CN113582209A - Preparation method and application of hexagonal flaky magnesium hydroxide - Google Patents
Preparation method and application of hexagonal flaky magnesium hydroxide Download PDFInfo
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- CN113582209A CN113582209A CN202110986798.1A CN202110986798A CN113582209A CN 113582209 A CN113582209 A CN 113582209A CN 202110986798 A CN202110986798 A CN 202110986798A CN 113582209 A CN113582209 A CN 113582209A
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- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
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Abstract
The invention provides a preparation method of hexagonal flaky magnesium hydroxide, which comprises the steps of mixing and stirring magnesium hydroxide, a dispersing agent and water to prepare a suspension, putting the suspension into a high-pressure reaction kettle for reaction, and filtering, washing, drying and grinding a product after the reaction to obtain the hexagonal flaky magnesium hydroxide, wherein the dispersing agent is polyvinylpyrrolidone or sodium dodecyl sulfate. The method takes common magnesium hydroxide as a raw material and SDS or PVP as a dispersing agent, the reaction process is simple, the energy consumption is low, the method is clean and environment-friendly, the production cost is low, and the obtained product is hexagonal flaky magnesium hydroxide with controllable and regular appearance.
Description
Technical Field
The invention relates to the technical field of flame retardants, in particular to a preparation method and application of hexagonal flaky magnesium hydroxide.
Background
The nano magnesium hydroxide (1-100 nm) has common characteristics of nano materials, such as small-size effect, quantum size effect, surface effect and the like, and can be applied to high polymers to strengthen the performance of the materials. Therefore, the preparation of nano-scale, high-dispersion, complete crystal form and low specific surface area magnesium hydroxide is an important direction of current domestic and foreign research. At present, the research on the flaky magnesium hydroxide mainly focuses on flame retardants, environment-friendly adsorbents, antibacterial agents, environment-friendly coatings and the like. As a flame retardant, magnesium hydroxide has the advantages of flame retardance, smoke suppression, easily available raw materials and the like, and is widely applied to fillers of materials such as engineering plastics, rubber, epoxy resin and the like.
Common preparation methods of the flame-retardant nano magnesium hydroxide mainly comprise a wet coprecipitation method, a hydrothermal method, a magnesium oxide hydrothermal method and the like. The hexagonal flaky nano magnesium hydroxide obtained by Zhao Jianhai et al through impinging stream reaction has small particle size, large specific surface area and excellent flame retardant property. Wu Jian Song takes bittern as raw material and sodium hydroxide is added into a special buffer solution system to obtain magnesium hydroxide with high purity, high crystallinity and excellent dispersibility. In the application of the method in the field of environmental protection, Zhang Yan and the like recover waste graphitized carbon from waste lithium ion batteries and modify the waste graphitized carbon by using magnesium hydroxide with a surface nano structure so as to treat excessive phosphate. This phosphate adsorbent showed one of the highest phosphate adsorption capacities to date, 588.4 mg/g (1 order of magnitude higher than the previously reported carbon-based adsorbents), and showed good stability. Researches such as Nigla Ponnomalifu and the like show that the lignin-magnesium hydroxide nano composite material (LH-MH) developed by utilizing the hydrolyzed lignin waste can be regenerated and recycled after absorbing metal. As an antibacterial agent, Huang Ziyang et al studied magnesium hydroxide particles for crop protection instead of copper bactericide with low cytotoxicity. Liushuzhao et al studied a process for preparing an integral oil-water separation material by modifying melamine sponge with a Magnesium Hydroxide (MH) coating that effectively separates immiscible oil-water mixtures and surfactant-stabilized emulsions. It may have a demulsification efficiency of over 99.7% for surfactant-stabilized emulsions.
The patent CN111547750A discloses a method for preparing a hexagonal flaky magnesium hydroxide flame retardant with controllable particle size, which comprises the steps of preparing magnesium oxide suspension from magnesium oxide and water, adding a certain amount of NaOH and an auxiliary agent, uniformly stirring, putting slurry into a high-pressure reaction kettle, reacting for a period of time, filtering, washing and drying to obtain the hexagonal flaky magnesium hydroxide flame retardant, and adjusting the particle size of hexagonal flaky magnesium hydroxide by adjusting the material ratio of a reaction system.
The conventional hydrothermal method for preparing magnesium hydroxide usually needs to add alkaline additives, such as ammonia water, sodium hydroxide, potassium hydroxide and the like, and has high price and strong corrosivity. And the hydration of magnesium oxide to prepare magnesium hydroxide has complex process and is not beneficial to industrial application.
Disclosure of Invention
The invention aims to solve the problems, and provides a preparation method of hexagonal flaky magnesium hydroxide, which adopts a more environment-friendly dispersing agent, can prepare hexagonal flaky magnesium hydroxide with regular appearance and high dispersion degree, and has the advantages of simple process flow and low production cost.
The purpose of the invention is realized by the following technical scheme:
a preparation method of hexagonal flaky magnesium hydroxide comprises the steps of mixing and stirring magnesium hydroxide, a dispersing agent and water to prepare a suspension, putting the suspension into a high-pressure reaction kettle for reaction, and filtering, washing, drying and grinding a product after the reaction to obtain the hexagonal flaky magnesium hydroxide, wherein the dispersing agent is polyvinylpyrrolidone or sodium dodecyl sulfate.
Preferably, the mass ratio of the magnesium hydroxide to the dispersant is 1 (0.02-0.5), and further preferably, the mass ratio of the magnesium hydroxide to the dispersant is 1: 0.2.
Preferably, the preparation process specifically comprises the following steps: mixing the dispersant with water, adding magnesium hydroxide after fully mixing, stirring for 30-120min, and putting the suspension into a high-pressure reaction kettle for reaction.
Preferably, the mass ratio of magnesium hydroxide to water is 1: 50-60.
Preferably, the reaction temperature is 150-200 ℃, and the reaction time is 4-30h, further preferably, the reaction temperature is 160 ℃, and the reaction time is 6-24 h.
Preferably, the washing times are 3-5 times, the drying temperature is 30-50 ℃, and the drying time is 22-26h, and further preferably, the drying is carried out in an oven, the drying temperature is 40 ℃, and the drying time is 24 h.
The application of the hexagonal flaky magnesium hydroxide prepared by the preparation method is that the hexagonal flaky magnesium hydroxide is used as a flame retardant.
The invention aims to provide a preparation method of hexagonal flaky magnesium hydroxide, which has the advantages of simple process and low cost, and the prepared magnesium hydroxide is hexagonal flaky, has the advantages of higher dispersity, large specific surface area, high crystallinity and the like, and can be used as a flame retardant or a template agent of a carbon material.
Compared with the conventional hydrothermal method for preparing magnesium hydroxide, the method usually needs to add alkaline additives, similar to ammonia water, sodium hydroxide, potassium hydroxide and the like, and has high price and strong corrosivity. And the hydration of magnesium oxide to prepare magnesium hydroxide has complex process. The invention adopts more environment-friendly dispersant, not only can prepare the hexagonal flaky magnesium hydroxide with regular appearance and high dispersity, but also has simple process flow and low production cost.
According to the method, common magnesium hydroxide and water are used as raw materials, a certain amount of Sodium Dodecyl Sulfate (SDS) or polyvinylpyrrolidone (PVP) is added, and the growth process of the crystal face of the magnesium hydroxide is inhibited by utilizing the electrostatic interaction between the SDS or the PVP and the surface of the magnesium hydroxide, so that the crystal face of the magnesium hydroxide grows along the direction favorable for the [001] crystal face, and the hexagonal flaky magnesium hydroxide is obtained. Stirring uniformly, and putting the suspension into a high-temperature high-pressure reaction kettle for hydro-thermal treatment to dissolve and recrystallize common magnesium hydroxide; and filtering, washing and drying a product obtained by the reaction to obtain the hexagonal flaky magnesium hydroxide.
Drawings
FIG. 1 is a scanning electron micrograph of hexagonal flaky magnesium hydroxide prepared in example 1.
Detailed Description
The invention is described in detail below with reference to the figures and specific embodiments.
Example 1
The hexagonal flaky magnesium hydroxide is prepared by the following steps:
0.2g of Sodium Dodecyl Sulfate (SDS) and 60mL of water are mixed uniformly, 1g of magnesium hydroxide is added, the mixture is stirred for 30min, and the suspension is transferred into a 100mL high-pressure reaction kettle (the filling rate of the reaction kettle is 63 percent), the reaction temperature is 160 ℃, and the reaction time is 24 h. And (4) carrying out suction filtration on the suspension obtained after the reaction, and washing, drying and crushing the obtained filter cake to obtain the magnesium hydroxide. The SEM image of the product is shown in figure 1. the product is micron-sized hexagonal sheet, high in crystallinity and regular in shape.
Example 2
The hexagonal flaky magnesium hydroxide is prepared by the following steps:
mixing 0.2g SDS and 60mL water uniformly, adding 1g magnesium hydroxide, stirring for 30min, transferring the suspension into a 100mL high-pressure reaction kettle (the filling rate of the reaction kettle is 63%), reacting at 160 ℃ for 6h, carrying out suction filtration on the suspension obtained after the reaction, and washing, drying and crushing the obtained filter cake to obtain the magnesium hydroxide.
Example 3
The hexagonal flaky magnesium hydroxide is prepared by the following steps:
after 0.2g of polyvinylpyrrolidone (PVP) was mixed with 60mL of water, 1g of magnesium hydroxide was added, the mixture was stirred for 30min, and the suspension was transferred to a 100mL autoclave (the filling rate of the autoclave was 63%), the reaction temperature was 160 ℃ and the reaction time was 24 h. And (4) carrying out suction filtration on the suspension obtained after the reaction, and washing, drying and crushing the obtained filter cake to obtain the magnesium hydroxide.
Example 4
The hexagonal flaky magnesium hydroxide is prepared by the following steps:
uniformly mixing 0.2g of PVP with 60mL of water, adding 1g of magnesium hydroxide, stirring for 30min, transferring the suspension into a 100mL high-pressure reaction kettle (the filling rate of the reaction kettle is 63%), reacting at 160 ℃ for 6h, carrying out suction filtration on the suspension obtained after the reaction, and washing, drying and crushing the obtained filter cake to obtain the magnesium hydroxide.
Comparative example 1
The synthesis of magnesium hydroxide is prepared by adopting a preparation method comprising the following steps: directly adding 1g of magnesium hydroxide into 60mL of water, adding no SDS or PVP, stirring for 30min for comparison, transferring the suspension into a 100mL high-pressure reaction kettle (the filling rate of the reaction kettle is 63%), reacting at 160 ℃ for 6h, carrying out suction filtration on the suspension obtained after reaction, washing, drying and crushing the obtained filter cake to obtain magnesium hydroxide, so that hexagonal flaky magnesium hydroxide cannot be obtained, and meanwhile, samples are gathered together.
The embodiments described above are described to facilitate an understanding and use of the invention by those skilled in the art. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above embodiments, and those skilled in the art should make improvements and modifications within the scope of the present invention based on the disclosure of the present invention.
Claims (10)
1. A preparation method of hexagonal flaky magnesium hydroxide is characterized in that the preparation method comprises the steps of mixing and stirring magnesium hydroxide, a dispersing agent and water to prepare a suspension, putting the suspension into a high-pressure reaction kettle for reaction, and filtering, washing, drying and grinding a product after the reaction to obtain the hexagonal flaky magnesium hydroxide, wherein the dispersing agent is polyvinylpyrrolidone or sodium dodecyl sulfate.
2. The method for preparing hexagonal flaky magnesium hydroxide according to claim 1, wherein the mass ratio of the magnesium hydroxide to the dispersant is 1 (0.02-0.5).
3. The method for preparing hexagonal flaky magnesium hydroxide according to claim 2, wherein the mass ratio of the magnesium hydroxide to the dispersant is 1: 0.2.
4. The method for preparing hexagonal flaky magnesium hydroxide according to claim 1, which is characterized in that the preparation process specifically comprises the following steps: mixing the dispersant with water, adding magnesium hydroxide after fully mixing, stirring for 30-120min, and putting the suspension into a high-pressure reaction kettle for reaction.
5. The method for preparing hexagonal flaky magnesium hydroxide according to claim 4, wherein the mass ratio of magnesium hydroxide to water is 1: 50-60.
6. The method as claimed in claim 4, wherein the reaction temperature is 150 ℃ to 200 ℃ and the reaction time is 4-30 h.
7. The method for preparing hexagonal flaky magnesium hydroxide according to claim 6, wherein the reaction temperature is 160 ℃ and the reaction time is 6-24 h.
8. The method for preparing hexagonal flaky magnesium hydroxide according to claim 6, wherein the washing times are 3 to 5, the drying temperature is 30 to 50 ℃, and the drying time is 22 to 26 hours.
9. The method for preparing hexagonal flaky magnesium hydroxide according to claim 8, wherein the drying is carried out in an oven at a drying temperature of 40 ℃ for 24 hours.
10. Use of the hexagonal flaky magnesium hydroxide prepared by the preparation method according to any one of claims 1 to 9 as a flame retardant.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114212768A (en) * | 2021-12-08 | 2022-03-22 | 上海应用技术大学 | Preparation method of nitrogen-doped two-dimensional flaky hexagonal hollow carbon material with open pores on surface |
| CN114318367A (en) * | 2022-01-10 | 2022-04-12 | 东莞理工学院 | High-dispersion modified nano magnesium hydroxide and preparation method thereof |
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| CN1810927A (en) * | 2006-02-23 | 2006-08-02 | 山东大学 | Prepn of magnesium hydroxide for fire retardant |
| CN101544387A (en) * | 2009-04-25 | 2009-09-30 | 中国科学院青海盐湖研究所 | Preparation technology of hexagonal plate magnesium hydroxide |
| CN101565193A (en) * | 2009-06-05 | 2009-10-28 | 河南科技大学 | Preparation method of highly pure magnesium hydroxide nanocrystal |
| CN102050472A (en) * | 2009-10-28 | 2011-05-11 | 中国科学院过程工程研究所 | Method for preparing submicron flaky magnesium hydroxide from magnesium oxide |
| CN102259898A (en) * | 2011-06-30 | 2011-11-30 | 武汉钢铁(集团)公司 | Method for preparing magnesium hydroxide utilizing light-burned dolomite powder |
| CN106587119A (en) * | 2016-12-24 | 2017-04-26 | 天津大学 | Method for preparing hexagonal flake magnesium hydroxide with dominant growth on (001) crystal face |
| CN111547750A (en) * | 2020-05-15 | 2020-08-18 | 洛阳中超新材料股份有限公司 | Preparation method of hexagonal flaky magnesium hydroxide flame retardant with controllable particle size |
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2021
- 2021-08-26 CN CN202110986798.1A patent/CN113582209A/en active Pending
Patent Citations (7)
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| CN1810927A (en) * | 2006-02-23 | 2006-08-02 | 山东大学 | Prepn of magnesium hydroxide for fire retardant |
| CN101544387A (en) * | 2009-04-25 | 2009-09-30 | 中国科学院青海盐湖研究所 | Preparation technology of hexagonal plate magnesium hydroxide |
| CN101565193A (en) * | 2009-06-05 | 2009-10-28 | 河南科技大学 | Preparation method of highly pure magnesium hydroxide nanocrystal |
| CN102050472A (en) * | 2009-10-28 | 2011-05-11 | 中国科学院过程工程研究所 | Method for preparing submicron flaky magnesium hydroxide from magnesium oxide |
| CN102259898A (en) * | 2011-06-30 | 2011-11-30 | 武汉钢铁(集团)公司 | Method for preparing magnesium hydroxide utilizing light-burned dolomite powder |
| CN106587119A (en) * | 2016-12-24 | 2017-04-26 | 天津大学 | Method for preparing hexagonal flake magnesium hydroxide with dominant growth on (001) crystal face |
| CN111547750A (en) * | 2020-05-15 | 2020-08-18 | 洛阳中超新材料股份有限公司 | Preparation method of hexagonal flaky magnesium hydroxide flame retardant with controllable particle size |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114212768A (en) * | 2021-12-08 | 2022-03-22 | 上海应用技术大学 | Preparation method of nitrogen-doped two-dimensional flaky hexagonal hollow carbon material with open pores on surface |
| CN114212768B (en) * | 2021-12-08 | 2023-04-28 | 上海应用技术大学 | Preparation method of nitrogen-doped two-dimensional flaky hexagonal hollow carbon material with surface open pores |
| CN114318367A (en) * | 2022-01-10 | 2022-04-12 | 东莞理工学院 | High-dispersion modified nano magnesium hydroxide and preparation method thereof |
| CN114318367B (en) * | 2022-01-10 | 2023-10-27 | 东莞理工学院 | High-dispersion modified nano magnesium hydroxide and preparation method thereof |
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Application publication date: 20211102 |