydrotalcite, and belongs to the technical field of hydrotalcite.
Background
Hydrotalcite-like compounds, also called layered double hydroxides, belong to anionic layered compounds, and typical hydrotalcite is magnesium aluminum carbonate hydrotalcite, has good heat stability, flame retardance, ultraviolet resistance and other properties, and is widely applied in the fields of plastics, rubber, glass and the like.
The preparation method of the hydrotalcite-like compound comprises a coprecipitation method, an ion exchange method, a hydrothermal method, a roasting recovery method, a nucleation/crystallization separation method and the like, but the prior art has certain defects: in the coprecipitation method, nucleation and crystallization are carried out simultaneously, so that the particle size distribution range of the product is wider, the particle size is irregular, a large amount of byproducts and wastewater are generated, and the cost is high; in the ion exchange method, the process is complex and tedious, and is time-consuming and labor-consuming; in the hydrothermal method, a large amount of wastewater is generated, and the yield is low; in the roasting recovery method, high-temperature roasting is needed, equipment investment is large, and the process is complex; in the nucleation/crystallization separation method, equipment needs to be specially manufactured, the complexity of the process is increased, the reaction concentration needs to be strictly controlled, and the purity of hydrotalcite is greatly reduced due to the too high concentration.
Disclosure of Invention
At least aiming at the problems existing in the prior art, the invention provides a method for synthesizing magnesium aluminum hydrotalcite, which has the advantages of high crystallinity of the obtained magnesium aluminum hydrotalcite, small particle size, good particle size dispersibility, high purity, no impurity and high yield.
In order to achieve the above purpose, the present invention adopts the following technical scheme: the synthesis method of the magnesium aluminum hydrotalcite comprises the following steps:
(1) Mixing magnesium oxide, magnesium bicarbonate, aluminum hydroxide and sodium hydroxide, adding ethanol aqueous solution for wet grinding, and grinding for 20-30 min;
(2) Continuously grinding, gradually heating, and preserving heat to finish the reaction;
(3) And (3) after the reaction is finished, recovering to normal temperature, filtering, washing with water and drying to obtain the magnesium aluminum hydrotalcite.
Preferably, in the step (1), magnesium oxide, magnesium bicarbonate, aluminum hydroxide and sodium hydroxide are mixed according to a molar ratio of 2:1:1:3.
Preferably, in the step (1), the amount of the aqueous ethanol solution added is 1 to 2 times the weight of magnesium oxide.
Preferably, in the step (1), the mass fraction of the ethanol aqueous solution is 70-80%, and the particle size uniformity of the product is improved during grinding.
Preferably, in the step (1) and the step (2), the grinding speed is 300-500 r/min.
Preferably, in the step (2), the temperature is gradually increased to 75-85 ℃, and the reaction is kept for 1-1.5 h.
Wherein, in the step (2), the gradual heating rate is 0.5-1 ℃/min.
Preferably, in the step (3), the water is washed for 2 to 3 times, and the pure water is 2 to 3 times of the ethanol water solution each time.
Preferably, in the step (3), the drying temperature is 90-100 ℃ for 6-8 hours.
Preferably, in the step (3), the product is ground in the drying process, and the grinding is carried out every 2-3 hours, so that the drying agglomeration is avoided, the crystallinity of the product is improved, and the particle size uniformity of the product is further improved.
Preferably, in step (1), the purity of the magnesium oxide is not less than 98%.
Preferably, in step (1), the purity of the magnesium bicarbonate is not less than 98%.
Preferably, in step (1), the purity of the aluminum hydroxide is not less than 99%.
The invention has the beneficial effects that: the magnesium aluminum hydrotalcite synthesis method takes magnesium oxide, magnesium bicarbonate, aluminum hydroxide and sodium hydroxide as raw materials, does not need carbon dioxide to provide carbonate source, and all the magnesium oxide, the magnesium bicarbonate and the aluminum hydroxide are converted into hydrotalcite at proper grinding and temperature, so that the maximum atomic economy is realized; meanwhile, the byproduct is less, the yield is high, the cost is low, and the product quality is stable; the magnesium aluminum hydrotalcite provided by the invention has the advantages of high crystallinity, good particle size uniformity, high purity and no impurity; the invention has simple preparation and convenient operation; the grinding lubrication adopts the ethanol water solution, which is beneficial to improving the particle size uniformity of the product on one hand, and is beneficial to dissolving byproducts and impurities on the other hand, so that the product is convenient to filter.
Detailed Description
The invention will now be more clearly and more fully described by way of the following specific examples, which are not intended to be limiting. The specific conditions are not noted in the examples and are carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents, instruments and components used are conventional products commercially available without identifying the manufacturer.
The purity of the magnesium oxide used in the invention is more than or equal to 98%; the purity of the magnesium bicarbonate is more than or equal to 98 percent; the purity of the aluminum hydroxide is more than or equal to 99 percent.
Example 1
The method for synthesizing the magnesium aluminum hydrotalcite comprises the following specific synthesis steps:
(1) Mixing 40.3g of magnesium oxide, 73.15g of magnesium bicarbonate, 39g of aluminum hydroxide and 40.3g of sodium hydroxide, adding 40.3g of 75wt% ethanol aqueous solution, wetting and grinding at a grinding speed of 400r/min for 25min;
(2) Continuously grinding at the rotating speed of 400r/min, gradually heating to 80 ℃ at the speed of 0.5-1 ℃/min, and preserving heat for reaction for 1.5h;
(3) And after the reaction is finished, the reaction is restored to normal temperature, filtered, washed for 2 times, the pure water dosage is 80.6g each time, and then dried for 6 hours at the temperature of 95 ℃ and ground for once every 2 hours, thus obtaining 147.96g of magnesium aluminum hydrotalcite.
Example 2
The method for synthesizing the magnesium aluminum hydrotalcite comprises the following specific synthesis steps:
(1) Mixing 60.45g of magnesium oxide, 109.725g of magnesium bicarbonate, 58.5g of aluminum hydroxide and 90g of sodium hydroxide, adding 60.45g of 75wt% ethanol aqueous solution, wetting and grinding at a grinding speed of 400r/min for 25min;
(2) Continuously grinding at the rotating speed of 400r/min, gradually heating to 80 ℃ at the speed of 0.5-1 ℃/min, and preserving heat for reaction for 1.5h;
(3) And after the reaction is finished, the reaction is restored to normal temperature, filtered, washed for 2 times, the pure water dosage is 120.9g each time, and then dried for 6 hours at the temperature of 95 ℃ and ground for once every 2 hours, thus obtaining 223.12g of magnesium aluminum hydrotalcite.
Example 3
The method for synthesizing the magnesium aluminum hydrotalcite comprises the following specific synthesis steps:
(1) Mixing 80.6g of magnesium oxide, 146.3g of magnesium bicarbonate, 78g of aluminum hydroxide and 120g of sodium hydroxide, adding 80.6g of 75wt% ethanol aqueous solution, wetting and grinding at a grinding speed of 400r/min for 25min;
(2) Continuously grinding at the rotating speed of 400r/min, gradually heating to 80 ℃ at the speed of 0.5-1 ℃/min, and preserving heat for reaction for 1.5h;
(3) And after the reaction is finished, the reaction is restored to normal temperature, filtered, washed for 2 times, and dried for 6 hours at the temperature of 95 ℃ with the pure water dosage of 161.2g each time, and ground for once every 2 hours to obtain 298.45g of magnesium aluminum hydrotalcite.
Example 4
The method for synthesizing the magnesium aluminum hydrotalcite comprises the following specific synthesis steps:
(1) Mixing 40.3g of magnesium oxide, 73.15g of magnesium bicarbonate, 39g of aluminum hydroxide and 40.3g of sodium hydroxide, adding 40.3g of 70wt% ethanol aqueous solution, wetting and grinding at a grinding speed of 400r/min for 25min;
(2) Continuously grinding at the rotating speed of 400r/min, gradually heating to 80 ℃ at the speed of 0.5-1 ℃/min, and preserving heat for reaction for 1.5h;
(3) And after the reaction is finished, the reaction is restored to normal temperature, filtered, washed for 2 times, the pure water dosage is 80.6g each time, and then dried for 6 hours at the temperature of 95 ℃ and ground for once every 2 hours, thus obtaining 146.83g of magnesium aluminum hydrotalcite.
Example 5
The method for synthesizing the magnesium aluminum hydrotalcite comprises the following specific synthesis steps:
(1) Mixing 40.3g of magnesium oxide, 73.15g of magnesium bicarbonate, 39g of aluminum hydroxide and 40.3g of sodium hydroxide, adding 40.3g of 80wt% ethanol aqueous solution, wetting and grinding at a grinding speed of 400r/min for 25min;
(2) Continuously grinding at the rotating speed of 400r/min, gradually heating to 80 ℃ at the speed of 0.5-1 ℃/min, and preserving heat for reaction for 1.5h;
(3) And after the reaction is finished, the reaction is restored to normal temperature, filtered, washed for 2 times, the pure water dosage is 80.6g each time, and then dried for 6 hours at the temperature of 95 ℃ and ground for once every 2 hours, thus obtaining 147.32g of magnesium aluminum hydrotalcite.
Example 6
The method for synthesizing the magnesium aluminum hydrotalcite comprises the following specific synthesis steps:
(1) Mixing 40.3g of magnesium oxide, 73.15g of magnesium bicarbonate, 39g of aluminum hydroxide and 40.3g of sodium hydroxide, adding 60.45g of 75wt% ethanol aqueous solution, wetting and grinding at a grinding speed of 500r/min for 20min;
(2) Continuously grinding at the rotating speed of 300r/min, gradually heating to 85 ℃ at the speed of 0.5-1 ℃/min, and preserving heat for reaction for 1h;
(3) And after the reaction is finished, the reaction is restored to normal temperature, filtered, washed for 2 times, the pure water dosage is 181g each time, and then dried for 8 hours at the temperature of 100 ℃ and ground for once every 3 hours, thus obtaining 146.68g of magnesium aluminum hydrotalcite.
Example 7
The method for synthesizing the magnesium aluminum hydrotalcite comprises the following specific synthesis steps:
(1) Mixing 40.3g of magnesium oxide, 73.15g of magnesium bicarbonate, 39g of aluminum hydroxide and 40.3g of sodium hydroxide, adding 80.6g of 75wt% ethanol aqueous solution, wetting and grinding at the grinding speed of 300r/min for 30min;
(2) Continuously grinding at the rotating speed of 300r/min, gradually heating to 85 ℃ at the speed of 0.5-1 ℃/min, and preserving heat for reaction for 1.2h;
(3) And after the reaction is finished, the reaction is restored to normal temperature, filtered, washed for 3 times, the pure water dosage is 200g each time, and then dried for 7 hours at the temperature of 90 ℃ and ground for once every 2 hours, thus obtaining 147.84g of magnesium aluminum hydrotalcite.
Example 8
The method for synthesizing the magnesium aluminum hydrotalcite comprises the following specific synthesis steps:
(1) Mixing 80.6g of magnesium oxide, 146.3g of magnesium bicarbonate, 78g of aluminum hydroxide and 120g of sodium hydroxide, adding 120.9g of 80wt% ethanol aqueous solution, wetting and grinding at a grinding speed of 400r/min for 25min;
(2) Continuously grinding at the rotating speed of 400r/min, gradually heating to 80 ℃ at the speed of 0.5-1 ℃/min, and preserving heat for reaction for 1.5h;
(3) And after the reaction is finished, the reaction is restored to normal temperature, filtered, washed for 3 times, the pure water dosage is 302.25g each time, and then dried for 8 hours at the temperature of 90 ℃ and ground for once every 3 hours, thus obtaining 297.78g of magnesium aluminum hydrotalcite.
Comparative example 1
The method for synthesizing the magnesium aluminum hydrotalcite comprises the following specific synthesis steps:
(1) Mixing 40.3g of magnesium oxide, 73.15g of magnesium bicarbonate, 39g of aluminum hydroxide and 40.3g of sodium hydroxide, adding 40.3g of 75wt% pure water, wetting and grinding at a grinding speed of 400r/min for 25min;
(2) Continuously grinding at the rotating speed of 400r/min, gradually heating to 80 ℃ at the speed of 0.5-1 ℃/min, and preserving heat for reaction for 1.5h;
(3) And after the reaction is finished, the reaction is restored to normal temperature, filtered, washed for 2 times, the pure water dosage is 80.6g each time, and then dried for 6 hours at the temperature of 95 ℃ and ground for once every 2 hours, thus obtaining 145.89g of magnesium aluminum hydrotalcite.
Unlike example 1, comparative example 1 was wet-ground using pure water.
Comparative example 2
A method for synthesizing magnesium-aluminum hydrotalcite,
the specific synthesis steps are as follows:
(1) Mixing 40.3g of magnesium oxide, 73.15g of magnesium bicarbonate, 39g of aluminum hydroxide and 40.3g of sodium hydroxide, adding 40.3g of 65wt% ethanol aqueous solution, wetting and grinding at a grinding speed of 400r/min for 25min;
(2) Continuously grinding at the rotating speed of 400r/min, gradually heating to 80 ℃ at the speed of 0.5-1 ℃/min, and preserving heat for reaction for 1.5h;
(3) And after the reaction is finished, the reaction is restored to normal temperature, filtered, washed for 2 times, the pure water dosage is 80.6g each time, and then dried for 6 hours at the temperature of 95 ℃ and ground for once every 2 hours, thus obtaining 146.55g of magnesium aluminum hydrotalcite.
Unlike example 1, comparative example 2 was wet-milled using a 65wt% aqueous ethanol solution.
Comparative example 3
The method for synthesizing the magnesium aluminum hydrotalcite comprises the following specific synthesis steps:
(1) Mixing 40.3g of magnesium oxide, 73.15g of magnesium bicarbonate, 39g of aluminum hydroxide and 40.3g of sodium hydroxide, adding 40.3g of 85wt% ethanol aqueous solution, wetting and grinding at a grinding speed of 400r/min for 25min;
(2) Continuously grinding at the rotating speed of 400r/min, gradually heating to 80 ℃ at the speed of 0.5-1 ℃/min, and preserving heat for reaction for 1.5h;
(3) And after the reaction is finished, the reaction is restored to normal temperature, filtered, washed for 2 times, the pure water dosage is 80.6g each time, and then dried for 6 hours at the temperature of 95 ℃ and ground for 2 hours, thus obtaining the magnesium aluminum hydrotalcite 147.39.
Unlike example 1, comparative example 3 was wet-milled using an 85wt% aqueous ethanol solution.
Comparative example 4
The method for synthesizing the magnesium aluminum hydrotalcite comprises the following specific synthesis steps:
(1) Mixing 40.3g of magnesium oxide, 73.15g of magnesium bicarbonate, 39g of aluminum hydroxide and 40.3g of sodium hydroxide, adding 40.3g of 75wt% ethanol aqueous solution, wetting and grinding at the grinding speed of 250r/min for 25min;
(2) Continuously grinding at the rotating speed of 400r/min, gradually heating to 80 ℃ at the speed of 0.5-1 ℃/min, and preserving heat for reaction for 1.5h;
(3) And after the reaction is finished, the reaction is restored to normal temperature, filtered, washed for 2 times, the pure water dosage is 80.6g each time, and then dried for 6 hours at the temperature of 95 ℃ and ground for once every 2 hours, thus obtaining 147.53g of magnesium aluminum hydrotalcite.
Unlike example 1, comparative example 4 had a polishing rate of 250r/min.
Comparative example 5
The method for synthesizing the magnesium aluminum hydrotalcite comprises the following specific synthesis steps:
(1) Mixing 40.3g of magnesium oxide, 73.15g of magnesium bicarbonate, 39g of aluminum hydroxide and 40.3g of sodium hydroxide, adding 40.3g of 75wt% ethanol aqueous solution, wetting and grinding at a grinding speed of 550r/min for 25min;
(2) Continuously grinding at the rotating speed of 400r/min, gradually heating to 80 ℃ at the speed of 0.5-1 ℃/min, and preserving heat for reaction for 1.5h;
(3) And after the reaction is finished, the reaction is restored to normal temperature, filtered, washed for 2 times, the pure water dosage is 80.6g each time, and then dried for 6 hours at the temperature of 95 ℃ and ground for once every 2 hours, thus obtaining 145.24g of magnesium aluminum hydrotalcite.
Unlike example 1, comparative example 5 had a polishing rate of 550r/min.
Comparative example 6
The method for synthesizing the magnesium aluminum hydrotalcite comprises the following specific synthesis steps:
(1) Mixing 40.3g of magnesium oxide, 73.15g of magnesium bicarbonate, 39g of aluminum hydroxide and 40.3g of sodium hydroxide, adding 40.3g of 75wt% ethanol aqueous solution, wetting and grinding at a grinding speed of 400r/min for 25min;
(2) Continuously grinding at the rotating speed of 400r/min, gradually heating to 80 ℃ at the speed of 2-5 ℃/min, and preserving heat for reaction for 1.5h;
(3) And after the reaction is finished, the reaction is restored to normal temperature, filtered, washed for 2 times, the pure water dosage is 80.6g each time, and then dried for 6 hours at the temperature of 95 ℃ and ground for once every 2 hours, thus obtaining 142.54g of magnesium aluminum hydrotalcite.
Unlike example 1, comparative example 6 had a heating rate of 2 to 5 ℃/min.
Comparative example 7
The method for synthesizing the magnesium aluminum hydrotalcite comprises the following specific synthesis steps:
(1) Mixing 40.3g of magnesium oxide, 73.15g of magnesium bicarbonate, 39g of aluminum hydroxide and 40.3g of sodium hydroxide, adding 40.3g of 75wt% ethanol aqueous solution, wetting and grinding at a grinding speed of 400r/min for 25min;
(2) Continuously grinding at the rotating speed of 400r/min, gradually heating to 80 ℃ at the speed of 0.5-1 ℃/min, and preserving heat for reaction for 1.5h;
(3) And after the reaction is finished, the reaction is restored to normal temperature, filtered, washed for 2 times, 80.6g of pure water is used each time, and then dried for 6 hours at the temperature of 95 ℃ to obtain 148.48g of magnesium aluminum hydrotalcite.
Unlike example 1, the drying process of comparative example 7 did not grind.
Comparative example 8
The method for synthesizing the magnesium aluminum hydrotalcite comprises the following specific synthesis steps:
(1) Mixing 40.3g of magnesium oxide, 29.26g of magnesium bicarbonate, 31.2g of aluminum hydroxide and 32g of sodium hydroxide, adding 40.3g of 75wt% ethanol aqueous solution, wetting and grinding at a grinding speed of 400r/min for 25min;
(2) Continuously grinding at the rotating speed of 400r/min, gradually heating to 85 ℃ at the speed of 0.5-1 ℃/min, and preserving heat for reaction for 1h;
(3) Then introducing carbon dioxide, and continuing to react for 2 hours;
(4) And after the reaction is finished, the reaction is restored to normal temperature, filtered, washed for 3 times, the pure water dosage is 200g each time, and then dried for 7 hours at the temperature of 90 ℃ and ground for once every 2 hours to obtain 111.35g of magnesium aluminum hydrotalcite.
Unlike example 1, the molar ratio of magnesium oxide, magnesium aluminum bicarbonate, sodium hydroxide of comparative example 8 was 5:1:2:4 without grinding during the drying process, and carbon dioxide was also required to provide the carbonate source.
Effect examples
The magnesium aluminum hydrotalcite prepared in examples 1 to 8 and comparative examples 1 to 8 was measured for particle size, particle dispersibility, crystallinity, purity, and the results are shown in table 1.
From the results of the above examples and comparative examples, it was found that the yield of the magnesium aluminum hydrotalcite obtained by the synthesis method of the present invention was high, the byproducts were few, and the maximized atomic economy was achieved; with reference to Table 1, the synthesized magnesium aluminum hydrotalcite has high crystallinity, particle size smaller than 0.2 micron, good particle size dispersibility, uniform and orderly particle size distribution, high purity and no impurity.
Finally, it should be noted that the above-mentioned embodiments are only for illustrating the technical solution of the present invention and not for limiting the technical solution of the present invention, and although the present invention has been described in detail with reference to the above-mentioned embodiments, it should be understood by those skilled in the art that the present invention may be modified or equivalently replaced without departing from the spirit and scope of the present invention, and any modification or partial replacement thereof should be included in the scope of the claims of the present invention.
Claims (9)
1. The method for synthesizing the magnesium aluminum hydrotalcite is characterized by comprising the following steps of:
(1) Mixing magnesium oxide, magnesium bicarbonate, aluminum hydroxide and sodium hydroxide, adding ethanol aqueous solution for wet grinding, and grinding for 20-30 min;
(2) Continuously grinding, gradually heating to 75-85 ℃, and reacting for 1-1.5 h at a temperature;
(3) And (3) after the reaction is finished, recovering to normal temperature, filtering, washing with water and drying to obtain the magnesium aluminum hydrotalcite.
2. The method according to claim 1, wherein in the step (1), the magnesium oxide, the magnesium bicarbonate, the aluminum hydroxide and the sodium hydroxide are mixed according to a molar ratio of 2:1:1:3.
3. The method for synthesizing magnesium aluminum hydrotalcite according to claim 1, wherein the mass fraction of the aqueous ethanol solution is 70 to 80%.
4. The method for synthesizing magnesium aluminum hydrotalcite according to claim 1, wherein in the step (1), the amount of the aqueous ethanol solution added is 1 to 2 times the weight of magnesium oxide.
5. The method according to claim 1, wherein in the steps (1) and (2), the grinding speed is 300-500 r/min.
6. The method for synthesizing magnesium aluminum hydrotalcite according to claim 1, wherein in the step (2), the gradual temperature rise rate is 0.5 to 1 ℃/min.
7. The method for synthesizing magnesium aluminum hydrotalcite according to claim 1, wherein in the step (3), the washing is performed 2 to 3 times; the consumption of pure water is 2-3 times of that of ethanol water solution each time.
8. The method for synthesizing magnesium aluminum hydrotalcite according to claim 1, wherein in the step (3), the drying temperature is 90 to 100 ℃ for 6 to 8 hours.
9. The method for synthesizing magnesium aluminum hydrotalcite according to claim 1 or 8, wherein in the step (3), the product is ground every 2 to 3 hours during the drying process.
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