CN100372771C - Preparation method of high purity nano-magnesium hydroxide - Google Patents
Preparation method of high purity nano-magnesium hydroxide Download PDFInfo
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- CN100372771C CN100372771C CNB2004100526649A CN200410052664A CN100372771C CN 100372771 C CN100372771 C CN 100372771C CN B2004100526649 A CNB2004100526649 A CN B2004100526649A CN 200410052664 A CN200410052664 A CN 200410052664A CN 100372771 C CN100372771 C CN 100372771C
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Abstract
The present invention discloses a preparation method of high-purity nanometer magnesium hydroxide, which uses hexammoniate magnesium chloride as a precursor, and the hexammoniate magnesium chloride is converted into high-purity nanometer magnesium hydroxide with a liquid phase alkali hydrolyzing method. The research proves that compared with the prior art, the preparation method of the present invention has the superiority in purity, grain diameter and distribution.
Description
Technical field
The present invention relates to a kind of preparation method of high-purity nm magnesium hydroxide.
Background technology
China is magnesium resource big country, and western salt lake magnesium resource is particularly abundant, mainly with bischofite (MgCl
26H
2O) form exists, and cost is very cheap.China's magnesium resource utilization is in lower level, mainly is with MgCl
26H
2The direct export of O form causes the waste of resource.Accelerate the research and development that high-purity, super fine magnesium hydroxide etc. has high added value magnesium series product and become the task of top priority.
Magnesium hydroxide is a kind of weak base, has resiliency, high adsorption capacity, does not have corrodibility, an advantage such as safe and reliable, nontoxic, is used widely in the environmental protection field at present: as neutralizing acid wastewater, removing and flue gas desulfurization etc. heavy metal.Magnesium hydroxide has decomposition temperature height, Heat stability is good, nontoxic, the smokeless characteristics such as pressing down cigarette that reach, and can be used as the high-performance inorganic fire retardant and is applied in the macromolecular material.Eco-friendly fire retardant magnesium hydroxide has been subjected to various countries' attention, about the focus of studying, activity in production is very active, especially high-purity, ultra-fine magnesium hydroxide flame retardant has become at present exploitation both at home and abroad and studied.
When magnesium hydroxide used as fire retardant, the addition in macromolecular material made the mechanical property of materials generally greater than 40%, particularly all remarkable deterioration of resistance to impact shock and elongation.One of solution to this problem is that magnesium hydroxide is carried out the ultra micro granulation.Nano-sized magnesium hydroxide uses as fire retardant has two big advantages: the one, when addition one regularly, particle diameter reduces, filling properties and dispersing property between itself and the superpolymer improve, thereby reduction is to the machinery of goods, the influence of physicals; The 2nd, because particle diameter reduces, specific surface area increases, and caloric receptivity rises, thereby has improved the flame retardant properties of material.The preparation nano-sized magnesium hydroxide can make its dispersiveness and consistency in rubber-plastics material improve greatly, and the influence of Drawing abillity and mechanical mechanics property is greatly reduced.
High-purity nano magnesia all has been widely used on pottery, enamel, medical science and aeronautical material.Matrix material such as high-purity nano magnesia and superpolymer has good microwave absorption coefficient, not only can be used as the compaction material of makeup, paint, face powder, and can be used as polish of fat-splitting agent or pharmaceuticals etc.
At present domestic and international superfine Mg (OH)
2The powder existing procucts are sold, but still exist many problems,, purity not high (90～95%) big as physics method products made thereby particle diameter, the ordinary chemical method products made thereby is reunited seriously, size distribution is inhomogeneous etc., and there are shortcomings such as equipment requirements height, complicated operation in sluggish precipitation and hydrothermal method etc.
Summary of the invention
The technical issues that need to address of the present invention are: the magnesium hydroxide particle of preparing purity height, particle diameter thin (less than 100 nanometers).
Technical scheme:
The preparation method of the said high-purity nm magnesium hydroxide of the present invention is characterized in that, with magnesium chloride hex-ammoniate (MgCl
26NH
3) be precursor, adopt liquid phase alkaline hydrolysis method to make magnesium chloride hex-ammoniate change into the high-purity nm magnesium hydroxide,
Wherein: said liquid phase alkaline hydrolysis method is: alkalitropism is better than and adds the magnesium chloride hex-ammoniate solid particulate in the dilute alkaline soln of ammoniacal liquor and carry out alkaline hydrolysis, after ageing, add dispersion agent and carry out surface treatment, the suspension filtered that obtains is washed to chlorion and can not be detected, and the filter cake that obtains obtains the high-purity nm magnesium hydroxide after drying.
Among the present invention: used magnesium chloride hex-ammoniate is by bischofite (MgCl
26H
2O) make with extra care and get, concrete preparation method is referring to ZL 01126495.0.The alkaline hydrolysis temperature of recommending is 10～100 ℃, and the time is 2～5 hours; It is preferred that said alkalescence is better than the dilute alkaline soln of ammoniacal liquor: concentration is sodium hydroxide or the potassium hydroxide solution of 2～25wt.%; Said dispersion agent is advisable with thanomin, trolamine, sodium oleate, sodium stearate, Sodium hexametaphosphate 99, sodium polyphosphate, titanate coupling agent, polyvinyl alcohol or silane coupling agent; Said washing can adopt low-viscosity (mobile) liquids such as water, ethanol, methyl alcohol, benzene or toluene to wash; Preferred drying temperature is 80～180 ℃, and be 2～5 hours time of drying.
The characteristics of maximum of the present invention are: be precursor with the magnesium chloride hex-ammoniate, adopt liquid phase alkaline hydrolysis method to make magnesium chloride hex-ammoniate change into the high-purity nm magnesium hydroxide.Studies have shown that: no matter be or aspect size and the distribution, the present invention all is better than prior art in purity.
Description of drawings
Fig. 1 is the Electronic Speculum figure of example 1 product.Fig. 2 is the Electronic Speculum figure of example 2 products.
Fig. 3 is the Electronic Speculum figure of example 3 products.Fig. 4 is the Electronic Speculum figure of example 4 products.
Embodiment
The invention will be further described below by embodiment, and the cited case does not influence protection scope of the present invention:
Embodiment 1
Under 25 ℃, take by weighing 1000 the gram magnesium chloride hex-ammoniates, under the mechanical stirring condition, join in the 20L10wt.% sodium hydroxide solution that has prepared, fully react 5h after, suspension ageing 12～24h.Add the surface treatment agent sodium oleate in suspension, after continuing to stir 1h,, and can not detect with washing with alcohol to chlorion and to end suspension filtered.The solid of washing was descended dry 3 hours at 120 ℃, obtain the high-purity nm magnesium hydroxide products.Product characterizes through instrumental analysis, reaches high-purity, nano level.Purity check result following (the Electronic Speculum test result is seen Fig. 1):
The purity check result
| Composition | Percentage composition |
| The magnesium hydroxide muriate is (with Cl -Meter) moisture content calcium oxide | 99.7 0.10 0.03 0.05 |
Embodiment 2
Under 30 ℃, take by weighing 1000 the gram magnesium chloride hex-ammoniates, under the clarifixator processing condition, join in the 20L 15wt.% potassium hydroxide solution that has prepared, fully react 3h after, suspension ageing 12～24h.Add the surface treatment agent sodium stearate in suspension, after continuing to stir 2h,, and can not detect with methanol wash to chlorion and to end suspension filtered.The solid of washing was descended dry 2 hours at 150 ℃, obtain the high-purity nm magnesium hydroxide products.Product characterizes through instrumental analysis, reaches high-purity, nano level.Purity check result following (the Electronic Speculum test result is seen Fig. 2):
The purity check result
| Composition | Percentage composition |
| The magnesium hydroxide muriate is (with Cl -Meter) moisture content calcium oxide | 99.8 0.10 0.02 0.04 |
Embodiment 3
Under 50 ℃, take by weighing 1000 the gram magnesium chloride hex-ammoniates, under the clarifixator processing condition, join in the 20L 20wt.% potassium hydroxide solution that has prepared, fully react 2h after, suspension ageing 12～24h.Add the surface treatment agent Sodium hexametaphosphate 99 in suspension, after continuing to stir 3h,, and be washed with water to chlorion and can not detect and end suspension filtered.The solid of washing was descended dry 1.5 hours at 170 ℃, obtain the high-purity nm magnesium hydroxide products.Product characterizes through instrumental analysis, reaches high-purity, nano level.Purity check result following (the Electronic Speculum test result is seen Fig. 3):
The purity check result
| Composition | Percentage composition |
| The magnesium hydroxide muriate is (with Cl -Meter) moisture content calcium oxide | 99.7 0.15 0.01 0.04 |
Embodiment 4
Under 10 ℃, take by weighing 1000 the gram magnesium chloride hex-ammoniates, under the clarifixator processing condition, join in the 20L 10wt.% sodium hydroxide dilute alkaline soln that has prepared, fully react 3h after, suspension ageing 12～24h.Add the surface treatment agent trolamine in suspension, after continuing to stir 3h, with suspension filtered, and with washing with alcohol 3 times, only can not detect to chlorion.The solid of washing was descended dry 3 hours at 120 ℃, obtain the high-purity nm magnesium hydroxide products.Product characterizes through instrumental analysis, reaches high-purity, nano level.Purity check result following (the Electronic Speculum test result is seen Fig. 4):
The purity check result
| Composition | Percentage composition |
| The magnesium hydroxide muriate is (with Cl -Meter) moisture content calcium oxide | 99.8 0.10 0.02 0.04 |
Claims (8)
1. the preparation method of a high-purity nm magnesium hydroxide is characterized in that, said preparation method is to be presoma with the magnesium chloride hex-ammoniate, adopts liquid phase alkaline hydrolysis method to make magnesium chloride hex-ammoniate change into the high-purity nm magnesium hydroxide,
Wherein: said liquid phase alkaline hydrolysis method is: alkalitropism is better than and adds the magnesium chloride hex-ammoniate solid particulate in the dilute alkaline soln of 2wt%～25wt% of ammoniacal liquor and carry out alkaline hydrolysis, after ageing, add dispersion agent and carry out surface treatment, the suspension filtered that obtains is washed to chlorion and can not be detected, and the filter cake that obtains obtains the high-purity nm magnesium hydroxide after drying.
2. preparation method as claimed in claim 1 is characterized in that, wherein the alkaline hydrolysis temperature is 10～100 ℃, and the time is 2～5 hours.
3. preparation method as claimed in claim 1 or 2 is characterized in that, wherein said dispersion agent is thanomin, trolamine, sodium oleate, sodium stearate, Sodium hexametaphosphate 99, sodium polyphosphate, titanate coupling agent, polyvinyl alcohol or silane coupling agent.
4. preparation method as claimed in claim 1 or 2 is characterized in that, wherein drying temperature is 80～180 ℃, and be 2～5 hours time of drying.
5. preparation method as claimed in claim 1 or 2 is characterized in that, wherein dilute alkaline soln is 2～25wt% sodium hydroxide or potassium hydroxide solution.
6. preparation method as claimed in claim 3 is characterized in that, wherein drying temperature is 80～180 ℃, and be 2～5 hours time of drying.
7. preparation method as claimed in claim 6 is characterized in that, wherein dilute alkaline soln is 2～25wt.% sodium hydroxide or potassium hydroxide solution.
8. preparation method as claimed in claim 7 is characterized in that, wherein said washing adopts water, ethanol, methyl alcohol, benzene or toluene to wash.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100526649A CN100372771C (en) | 2004-07-09 | 2004-07-09 | Preparation method of high purity nano-magnesium hydroxide |
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|---|---|---|---|
| CNB2004100526649A CN100372771C (en) | 2004-07-09 | 2004-07-09 | Preparation method of high purity nano-magnesium hydroxide |
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|---|---|
| CN1718542A CN1718542A (en) | 2006-01-11 |
| CN100372771C true CN100372771C (en) | 2008-03-05 |
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104030325A (en) * | 2014-05-15 | 2014-09-10 | 宁波职业技术学院 | Method for preparing magnesium hydroxide by using magnesium chloride hexammoniate |
| CN104495883A (en) * | 2014-12-02 | 2015-04-08 | 中国科学院青海盐湖研究所 | Preparation method of magnesium hydrate with high-concentration slurry |
| CN104611763A (en) * | 2014-12-25 | 2015-05-13 | 武汉工程大学 | Technology of using phosphate tailing as raw material to produce in-situ modified nano-magnesium hydroxide whisker |
| CN106317706A (en) * | 2016-09-04 | 2017-01-11 | 淄博夸克医药技术有限公司 | High-temperature-resistant anti-cracking flame-retardant cable material and preparation method thereof |
| CN106430263B (en) * | 2016-09-13 | 2017-09-15 | 苏州市泽镁新材料科技有限公司 | A kind of preparation method of magnesium oxide nanoparticle |
| CN111073666A (en) * | 2019-12-24 | 2020-04-28 | 合肥中科阻燃新材料有限公司 | Superfine modified magnesium hydroxide flame retardant and preparation method thereof |
| CN113789185A (en) * | 2021-10-14 | 2021-12-14 | 华北理工大学 | Preparation method of coal spontaneous combustion inhibitor based on magnesium ion compound |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1341694A (en) * | 2001-09-19 | 2002-03-27 | 北京化工大学 | Preparation process of magnesium hydroxide fire-retarding nanomaterial |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1341694A (en) * | 2001-09-19 | 2002-03-27 | 北京化工大学 | Preparation process of magnesium hydroxide fire-retarding nanomaterial |
Non-Patent Citations (1)
| Title |
|---|
| 纳米氢氧化镁制备技术研究. 林慧博，印万忠，南黎，韩跃新.有色矿冶，第19卷第1期. 2003 * |
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