CN109354049B - Synthesis method of intercalated hydrotalcite stabilizer - Google Patents
Synthesis method of intercalated hydrotalcite stabilizer Download PDFInfo
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- CN109354049B CN109354049B CN201811575818.0A CN201811575818A CN109354049B CN 109354049 B CN109354049 B CN 109354049B CN 201811575818 A CN201811575818 A CN 201811575818A CN 109354049 B CN109354049 B CN 109354049B
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- 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
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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Abstract
The invention discloses a method for synthesizing an intercalated hydrotalcite stabilizer, which comprises the steps of preparing a solid magnesium source and an aluminum source into a suspension according to a proportion, adding a proper amount of water to prepare a reaction solution, and placing the reaction solution into a reaction kettle for reaction; then introducing a proper amount of carbon dioxide to continue reacting, cooling and decompressing after reacting for a certain time, adding a proper amount of stearic acid or stearate to obtain a solid crude product, and filtering and drying the solid crude product to obtain a product intercalated hydrotalcite stabilizer; the synthesis process is simple, the reaction temperature of the magnesium source and the aluminum source in the reaction kettle is low, the pH value of the solution is changed slightly in the reaction process, magnesium and aluminum are stable, the obtained solid crude product is washed and filtered, and the filtered filtrate can be circularly used for being added into the suspension for reaction, so that the wastewater amount is greatly reduced.
Description
Technical Field
The invention belongs to the field of hydrotalcite preparation, and particularly relates to a synthesis method of an intercalated hydrotalcite stabilizer.
Background
Hydrotalcite is Layered Double Hydroxides (LDHs, molecular formula is [ MM (OH) ] A. mHO), belongs to anion Layered materials, and is typically represented by magnesium aluminum carbonate type hydrotalcite, wherein magnesium aluminum hydroxide forms Layered plates, and carbonate ions are anions between the Layered plates. Due to the variety and quantity of interlayer anions and the adjustability of the laminate, the hydrotalcite is endowed with many characteristics, such as ion exchangeability, catalytic performance, thermal stability, alkalescence and the like, and is widely applied to the fields of materials, catalysis, medicines and the like at present.
In the related technology, hydrotalcite is prepared by a hydrothermal method, and magnesium oxide/magnesium hydroxide, aluminum oxide/aluminum hydroxide and sodium carbonate are used as raw materials and are prepared at 140 ℃. The preparation process is simple, but as the reaction proceeds, the pH of the reaction solution tends to rise, so that an aluminum source substance is dissolved in a strong alkaline solution, and the fluctuation of the ratio of magnesium to aluminum is large; and a large amount of alkaline wastewater is generated, so that the cost of the later-stage water treatment is high.
Disclosure of Invention
In view of this, the embodiment of the present invention provides a method for preparing an intercalated hydrotalcite stabilizer, which has a simple preparation process, easily controlled pH of a reaction solution, and a very small amount of wastewater generated by the reaction.
In order to solve the technical problems, the embodiment of the invention adopts the technical scheme that the synthesis method of the intercalated hydrotalcite stabilizer comprises the following steps:
(1) preparing a solid magnesium source and an aluminum source into a suspension according to a proportion, adding a proper amount of water to prepare a reaction solution, and placing the reaction solution into a reaction kettle for reaction;
(2) closing the reaction kettle after the reaction is finished, introducing a proper amount of carbon dioxide into the reaction kettle, then opening the reaction kettle for reaction, cooling and decompressing after the reaction is carried out for a certain time, and adding a proper amount of stearic acid or stearate;
(3) obtaining a solid crude product after the reaction is finished, washing, filtering and drying the solid crude product to obtain a product intercalated hydrotalcite stabilizer;
(4) the filtered filtrate was repeatedly used for preparing the reaction solution in the step (1).
Preferably, in the step (1), the reaction conditions of the reaction kettle are as follows: stirring at the rotating speed of 150-200 rpm, heating to 90-100 ℃ at normal pressure, and keeping the temperature for 10-20 minutes; the ratio of the magnesium source to the aluminum source in the reaction liquid is 2: 1; the amount of water added is 3-4 times of the weight of the suspension.
Preferably, in the step (1), the solid magnesium source is a mixture of magnesium hydroxide and magnesium oxide, and the aluminum source is aluminum hydroxide; respectively preparing the magnesium hydroxide, the magnesium oxide and the aluminum hydroxide into 20% suspension, and shearing the suspension by using a nano-emulsion pump until the particle size D50 of solid particles in the suspension is less than 300 nanometers.
Preferably, in the step (1), the molar ratio of magnesium oxide, magnesium hydroxide and aluminum hydroxide in the suspension is 1-2: 3-2: 2.
preferably, in the step (2), the amount of the introduced carbon dioxide is 50 to 70 percent of the molar weight of the aluminum hydroxide; after carbon dioxide is introduced, the temperature of the reaction kettle is increased to 150-200 ℃ for reaction for 5-10 hours, the temperature is decreased to 90 ℃, the pressure is released, the stearic acid or stearate is added, and the reaction is carried out for 1-2 hours, wherein the amount of the stearic acid or stearate is 4-10 times of the molar amount of the aluminum hydroxide.
Preferably, in the step (3), the drying temperature is 120 ℃.
Compared with the related art, the technical scheme provided by the embodiment of the invention has the following beneficial effects: the synthesis method of the intercalated hydrotalcite stabilizer provided by the embodiment of the invention has the advantages that the synthesis process is simple, the reaction temperature of the magnesium source and the aluminum source in the reaction kettle is low, the pH value of the solution is slightly changed in the reaction process, the magnesium and the aluminum are relatively stable, the obtained solid crude product is washed and filtered, and the filtered filtrate can be circularly used for being added into the suspension for reaction, so that the wastewater amount is greatly reduced.
Drawings
FIG. 1 is a flow chart of a synthetic method of an intercalated hydrotalcite stabilizer according to an embodiment of the present invention;
FIG. 2 is an XRD pattern of an intercalated hydrotalcite stabilizer according to an embodiment of the present invention;
FIG. 3 is a comparative graph of the stability test of the intercalated hydrotalcite prepared by the embodiment of the present invention applied to the resin.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, embodiments of the present invention will be further described with reference to the accompanying drawings.
Example one
Referring to fig. 1, an embodiment of the present invention provides a method for synthesizing an intercalated hydrotalcite stabilizer, including the following steps:
(1) preparing a solid magnesium source and an aluminum source into a suspension according to a proportion, adding a proper amount of water to prepare a reaction solution, and placing the reaction solution into a reaction kettle for reaction; wherein the reaction conditions of the reaction kettle are as follows: stirring at the rotating speed of 150-200 rpm, heating to 90-100 ℃ at normal pressure, and keeping the temperature for 10-20 minutes; the ratio of the magnesium source to the aluminum source in the reaction liquid is 2: 1; adding water in an amount which is 3-4 times the weight of the suspension; the solid magnesium source is a mixture of magnesium hydroxide and magnesium oxide, and the aluminum source is aluminum hydroxide; respectively preparing the magnesium hydroxide, the magnesium oxide and the aluminum hydroxide into 20% solution, and shearing the solution by using a nano emulsification pump until the particle size D50 of solid particles of the suspension is less than 300 nanometers; the mol ratio of magnesium oxide to magnesium hydroxide to aluminum hydroxide in the suspension is 1-2: 3-2: 2; in the embodiment of the invention, the magnesium source and the aluminum source suspension are adopted, the magnesium source and the aluminum source are uniformly mixed during reaction, and the particle size of particles in the suspension is small, so that the reaction rate can be increased, and the reaction time can be shortened; magnesium hydroxide, magnesium oxide and aluminum hydroxide are used as raw materials, sodium hydroxide or ammonia water and the like are not needed, and the generation of byproducts due to large alkali consumption in the reaction process is avoided;
(2) closing the reaction kettle after the reaction is finished, introducing a proper amount of carbon dioxide into the reaction kettle, then opening the reaction kettle for reaction, cooling and decompressing after the reaction is carried out for a certain time, and adding a proper amount of stearic acid or stearate; according to the embodiment of the invention, carbon dioxide is added after the magnesium source and the aluminum source are reacted, the magnesium source and the aluminum source are reacted to form a mixed colloidal compound, and the mixed colloidal compound is reacted after the carbon dioxide is added, so that no by-product is generated in the reaction process, and the reaction rate can be increased;
wherein, the amount of the introduced carbon dioxide is 50 to 70 percent of the molar weight of the aluminum hydroxide; after carbon dioxide is introduced, heating the temperature of the reaction kettle to 150-200 ℃ for reaction for 5-10 hours, cooling to 90 ℃, decompressing, adding stearic acid or stearate for reaction for 1-2 hours, wherein the amount of the stearic acid or stearate is 4-10 times of the molar amount of aluminum hydroxide; stearic acid or stearate not only plays a role of intercalation anion in the reaction, but also plays a role of heat stabilizer, and other stabilizers are not required to be added in the reaction, thereby reducing the reaction cost.
(3) Obtaining a solid crude product after the reaction is finished, washing, filtering and drying the solid crude product to obtain a product intercalated hydrotalcite stabilizer; the drying temperature is 120 ℃;
(4) the filtered filtrate was repeatedly used for preparing the reaction solution in the step (1). The filtered filtrate only contains a magnesium source and an aluminum source, and can be recycled for reaction, thereby greatly reducing the discharge of waste water and improving the environmental protection.
The coprecipitation method is easy to react, but the generated product is colloidal, washing and filtering are difficult, a large amount of sodium hydroxide is consumed in the reaction process, and more byproducts are generated; the hydrothermal method has the advantages that the pH value changes along with the reaction, and the reaction process is unstable and difficult to control; the embodiment of the invention has the advantages of stable reaction, small alkali consumption, stable and easily separated product, little waste water discharge, reaction cost reduction and good environmental protection effect.
Example two
According to the method of the first embodiment of the invention, 200g of magnesium oxide (with the content of 99.7%) is added into 800ml of water and sheared for 1 hour by a nano emulsifying pump, and the test particle size D50 is 250nm for standby; adding 300g of magnesium hydroxide (with the content of 99.8%) into 1200ml of water, shearing for 1 hour by using a nano emulsification pump, and testing the particle size D50 to be 260nm for later use; 300g of aluminium hydroxide (content 99.7%) is added to 1200ml of water and sheared by a nanoemulsification pump for 1.5 hours, the test particle size D50 is 240nm for use.
Preparing reaction liquid from 100g of prepared magnesium oxide suspension, 337g of magnesium hydroxide suspension, 323g of aluminum hydroxide suspension and 2720L of water, reacting in a high-pressure reaction kettle, starting stirring at a rotating speed of 170rpm, heating to 90-100 ℃, keeping the temperature at normal pressure for 20 minutes, sealing the reaction kettle, adding 22g of carbon dioxide, heating to 170-180 ℃, keeping the temperature for 8 hours, cooling to 90 ℃, decompressing, adding 10.5g of stearic acid, reacting at 80-90 ℃ for 2 hours, stopping reaction and filtering; drying the filtered solid crude product for 12 hours at 120 ℃ to obtain 392g of white intercalated hydrotalcite solid; the filtered filtrate can be repeatedly applied to the preparation of reaction liquid. The rest is the same as the first embodiment.
EXAMPLE III
Taking 124.5g of the magnesium oxide suspension prepared in the second embodiment, 301g of the magnesium hydroxide suspension, 323g of the aluminum hydroxide suspension and 2650L of water to prepare a reaction solution, reacting in a high-pressure reaction kettle, starting stirring at a rotating speed of 200rpm, heating to 90-100 ℃, keeping the temperature for 20 minutes under normal pressure, sealing the reaction kettle, adding 20g of carbon dioxide, heating to 150-160 ℃, keeping the temperature for 10 hours, cooling to 90 ℃, decompressing, adding 12g of stearic acid, reacting at 80-90 ℃ for 2 hours, stopping reaction and filtering, and drying a filtered solid crude product at 120 ℃ for 12 hours to obtain 389g of white intercalated hydrotalcite solid; the filtered filtrate was repeatedly used for preparing the reaction solution. The rest is the same as the first embodiment.
Example four
Preparing 166g of the magnesium oxide suspension, 241g of the magnesium hydroxide suspension, 323g of the aluminum hydroxide suspension and 2700L of water prepared in the second embodiment into a reaction solution, reacting in a high-pressure reaction kettle, starting stirring at a speed of 200rpm, heating to 90-100 ℃, keeping the temperature for 20 minutes at normal pressure, sealing the reaction kettle, adding 20g of carbon dioxide, heating to 180-195 ℃, keeping the temperature for 6 hours, cooling to 90 ℃, decompressing, adding 12g of stearic acid, reacting for 2 hours at 80-90 ℃, stopping reaction and filtering, filtering to obtain a solid crude product, and drying at 120 ℃ for 12 hours to obtain 394g of white intercalated hydrotalcite solid; the filtered filtrate was repeatedly used for preparing the reaction solution. The rest is the same as the first embodiment.
EXAMPLE five
Preparing 100g of magnesium oxide suspension prepared in the second embodiment, 337g of magnesium hydroxide suspension, 323g of aluminum hydroxide suspension and 2720L of filtrate in the second embodiment into a reaction solution, reacting in a high-pressure reaction kettle, starting stirring at a rotating speed of 170rpm, heating to 90-100 ℃, keeping the temperature for 20 minutes under normal pressure, sealing the reaction kettle, adding 22g of carbon dioxide, heating to 170-180 ℃, keeping the temperature for 8 hours, cooling to 90 ℃, decompressing, adding 10.5g of stearic acid, reacting at 80-90 ℃ for 2 hours, stopping reaction and filtering, filtering to obtain a solid crude product, and drying at 120 ℃ for 12 hours to obtain 391.5g of white intercalated hydrotalcite solid; the filtrate was used to prepare the reaction solution repeatedly. The rest is the same as the first embodiment.
EXAMPLE six
Preparing a reaction solution from 100g of the magnesium oxide suspension prepared in the second embodiment, 337g of the magnesium hydroxide suspension, 323g of the aluminum hydroxide suspension and 2720L of the filtrate prepared in the fifth embodiment into a high-pressure reaction kettle, reacting at a stirring rotation speed of 170rpm, heating to 90-100 ℃, keeping the temperature for 20 minutes at normal pressure, sealing the reaction kettle, adding 22g of carbon dioxide, heating to 170-180 ℃, keeping the temperature for 8 hours, cooling to 90 ℃, decompressing, adding 10.5g of stearic acid, reacting at 80-90 ℃ for 2 hours, stopping reaction, filtering, and drying a filtered solid crude product at 120 ℃ for 12 hours to obtain 391.5g of white intercalated hydrotalcite solid; the filtrate was repeatedly used for preparing the reaction solution. The rest is the same as the first embodiment.
Referring to fig. 2, the intercalated hydrotalcite prepared in the embodiment of the present invention and the intercalated hydrotalcite obtained from the reaction solution prepared by repeating the filtrate have distinct characteristic peaks 003, 006, 009, and 110, and have a layered structure, and the intercalation reaction is complete.
EXAMPLE seven
The intercalated hydrotalcite prepared in the second, third, fourth and sixth embodiments of the invention is applied to resin for stability detection in comparison with the commercial resin, wherein the resin formula is shown in table 1, the detection conditions are that the double rollers are 185 ℃, the thickness is 0.5mm, the rotating speed is 17/15rpm, the sheet is pulled for 4 minutes, and the oven temperature is 195 ℃ for test.
TABLE 1 formulation of hydrotalcite prepared in example of the present invention applied to resin
Referring to fig. 3, the stability of the intercalated hydrotalcite prepared in the second, third, fourth and sixth embodiments of the present invention applied to resin is good, and the initial whiteness and the whiteness retention time are better than those of the commercially available resin; the intercalated hydrotalcite prepared by recycling the filtrate has good stability.
In this document, the terms front, back, upper and lower are used to define the components in the drawings and the positions of the components relative to each other, and are used for clarity and convenience of the technical solution. It is to be understood that the use of the directional terms should not be taken to limit the scope of the claims.
The features of the embodiments and embodiments described herein above may be combined with each other without conflict.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (8)
1. A synthetic method of an intercalated hydrotalcite stabilizer is characterized by comprising the following steps:
(1) preparing a solid magnesium source and an aluminum source into a suspension according to a proportion, adding a proper amount of water to prepare a reaction solution, and placing the reaction solution into a reaction kettle for reaction; wherein the reaction conditions of the reaction kettle are as follows: stirring at the rotating speed of 150-200 rpm, heating to 90-100 ℃ at normal pressure, and keeping the temperature for 10-20 minutes; the ratio of the magnesium source to the aluminum source in the reaction liquid is 2: 1; adding water in an amount which is 3-4 times the weight of the suspension;
(2) closing the reaction kettle after the reaction, introducing a proper amount of carbon dioxide into the reaction kettle, then opening the reaction kettle for reaction, cooling and decompressing after the reaction for a certain time, and adding a proper amount of stearic acid or stearate; the amount of the introduced carbon dioxide is 50 to 70 percent of the molar weight of the aluminum hydroxide; after carbon dioxide is introduced, heating the temperature of the reaction kettle to 150-200 ℃ for reaction for 6-10 hours, cooling to 90 ℃, decompressing, adding stearic acid or stearate for reaction for 1-2 hours, wherein the amount of the stearic acid or stearate is 4-10 times of the molar amount of aluminum hydroxide;
(3) after the reaction is finished, obtaining a solid crude product, and filtering and drying the solid crude product to obtain a product intercalated hydrotalcite stabilizer;
(4) the filtered filtrate was repeatedly used for preparing the reaction solution in the step (1).
2. The method for synthesizing intercalated hydrotalcite stabilizer according to claim 1, wherein in step (1), the solid magnesium source is a mixture of magnesium hydroxide and magnesium oxide, and the aluminum source is aluminum hydroxide; respectively preparing the magnesium hydroxide, the magnesium oxide and the aluminum hydroxide into 20% suspension, and shearing solid particles in the suspension to a particle size D50 of less than 300 nanometers by using a nano-emulsion pump.
3. The method for synthesizing the intercalated hydrotalcite stabilizer according to claim 2, wherein in the step (1), the molar ratio of magnesium oxide, magnesium hydroxide and aluminum hydroxide in the suspension is 1-2: 3-2: 2.
4. the method for synthesizing the intercalated hydrotalcite stabilizer according to claim 1, wherein in the step (2), the temperature of the reaction kettle is raised to 170-180 ℃ after carbon dioxide is introduced, and the reaction is carried out for 8 hours.
5. The method for synthesizing the intercalated hydrotalcite stabilizer according to claim 1, wherein in the step (2), the temperature of the reaction kettle is raised to 150-160 ℃ after carbon dioxide is introduced, and the reaction is carried out for 10 hours.
6. The method for synthesizing the intercalated hydrotalcite stabilizer according to claim 1, wherein in the step (2), the temperature of the reaction kettle is increased to 180-195 ℃ after carbon dioxide is introduced, and the reaction is carried out for 6 hours.
7. The method for synthesizing intercalated hydrotalcite stabilizer according to claim 1, wherein in the step (3), the drying temperature is 120 ℃.
8. The method for synthesizing the intercalated hydrotalcite stabilizer according to any one of claims 1 to 7, wherein the synthesized intercalated hydrotalcite stabilizer can be applied to resin.
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| CN110498471B (en) * | 2019-08-28 | 2022-01-04 | 日照市新正泓环保科技有限公司 | Sewage treatment agent and preparation method thereof |
| CN111453750B (en) * | 2020-05-29 | 2021-09-03 | 山东长泽新材料科技有限公司 | Clean synthesis process of magnesium aluminum hydrotalcite |
| CN113620326A (en) * | 2021-08-20 | 2021-11-09 | 云南创能斐源金属燃料电池有限公司 | Method for preparing magnesium-aluminum-zinc hydrotalcite from aluminum-air battery electrolysis waste liquid and application thereof |
| CN114904457A (en) * | 2022-03-28 | 2022-08-16 | 自然资源部天津海水淡化与综合利用研究所 | Continuous production equipment and process for carbonate type layered magnesium aluminum hydroxide neutralized by mother liquor carbon |
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