CN104495883A - Preparation method of magnesium hydrate with high-concentration slurry - Google Patents
Preparation method of magnesium hydrate with high-concentration slurry Download PDFInfo
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- CN104495883A CN104495883A CN201410722751.4A CN201410722751A CN104495883A CN 104495883 A CN104495883 A CN 104495883A CN 201410722751 A CN201410722751 A CN 201410722751A CN 104495883 A CN104495883 A CN 104495883A
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- magnesium
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- magnesium hydroxide
- chloride solution
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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
- C01F5/20—Magnesium hydroxide by precipitation from solutions of magnesium salts with ammonia
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- Inorganic Chemistry (AREA)
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Abstract
The invention discloses a preparation method of magnesium hydrate with high-concentration slurry. The method comprises the following steps: 1) preparing a magnesium hydrate solution; 2) heating the magnesium hydrate solution to 60-80 DEG C under the stirring strength of 250-350r/min; 3) continuously introducing ammonia gas at the flow of 300-500mL/min at 60-80 DEG C under the stirring strength of 250-350r/min until the molar ratio of NH4<+> to Mg<2+> is (2:1) to (3:1), and reacting; 4) aging at 60-80 DEG C under the stirring strength of 250-350r/min for 100-180min, so as to obtain Mg(OH)2 slurry; and 5) filtering the Mg(OH)2 slurry to obtain a flake magnesium hydroxide product. The high-concentration magnesium hydrate slurry is prepared by the method disclosed by the invention; and high-purity and high-quality magnesium hydrate 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 the magnesium hydroxide of high concentration ground paste.
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.And the pulp density that the existing technique with bischofite being magnesium hydroxide prepared by raw material obtains is lower, and pulp density is up to 7%-9%, and the productivity of unit equipment is low.
Summary of the invention
The invention provides and a kind ofly prepare the magnesium hydroxide technique with high concentration ground paste, improve the preparation efficiency of magnesium hydroxide and obtain the magnesium hydroxide products of high-quality.
For reaching the object of the invention, this preparation method with the magnesium hydroxide of high concentration ground paste, is characterized in that, comprise the following steps:
1) magnesium chloride solution is prepared;
2) by magnesium chloride solution at stirring intensity be 250-350r/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 300-500mL/min, to NH
4 +with Mg
2+mol ratio be 2:1-3:1, react;
4) ageing 100-180min at above temperature and stirring intensity condition, obtains Mg (OH)
2slip;
5) Mg (OH) is filtered
2slip obtains hydroxide flake magnesium products.
Wherein, step 1) be by bischofite deionized water dissolving, filtration, configuration concentration is the magnesium chloride solution of 3.0-4.4mol/L.
Preferably, step 5) also comprise with deionized water wash filter cake to without chlorion, and under 110 DEG C of conditions dry 6h, obtain magnesium hydroxide products.
Wherein, Büchner funnel vacuum filtration is filtered into.
Method provided by the invention prepares high density magnesium hydroxide slurry and finally prepares high purity, high-quality magnesium hydroxide.
Accompanying drawing explanation
Fig. 1 is the particle size distribution figure of embodiment 1 the finished product magnesium hydroxide.
Fig. 2 is the SEM figure of embodiment 1 the finished product magnesium hydroxide.
Fig. 3 is the XRD figure of embodiment 1 the finished product magnesium hydroxide.
Fig. 4 is the particle size distribution figure of embodiment 2 the finished product magnesium hydroxide.
Fig. 5 is the SEM figure of embodiment 2 the finished product magnesium hydroxide.
Fig. 6 is the XRD figure of embodiment 2 the finished product magnesium hydroxide.
Fig. 7 is the particle size distribution figure of embodiment 3 the finished product magnesium hydroxide.
Fig. 8 is the SEM figure of embodiment 3 the finished product magnesium hydroxide.
Fig. 9 is the XRD figure of embodiment 3 the finished product magnesium hydroxide.
Figure 10 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) magnesium chloride solution is prepared: by bischofite deionized water dissolving, filtration, configuration concentration is the magnesium chloride solution of 4.4mol/L;
2) by magnesium chloride 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 300mL/min, to NH
4 +with Mg
2+mol ratio be 3:1, carry out building-up reactions;
4) ageing 100min 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 hydroxide flake magnesium products.Finally record Mg (OH)
2pulp density is 14.77%, magnesium yield 82.71%, magnesium hydroxide purity 99.75%.Particle size distribution figure, the SEM figure of the finished product and XRD figure are shown in Fig. 1 to Fig. 3, and wherein showing size distribution in Fig. 1 is D
50=1.38 μm, D
90=2.53 μm.
Embodiment 2
1) magnesium chloride solution is prepared: by bischofite deionized water dissolving, filtration, configuration concentration is the magnesium chloride solution of 4.0mol/L;
2) by magnesium chloride solution at stirring intensity be 250r/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 400mL/min, to NH
4 +with Mg
2+mol ratio be 2:1, carry out building-up reactions;
4) ageing 100min 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 hydroxide flake magnesium products.Finally record Mg (OH)
2pulp density is 11.99%, magnesium yield 69.65%, magnesium hydroxide purity 99.23%.Particle size distribution figure, the SEM figure of the finished product and XRD figure are shown in Fig. 4 to Fig. 6, and wherein showing size distribution in Fig. 4 is D
50=2.88 μm, D
90=6.04 μm.
Embodiment 3
1) magnesium chloride solution is prepared: by bischofite deionized water dissolving, filtration, configuration concentration is the magnesium chloride solution of 4.0mol/L;
2) by magnesium chloride 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 500mL/min, to NH
4 +with Mg
2+mol ratio be 3:1, carry out building-up reactions;
4) ageing 180min 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 hydroxide flake magnesium products.Finally record Mg (OH)
2pulp density is 13.82%, magnesium yield 81.55%, magnesium hydroxide purity 99.53%.Particle size distribution figure, the SEM figure of the finished product and XRD figure are shown in Fig. 7 to Fig. 9, and wherein showing size distribution in Fig. 7 is D
50=4.13 μm, D
90=7.88 μm.
Embodiment 4
1) magnesium chloride solution is prepared: by bischofite deionized water dissolving, filtration, configuration concentration is the magnesium chloride solution of 3.0mol/L;
2) by magnesium chloride 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 2:1, carry out building-up reactions;
4) ageing 180min 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 hydroxide flake magnesium products.Finally record Mg (OH)
2pulp density is 9.03%, magnesium yield 67.95%, magnesium hydroxide purity 98.89%.The particle size distribution figure of the finished product is shown in Figure 10, and size distribution is D
50=9.87 μm, D
90=38.56 μm.
Analyze above each figure, can see that the magnesium hydroxide form obtained in above four embodiment condition and ranges is sheet, centralized particle diameter, good uniformity, and 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, product is high purity magnesium hydroxide.
Claims (4)
1. there is a preparation method for the magnesium hydroxide of high concentration ground paste, it is characterized in that, comprise the following steps:
1) magnesium chloride solution is prepared;
2) by magnesium chloride solution at stirring intensity be 250-350r/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 300-500mL/min, to NH
4 +with Mg
2+mol ratio be 2:1-3:1, react;
4) ageing 100-180min at above temperature and stirring intensity condition, obtains Mg (OH)
2slip;
5) Mg (OH) is filtered
2slip obtains hydroxide flake magnesium products.
2. preparation method according to claim 1, is characterized in that, described step 1) be by bischofite deionized water dissolving, filtration, configuration concentration is the magnesium chloride solution of 3.0-4.4mol/L.
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 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.
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| CN201410722751.4A CN104495883A (en) | 2014-12-02 | 2014-12-02 | Preparation method of magnesium hydrate with high-concentration slurry |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110078101A (en) * | 2019-05-30 | 2019-08-02 | 福建农林大学 | A kind of preparation and application of anti-tealeaves fungal disease nano-sized magnesium hydroxide |
| CN110980780A (en) * | 2019-12-21 | 2020-04-10 | 聊城大学 | Preparation method of flaky magnesium hydroxide flame retardant |
| CN112897559A (en) * | 2021-02-26 | 2021-06-04 | 绵阳远达电子材料有限公司 | Production process of magnesium hydroxide |
| RU2801733C1 (en) * | 2023-03-15 | 2023-08-15 | Общество с ограниченной ответственностью "ИРКУТСКАЯ НЕФТЯНАЯ КОМПАНИЯ" | Method for extraction of magnesium hydroxide from polycomponent hydromineral raw |
| WO2024191320A1 (en) * | 2023-03-15 | 2024-09-19 | Общество с ограниченной ответственностью "ИРКУТСКАЯ НЕФТЯНАЯ КОМПАНИЯ" | Method for extracting magnesium hydroxide from a multi-component naturally occuring mineral solutions |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1542036A (en) * | 2003-11-04 | 2004-11-03 | 上海大学 | Method for manufacturing nanometer magnesium hydroxide fire retardant |
| CN1718542A (en) * | 2004-07-09 | 2006-01-11 | 华东理工大学 | Preparation method of high purity nano-magnesium hydroxide |
| CN101054190A (en) * | 2007-04-25 | 2007-10-17 | 中国日用化学工业研究院 | Method of preparing surface modified nano magnesium hydroxide |
| CN101700899A (en) * | 2009-10-28 | 2010-05-05 | 钟辉 | Technology for producing and preparing high-purity lamellar magnesium hydroxide |
| CN101723417A (en) * | 2009-12-23 | 2010-06-09 | 沈阳化工学院 | Process for preparing high dispersivity square blocky superfine magnesium hydroxide by one-step method |
| CN103130252A (en) * | 2011-12-01 | 2013-06-05 | 孟宪清 | Fire retardant preparation method |
-
2014
- 2014-12-02 CN CN201410722751.4A patent/CN104495883A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1542036A (en) * | 2003-11-04 | 2004-11-03 | 上海大学 | Method for manufacturing nanometer magnesium hydroxide fire retardant |
| CN1718542A (en) * | 2004-07-09 | 2006-01-11 | 华东理工大学 | Preparation method of high purity nano-magnesium hydroxide |
| CN101054190A (en) * | 2007-04-25 | 2007-10-17 | 中国日用化学工业研究院 | Method of preparing surface modified nano magnesium hydroxide |
| CN101700899A (en) * | 2009-10-28 | 2010-05-05 | 钟辉 | Technology for producing and preparing high-purity lamellar magnesium hydroxide |
| CN101723417A (en) * | 2009-12-23 | 2010-06-09 | 沈阳化工学院 | Process for preparing high dispersivity square blocky superfine magnesium hydroxide by one-step method |
| CN103130252A (en) * | 2011-12-01 | 2013-06-05 | 孟宪清 | Fire retardant preparation method |
Non-Patent Citations (1)
| Title |
|---|
| 宋雪雪等: ""氨气法制备氢氧化镁工艺研究"", 《化学工程》 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110078101A (en) * | 2019-05-30 | 2019-08-02 | 福建农林大学 | A kind of preparation and application of anti-tealeaves fungal disease nano-sized magnesium hydroxide |
| CN110078101B (en) * | 2019-05-30 | 2022-02-01 | 福建农林大学 | Preparation and application of tea fungus disease resistant nano magnesium hydroxide |
| CN110980780A (en) * | 2019-12-21 | 2020-04-10 | 聊城大学 | Preparation method of flaky magnesium hydroxide flame retardant |
| CN110980780B (en) * | 2019-12-21 | 2022-06-07 | 聊城大学 | Preparation method of flaky magnesium hydroxide flame retardant |
| CN112897559A (en) * | 2021-02-26 | 2021-06-04 | 绵阳远达电子材料有限公司 | Production process of magnesium hydroxide |
| RU2801733C1 (en) * | 2023-03-15 | 2023-08-15 | Общество с ограниченной ответственностью "ИРКУТСКАЯ НЕФТЯНАЯ КОМПАНИЯ" | Method for extraction of magnesium hydroxide from polycomponent hydromineral raw |
| WO2024191320A1 (en) * | 2023-03-15 | 2024-09-19 | Общество с ограниченной ответственностью "ИРКУТСКАЯ НЕФТЯНАЯ КОМПАНИЯ" | Method for extracting magnesium hydroxide from a multi-component naturally occuring mineral solutions |
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Application publication date: 20150408 |
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