CN101935058B - Preparation method of magnesium hydroxide hexagonal crystal - Google Patents
Preparation method of magnesium hydroxide hexagonal crystal Download PDFInfo
- Publication number
- CN101935058B CN101935058B CN 201010284921 CN201010284921A CN101935058B CN 101935058 B CN101935058 B CN 101935058B CN 201010284921 CN201010284921 CN 201010284921 CN 201010284921 A CN201010284921 A CN 201010284921A CN 101935058 B CN101935058 B CN 101935058B
- Authority
- CN
- China
- Prior art keywords
- crystal
- magnesium
- hydroxide
- hexagonal crystal
- percent
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Images
Landscapes
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention discloses a preparation method of a magnesium hydroxide hexagonal crystal, relating to the technology of chemical engineering. The method comprises the following steps of: (1) placing magnesium nitrate in a mixture of sodium hydroxide and potassium hydroxide with the mass ratio of 25 percent: 75 percent-48.5 percent: 51.5 percent, wherein the molar ratio of magnesium nitrate to potassium hydroxide is 30:393-50:393; (2) raising the temperature to 160-200 DEG C so that sodium hydroxide and potassium hydroxide are in a molten liquid state, and keeping the temperature to prepare a magnesium hydroxide crystal under the condition to grow for 12-24 hours; and (3) dissolving, filtering and drying the grown crystal and growth medium to obtain the magnesium hydroxide hexagonal crystal with regular shapes. In the invention, the magnesium hydroxide hexagonal crystal with regular shapes is grown through a certain temperature condition and time by using the magnesium nitrate as a raw material and molten strong base as the growth medium, so as to avoid the traditional method which needs the assistance of adding a complexing agent or a surfactant, and the crystal has the diameter of 4-10mum, uniform grain diameter and excellent dispersibility, and is in a hexagonal sheet structure.
Description
Technical field
The present invention relates to the chemical industry technology.
Background technology
The Marinco H function is extensive; As fire retardant have concurrently fire-retardant, press down functions such as cigarette, resistance drip, antiacid and filling; And itself is nonpoisonous and tasteless, does not produce toxic gas and etchant gas during burning, does not corrode mould; Do not produce secondary pollution, especially be fit to polymkeric substance such as the PP high, PA and be used with processing temperature.Mostly ordinary hydrogen Natural manganese dioxide is hexagonal structure or amorphous, but the Marinco H granularity of preparation is little at present, filtration difficulty; Be prone to foreign ions such as absorption silicon, calcium, iron, gained hexagonal flake crystal thickness is little, and the microcosmic internal strain increases; Serious agglomeration realizes that the high dispersive of product is relatively more difficult, is difficult for reaching the product application standard; Therefore, limited it in Industrial Application.
The magnesium hydroxide crystal of ordinary method growth often exists and is easy between particle reunite, and size distribution is inhomogeneous, and the irregular grade of crystal shape directly has influence on the performance of its application.How to realize that the good magnesium hydroxide crystal of processability is just becoming the focus of people's growing interest.The method for preparing magnesium hydroxide crystal commonly used has: compound methods such as direct precipitation method, sluggish precipitation, hypergravity and hydro-thermal.Mostly traditional preparation method is in liquid environment growing crystal.Generally also one or more alkali sources grow Marinco H (Y.Ding, G.T.Zhang, H.Wu, B.Hai, L.B.Wang of adopting more; Y.T.Qian, Chem.Mater., 2001:13,435-440), still; The uniform crystal of the particle diameter of growing needs to add certain dispersion agent (Y.D.Li, M.Sui, Y.Ding, G.H.Zhang; J.Zhuang, C.Wang, Adv.Mater.2000,12 (11) 818).
Chinese patent CN1740269A proposes be a kind of be raw material with the magnesium chloride, the method through liquefied ammonia pressurized precipitation-hydrothermal modification prepares Marinco H.
Japanese Patent JP20053364 is disclosed to be a kind of Lithium Hydroxide MonoHydrate or sodium hydroxide are mixed with Marinco H to form suspension liquid, and carries out the Marinco Hs that modification prepares at 180 ℃ with 220 ℃ of reaction pair Marinco Hs.
Chinese patent CN101544387A is disclosed to be a kind ofly the Marinco H slip is joined Lithium Hydroxide MonoHydrate to mix the compound transformation system that forms with sodium hydroxide or Pottasium Hydroxide.
The growing environment of the Marinco H of above method is liquid solution.
Summary of the invention
Technical problem to be solved by this invention is; A kind of new preparation method of the Marinco H of growing is provided; In the fused strong alkali environment, the growth magnesium hydroxide crystal need not the auxiliary of any complexing agent or tensio-active agent; Realized the magnesium hydrate hexagonal crystalline growth of regular shape, the synthetic magnesium hydroxide crystal of industry has been had positive meaning.
The technical scheme that the present invention solve the technical problem employing is that magnesium hydrate hexagonal crystal preparation method is characterized in that, comprises the steps:
1) magnesium nitrate is placed sodium hydroxide and Pottasium Hydroxide mixture, the mass ratio of sodium hydroxide and Pottasium Hydroxide is 25%: 75%～48.5%: 51.5%, and magnesium nitrate and mol ratio hydroxy are 30: 393～50: 393;
2) be warming up to 160～200 ℃, make sodium hydroxide and Pottasium Hydroxide become the fused liquid state, keep temperature, prepare magnesium hydroxide crystal with this understanding, growth time is 12～24 hours;
3) will grow good crystal and growth medium dissolving thereof, filtration, drying have obtained the magnesium hydrate hexagonal crystal of regular shape.
Step 2) in, heats up and in polytetrafluoroethylcontainer container, carry out.
The present invention is to be raw material with the magnesium nitrate; Fused highly basic is growth medium, grows the magnesium hydrate hexagonal crystal of regular shape through certain temperature condition and time, has avoided traditional method and need add the auxiliary of complexing agent or tensio-active agent; This crystal diameter is 4～10um; Be the hexagonal flake structure, particle diameter is even, has good dispersiveness.
Below in conjunction with accompanying drawing and embodiment the present invention is further described.
Description of drawings
Fig. 1 is the XRD figure spectrum of embodiment 1 products therefrom;
Fig. 2 is the stereoscan photograph of embodiment 1 products therefrom;
Fig. 3 is the XRD figure of the different magnesium of instance 2 gained samples source growth, and wherein magnesium nitrate and mol ratio hydroxy are (a) 30: 393; (b) 40: 393; (c) 50: 393.
Fig. 4～6th, the sem photograph of the different magnesium of instance 2 gained samples source growth, wherein magnesium nitrate and mol ratio hydroxy are (Fig. 4) 30: 393; (Fig. 5) 40: 393; (Fig. 6) 50: 393.
Embodiment
Embodiment 1:
Mg (NO
3)
26H
2O gets 7.697g (30mmol); With gross weight is that sodium hydroxide and the Pottasium Hydroxide (wherein NaOH and KOH weight ratio are 1: 3) of 20g mixes, and puts into together in the polytetrafluoroethylcontainer container, and control crystalline growth temperature is 180 ℃; Treat the complete fusion of NaOH and KOH; It is rocked evenly, be incubated 24 hours with this understanding, growth Mg (OH)
2Crystal.The Mg (OH) that generates
2Crystalline XRD is as shown in Figure 1, and each diffraction peak position is consistent with the standard card (JCPDS NO.74-2220) of Marinco H among the figure, explains that the gained sample is the Mg (OH) of single phase
2Fig. 2 is the stereoscan photograph of this routine products therefrom, and as can be seen from the figure product is a hexagonal structure, the about 4～10um of diameter range, crystal grain good dispersivity.
Embodiment 2:
Mg (NO
3)
26H
2The amount of substance of O is got 7.697g (30mmol), 10.26g (40mmol), 12.83g (50mmol); With gross weight is that 20g (393mmol) (wherein NaOH and KOH weight ratio are 1: 3) mixes; Put into together in the polytetrafluoroethylcontainer container, control crystalline growth temperature is 160 ℃, treats the complete fusion of NaOH and KOH; It is rocked evenly, be incubated 24 hours with this understanding.The Mg (OH) that generates
2Crystalline XRD is as shown in Figure 3, and each diffraction peak position is consistent with the standard card (JCPDS NO.74-2220) of Marinco H among the figure, explains that the gained sample is the Mg (OH) of single phase
2Fig. 4～6 are the stereoscan photograph of this routine products therefrom, and as can be seen from the figure product is a hexagonal structure, the about 4～15um of diameter range, and crystal grain does not have reunion, good dispersivity.
Embodiment 3:
Magnesium hydrate hexagonal crystal preparation method comprises the steps:
1) magnesium nitrate is placed sodium hydroxide and Pottasium Hydroxide mixture, the mass ratio of sodium hydroxide and Pottasium Hydroxide is 25%: 75%, and magnesium nitrate and mol ratio hydroxy are 1: 262;
2) be warming up to 160～200 ℃, make sodium hydroxide and Pottasium Hydroxide become the fused liquid state, keep temperature, prepare magnesium hydroxide crystal with this understanding, growth time is 12～24 hours;
3) will grow good crystal and growth medium dissolving thereof, filtration, drying have obtained the magnesium hydrate hexagonal crystal of regular shape.
Embodiment 4:
Magnesium hydrate hexagonal crystal preparation method comprises the steps:
1) magnesium nitrate is placed sodium hydroxide and Pottasium Hydroxide mixture, the mass ratio of sodium hydroxide and Pottasium Hydroxide is 48.5%: 51.5%, and magnesium nitrate and mol ratio hydroxy are 2: 262;
2) be warming up to 160～200 ℃, make sodium hydroxide and Pottasium Hydroxide become the fused liquid state, keep temperature, prepare magnesium hydroxide crystal with this understanding, growth time is 12～24 hours;
3) will grow good crystal and growth medium dissolving thereof, filtration, drying have obtained the magnesium hydrate hexagonal crystal of regular shape.
Claims (2)
1. magnesium hydrate hexagonal crystal preparation method is characterized in that, comprises the steps:
1) magnesium nitrate is placed sodium hydroxide and Pottasium Hydroxide mixture, the mass ratio of sodium hydroxide and Pottasium Hydroxide is 25%: 75%～48.5%: 51.5%, and magnesium nitrate and mol ratio hydroxy are 30: 393～50: 393;
2) be warming up to 160～200 ℃, make sodium hydroxide and Pottasium Hydroxide become the fused liquid state, keep temperature, prepare magnesium hydroxide crystal with this understanding, growth time is 12～24 hours;
3) will grow good crystal and growth medium dissolving thereof, filtration, drying have obtained the magnesium hydrate hexagonal crystal of regular shape.
2. magnesium hydrate hexagonal crystal preparation method as claimed in claim 1 is characterized in that step 2) in, heat up and in polytetrafluoroethylcontainer container, carry out.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010284921 CN101935058B (en) | 2010-09-17 | 2010-09-17 | Preparation method of magnesium hydroxide hexagonal crystal |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010284921 CN101935058B (en) | 2010-09-17 | 2010-09-17 | Preparation method of magnesium hydroxide hexagonal crystal |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101935058A CN101935058A (en) | 2011-01-05 |
| CN101935058B true CN101935058B (en) | 2012-05-23 |
Family
ID=43388666
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 201010284921 Expired - Fee Related CN101935058B (en) | 2010-09-17 | 2010-09-17 | Preparation method of magnesium hydroxide hexagonal crystal |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101935058B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109896548B (en) * | 2018-08-28 | 2022-04-08 | 福建省农业科学院农业工程技术研究所 | Porous magnetic iron oxide red rich in lattice defects and preparation method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1359853A (en) * | 2000-12-19 | 2002-07-24 | 中国科学技术大学 | Acidular or flaky nano magnesium hydroxide and its preparing process |
| JP2006306659A (en) * | 2005-04-28 | 2006-11-09 | Tateho Chem Ind Co Ltd | Magnesium hydroxide particle, method for producing the same, and resin composition containing the same |
| CN101376512A (en) * | 2008-06-13 | 2009-03-04 | 河南科技大学 | Preparation of magnesium hydrate nanocrystalline |
| CN101607722A (en) * | 2008-05-27 | 2009-12-23 | 浙江理工大学 | A kind of synthetic method of magnesium hydrate hexagonal nano-flake |
-
2010
- 2010-09-17 CN CN 201010284921 patent/CN101935058B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1359853A (en) * | 2000-12-19 | 2002-07-24 | 中国科学技术大学 | Acidular or flaky nano magnesium hydroxide and its preparing process |
| JP2006306659A (en) * | 2005-04-28 | 2006-11-09 | Tateho Chem Ind Co Ltd | Magnesium hydroxide particle, method for producing the same, and resin composition containing the same |
| CN101607722A (en) * | 2008-05-27 | 2009-12-23 | 浙江理工大学 | A kind of synthetic method of magnesium hydrate hexagonal nano-flake |
| CN101376512A (en) * | 2008-06-13 | 2009-03-04 | 河南科技大学 | Preparation of magnesium hydrate nanocrystalline |
Non-Patent Citations (1)
| Title |
|---|
| Jin Dl et al..Hydrothermal synthesis and characterization of hexagonal Mg(OH)2 nano-flake as a flame retardant.《Materials Chemistry and Physics》.2008,第112卷962-965. * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101935058A (en) | 2011-01-05 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Wang et al. | Single-crystalline ZnSn (OH) 6 hollow cubes via self-templated synthesis at room temperature and their photocatalytic properties | |
| CN102491403B (en) | Method for preparing copper oxide powder by using complexed-precipitation method | |
| CN103663527A (en) | Preparation method of cubic ultra-fine calcium carbonate particles | |
| Hao et al. | Controlled growth of hydroxyapatite fibers precipitated by propionamide through hydrothermal synthesis | |
| CN102139869B (en) | Method for preparing spherical iron phosphate by combining sedimentation method and hydrothermal method | |
| CN104129770B (en) | A kind of nanoscale iron phosphate and preparation method thereof | |
| CN101891165A (en) | Production method of macrocrystalline hexagonal boron nitride | |
| CN102649590A (en) | Method for preparing mesoporous material NiAl2O4 without specific surface active agent | |
| KR20130074806A (en) | Metal doped crystalline iron phosphate, method for preparation thereof and lithium composite metal phosphorus oxide prepared using the same | |
| Zeng et al. | A general method to prepare metal ammonium phosphate nanoflake constructed microspheres | |
| CN104117372A (en) | Hydrothermal preparation method of load-type nickel phosphide catalyst using nano red phosphorus as phosphorus source | |
| Vasquez-Elizondo et al. | Urea decomposition enhancing the hydrothermal synthesis of lithium iron phosphate powders: Effect of the lithium precursor | |
| CN101935058B (en) | Preparation method of magnesium hydroxide hexagonal crystal | |
| CN103936034B (en) | Preparation method of high-purity sodium iodide powder | |
| CN101607722B (en) | Method for synthesizing magnesium hydrate hexagonal nano-flake | |
| CN105645422B (en) | The technique that a kind of liquid phase method prepares spherical super fine zirconium boride powder | |
| CN105502450B (en) | Preparing method and application of subspheroidal alpha-alumina micro powder | |
| CN104261417A (en) | Preparation method of micro-nano hydroxyl magnesium silicate | |
| CN109467102A (en) | A method of SBA-15 molecular sieve is synthesized using SILICA FUME | |
| CN103922594B (en) | A kind of large red color crystal bead blank and preparation method thereof | |
| CN102910611A (en) | Method for preparing ferrous phosphate-based lithium salt | |
| CN101565564B (en) | SiO2 enveloped spherical nanometer calcium carbonate and preparation method thereof | |
| Deng et al. | A generic in situ seed-mediated size-control method in the case of cuprous oxide nanocubes and their antibacterial activities | |
| CN102910910A (en) | Method for preparing micro-nano titanium carbonitride powder with controllable carbon-nitrogen ratio by adopting solid state nitrogen source | |
| CN103304228A (en) | Self-propagating combustion synthesis method for palladium-copper ferrite nano-powder |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C17 | Cessation of patent right | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20120523 Termination date: 20130917 |