CN101905896B - Method for preparing magnesium hydroxide from brucite ore - Google Patents
Method for preparing magnesium hydroxide from brucite ore Download PDFInfo
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- CN101905896B CN101905896B CN2009100849741A CN200910084974A CN101905896B CN 101905896 B CN101905896 B CN 101905896B CN 2009100849741 A CN2009100849741 A CN 2009100849741A CN 200910084974 A CN200910084974 A CN 200910084974A CN 101905896 B CN101905896 B CN 101905896B
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- marinco
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- brucite
- magnesium hydroxide
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Abstract
The invention provides a method for preparing magnesium hydroxide from brucite ore, which comprises the following steps of: mixing the brucite ore and water in a weight ratio of 1-60:100, and pre-breaking the obtained mixture; and stirring the pre-broken product at the temperature of between 100 and 400 DEG C and under the pressure of between 0.1 and 30MPa for 0.5 to 240 hours. The magnesium hydroxide prepared by the method has high purity, small and uniform grains, and is suitable to be used as a flame retardant of organic polymer materials. Besides, only the brucite ore is used in the reaction process, other chemical raw materials are not used in the method, so the reaction product can be directly dried to form the pure product; therefore, the water resource used for cleaning is greatly saved, the environment is protected, and the method is a clean method for preparing superfine magnesium hydroxide.
Description
Technical field
The present invention relates to a kind of method for preparing Marinco H by brucite mineral.
Background technology
The fast development of Polymer Synthesizing polymer industry; Great promoter action has been played in application and update to building materials, packing, electric appliance and electronic product, product for agriculture, auto parts machinery, defence and military material, aerospace material, medical material etc., and the Application Areas of Polymer Synthesizing polymkeric substance has been penetrated into the every field of national economy.Except satisfying domestic needs, the exported product that China is main has all used the Polymer Synthesizing polymer materials in large quantities like various electrical equipment, electric wire, toy, synthetic textile etc.
Be accompanied by the progress of development of science and technology and society, international community also constantly promotes environment and the healthy level that requires, with the negative impact of reply rapid economic development to ecotope and human health.In European Union's " ROHS ", clearly stipulate to rise on July 1st, 2006 use of completely forbidding PBB (PBBs) and PBDE bromide fire retardants such as (polybromodiphenyl ether).The fire retardant that plastic fittings on the products such as the present just China of above-mentioned many bromine flame retardants outlet household electrical appliance, IT and signal equipment and printed substrate etc. adopt.
Two kinds of inorganic combustion inhibitors that generally use in the world at present are Marinco H and white lake, and that Marinco H has is lower than white lake material cost, tolerable temperature is high, the better advantage of various physicals, therefore more receives user's favor.The magnesium hydrate powder material be inorganic, press down cigarette, nontoxic fire retardant, widespread use in the high polymeric fire-retardant field is applicable to the fire-retardant of macromolecular materials such as Vestolen PP 7052, Vilaterm, SE, terpolymer EP rubber and unsaturated polyester and presses down cigarette.
The chemical process of preparation Marinco H mainly contains vapor phase process, metal alkoxide method and direct precipitation method etc.Vapor phase process is few to equipment and technical requirements height and output; Metal alkoxide method raw materials cost is high, complex process; Direct precipitation method is easy and simple to handle, and raw material is easy to get, and production cost is low, and product purity is high, is a kind of industrialized compound method that is easy to.At present, when producing high purity magnesium hydroxide, adopt direct precipitation method both at home and abroad mostly.
Comparing with chemical method, benefit from the natural brucite ore deposit of a large amount of storages of China, is the another kind of method that obtains magnesium hydrate powder to the brucite mineral dry ground.Compare with chemical method, the Marinco H purity that this method obtains receives the brucite mineral purity tolerances, and product purity is low, and is with low cost.But because the physical properties of Marinco H, the fineness of pulverizing is restricted, and generally can only be crushed to 1250 orders, adopt special methods also can only accomplish 5000 orders, and size-grade distribution is wide.The particle crystalline form that under Electronic Speculum, can be observed dry ground is sharp-pointed, makes the coating modification effect bad.
Summary of the invention
The objective of the invention is to overcome in the prior art that the product purity that the method for using brucite mineral to prepare Marinco H obtains is low, granularity is big and the uneven shortcoming of granularity, provide that a kind of product purity is high, granularity is little and the even-grained method that is prepared Marinco H by brucite mineral.
The invention provides and a kind ofly prepare the method for Marinco H by brucite mineral, wherein, this method comprises: with brucite mineral and water by weight 1-60: 100 mix, and then the gained mixture are carried out precomminution; Is that 100-400 ℃, pressure are to stir 0.5-240 hour under the 0.1-30MPa with the product after the precomminution in temperature.
Contriver of the present invention is surprised to find that: though most metal oxyhydroxide is insoluble in water; Its solubility product constant is very little; But through regulating and controlling temperature, pressure, the water yield and means such as filter; Still can realize the conversion from the brucite mineral to the super fine magnesium hydroxide, remove partial impurities simultaneously, thereby obtain the higher super fine magnesium hydroxide of purity.This mainly is because Mg (OH)
2In water, still have certain solubleness, and solubleness can access further increase under the HTHP.
Not only purity is high to use the Marinco H that method of the present invention makes, and granularity is little and even, is suitable for the fire retardant as the organic high molecular polymer material.In addition, because method of the present invention has only been used brucite mineral in reaction process, do not use other industrial chemicals; Reaction product can directly be carried out drying and obtained pure product; Having practiced thrift the water resources that is used to clean greatly, protected environment, is a kind of clean method for preparing of super fine magnesium hydroxide.
Description of drawings
X-ray diffraction (XRD) figure of the Marinco H that Fig. 1 makes for embodiment 1.
Embodiment
The method for preparing Marinco H by brucite mineral provided by the invention comprises: with brucite mineral and water by weight 1-60: 100 mix, and then the gained mixture are carried out precomminution; Is that 100-400 ℃, pressure are to stir 0.5-240 hour under the 0.1-30MPa with the product after the precomminution in temperature.
According to method provided by the invention, wherein,, can use through the brucite mineral after the dry ground processing of various degree in order to make the Marinco H particle diameter that makes littler.Under the preferable case, the granularity of said brucite mineral can be 100-5000 order, more preferably 500-5000 order.Wherein, the equipment of said dry ground and method are conventionally known to one of skill in the art, repeat no more here.
The staple of said brucite mineral is a Marinco H, and its content can be 90-97 weight %, is preferably 95-97 weight %; All the other components are generally FeO, Fe
2O
3, SiO
2, Al
2O
3And CaO.
According to method provided by the invention, wherein, the weight ratio when brucite mineral is mixed with water is preferably 2-50: 100, and 5-40 more preferably: 100.
According to method provided by the invention, wherein, the mode of said precomminution can be a various water mill grinding mode of the prior art, for example, can use colloidal mill, ball mill or high dispersive stirrer to carry out precomminution.Under the preferable case, more even in order to make pulverizing, use colloidal mill to pulverize, the rotating speed of said colloidal mill can be 500-10000 rev/min, is preferably 1000-8000 rev/min, the time of pulverizing can be 5-120 minute, is preferably 5-60 minute.
According to method provided by the invention, under the preferable case, the granularity in the water in products magnesite ore deposit after the said precomminution can be 1000-8000 order, more preferably 5000-8000 order.
According to method provided by the invention, wherein, the temperature of said stirring is preferably 150-350 ℃, and the pressure of stirring is preferably 0.4-17MPa, and the time of stirring is preferably 1-180 hour.Under this preferred whipping temp, pressure and churning time, the Marinco H granularity that makes is littler, and practices thrift the energy consumption of preparation.The speed of said stirring can be 100-5000 rev/min, is preferably 1000-4000 rev/min.
According to method provided by the invention, wherein, in order to obtain more purified magnesium hydroxide products, this method can also comprise filters the product that obtains after stirring, and with solid drying, said exsiccant temperature can be 50-100 ℃, is preferably 60-90 ℃.
Below, will be described in more detail the present invention through embodiment.
Embodiment 1
Present embodiment is used to explain the method that is prepared Marinco H by brucite mineral provided by the invention.
The staple of the brucite mineral that uses is: Mg (OH)
296.47 weight %, CaO 0.45 weight %, Fe
2O
30.48 weight %, Al
2O
30.14 weight %, SiO
22.26 weight %.
With the above-mentioned brucite mineral of 5000 purposes and deionized water by weight the mixed that is 20: 100; With colloidal mill (Hangtian Xinguang Super Microcrushing Machinery Co., Ltd., Shenyang; The JTM51AB type) pulverized 30 minutes with 3000 rev/mins speed, then the product that obtains is all joined in the reaction kettle.Under agitation condition, be warming up to 350 ℃ in still, reaction is 32 hours under the pressure of 17MPa, and the product that obtains is filtered the back 70 ℃ of dryings 8 hours, and the Marinco H that obtains note is made A1.
Embodiment 2
Present embodiment is used to explain the method that is prepared Marinco H by brucite mineral provided by the invention.
The staple of the brucite mineral that uses is: Mg (OH)
296.47 weight %, CaO 0.45 weight %, Fe
2O
30.48 weight %, Al
2O
30.14 weight %, SiO
22.26 weight %.
With the above-mentioned brucite mineral of 2000 purposes and deionized water by weight the mixed that is 10: 100; With colloidal mill (Hangtian Xinguang Super Microcrushing Machinery Co., Ltd., Shenyang; The JTM51AB type) pulverized 100 minutes with 2000 rev/mins speed, then the product that obtains is all joined in the reaction kettle.Under agitation condition, be warming up to 150 ℃ in still, reaction is 180 hours under the pressure of 0.5MPa, and the product that obtains is filtered the back 90 ℃ of dryings 6 hours, and the Marinco H that obtains note is made A2.
Embodiment 3
Present embodiment is used to explain the method that is prepared Marinco H by brucite mineral provided by the invention.
The staple of the brucite mineral that uses is: Mg (OH)
296.47 weight %, CaO 0.45 weight %, Fe
2O
30.48 weight %, Al
2O
30.14 weight %, SiO
22.26 weight %.
With the above-mentioned brucite mineral of 500 purposes and deionized water by weight the mixed that is 30: 100; With colloidal mill (Hangtian Xinguang Super Microcrushing Machinery Co., Ltd., Shenyang; The JTM51AB type) pulverized 10 minutes with 8000 rev/mins speed, then the product that obtains is all joined in the reaction kettle.Under agitation condition, be warming up to 300 ℃ in still, reaction is 6 hours under the pressure of 8.7MPa, and the product that obtains is filtered the back 90 ℃ of dryings 6 hours, and the Marinco H that obtains note is made A3.
Embodiment 4
Present embodiment is used to explain the method that is prepared Marinco H by brucite mineral provided by the invention.
The staple of the brucite mineral that uses is: Mg (OH)
296.47 weight %, CaO 0.45 weight %, Fe
2O
30.48 weight %, Al
2O
30.14 weight %, SiO
22.26 weight %.
With the above-mentioned brucite mineral of 1000 purposes and deionized water by weight the mixed that is 25: 100; With colloidal mill (Hangtian Xinguang Super Microcrushing Machinery Co., Ltd., Shenyang; The JTM51AB type) pulverized 20 minutes with 5000 rev/mins speed, then the product that obtains is all joined in the reaction kettle.Under agitation condition, be warming up to 200 ℃ in still, reaction is 150 hours under the pressure of 1.6MPa, and the product that obtains is filtered the back 60 ℃ of dryings 12 hours, and the Marinco H that obtains note is made A4.
Products measure
(1) XRD test
The Marinco H that the XRD-6000 type X-ray powder diffraction appearance of employing day island proper Tianjin company makes embodiment 1 carries out crystalline structure and characterizes.Fig. 1 is the XRD figure of the Marinco H that makes of embodiment 1, and as can be seen from the figure, each characteristic diffraction peak peak shape point of reflection Marinco H structure is alarmmed, and baseline is low flat, and the inclusion-free peak occurs, and the interpret sample crystalline phase is single.
(2) constituent content analysis
Adopt in the Marinco H that day island proper Tianjin ICPS-7500 type elemental analyser makes embodiment 1-4 magnesium element content to analyze, and the content through this cubage Marinco H.The result lists in table 1.
(3) sreen analysis
Employing Ma Erwen Mastsizer-2000 type particle size analyzer is analyzed the granularity of the Marinco H that embodiment 1-4 makes.The result lists in table 1.
Table 1
| Numbering | A1 | A2 | A3 | A4 |
| Content/weight the % of magnesium elements | 41.14 | 40.65 | 41.09 | 41.00 |
| Content/weight the % of Marinco H | 99.42 | 98.24 | 99.30 | 99.08 |
| Average particulate diameter/μ m | 0.11 | 2.35 | 0.96 | 1.48 |
| Particle diameter is the particulate content/weight % of MV ± 5% | 95 | 89 | 94 | 90 |
Can find out that through the data in the table 1 not only purity is high to use the magnesium hydroxide particle that method of the present invention makes, and grain diameter is little, is evenly distributed.In addition, because method of the present invention has only been used brucite mineral in reaction process, do not use other industrial chemicals; Reaction product can directly be carried out drying and obtained pure product; Having practiced thrift the water resources that is used to clean greatly, protected environment, is a kind of clean method for preparing of super fine magnesium hydroxide.
Claims (7)
1. method for preparing Marinco H by brucite mineral; It is characterized in that; This method comprises: with brucite mineral and water by weight 1-60: 100 mix; The content of Marinco H is 90-97 weight % in the said brucite mineral, and granularity is the 100-5000 order, then the gained mixture is carried out precomminution; Is that 100-400 ℃, pressure are to stir 0.5-240 hour under the 0.1-30MPa with the product after the precomminution in temperature, and the granularity in the water in products magnesite ore deposit after the said precomminution is the 1000-8000 order.
2. method according to claim 1, wherein, the weight ratio of said brucite mineral and water is 2-40: 100.
3. method according to claim 1, wherein, said precomminution is carried out in colloidal mill, ball mill or high dispersive stirrer.
4. method according to claim 3, wherein, said precomminution is carried out in colloidal mill, and the rotating speed of colloidal mill is 500-10000 rev/min, and the pulverizing time is 5-120 minute.
5. method according to claim 1, wherein, the temperature of said stirring is 150-350 ℃, the time of stirring is 1-180 hour.
6. according to claim 1 or 5 described methods, wherein, the speed of said stirring is 100-5000 rev/min.
7. according to any described method in the claim 1,2 and 5, wherein, this method also comprises filters the product after stirring, and with solid drying, said exsiccant temperature is 50-100 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009100849741A CN101905896B (en) | 2009-06-05 | 2009-06-05 | Method for preparing magnesium hydroxide from brucite ore |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009100849741A CN101905896B (en) | 2009-06-05 | 2009-06-05 | Method for preparing magnesium hydroxide from brucite ore |
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| Publication Number | Publication Date |
|---|---|
| CN101905896A CN101905896A (en) | 2010-12-08 |
| CN101905896B true CN101905896B (en) | 2012-04-25 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2009100849741A Expired - Fee Related CN101905896B (en) | 2009-06-05 | 2009-06-05 | Method for preparing magnesium hydroxide from brucite ore |
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|---|---|
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1174171A (en) * | 1996-08-12 | 1998-02-25 | 大赛璐网干产业株式会社 | Magnesium hydroxide and method of preparing water suspension |
| CN1557711A (en) * | 2004-02-12 | 2004-12-29 | 大连市中山区鑫阳矿业化工研究所 | Method for preparing brucite or sintered magnesia ultrafine powder by wet method |
-
2009
- 2009-06-05 CN CN2009100849741A patent/CN101905896B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1174171A (en) * | 1996-08-12 | 1998-02-25 | 大赛璐网干产业株式会社 | Magnesium hydroxide and method of preparing water suspension |
| CN1557711A (en) * | 2004-02-12 | 2004-12-29 | 大连市中山区鑫阳矿业化工研究所 | Method for preparing brucite or sintered magnesia ultrafine powder by wet method |
Non-Patent Citations (2)
| Title |
|---|
| JP特开2002-167219A 2002.06.11 |
| 郑水林等.用水镁石制备超细氢氧化镁的研究.《矿冶》.2004,第13卷(第2期),43-46，60. * |
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