CN111547750B - Preparation method of hexagonal flaky magnesium hydroxide flame retardant with controllable particle size - Google Patents
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Abstract
The invention relates to a preparation method of a hexagonal flaky magnesium hydroxide flame retardant with controllable particle size, belonging to the technical field of inorganic material preparation. The invention discloses a hexagonal flaky magnesium hydroxide flame retardant which is prepared by preparing magnesium oxide suspension from magnesium oxide and water as raw materials, 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, and modulating the particle size of hexagonal flaky magnesium hydroxide by modulating the material ratio of a reaction system. The preparation method has the advantages of simple reaction process, cleanness, environmental protection, low energy consumption, low production cost and the like, and the obtained product is the hexagonal flaky magnesium hydroxide flame retardant with controllable particle size, narrow particle size distribution, regular appearance and low specific surface area.
Description
Technical Field
The invention relates to a preparation method of a hexagonal flaky magnesium hydroxide flame retardant with controllable particle size, belonging to the field of preparation of inorganic materials.
Background
Magnesium hydroxide has wide application as an important inorganic chemical product in the fields of materials, chemical industry, environmental protection and the like. As an inorganic flame retardant, the flame retardant has the triple effects of filling, flame retarding and smoke control, and is an excellent inorganic additive flame retardant. Compared with aluminum hydroxide which is an inorganic additive flame retardant, the magnesium hydroxide has the advantages of higher decomposition temperature (340-. The research on the preparation technology of the magnesium hydroxide flame retardant and the flame retardant performance of the magnesium hydroxide flame retardant in different materials is more at home and abroad.
Because magnesite resources are rich in China, the preparation of magnesium hydroxide by using magnesite as a raw material through calcination, grinding, impurity removal and hydration is a hot point of industrial research. Wanyan et al [ university of wuhan project, 2013, month 01, volume 35, phase 1: 41-45, adopting light-burned magnesium powder as raw material and ammonia water as bottom-precipitation agent to prepare flaky magnesium hydroxide with the granularity D50 of about 1 micron, and seriously agglomerating. Plum man et al [ functional material, vol 2 No. 51 in 2020: 02131-02136 is prepared from light-burned magnesium and distilled water through grinding and hydrating to obtain nano-class magnesium hydroxide flakes, but the aggregation is serious. CN110642275A takes light-burned magnesium as a raw material, and after the light-burned magnesium is crushed, hydrated and deironized, a nucleating agent is added and ground, a catalyst is added to react for a period of time, and after the iron is removed for the second time, the mixture is filtered, a dispersing agent is added and ground, and then the magnesium hydroxide is obtained after centrifugation and drying. CN106366700B takes brucite as a raw material, and prepares the magnesium hydroxide flame retardant through wet grinding, desanding and purifying, flotation and classification, filter pressing after purification, drying and crushing, but the product belongs to the middle and low end of magnesium hydroxide flame retardant products. The patent CN109761252A takes active magnesium oxide as raw material, adopts hydration method to prepare magnesium hydroxide powder, applies pulse current in hydration process, and obtains layered, rod-like and granular nano magnesium hydroxide by modulating pulse current and pulse frequency.
The magnesium hydroxide prepared by hydration of magnesium oxide has the following defects: the appearance and the granularity are difficult to control (particularly the difficulty is higher when micron-sized magnesium hydroxide is prepared), the crystallinity is low, the specific surface area is large, the particles are fine, the agglomeration is easy, and the like. The flame retardant has poor dispersibility and compatibility in high polymers such as resin and the like, and is easy to cause poor mechanical property and processability of materials. The crystallinity, morphology, granularity, specific surface area and the like of magnesium hydroxide all affect the flame retardant property, and researches show that: the hexagonal magnesium hydroxide has good dispersibility in resin materials, good toughness, reinforcing property and can enhance the flexural strength and ductility of polymer materials.
Disclosure of Invention
The invention provides a novel process for preparing a magnesium hydroxide flame retardant by a magnesium oxide hydration method, which is used for overcoming or avoiding the defects of low crystallinity, fine granularity, large specific surface area, poor dispersibility and the like of the existing product.
In order to achieve the above object, a first aspect of the present invention provides a method for controlling the particle size and morphology of magnesium hydroxide, wherein the method comprises: (1) preparing magnesium oxide suspension with magnesium oxide and water, adding a certain amount of alkali NaOH and an auxiliary agent, uniformly stirring, and then putting into a high-pressure reaction kettle for reaction. (2) In the reaction system, MgO, water, NaOH and an auxiliary agent are carried out within a specific mass ratio range, and the particle size and the morphology of a final product are controlled by adjusting the mass ratio of the MgO, the water, the NaOH and the auxiliary agent. (3) And filtering, washing, drying and grinding the slurry after reaction to obtain the hexagonal flaky magnesium hydroxide.
The second aspect of the invention provides hexagonal flaky magnesium hydroxide with controllable particle size, which is prepared by the method. According to the technical scheme, the magnesium hydroxide with controllable granularity and hexagonal sheet shape is prepared by taking magnesium oxide, NaOH, an auxiliary agent and water as raw materials, and the granularity and the shape of a final product are controlled by adjusting the material ratio of a reaction system and the hydrothermal synthesis condition.
The concentration of magnesium oxide in the magnesium oxide suspension is 10 to 45% (mass percentage concentration), more preferably 15 to 30% (mass percentage concentration). If so. The concentration is too high, and the reaction is incomplete; the concentration is too low, and the product granularity is too large.
The selected auxiliary agent is one or more of magnesium nitrate, magnesium acetate and magnesium carbonate; the addition amount of the auxiliary agent is 0.2-3.5% (mass percentage concentration), more preferably 1-2.5% (mass percentage concentration).
In the reaction system, m (NaOH)/m (MgO) is 0.65-1.5, preferably m (NaOH)/m (MgO) is 0.9-1.2, corresponding to the product of hexagonal sheet magnesium hydroxide with micron size, and the average grain size is 1.2-4 microns. m (NaOH)/m (MgO) is 0.04-0.50, preferably m (NaOH)/m (MgO) is 0.05-0.20, corresponding to the product being submicron hexagonal sheet magnesium hydroxide, with an average particle size of 0.4-0.7 micron.
The reaction temperature is 160-220 ℃, the reaction time is 3-15 hours, the more preferable reaction temperature is 180-210 ℃, and the reaction time is 4-10 hours.
The filling rate of the reaction kettle is 30-80% (volume percentage of the reaction kettle), and more preferably 55-70% (volume percentage of the reaction kettle).
The third aspect of the invention provides the application of the hexagonal flaky magnesium hydroxide in flame retardance.
The hexagonal magnesium hydroxide flame retardant is prepared from magnesium oxide, a selected auxiliary agent and sodium hydroxide for the first time by a novel hydration method, submicron magnesium hydroxide and micron magnesium hydroxide with selected particle sizes are obtained by a selected proportion, the two flame retardants both have regular shapes and narrow particle size distribution, so that a lower specific surface area is obtained, the flame retardants with the characteristics have good dispersibility, can be added into application materials in a large proportion, and have a good flame retardant effect.
Drawings
FIG. 1 is an SEM photograph of a product (A1) of example 1 of the present invention.
FIG. 2 is an XRD pattern of the product of example 1 of the present invention (A1).
FIG. 3 is an SEM photograph of a product (A2) of example 2 of the present invention.
FIG. 4 is an XRD pattern of the product of example 2 of the present invention (A2).
Detailed Description
The endpoints of the ranges and any values disclosed herein are not limited to the precise range or value, and such ranges or values should be understood to encompass values close to those ranges or values. For ranges of values, between the endpoints of each of the ranges and the individual points, and between the individual points may be combined with each other to give one or more new ranges of values, and these ranges of values should be considered as specifically disclosed herein.
In the embodiment of the invention, the hydrothermal reaction is carried out in a high-pressure reaction kettle, the 2L high-pressure reaction kettle is purchased from West Anita instruments and technology Co., Ltd, the model is FCF-2L, and the 1L high-pressure reaction kettle is purchased from West Anita instruments and technology Co., Ltd, the model is FCF-1L. The 0.2L reaction kettle is purchased from Weihai-Huan-Yu chemical machinery Co., Ltd, and the model is GSH-0.2. Magnesium oxide was purchased from yurt magnesium industries, ltd; NaOH was purchased from IS-IT-1, Tai chemical Co., Ltd, Sinkiang; magnesium acetate is provided by Tianjin Damao chemical reagent factory and is AR pure; magnesium carbonate is provided by the Hongze chemical industry, model ZH-1; magnesium nitrate is provided by Shanxi Jinlan chemical products company, 99%.
Example 1:
300g of light-burned magnesia powder as a raw material and 810g of water are mixed into a suspension, 360g of NaOH and 24g of magnesium acetate are added and stirred uniformly, and then the slurry is transferred into a 2L high-pressure reaction kettle (the filling rate of the reaction kettle is 65 percent), the reaction temperature is 200 ℃, and the reaction time is 8 hours. And (4) carrying out suction filtration on the slurry obtained after the reaction, and washing, drying and crushing the obtained filter cake to obtain the magnesium hydroxide A1. The SEM image and XRD of product A1 are shown in figures 1 and 2. As can be seen from the figure, the obtained product is in a micron-scale hexagonal sheet shape, and has high crystallinity, good appearance and narrow particle size distribution.
Example 2:
raw material 210g of light-burned magnesia powder and 590g of water are mixed into suspension, 40g of NaOH and 17 g of magnesium acetate are added and stirred uniformly, and then the slurry is transferred into a 1L high-pressure reaction kettle (the filling rate of the reaction kettle is 70 percent), the reaction temperature is 200 ℃, and the reaction time is 6 hours. And (4) carrying out suction filtration on the slurry obtained after the reaction, and washing, drying and crushing the obtained filter cake to obtain the magnesium hydroxide A2. The SEM image and XRD of product A2 are shown in figures 3 and 4. As can be seen from the figure, the obtained product is in a submicron hexagonal sheet shape, and has high crystallinity, good appearance and narrow particle size distribution.
Example 3:
300g of light-burned magnesia powder as a raw material and 810g of water are mixed into a suspension, 360g of NaOH and 24g of magnesium acetate are added and stirred uniformly, and then the slurry is transferred into a 2L high-pressure reaction kettle (the filling rate of the reaction kettle is 65 percent), the reaction temperature is 160 ℃, and the reaction time is 6 hours. And (4) carrying out suction filtration on the slurry obtained after the reaction, and washing, drying and crushing the obtained filter cake to obtain the magnesium hydroxide A3.
Example 4:
after 10g of light-burned magnesia powder as a raw material and 120g of water are mixed into a suspension, 24g of NaOH and 1.7 g of magnesium acetate are added and stirred uniformly, the slurry is transferred into a 0.2L high-pressure reaction kettle (the filling rate of the reaction kettle is 70 percent), the reaction temperature is 200 ℃, and the reaction time is 6 hours. And (4) carrying out suction filtration on the slurry obtained after the reaction, and washing, drying and crushing the obtained filter cake into sheet-shaped magnesium hydroxide A4. In this example, low-concentration magnesia suspension slurry was used as the starting material (8.5%) and the resulting product was in the form of submicron, irregular flakes.
Example 5:
after 37.2g of light-burned magnesia powder as a raw material and 110g of water are mixed into a suspension, 22g of NaOH and 3 g of magnesium acetate are added and stirred uniformly, the slurry is transferred into a 0.2L high-pressure reaction kettle (the filling rate of the reaction kettle is 70 percent), the reaction temperature is 200 ℃, and the reaction time is 6 hours. And (4) carrying out suction filtration on the slurry obtained after the reaction, and washing, drying and crushing the obtained filter cake to obtain the magnesium hydroxide A5. In the embodiment, the ratio of m (NaOH)/m (MgO) in the raw materials is 0.59, the product is a mixture of nano flaky magnesium hydroxide and micron hexagonal flaky magnesium hydroxide, and the product shows wider particle size distribution and poor appearance and is irregular flaky.
Example 6:
after mixing 37.2g of light-burned magnesia powder as a raw material with 110g of water to form a suspension, adding 1g of NaOH and 3 g of magnesium acetate, uniformly stirring, transferring the slurry into a 0.2L high-pressure reaction kettle (the filling rate of the reaction kettle is 70%), reacting at 200 ℃ for 6 hours. And (4) carrying out suction filtration on the slurry obtained after the reaction, and washing, drying and crushing the obtained filter cake to obtain the nano magnesium hydroxide A6. In this example, the ratio of m (NaOH)/m (MgO) in the raw material was 0.027, and the product was in the form of submicron irregular flakes.
Example 7
The same procedure for preparing magnesium hydroxide as in example 1 was repeated, except that the reaction temperature was 140 ℃ and the reaction time was 4 hours, to obtain magnesium hydroxide A7. The reaction temperature and the reaction time are lower, and the product is submicron and irregular flake.
Example 8
The same procedure for preparing magnesium hydroxide as in example 1 was repeated, except that the reaction temperature was 200 ℃ and the reaction time was 16 hours, to obtain magnesium hydroxide A8. The experimental results show that too long reaction times have an adverse effect on the results.
Example 9
The same procedures used in example 1 were repeated except that the reaction was carried out in a 5L autoclave, to obtain magnesium hydroxide A9. The filling rate of the reaction kettle is 26 percent in the embodiment, and the product has wide and irregular flake-shaped particle size distribution. From experimental results, the filling rate of the reaction kettle is too low, and the result is unfavorable because the pressure in the reaction kettle is low in the reaction process.
Example 10
300g of light-burned magnesium powder as a raw material and 810g of water are mixed to form a suspension, 360g of NaOH and 0.3 g of magnesium acetate are added to be uniformly stirred, and then the slurry is transferred to a 2L high-pressure reaction kettle (the filling rate of the reaction kettle is 65 percent), the reaction temperature is 200 ℃, and the reaction time is 8 hours. And (4) carrying out suction filtration on the slurry obtained after the reaction, and washing, drying and crushing the obtained filter cake to obtain the magnesium hydroxide A10. The amount of the additive added in the embodiment is too low, and the product is submicron and irregular flake.
Example 11
300g of light-burned magnesium powder as a raw material and 810g of water are mixed to form a suspension, 360g of NaOH and 68 g of magnesium acetate are added to be uniformly stirred, and then the slurry is transferred to a 2L high-pressure reaction kettle (the filling rate of the reaction kettle is 65 percent), the reaction temperature is 200 ℃, and the reaction time is 8 hours. And (4) carrying out suction filtration on the slurry obtained after the reaction, and washing, drying and crushing the obtained filter cake to obtain the magnesium hydroxide A11. The amount of the additive added in the embodiment is too high, the particle size distribution of the product is wider from 0.3 micron to 16.8 micron, and the shape of the product is irregular and flaky.
Comparative example 1:
after 408g of light-burned magnesium powder as a raw material and 1100g of water were mixed into a suspension, 32.6 g of magnesium acetate was added and stirred uniformly, and then the slurry was transferred to a 2L high-pressure reaction kettle (the filling rate of the reaction kettle was 65%), the reaction temperature was 200 ℃ and the reaction time was 8 hours. And (4) carrying out suction filtration on the slurry obtained after the reaction, and washing, drying and crushing the obtained filter cake to obtain the magnesium hydroxide D1.
Comparative example 2:
300g of light-burned magnesium powder as a raw material and 810g of water are mixed into a suspension, 360g of NaOH is added and uniformly stirred, and then the slurry is transferred into a 2L high-pressure reaction kettle (the filling rate of the reaction kettle is 65 percent), the reaction temperature is 200 ℃, and the reaction time is 8 hours. And (4) carrying out suction filtration on the slurry obtained after the reaction, and washing, drying and crushing the obtained filter cake to obtain the magnesium hydroxide D2.
Table 1 shows physical property indexes of the products obtained in examples 1 to 11 of the present invention and comparative examples 1 to 2.
TABLE 1 physical Properties of the products obtained in examples 1-11 and comparative examples 1 and 2
*
The preferred embodiments of the invention disclosed above are intended to be illustrative only. The preferred embodiments are not intended to be exhaustive or to limit the invention to the precise embodiments disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best utilize the invention. The specific parameters given in the above examples, which may vary within suitable ranges, may have the same or similar effect, e.g. the average particle size value varies within 5 microns, preferably within 3 or 2 microns. The invention is limited only by the claims and their full scope and equivalents.
Claims (1)
1. A preparation method of hexagonal flaky magnesium hydroxide flame retardant with controllable particle size is characterized in that: preparing magnesium oxide and water into magnesium oxide suspension, adding NaOH and an auxiliary agent, stirring uniformly, and then putting into a high-pressure reaction kettle for reaction; (2) the mass ratio of NaOH to MgO in the reaction system is 0.65-1.5, (3) slurry after reaction is filtered, washed, dried and ground to obtain hexagonal flaky magnesium hydroxide, wherein the mass concentration of magnesium oxide in the magnesium oxide suspension is 10-45%, and the auxiliary agent is one or more of magnesium nitrate, magnesium acetate and magnesium carbonate; the addition amount of the auxiliary agent is 0.2-3.5% of the mass of the magnesium oxide suspension, the reaction temperature is 160-220 ℃, the reaction time is 3-15 hours, and the filling rate of the reaction kettle is 30-80% by volume.
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| CN112408439B (en) * | 2020-11-20 | 2021-09-17 | 洛阳中超新材料股份有限公司 | Method for preparing superfine magnesium hydroxide for flame retardant by using magnesium hydroxide coarse powder as raw material |
| CN113044861A (en) * | 2021-04-16 | 2021-06-29 | 乌兰中钰新材料有限公司 | Preparation method of high-purity flame retardant magnesium hydroxide |
| CN113548682A (en) * | 2021-07-22 | 2021-10-26 | 安徽大学绿色产业创新研究院 | Method for preparing hexagonal flaky flame-retardant magnesium hydroxide from natural hydromagnesite |
| CN113582209A (en) * | 2021-08-26 | 2021-11-02 | 上海应用技术大学 | Preparation method and application of hexagonal flaky magnesium hydroxide |
| CN114394611B (en) * | 2022-01-21 | 2024-05-24 | 洛阳中超新材料股份有限公司 | Preparation method of high aspect ratio flaky magnesium hydroxide |
| CN114436301B (en) * | 2022-02-18 | 2024-04-05 | 洛阳中超新材料股份有限公司 | Preparation method of magnesium hydroxide large monocrystal |
| CN114874494B (en) * | 2022-03-28 | 2023-10-17 | 洛阳中超新材料股份有限公司 | High-flow magnesium hydroxide flame retardant, preparation method thereof and low-smoke halogen-free cable |
| CN115417436B (en) * | 2022-09-20 | 2023-08-11 | 西部金属材料股份有限公司 | Preparation method of two-dimensional magnesium hydroxide nano-sheet |
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