CN104445302A - Method for preparing magnesium hydrate - Google Patents
Method for preparing magnesium hydrate Download PDFInfo
- Publication number
- CN104445302A CN104445302A CN201410722681.2A CN201410722681A CN104445302A CN 104445302 A CN104445302 A CN 104445302A CN 201410722681 A CN201410722681 A CN 201410722681A CN 104445302 A CN104445302 A CN 104445302A
- Authority
- CN
- China
- Prior art keywords
- magnesium
- magnesium hydroxide
- stirring intensity
- ion solution
- ammonia
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Classifications
-
- 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
- C01F5/20—Magnesium hydroxide by precipitation from solutions of magnesium salts with ammonia
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/51—Particles with a specific particle size distribution
-
- 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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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention discloses a method for preparing magnesium hydrate. The method comprises the following steps: 1) preparing a magnesium ion solution; 2) heating the magnesium ion solution to 60-80 DEG C under the condition that the stirring intensity is 350-450r/min; 3) continuously introducing ammonia gas at the flow rate of 200-500mL/min at the temperature and the stirring intensity until the molar ratio of ammonia ions to magnesium ions is (2:1) to (3:1), and reacting; 4) aging at the temperature and the stirring intensity for 60-80 minutes to obtain Mg(OH)2 slurry; and 5) filtering the Mg(OH)2 slurry to obtain a magnesium hydrate product. According to the preparation method, the magnesium hydrate with high purity, high quality, large particle size and low superficial area is finally prepared.
Description
Technical field
The present invention relates to a kind of magnesium hydroxide of fire-fighting purposes, particularly there is the preparation method of magnesium hydroxide.
Background technology
Magnesium hydroxide, as novel interpolation inorganic combustion inhibitor that is efficient, superior, environmental protection, at home and abroad day by day comes into one's own, obtains significant progress in inorganic combustion inhibitor field.The multi-functionals such as it is fire-retardant, eliminate smoke, resistance is dripped, filling, are used widely in polymer materials industry.Magnesium hydroxide has the mechanism of flame-retardant nature to be: decompose when magnesium hydroxide is more than 340 DEG C, generates magnesium oxide and water, absorbs the heat on combustionmaterial surface; Generate the effect that a large amount of moisture has dilution and isolated combustionmaterial superficial air, decomposing the magnesium oxide solid generated is then high temperature resistant material, and the surface being attached to combustionmaterial can stop burning to proceed.
The production technique of existing magnesium hydroxide has multiple, can be divided into lime method, ammonia process, sodium hydroxide method etc. by the kind difference of precipitation agent.The magnesium hydroxide products purity that lime method obtains is low, sodium hydroxide method cost is high, filtration washing difficulty, mother liquor not easily reclaims, and ammonia process, because the alkalescence of ammonia is weak, the solubleness of magnesium hydroxide can be made to strengthen, and thus reaction process is easy to control, and can obtain the magnesium hydroxide of high-purity fine, also can obtain the product that large grain size easily washs, therefore the method is the method that China's production magnesium hydroxide generally adopts.And to study more in ammonia process be Ammonia Process, the research of ammonia method is considerably less.Magnesium hydroxide surface polarity is comparatively strong, and particle diameter is little, be then easy to reunite form offspring, cause with polymer materials consistency very poor, dispersed bad in the polymeric material, have a strong impact on the mechanical property of polymer materials, therefore cannot be directly used in polymer materials to improve its flame-retarding characteristic.
Summary of the invention
The invention provides one and prepare magnesium hydroxide technique, improve the preparation efficiency of magnesium hydroxide and obtain the magnesium hydroxide products of high-quality.
For reaching the object of the invention, the preparation method of this magnesium hydroxide, is characterized in that, comprises the following steps:
1) magnesium ion solution is prepared;
2) by magnesium ion solution at stirring intensity be 350-450r/min condition under be warming up to 60-80 DEG C;
3) at above temperature and stirring intensity condition, continue to pass into ammonia, the flow passing into ammonia is 200-500mL/min, and the mol ratio to ammonium ion and magnesium ion is 2:1-3:1, reacts;
4) ageing 60-80min at above temperature and stirring intensity condition, obtains Mg (OH)
2slip;
5) Mg (OH) is filtered
2slip obtains magnesium hydroxide products.
Wherein, described step 1) be by bischofite, magnesium sulfate heptahydrate deionized water dissolving, filtration, configuration concentration is the magnesium ion solution of 0.5-2.5mol/L, and wherein, the mol ratio of chlorion and sulfate ion is 0.5-10.
Preferably, step 5) also comprise with deionized water wash filter cake to without chlorion and sulfate ion, and under 110 DEG C of conditions dry 6h, obtain magnesium hydroxide products.
Wherein, Büchner funnel vacuum filtration is filtered into described in.
The magnesium hydroxide finally preparing high purity, high-quality acquisition Large stone low surface area provided by the invention.
Accompanying drawing explanation
Fig. 1 is the particle size distribution figure of embodiment 1 the finished product magnesium hydroxide.
Fig. 2 is the particle size distribution figure of embodiment 2 the finished product magnesium hydroxide.
Fig. 3 is the particle size distribution figure of embodiment 3 the finished product magnesium hydroxide.
Fig. 4 is the particle size distribution figure of embodiment 4 the finished product magnesium hydroxide.
Embodiment
Below will the present invention is further described by embodiment and accompanying drawing.
Embodiment 1
1) prepare magnesium ion solution: be that 5:1 measures bischofite, magnesium sulfate heptahydrate deionized water dissolving, filtration by the mol ratio of chlorion and sulfate ion, configuration concentration is the magnesium ion solution of 1mol/L;
2) by magnesium ion solution at stirring intensity be 350r/min condition under be warming up to 60 DEG C;
3) at above temperature and stirring intensity condition, continue to pass into ammonia, the flow passing into ammonia is 200mL/min, to NH
4 +with Mg
2+mol ratio be 2:1, carry out building-up reactions;
4) ageing 80min at above temperature and stirring intensity condition, obtains Mg (OH)
2slip;
5) Mg (OH) is filtered with Büchner funnel vacuum filtration
2slip obtains filter cake, with deionized water wash filter cake to without chlorion, and under 110 DEG C of conditions dry 6h, obtain the magnesium hydroxide products of Large stone low surface area.Finally record Mg (OH)
2pulp density is 3.14%, magnesium yield 66.21%, magnesium hydroxide purity 95.38%.The particle size distribution figure of the finished product is shown in Fig. 1, and size distribution is D
50=50.34 μm, D
90=77.56 μm.
Embodiment 2
1) prepare magnesium ion solution: be that 10:1 measures bischofite, magnesium sulfate heptahydrate deionized water dissolving, filtration by the mol ratio of chlorion and sulfate ion, configuration concentration is the magnesium ion solution of 2.5mol/L;
2) by magnesium ion solution at stirring intensity be 350r/min condition under be warming up to 80 DEG C;
3) at above temperature and stirring intensity condition, continue to pass into ammonia, the flow passing into ammonia is 500mL/min, to NH
4 +with Mg
2+mol ratio be 3:1, carry out building-up reactions;
4) ageing 60min at above temperature and stirring intensity condition, obtains Mg (OH)
2slip;
5) Mg (OH) is filtered with Büchner funnel vacuum filtration
2slip obtains filter cake, with deionized water wash filter cake to without chlorion, and under 110 DEG C of conditions dry 6h, obtain the magnesium hydroxide products of Large stone low surface area.Finally record Mg (OH)
2pulp density is 8.78%, magnesium yield 79.56%, magnesium hydroxide purity 95.89%.The particle size distribution figure of the finished product is shown in Fig. 2, and size distribution is D
50=31.78 μm, D
90=46.59 μm.
Embodiment 3
1) prepare magnesium ion solution: be that 0.5:1 measures bischofite, magnesium sulfate heptahydrate deionized water dissolving, filtration by the mol ratio of chlorion and sulfate ion, configuration concentration is the magnesium ion solution of 0.5mol/L;
2) by magnesium ion solution at stirring intensity be 450r/min condition under be warming up to 70 DEG C;
3) at above temperature and stirring intensity condition, continue to pass into ammonia, the flow passing into ammonia is 500mL/min, to NH
4 +with Mg
2+mol ratio be 3:1, carry out building-up reactions;
4) ageing 70min at above temperature and stirring intensity condition, obtains Mg (OH)
2slip;
5) Mg (OH) is filtered with Büchner funnel vacuum filtration
2slip obtains filter cake, with deionized water wash filter cake to without chlorion, and under 110 DEG C of conditions dry 6h, obtain the magnesium hydroxide products of Large stone low surface area.Finally record Mg (OH)
2pulp density is 1.89%, magnesium yield 77.56%, magnesium hydroxide purity 95.91%.The particle size distribution figure of the finished product is shown in Fig. 3, and size distribution is D
50=23.93 μm, D
90=37.57 μm.
Embodiment 4
1) prepare magnesium ion solution: be that 2:1 measures bischofite, magnesium sulfate heptahydrate deionized water dissolving, filtration by the mol ratio of chlorion and sulfate ion, configuration concentration is the magnesium ion solution of 2.5mol/L;
2) by magnesium ion solution at stirring intensity be 350r/min condition under be warming up to 70 DEG C;
3) at above temperature and stirring intensity condition, continue to pass into ammonia, the flow passing into ammonia is 500mL/min, to NH
4 +with Mg
2+mol ratio be 2:1, carry out building-up reactions;
4) ageing 70min at above temperature and stirring intensity condition, obtains Mg (OH)
2slip;
5) Mg (OH) is filtered with Büchner funnel vacuum filtration
2slip obtains filter cake, with deionized water wash filter cake to without chlorion, and under 110 DEG C of conditions dry 6h, obtain the magnesium hydroxide products of Large stone low surface area.Finally record Mg (OH)
2pulp density is 7.08%, magnesium yield 66.29%, magnesium hydroxide purity 95.21%.The particle size distribution figure of the finished product is shown in Fig. 4, and size distribution is D
50=34.02 μm, D
90=49.67 μm.
Analyze above each figure, the magnesium hydroxide obtaining Large stone low surface area in above four embodiment condition and ranges can be seen, and Particle dispersity is good, the XRD diffraction peak of product is consistent with the PDF2-2003 No.84-2164 magnesium hydroxide standard spectrogram that joint committee (ICDD) is issued, and product is high purity magnesium hydroxide.
Claims (4)
1. a preparation method for magnesium hydroxide, is characterized in that, comprises the following steps:
1) magnesium ion solution is prepared;
2) by magnesium ion solution at stirring intensity be 350-450r/min condition under be warming up to 60-80 DEG C;
3) at above temperature and stirring intensity condition, continue to pass into ammonia, the flow passing into ammonia is 200-500mL/min, and the mol ratio to ammonium ion and magnesium ion is 2:1-3:1, reacts;
4) ageing 60-80min at above temperature and stirring intensity condition, obtains Mg (OH)
2slip;
5) Mg (OH) is filtered
2slip obtains magnesium hydroxide products.
2. preparation method according to claim 1, it is characterized in that, described step 1) for bischofite, magnesium sulfate heptahydrate are used deionized water dissolving, filtration respectively, configuration concentration is the magnesium ion solution of 0.5-2.5mol/L, wherein, the mol ratio of chlorion and sulfate ion is 0.5-10.
3. preparation method according to claim 1, is characterized in that, described step 5) also comprise with deionized water wash filter cake to without chlorion and sulfate ion, and under 110 DEG C of conditions dry 6h, obtain magnesium hydroxide products.
4. preparation method according to claim 3, is characterized in that, described in be filtered into Büchner funnel vacuum filtration.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410722681.2A CN104445302A (en) | 2014-12-02 | 2014-12-02 | Method for preparing magnesium hydrate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410722681.2A CN104445302A (en) | 2014-12-02 | 2014-12-02 | Method for preparing magnesium hydrate |
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| CN104445302A true CN104445302A (en) | 2015-03-25 |
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| CN201410722681.2A Pending CN104445302A (en) | 2014-12-02 | 2014-12-02 | Method for preparing magnesium hydrate |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110203951A (en) * | 2019-06-26 | 2019-09-06 | 青海盐湖工业股份有限公司 | A kind of preparation method of magnesium hydroxide with coproduction dichloride hexamine nickel |
| CN111268706A (en) * | 2020-03-30 | 2020-06-12 | 西部矿业股份有限公司 | Method for producing high-purity magnesium hydroxide, high-purity magnesium oxide and high-purity magnesite serial magnesium products by using salt lake brine |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102849761A (en) * | 2012-09-30 | 2013-01-02 | 河北工业大学 | Preparation method of magnesium hydrate |
-
2014
- 2014-12-02 CN CN201410722681.2A patent/CN104445302A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102849761A (en) * | 2012-09-30 | 2013-01-02 | 河北工业大学 | Preparation method of magnesium hydrate |
Non-Patent Citations (4)
| Title |
|---|
| 姚建平等: "氨状态对氨法制备氢氧化镁颗粒性质的影响", 《化工学报》 * |
| 宋雪雪等: "氨气法制备氢氧化镁工艺研究", 《化学工程》 * |
| 柴多里等: "沉淀法制备氢氧化镁及其对砷溶液的吸附特性", 《硅酸盐学报》 * |
| 范天博等: "氯化镁溶液氨气鼓泡反应制备纳米氢氧化镁", 《化工学报》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110203951A (en) * | 2019-06-26 | 2019-09-06 | 青海盐湖工业股份有限公司 | A kind of preparation method of magnesium hydroxide with coproduction dichloride hexamine nickel |
| CN110203951B (en) * | 2019-06-26 | 2021-08-31 | 青海盐湖工业股份有限公司 | Preparation method for magnesium hydroxide and coproduction of nickel hexammine dichloride |
| CN111268706A (en) * | 2020-03-30 | 2020-06-12 | 西部矿业股份有限公司 | Method for producing high-purity magnesium hydroxide, high-purity magnesium oxide and high-purity magnesite serial magnesium products by using salt lake brine |
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Application publication date: 20150325 |
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