CN113716588A - Low-cost preparation method of magnesium-aluminum hydrotalcite - Google Patents
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- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D5/00—Sulfates or sulfites of sodium, potassium or alkali metals in general
- C01D5/14—Preparation of sulfites
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Abstract
A low-cost preparation method of magnesium-aluminum hydrotalcite relates to the technical field of magnesium-aluminum hydrotalcite preparation, and comprises the steps of taking light-burned magnesia powder as a raw material, adding the light-burned magnesia powder into a reaction kettle, mixing the light-burned magnesia powder with a proper amount of water, and introducing sulfur dioxide gas to form a soluble magnesium bisulfite solution; simultaneously, adding aluminum hydroxide into a sodium hydroxide solution, heating and dissolving, and adding sodium carbonate to prepare sodium metaaluminate and sodium carbonate solution; then adding sodium metaaluminate and sodium carbonate solution into the prepared magnesium bisulfite solution, heating and stirring to obtain reaction slurry, namely magnesium aluminum hydrotalcite precipitate and sodium sulfite solution; then filtering and washing the obtained reaction slurry to obtain a magnesium-aluminum hydrotalcite filter cake, a sodium sulfite filtrate and a washing liquid; finally, drying the magnalium hydrotalcite filter cake to obtain a magnalium hydrotalcite product; and simultaneously, sodium sulfite filtrate can be concentrated to co-produce sodium sulfite products.
Description
Technical Field
The invention relates to the technical field of preparation of magnesium-aluminum hydrotalcite, in particular to a low-cost preparation method of magnesium-aluminum hydrotalcite.
Background
The magnesium-aluminum hydrotalcite, namely Mg/Al-LDHs, is a functional material, can be applied to the field of preparation of flame retardant materials as a flame retardant, and can be applied to the industry of plastic heat stabilizers as an acid acceptor. When the molar ratio of magnesium to aluminum is 2, the molecular formula of the magnesium-aluminum hydrotalcite can be expressed as 4Mg2Al (OH)12 CO3.4H2O.
The magnesium-aluminum hydrotalcite is prepared from the following raw materials of magnesium chloride or magnesium sulfate, aluminum chloride, sodium hydroxide and sodium carbonate:
4MgCl2+2AlCl3+ Na2CO3+12NaOH +4H2O =4Mg2Al (OH)12CO 3.4h2o +14NaCl formula (1)
As can be seen from formula (1), the preparation process consumes a large amount of sodium hydroxide solution, which results in high production cost, and a large amount of brine solution, i.e., sodium chloride wastewater, is formed, and the sodium chloride wastewater is difficult to be recycled in actual production, so that industrial production is difficult to realize.
In order to reduce the production cost and the discharge amount of waste liquid, some existing manufacturers directly adopt high-purity aluminum hydroxide and high-purity magnesium hydroxide or magnesium oxide and sodium carbonate as raw materials to prepare a magnesium-aluminum hydrotalcite product, and the process principle is as follows:
4Mg (OH)2+2al (OH)3+ Na2CO3+4H2O =4Mg2Al (OH)12CO 3.4h2o +2NaOH formula (2)
As can be seen from the formula (2), in the production process, a low-concentration sodium hydroxide solution is generated, and the formed wastewater still needs to be treated, so that high-purity magnesium oxide or high-purity magnesium hydroxide is prepared by taking a soluble magnesium salt as a raw material and adding alkali by a company specially producing magnesium oxide or magnesium hydroxide, the preparation cost is high, and the sale price is also high. Therefore, the problem of higher preparation cost at the early stage still exists when magnesium-aluminum hydrotalcite is prepared by adopting high-purity magnesium oxide or magnesium hydroxide.
Sodium sulfite is a basic chemical raw material, and for manufacturers producing sulfuric acid, sodium carbonate or sodium hydroxide is usually adopted to absorb purified sulfur dioxide gas, so that a sodium sulfite product is formed, the production cost of the sodium sulfite is mainly the cost of the raw material of the sodium carbonate or sodium hydroxide, and the preparation process of the magnesium-aluminum hydrotalcite just needs the sodium carbonate and the sodium hydroxide, so that if the sodium carbonate and the sodium hydroxide are used as the raw materials, the co-production of the magnesium-aluminum hydrotalcite and the sodium sulfite is realized, and the problems of high production cost and wastewater treatment need to be effectively solved.
Disclosure of Invention
The invention aims to provide a low-cost preparation method of magnesium-aluminum hydrotalcite, which can reduce the production cost through the form phase change of the co-production with sodium sulfite products and reduce the generation of waste water.
In order to solve the technical problems, the invention adopts the following technical scheme: a low-cost preparation method of magnesium-aluminum hydrotalcite comprises the following steps:
step one, adding light-burned magnesia powder serving as a raw material into a reaction kettle, mixing the light-burned magnesia powder with a proper amount of water, introducing sulfur dioxide gas to form a soluble magnesium bisulfite solution, and filtering out insoluble impurities. The main component of the light-burned magnesia powder is magnesia, the other impurities comprise alumina, ferric oxide and silicon dioxide, sulfur dioxide gas introduced into the reaction kettle does not react with the components in the impurities, but only reacts with the magnesia to generate magnesium bisulfite, and therefore, the main reaction principle in the step is as follows:
MgO +2SO2+ H2O = Mg (HSO3)2 formula (3)
In order to prepare the magnesium bisulfite solution, light-burned magnesia powder is taken as a raw material and mixed with a proper amount of water in a reaction kettle to obtain magnesia slurry with the concentration controlled within the range of 2-6 percent.
And secondly, adding aluminum hydroxide into the sodium hydroxide solution, heating and dissolving, and adding sodium carbonate to prepare sodium metaaluminate and sodium carbonate solution.
Step three, adding the sodium metaaluminate and sodium carbonate solution prepared in the step two into the magnesium bisulfite solution prepared in the step one, heating and stirring the mixture to obtain reaction slurry, namely magnesium aluminum hydrotalcite precipitate and sodium sulfite solution, wherein the reaction principle in the step is as follows:
4Mg (HSO3)2+2naal (OH)4+12NaOH + Na2CO3=4Mg2Al (OH)12 co3.4h2o ↓ +8Na2SO3+4H 2O; formula (4)
And step four, filtering and washing the reaction slurry obtained in the step three to obtain a magnesium-aluminum hydrotalcite filter cake, a sodium sulfite filtrate and a washing liquid.
Step five, drying the magnalium hydrotalcite filter cake to obtain a magnalium hydrotalcite product; the sodium sulfite filtrate is concentrated to obtain a sodium sulfite product.
And step six, sending the washing liquid obtained in the step four into the reaction kettle in the step one to repeatedly prepare the magnesium bisulfite solution.
Preferably, the content of magnesium oxide in the light-burned magnesia powder is 90%.
Preferably, the reaction temperature in the reaction kettle in the step one is 25-65 ℃, and the reaction time is 6-12 hours.
More preferably, the mass concentration of the magnesium bisulfite solution prepared in the step one is 6-16%.
More preferably, the mass concentration of the sodium hydroxide solution in the second step is 20-32%.
More preferably, the reaction temperature in step three is 85-105 ℃ and the reaction time is 8-16 hours.
More preferably, the whiteness of the aluminum hydroxide is more than or equal to 90 percent, the effective content is more than or equal to 99 percent, and the granularity is more than 200 meshes; the volume content of sulfur dioxide in the sulfur dioxide gas is more than 8 percent.
The principle of the invention is as follows: the main component of the light-burned magnesia powder raw material, namely magnesia, is mixed with sulfur dioxide gas in a reaction kettle to prepare high-purity magnesium hydrogen sulfite solution, and then the high-purity magnesium hydrogen sulfite solution reacts with sodium metaaluminate, sodium carbonate solution and sodium hydroxide to obtain a magnesium-aluminum hydrotalcite product and co-produce sodium sulfite.
Compared with the prior art, the invention has the beneficial effects that:
1. the light-burned magnesia powder is used as a raw material, the magnesia which is the main component in the light-burned magnesia powder can be dissolved and reacted with sulfur dioxide, and other impurities do not react, so that the raw material of high-purity magnesium hydroxide or magnesia does not need to be selected intentionally, and the use cost is low.
2. The method adopts sulfur dioxide gas as one of the raw materials, has great application value for sulfur plants, can utilize the discharged and collected sulfur dioxide gas to the maximum extent for production and preparation, and can coproduce sodium sulfite while preparing the magnesium-aluminum hydrotalcite product, so compared with the traditional method for preparing the magnesium-aluminum hydrotalcite, the method provided by the invention is more suitable for the chemical plants, and the generated actual benefit is more obvious.
3. The existing process method needs to consume a large amount of sodium carbonate or sodium hydroxide raw materials to obtain a single product of the magnesium-aluminum hydrotalcite, but the process method provided by the invention not only can prepare the magnesium-aluminum hydrotalcite after consuming the sodium hydroxide raw materials, but also can coproduce and prepare sodium sulfite, so that the application of the sodium hydroxide raw materials can generate a value beyond expectation, and from the perspective of preparing the magnesium-aluminum hydrotalcite, the extra sodium hydroxide raw materials are not needed to be consumed any more, and the production cost is reduced in a phase-changing manner.
4. The method provided by the invention can also send the washing liquid obtained by washing the magnesium-aluminum hydrotalcite sediment and the sodium sulfite solution back to the initial step for preparing the magnesium bisulfite solution repeatedly, thereby achieving the process effect of resource recycling and basically no waste liquid formation, which has great significance for industrial production and good market prospect.
Detailed Description
The present invention will be further described with reference to the following examples for facilitating understanding of those skilled in the art, and the description of the embodiments is not intended to limit the present invention.
Example 1
Adding 20m3 of industrial water into a stirring reaction kettle of 30m3, adding 1 ton of light-burned magnesia powder (the magnesia content is 90 percent), stirring, introducing high-concentration sulfur dioxide, reacting for 10 hours at 45 ℃, converting the magnesia into a soluble magnesium bisulfite solution, filtering, and removing impurities to obtain the refined magnesium bisulfite solution.
Wherein the molar ratio of the magnesium oxide to the sulfur dioxide is 1.4.
8.44 tons of 32 percent sodium hydroxide solution and 0.8775 tons of aluminum hydroxide are added into a dissolving tank with the thickness of 15 m3, and after the mixture is heated to 95 ℃ to be dissolved, 0.6 ton of sodium carbonate is added and stirred until the sodium metaaluminate and the sodium carbonate solution are dissolved, thus obtaining the sodium metaaluminate and sodium carbonate solution.
Adding a 20m3 magnesium bisulfite solution into a 50 m3 reaction tank, adding sodium metaaluminate, sodium carbonate and sodium hydroxide solution, stirring, heating to 95 ℃, reacting for 10 hours to obtain reaction slurry of magnesium aluminum hydrotalcite precipitate and sodium sulfite solution, pumping the reaction slurry into a filter press for filter pressing and washing to obtain a magnesium aluminum hydrotalcite filter cake, sodium sulfite filtrate and washing liquid, wherein the magnesium aluminum hydrotalcite filter cake is a filter cake with solid content of 48%.
It should be noted that, as will be understood by those skilled in the art, the solid content represents the mass percentage of the remainder of the slurry of magnesium aluminum hydrotalcite after filter pressing and washing.
Further, drying and crushing the filter cake to obtain a magnesium-aluminum hydrotalcite product, removing MVR from the sodium sulfite filtrate, concentrating and crystallizing to obtain a sodium sulfite product, and feeding the washing solution into a reaction kettle for batching to repeatedly prepare a magnesium bisulfite solution.
The proper amount of the magnalium hydrotalcite product is taken as a sample, the sample is respectively characterized and analyzed by means of X-ray diffraction (XDR), plasma emission spectrum (ICP), Transmission Electron Microscope (TEM), laser particle size analysis and the like, the particle size of the sample is measured to be between 20 and 92nm, the purity is 94.6 percent, and the magnalium hydrotalcite product has higher crystallinity and meets the performance index of the magnalium hydrotalcite product prepared by the existing industrial-grade preparation method.
Example 2
This example differs from example 1 only in that the reaction conditions of the light-burned magnesia powder and the high concentration of sulfur dioxide were at 25 ℃ for 6 hours; the molar ratio of the magnesium oxide to the sulfur dioxide is 1.6; heating to 85 ℃ in the process of preparing sodium metaaluminate and sodium carbonate solution; the magnesium bisulfite solution, the sodium aluminate, the sodium carbonate and the sodium hydroxide solution are mixed and stirred to react under the condition that the temperature is raised to 85 ℃ and the reaction lasts 8 hours.
Taking a proper amount of the magnesium-aluminum hydrotalcite product obtained in the preparation process as a sample, adopting the same detection means and analysis as in example 1 to determine that the particle size of the sample is between 20 and 94nm and the purity is 94.3 percent, thus proving that the product has higher crystallinity and meets the performance index of the magnesium-aluminum hydrotalcite product prepared by the existing industrial preparation method.
Example 3
This example differs from example 1 only in that the reaction conditions of the light-burned magnesia powder and the high concentration of sulfur dioxide were 65 ℃ for 12 hours; the molar ratio of the magnesium oxide to the sulfur dioxide is 1.8; heating to 105 ℃ in the process of preparing sodium metaaluminate and sodium carbonate solution; the magnesium bisulfite solution, the sodium aluminate, the sodium carbonate and the sodium hydroxide solution are mixed and stirred to react under the condition that the temperature is raised to 105 ℃ and the reaction lasts for 16 hours.
Taking a proper amount of the magnalium hydrotalcite product obtained in the preparation process as a sample, adopting the same detection means and analysis as in example 1 to detect that the particle size of the sample is between 20 and 97nm and the purity is 94.2 percent, thus proving that the product has higher crystallinity and meets the performance index of the magnalium hydrotalcite product prepared by the existing industrial preparation method.
Example 4
This example differs from example 1 only in that the reaction conditions of the light-burned magnesia powder and the high concentration of sulfur dioxide were 50 ℃ for 8 hours; the molar ratio of the magnesium oxide to the sulfur dioxide is 1.2; heating to 100 ℃ in the process of preparing sodium metaaluminate and sodium carbonate solution; the magnesium bisulfite solution, the sodium aluminate, the sodium carbonate and the sodium hydroxide solution are mixed and stirred to react under the condition that the temperature is raised to 100 ℃ and the reaction lasts for 13 hours.
Taking a proper amount of the magnesium-aluminum hydrotalcite product obtained in the preparation process as a sample, adopting the same detection means and analysis as in example 1 to determine that the particle size of the sample is between 20 and 95nm and the purity is 94.5 percent, thus proving that the product has higher crystallinity and meets the performance index of the magnesium-aluminum hydrotalcite product prepared by the existing industrial preparation method.
In the above embodiments, firstly, sulfur dioxide gas reacts with magnesium oxide in light-burned magnesium oxide powder in water to prepare a magnesium bisulfite solution, and meanwhile, the other side can be dissolved by adding aluminum hydroxide into the sodium hydroxide solution and heating, and sodium carbonate is added to prepare a sodium metaaluminate and sodium carbonate solution, then the sodium metaaluminate and sodium carbonate solution are added into the magnesium bisulfite solution and heated and stirred to obtain a magnesium-aluminum hydrotalcite precipitate and a sodium sulfite solution, and then, the magnesium-aluminum hydrotalcite precipitate and the sodium sulfite solution are subjected to subsequent filtration, washing and corresponding drying or concentration treatment, so that a magnesium-aluminum hydrotalcite product and a sodium sulfite product can be produced. The sulfur dioxide gas can be added to prepare magnesium bisulfite solution by matching with magnesium oxide, and the aim of recovering and treating tail gas produced by a sulfur production process can be achieved. Compared with the prior art that a single product of the magnesium-aluminum hydrotalcite is obtained by consuming a large amount of sodium carbonate or sodium hydroxide raw material, the preparation method provided by the invention can be used for preparing the magnesium-aluminum hydrotalcite and co-producing sodium sulfite after consuming the sodium hydroxide raw material, so that the application of the sodium hydroxide raw material can generate a value beyond expectation, and in view of preparing the magnesium-aluminum hydrotalcite, the extra sodium hydroxide raw material is not required to be consumed, so that the production cost is reduced in a phase-changing manner.
It should be understood by those skilled in the art that, as can be seen from the reaction principle of formula (3), the concentration of the magnesium oxide slurry is controlled within the range of 2-6%, so that the mass concentration of the prepared magnesium bisulfite solution can reach 6-16%, and then can be calculated by formula (4), and the magnesium bisulfite within the mass concentration range accounts for a lower proportion in the reaction system than the sodium metaaluminate, sodium carbonate solution and sodium hydroxide solution, so that correspondingly, the reactants (sodium metaaluminate, sodium carbonate solution and sodium hydroxide solution) with relatively more mass concentrations are properly used, so that the conversion rate of the magnesium bisulfite raw material can be increased, and thus the magnesium bisulfite raw material is fully utilized, and the production cost is reduced.
In addition, it is worth mentioning that, from the reaction principle of formula (4), the finally obtained product only comprises a certain amount of aqueous solution besides the magnesium-aluminum hydrotalcite and sodium sulfite, which indicates that the magnesium-aluminum hydrotalcite prepared by the preparation method does not generate chemical waste liquid needing additional treatment basically, thereby greatly reducing the trouble degree of reaction product treatment and playing a good role in environmental protection. Furthermore, the reaction slurry obtained in the formula (4) actually needs to be filtered and washed, and a large amount of washing liquid generated in the washing process is mainly aqueous solution and can be sent to the first step for preparing the magnesium bisulfite solution, so that the resource recycling is realized, the production cost of enterprises is reduced, and a green and sustainable circular production preparation system is realized.
Comparative example 1
The particle size of some commercial non-nano-scale magnalium hydrotalcite is 0.6-1 μm, and the purity is more than 93%.
Comparative example 2
The average grain diameter of a certain commercial nano-scale magnalium hydrotalcite is 50nm, and the purity is more than 93 percent.
Test detection
The magnesium-aluminum hydrotalcite is a layered double metal hydroxide, has the advantages of magnesium hydroxide and aluminum hydroxide flame retardant, overcomes the defects of the magnesium hydroxide and the aluminum hydroxide, has three functions of flame retardance, smoke abatement and filling, and is a promising novel environment-friendly flame retardant with high efficiency, no halogen, no toxicity and low smoke. When the magnalium hydrotalcite fire retardant is heated and decomposed, the surface temperature of the polymer is reduced due to heat absorption, and the released inert carbon dioxide gas and water vapor can dilute the concentration of combustible gas, weaken the fire behavior and play a role in gas phase flame retardance. In order to verify that the magnalium hydrotalcite prepared by the invention has excellent flame retardant effect, the magnalium hydrotalcite is verified by the following test.
The magnesium-aluminum hydrotalcite in each example and comparative example is used as a flame retardant, and corresponding EVA foaming materials are prepared respectively according to the same components, wherein the foaming materials mainly comprise EVA, a foaming agent, a coupling agent, a cross-linking agent, a flame retardant (magnesium-aluminum hydrotalcite) and a mold release agent. The EVA foaming materials prepared in examples 1-4 and comparative examples 1-2 are subjected to mechanical property and flame retardant property detection, wherein the detection method comprises the following steps: performing hardness measurement according to the national standard GB/T3903.4-2008; measuring the tensile strength according to the national standard GB/T528-2009; testing a Limiting Oxygen Index (LOI) on an HC-2 type oxygen index instrument according to the national standard GB/T2406-93; testing a vertical combustion test on an CZF-3 type horizontal vertical combustion tester according to the national standard GB 2408-80; the cone calorimeter test was carried out to measure the maximum heat release rate (PHRR) according to the 1SO5600 standard test method. The test results are shown in table 1.
TABLE 1
It can be seen from table 1 that each group of EVA foam materials has certain mechanical properties and flame retardancy, and when compared with comparative example 1 and example 1, under the same dosage, the commercially available micron-sized magnesium aluminum hydrotalcite is used as a flame retardant, and compared with the nano-sized magnesium aluminum hydrotalcite, the tensile strength and flame retardancy of the EVA foam material are reduced, because the nano-sized magnesium aluminum hydrotalcite prepared in example 1 has better dispersibility and compatibility, and as a flame retardant, the EVA foam material can maintain relatively better mechanical properties and flame retardancy.
In addition, compared with the comparative example 2 and the example 1, under the condition of the same dosage, the difference between the mechanical property and the flame retardant property of the comparative example 2 and the example 1 is not large, which shows that the magnalium hydrotalcite prepared by the invention can also play an excellent flame retardant effect when being used as a flame retardant compared with the same products on the market. However, compared with the same product on the market, the magnesium-aluminum hydrotalcite product obtained by the preparation method provided by the invention has lower preparation cost, so that the magnesium-aluminum hydrotalcite product has better market prospect and application value.
The above embodiments are preferred implementations of the present invention, and the present invention can be implemented in other ways without departing from the spirit of the present invention.
Claims (7)
1. The preparation method of the low-cost magnesium-aluminum hydrotalcite is characterized by comprising the following steps:
firstly, adding light-burned magnesia powder serving as a raw material into a reaction kettle, mixing the light-burned magnesia powder with a proper amount of water, and introducing sulfur dioxide gas to form a soluble magnesium bisulfite solution;
adding aluminum hydroxide into a sodium hydroxide solution, heating and dissolving, and adding sodium carbonate to prepare sodium metaaluminate and sodium carbonate solution;
step three, adding the sodium metaaluminate and sodium carbonate solution prepared in the step two into the magnesium bisulfite solution prepared in the step one, heating and stirring to obtain reaction slurry, namely magnesium aluminum hydrotalcite precipitate and sodium sulfite solution;
step four, filtering and washing the reaction slurry obtained in the step three to obtain a magnesium-aluminum hydrotalcite filter cake, a sodium sulfite filtrate and a washing liquid;
step five, drying the magnalium hydrotalcite filter cake to obtain a magnalium hydrotalcite product; concentrating the sodium sulfite filtrate to obtain a sodium sulfite product;
and step six, sending the washing liquid obtained in the step four into the reaction kettle in the step one to repeatedly prepare the magnesium bisulfite solution.
2. The method for preparing the low-cost magnesium aluminum hydrotalcite of claim 1, wherein the method comprises the following steps: the content of magnesium oxide in the light-burned magnesium oxide powder is 90 percent.
3. The method for preparing the low-cost magnesium aluminum hydrotalcite of claim 1, wherein the method comprises the following steps: in the first step, the reaction temperature in the reaction kettle is 25-65 ℃, and the reaction time is 6-12 hours.
4. The method for preparing the low-cost magnesium aluminum hydrotalcite of claim 3, wherein the method comprises the following steps: the mass concentration of the magnesium bisulfite solution prepared in the step one is 6-16%.
5. The method for preparing the low-cost magnesium aluminum hydrotalcite of claim 1, wherein the method comprises the following steps: and in the second step, the mass concentration of the sodium hydroxide solution is 20-32%.
6. The method for preparing the low-cost magnesium aluminum hydrotalcite of claim 1, wherein the method comprises the following steps: the reaction temperature in the third step is 85-105 ℃, and the reaction time is 8-16 hours.
7. The method for preparing the low-cost magnesium aluminum hydrotalcite of claim 1, wherein the method comprises the following steps: the whiteness of the aluminum hydroxide is more than or equal to 90 percent, the effective content is more than or equal to 99 percent, and the granularity is more than 200 meshes; the volume content of sulfur dioxide in the sulfur dioxide gas is more than 8 percent.
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| WO2023019746A1 (en) | 2023-02-23 |
| CN113716588B (en) | 2023-04-18 |
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