CN110642275A - Preparation method of magnesium hydroxide - Google Patents
Preparation method of magnesium hydroxide Download PDFInfo
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- CN110642275A CN110642275A CN201911073270.4A CN201911073270A CN110642275A CN 110642275 A CN110642275 A CN 110642275A CN 201911073270 A CN201911073270 A CN 201911073270A CN 110642275 A CN110642275 A CN 110642275A
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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
- C01F5/00—Compounds of magnesium
- C01F5/14—Magnesium hydroxide
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- C—CHEMISTRY; METALLURGY
- 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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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
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Abstract
The invention relates to a preparation method of magnesium hydroxide, belonging to the field of chemical materials. The preparation method comprises the following steps: firstly, crushing the light burned magnesium and sieving the crushed light burned magnesium by a 200-mesh sieve; secondly, mixing water with the product obtained in the first step according to the mass ratio of (0.5-10): 1, uniformly mixing, and reacting for 0.5-2 h; thirdly, adding a nucleating agent into the product obtained in the second step after iron removal and filtration; grinding the product obtained in the step III; fifthly, adding a catalyst into the product obtained in the step IV, and reacting for 0.5-12 h; sixthly, removing iron and filtering the product obtained in the fifth step, and adding a dispersing agent into the product; seventhly, grinding the product obtained in the step I; eighthly, centrifuging and drying the product obtained in the step seventhly. The invention realizes the control of the performance of the magnesium hydroxide product from the aspect of process flow, and obtains the magnesium hydroxide powder with high purity, high yield, narrow particle size distribution and good dispersibility.
Description
Technical Field
The invention relates to a preparation method of magnesium hydroxide, belonging to the field of chemical materials.
Background
The preparation method of the magnesium hydroxide mainly comprises two methods, one is a magnesium oxide hydration method, and the other is a chemical precipitation method. At present, the chemical precipitation method is mainly used industrially, the ammonia method is mainly used for magnesium precipitation, and the ammonia water method is used for producing the magnesium chloride as the raw material. Due to the problem of system uniformity in the intermittent process of the ammonia water method, great technical difficulty exists in the aspect of controlling the shape and the particle size of magnesium hydroxide product particles.
The light-burned magnesium oxide is called light-burned magnesium for short, and is an important product of magnesium-containing minerals after calcination or other processing. The light-burned magnesium has rich sources and is obtained by taking magnesite as a raw material. In recent years, a method for producing magnesium hydroxide from light-burned magnesium has been attracting much attention. How to control the particle size and the particle size distribution of the magnesium hydroxide becomes a key technology for preparing the magnesium hydroxide.
CN106745103A discloses a method for preparing magnesium oxide or magnesium oxide and fibrous magnesium hydroxide by magnesite, which comprises the steps of calcining magnesite to obtain light-burned magnesium powder; adding the light-burned magnesium powder into an ammonium salt solution for leaching under the conditions of reduced pressure, water bath heating and stirring, and filtering to obtain a magnesium salt leaching solution; and (3) reacting the magnesium salt leaching solution with ammonia water to obtain magnesium hydroxide precipitate.
CN103613108B discloses a method for preparing a magnesium hydroxide flame retardant by an ammonia gas method, which comprises the steps of preparing a dilute sulfuric acid solution with a certain concentration, and adding light-burned powder (light-burned magnesium powder) to prepare a magnesium sulfate solution; introducing ammonia gas into the solution through a bubbler to perform reaction; adding a compound surfactant, aging, washing, filtering and drying to obtain the narrow-distribution micron-sized magnesium hydroxide. The product is in the shape of flower-ball particles, and the particle size is intensively distributed at 7-8 μm.
CN103101936B discloses a method for preparing magnesium hydroxide by an ammonia gas injection method, which takes light-burned magnesium and ammonium salt as raw materials, obtains ammonia gas and magnesium salt solution by ammonia evaporation reaction, and the ammonia gas and the magnesium salt solution are contacted in an injection type reactor and generate magnesium hydroxide precipitation reaction, thus obtaining a magnesium hydroxide product with uniform shape and good dispersion condition.
CN107032374A discloses a preparation method of magnesium hydroxide, which adopts light-burned magnesium powder and ammonium chloride to obtain a clear magnesium chloride solution; fully dissolving a surfactant in a magnesium chloride solution; dropwise adding ammonia water for precipitation reaction, and carrying out hydrothermal modification on the white magnesium hydroxide powder to obtain a hydrothermal modified white magnesium hydroxide precipitate.
CN10214979A discloses a method for synthesizing active magnesium hydroxide, which comprises the steps of calcining cheap magnesite as a raw material to obtain light-burned magnesium, and carrying out neutralization reaction with water in the presence of an alkaline agent or a high molecular agent to synthesize the magnesium hydroxide with low viscosity and high activity.
CN1088548A discloses a method for adjusting active magnesium hydroxide, which is characterized in that pulverized or granulated lightly calcined magnesium obtained by calcining natural magnesite is added to a warm aqueous solution in which an anionic surfactant containing an alkali metal salt of a fatty acid as a main component is dissolved, and the prepared magnesium hydroxide slurry has good fluidity, non-settling property and non-coagulation property.
CN1070154C discloses a method for preparing magnesium hydroxide, which adopts light-burned magnesium and water to wet, and adopts dry mixing or dry grinding to prepare powder-particle magnesium hydroxide.
CN1174171A discloses a method for preparing magnesium hydroxide and its aqueous suspension, which uses light-burned magnesium as raw material, and after wetting with water, grinding and aging at 100 deg.C, the powder-like magnesium hydroxide is obtained.
CN1680191A discloses a method for producing industrial magnesium hydroxide, which adopts light-burned magnesium powder as raw material, directly hydrates the raw material, hydrates the raw material in a water pool for 12-24h, and obtains the magnesium hydroxide.
The prior art shows that the magnesium hydroxide is prepared by using light-burned magnesium as a raw material and mainly adopting ammonium salt to obtain a magnesium salt solution and then carrying out a precipitation reaction, and the process is similar to the process of magnesium precipitation by an ammonia method and is relatively complex. The method for directly hydrating the light-burned magnesium has the advantages of long reaction time, easy residue of unreacted magnesium oxide, and great difficulty in effectively obtaining well-dispersed magnesium hydroxide powder from the aqueous slurry.
The macroscopic production of magnesium hydroxide powder by using light-burned magnesium as a raw material has the following technical difficulties: (1) the hydration rate is limited by a reaction mechanism, and the improvement of the hydration rate in a short reaction time has great technical difficulty; (2) purity, salt, alkali, catalyst, dispersant and the like are introduced in the reaction, which is not beneficial to improving the purity of the magnesium hydroxide; (3) the morphology and the particle size, the uniformity of a reaction system and a reaction method make the obtaining of magnesium hydroxide powder with certain morphology and particle size distribution difficult; (4) redispersibility, in which magnesium hydroxide particles are easily agglomerated in the process of obtaining powder from slurry, resulting in poor redispersibility; (5) the technical process is taken as two main methods, the technical process of the ammonia method is complex, and the direct hydration reaction period is longer, so that the scale production is not facilitated; (6) energy consumption, namely, a large amount of energy consumption is needed for directly obtaining powder from slurry, and the development requirement of green energy conservation is not met; (7) environmental impact, the use of ammonia and other compounds may cause potential environmental hazards, and the recycling, treatment and discharge of aqueous solutions need to be solved.
Disclosure of Invention
The method has simple process, realizes the control of the hydration process based on the nucleation and diffusion mechanisms, improves the hydration rate, regulates and controls the grain diameter of the product, has full reaction, and obtains the magnesium hydroxide powder with high purity, high yield, controllable grain diameter distribution and good dispersibility. The method reduces production energy consumption, has no harmful substance emission, and is an environment-friendly method for preparing the magnesium hydroxide powder.
The invention provides a preparation method of magnesium hydroxide, which comprises the following steps: firstly, crushing the light burned magnesium and sieving the crushed light burned magnesium by a 200-mesh sieve; secondly, mixing water with the product obtained in the first step according to the mass ratio of (0.5-10): 1, uniformly mixing, and reacting for 0.5-2 h; thirdly, adding a nucleating agent into the product obtained in the second step after iron removal and filtration; grinding the product obtained in the step III; fifthly, adding a catalyst into the product obtained in the step IV, and reacting for 0.5-12 h; sixthly, removing iron and filtering the product obtained in the fifth step, and adding a dispersing agent into the product; seventhly, grinding the product obtained in the step I; eighthly, centrifuging and drying the product obtained in the step seventhly.
In the invention, the nucleating agent is preferably at least one of nano titanium oxide, nano aluminum oxide, nano zinc oxide and nano silicon oxide; the mass ratio of the nucleating agent to the light-burned magnesium is (0-0.02): 1.
in the invention, the catalyst is preferably one of fatty acid and salt thereof, polyacrylic acid and salt thereof, and polyphosphoric acid and salt thereof; the mass ratio of the catalyst to the light-burned magnesium is (0-0.05): 1.
the preferable dispersing agent is one of sodium dodecyl sulfate, glyceryl stearate, polyethylene glycol, polyoxyethylene ether and organic silicon; the mass ratio of the dispersing agent to the light-burned magnesium is (0-0.10): 1.
the reaction temperature in the step (v) is preferably 10-80 ℃.
The invention has the beneficial effects that:
the method adopts a direct hydration method to prepare the magnesium hydroxide, has simple process and full reaction, and can achieve the control of the hydration rate through shorter reaction time.
The invention realizes the control of the performance of the magnesium hydroxide product from the aspect of process flow, and obtains the magnesium hydroxide powder with high purity, high yield, narrow particle size distribution and good dispersibility.
The method takes the light calcined powder as the raw material, reduces the production cost of preparing the magnesium hydroxide by a synthesis method, has better performance than the product prepared by brucite, and accords with the development direction of the magnesium hydroxide.
The method obtained by the invention is simple and feasible, mature in related equipment, reasonable in process route, small in pollution, low in energy consumption and suitable for large-scale production.
Drawings
In the figure 1 of the attached drawings of the invention,
FIG. 1 is an XRD pattern of magnesium hydroxide prepared in examples 1-3.
Detailed Description
The following non-limiting examples are presented to enable those of ordinary skill in the art to more fully understand the present invention and are not intended to limit the invention in any way.
Example 1
A method for preparing magnesium hydroxide, comprising the steps of:
firstly, carrying out jet milling on a light-burned magnesium raw material, and sieving the light-burned magnesium raw material by a 200-mesh sieve;
secondly, mixing water with the product obtained in the first step according to a mass ratio of 2: 1, uniformly mixing, and reacting for 0.5 h;
thirdly, removing iron and filtering the product obtained in the second step;
fourthly, conveying the product obtained in the third step to grinding equipment, and grinding for 2 hours;
fifthly, conveying the product obtained in the step IV to an aging tank, and reacting for 2 hours at room temperature;
sixthly, removing iron and filtering the product obtained in the fifth step;
seventhly, conveying the product obtained in the step sixthly to grinding equipment, and grinding for 1 hour;
eighthly, centrifuging the product obtained in the step seventhly, and then carrying out spray drying to obtain the magnesium hydroxide with the average particle size of 3.0 microns and uniform particle size distribution.
Example 2
A method for preparing magnesium hydroxide, comprising the steps of:
firstly, carrying out jet milling on a light-burned magnesium raw material, and sieving the light-burned magnesium raw material by a 200-mesh sieve;
secondly, mixing water with the product obtained in the first step according to a mass ratio of 2: 1, uniformly mixing, and reacting for 0.5 h;
thirdly, removing iron and filtering the product obtained in the second step, and adding nano titanium oxide into the product, wherein the mass ratio of the nano titanium oxide to the light-burned magnesium is 0.01: 1;
fourthly, conveying the product obtained in the third step to grinding equipment, and grinding for 2 hours;
fifthly, conveying the product obtained in the step IV to an aging tank, adding fatty acid magnesium, wherein the mass ratio of the fatty acid magnesium to the light-burned magnesium is 0.02: 1, reacting at room temperature for 2 hours;
sixthly, removing iron and filtering the product obtained in the fifth step, and adding polyoxyethylene ether into the product, wherein the mass ratio of the polyoxyethylene ether to the light-burned magnesium is 0.05: 1;
seventhly, conveying the product obtained in the step sixthly to grinding equipment, and grinding for 1 hour;
eighthly, centrifuging the product obtained in the step seventhly, and then carrying out spray drying to obtain the magnesium hydroxide with the average particle size of 1.5 microns and uniform particle size distribution.
Example 3
A method for preparing magnesium hydroxide, comprising the steps of:
firstly, carrying out jet milling on a light-burned magnesium raw material, and sieving the light-burned magnesium raw material by a 200-mesh sieve;
secondly, mixing water with the product obtained in the first step according to a mass ratio of 3: 1, uniformly mixing, and reacting for 1.0 h;
thirdly, after iron removal and filtration are carried out on the product obtained in the second step, nano silicon oxide is added into the product, and the mass ratio of the nano silicon oxide to the light-burned magnesium is 0.02: 1;
fourthly, conveying the product obtained in the third step to grinding equipment, and grinding for 2 hours;
fifthly, conveying the product obtained in the step IV to an aging tank, and adding sodium polyacrylate, wherein the mass ratio of the sodium polyacrylate to the light-burned magnesium is 0.02: 1, reacting at room temperature for 2 hours;
sixthly, removing iron and filtering the product obtained in the fifth step, and adding sodium dodecyl sulfate into the product, wherein the mass ratio of the sodium dodecyl sulfate to the light-burned magnesium is 0.08: 1;
seventhly, conveying the product obtained in the step sixthly to grinding equipment, and grinding for 2 hours;
eighthly, centrifuging the product obtained in the step seventhly, and then carrying out spray drying to obtain the magnesium hydroxide with the average particle size of 0.8 micron and uniform particle size distribution.
Claims (5)
1. A preparation method of magnesium hydroxide is characterized by comprising the following steps: the preparation method comprises the following steps:
firstly, crushing the light burned magnesium and sieving the crushed light burned magnesium by a 200-mesh sieve;
secondly, mixing water with the product obtained in the first step according to the mass ratio of (0.5-10): 1, uniformly mixing, and reacting for 0.5-2 h;
thirdly, adding a nucleating agent into the product obtained in the second step after iron removal and filtration;
grinding the product obtained in the step III;
fifthly, adding a catalyst into the product obtained in the step IV, and reacting for 0.5-12 h;
sixthly, removing iron and filtering the product obtained in the fifth step, and adding a dispersing agent into the product;
seventhly, grinding the product obtained in the step I;
eighthly, centrifuging and drying the product obtained in the step seventhly.
2. The method for producing magnesium hydroxide according to claim 1, characterized in that: the nucleating agent is at least one of nano titanium oxide, nano aluminum oxide, nano zinc oxide and nano silicon oxide;
the mass ratio of the nucleating agent to the light-burned magnesium is (0-0.02): 1.
3. the method for producing magnesium hydroxide according to claim 2, characterized in that: the catalyst is one of fatty acid and salt thereof, polyacrylic acid and salt thereof, and polyphosphoric acid and salt thereof;
the mass ratio of the catalyst to the light-burned magnesium is (0-0.05): 1.
4. the method for producing magnesium hydroxide according to claim 3, characterized in that: the dispersing agent is one of sodium dodecyl sulfate, glyceryl stearate, polyethylene glycol, polyoxyethylene ether and organic silicon;
the mass ratio of the dispersing agent to the light-burned magnesium is (0-0.10): 1.
5. the method for producing magnesium hydroxide according to claim 4, characterized in that: the reaction temperature in the fifth step is 10-80 ℃.
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| CN201911073270.4A CN110642275A (en) | 2019-11-05 | 2019-11-05 | Preparation method of magnesium hydroxide |
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| CN201911073270.4A CN110642275A (en) | 2019-11-05 | 2019-11-05 | Preparation method of magnesium hydroxide |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114394611A (en) * | 2022-01-21 | 2022-04-26 | 洛阳中超新材料股份有限公司 | Preparation method of high-aspect-ratio flaky magnesium hydroxide |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1309087A (en) * | 1996-08-12 | 2001-08-22 | 大赛璐网干产业株式会社 | Method for producing magnesium hydroxide and its aqueous suspension |
| CN101214979A (en) * | 2008-01-08 | 2008-07-09 | 李淑荣 | Method for synthesizing active magnesium hydroxide |
-
2019
- 2019-11-05 CN CN201911073270.4A patent/CN110642275A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1309087A (en) * | 1996-08-12 | 2001-08-22 | 大赛璐网干产业株式会社 | Method for producing magnesium hydroxide and its aqueous suspension |
| CN101214979A (en) * | 2008-01-08 | 2008-07-09 | 李淑荣 | Method for synthesizing active magnesium hydroxide |
Non-Patent Citations (2)
| Title |
|---|
| 王飞等: ""镁盐及晶种对氧化镁水化合成氢氧化镁的影响"", 《中国粉体技术》 * |
| 胡庆福等: ""轻烧粉水化法制取阻燃级氢氧化镁新工艺"", 《无机盐工业》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114394611A (en) * | 2022-01-21 | 2022-04-26 | 洛阳中超新材料股份有限公司 | Preparation method of high-aspect-ratio 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 |
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Application publication date: 20200103 |