CN100506696C - Method of preparing basic magnesium carbonate three-dimensional nanostructure - Google Patents
Method of preparing basic magnesium carbonate three-dimensional nanostructure Download PDFInfo
- Publication number
- CN100506696C CN100506696C CNB2007100114727A CN200710011472A CN100506696C CN 100506696 C CN100506696 C CN 100506696C CN B2007100114727 A CNB2007100114727 A CN B2007100114727A CN 200710011472 A CN200710011472 A CN 200710011472A CN 100506696 C CN100506696 C CN 100506696C
- Authority
- CN
- China
- Prior art keywords
- magnesium carbonate
- dimensional nanostructure
- basic magnesium
- preparing basic
- dispersion agent
- 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
- 238000000034 method Methods 0.000 title claims abstract description 13
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 title claims description 17
- 239000002086 nanomaterial Substances 0.000 title claims description 16
- 239000001095 magnesium carbonate Substances 0.000 title claims description 15
- 229910000021 magnesium carbonate Inorganic materials 0.000 title claims description 15
- 229940050906 magnesium chloride hexahydrate Drugs 0.000 claims abstract description 6
- DHRRIBDTHFBPNG-UHFFFAOYSA-L magnesium dichloride hexahydrate Chemical compound O.O.O.O.O.O.[Mg+2].[Cl-].[Cl-] DHRRIBDTHFBPNG-UHFFFAOYSA-L 0.000 claims abstract description 6
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 4
- 230000032683 aging Effects 0.000 claims abstract description 4
- 238000001035 drying Methods 0.000 claims abstract description 4
- 150000002500 ions Chemical class 0.000 claims abstract description 4
- JLVVSXFLKOJNIY-UHFFFAOYSA-N Magnesium ion Chemical compound [Mg+2] JLVVSXFLKOJNIY-UHFFFAOYSA-N 0.000 claims abstract description 3
- 229910001425 magnesium ion Inorganic materials 0.000 claims abstract description 3
- 238000003756 stirring Methods 0.000 claims abstract description 3
- 239000003795 chemical substances by application Substances 0.000 claims description 7
- 239000006185 dispersion Substances 0.000 claims description 6
- 239000012065 filter cake Substances 0.000 claims description 6
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 4
- -1 polyoxyethylene Polymers 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 229920004890 Triton X-100 Polymers 0.000 claims description 3
- 239000013504 Triton X-100 Substances 0.000 claims description 3
- 239000004202 carbamide Substances 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 238000000967 suction filtration Methods 0.000 claims description 3
- 239000007864 aqueous solution Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 239000013049 sediment Substances 0.000 abstract 3
- UOVKYUCEFPSRIJ-UHFFFAOYSA-D hexamagnesium;tetracarbonate;dihydroxide;pentahydrate Chemical compound O.O.O.O.O.[OH-].[OH-].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[O-]C([O-])=O.[O-]C([O-])=O.[O-]C([O-])=O.[O-]C([O-])=O UOVKYUCEFPSRIJ-UHFFFAOYSA-D 0.000 abstract 2
- 229940031958 magnesium carbonate hydroxide Drugs 0.000 abstract 2
- 229940059741 aqua care Drugs 0.000 abstract 1
- 239000002270 dispersing agent Substances 0.000 abstract 1
- 239000008236 heating water Substances 0.000 abstract 1
- 238000005406 washing Methods 0.000 abstract 1
- 239000000047 product Substances 0.000 description 6
- 238000002360 preparation method Methods 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 2
- OGWLTJRQYVEDMR-UHFFFAOYSA-F tetramagnesium;tetracarbonate Chemical compound [Mg+2].[Mg+2].[Mg+2].[Mg+2].[O-]C([O-])=O.[O-]C([O-])=O.[O-]C([O-])=O.[O-]C([O-])=O OGWLTJRQYVEDMR-UHFFFAOYSA-F 0.000 description 2
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 159000000003 magnesium salts Chemical class 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 239000000825 pharmaceutical preparation Substances 0.000 description 1
- 229940127557 pharmaceutical product Drugs 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000005060 rubber Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
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
- C01F5/24—Magnesium carbonates
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
-
- 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
Landscapes
- 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 making method of three-dimensional nanometer flower structure of magnesium carbonate hydroxide, which comprises the following steps: allocating magnesium chloride hexahydrate and aquacare with molar rate at 1:1-1:4 into solution with magnesium ion density at 0. 5-3mol/L; adding 1-3% dispersant corresponding to the quality of magnesium carbonate hydroxide; heating water bath to 80-99 deg. c; stirring 3-8h; aging 1-3h; obtaining sediment; sucking the sediment reciprocally; washing the sediment until not existing purity ion; drying under 100 deg. c for 3h in the baker; obtaining the product with the thickness of petal at 100nm. The method possesses simple technique and low manufacturing cost, which is easy to realize industrialization.
Description
Technical field
The invention belongs to the preparing technical field of nano material, be specifically related to a kind of method for preparing basic magnesium carbonate three-dimensional nanostructure.
Background technology
Magnesium basic carbonate is a kind of important inorganic chemical product.It not only can be used as the raw material of preparation magnesium salts series product, also can be used as the additive and the modifying agent of rubber, pharmaceutical products, insulating material, paint, papermaking, makeup, food, dentistry preparation, high glass, material of construction, stupalith and various Chemicals, application prospect is very wide.Therefore, how preparing high-quality basic carbonate magnesium products, particularly nano level basic carbonate magnesium products, is a problem that is worth discussion.At present, about the more existing reports of the preparation method of common magnesium basic carbonate product, but also there is not the report of synthetic method for basic magnesium carbonate three-dimensional nanostructure.
Summary of the invention
The purpose of this invention is to provide that a kind of technology is simple, low production cost, be easy to realize the preparation method of the high-quality basic magnesium carbonate three-dimensional nanostructure of suitability for industrialized production.
Technical solution of the present invention may further comprise the steps:
(1) magnesium chloride hexahydrate and urea are mixed with the aqueous solution that magnesium ion concentration is 0.5～3mol/L for 1:1～1:4 in molar ratio, the dispersion agent that adds magnesium chloride hexahydrate quality 1～3% again, heating in water bath to 80～99 ℃, stirring reaction 3～8 hours, ageing 1～3 hour obtains throw out;
(2) with throw out repeatedly suction filtration, be washed to the inclusion-free ion, obtain filter cake;
(3) filter cake is placed baking oven, drying is 3 hours under 100 ℃, obtains the basic magnesium carbonate three-dimensional nanostructure that petal thickness is about 100nm.
Dispersion agent is a kind of in polyoxyethylene glycol-1000, polyoxyethylene glycol-6000, the Triton X-100.
The beneficial effect that the present invention reached is: preparation technology is simple, low production cost, and process is controlled easily, is easy to realize suitability for industrialized production.Present method synthetic basic magnesium carbonate three-dimensional nanostructure product has characteristics such as well-crystallized, purity height.
Description of drawings
The present invention is further illustrated below in conjunction with drawings and Examples.
Fig. 1 is the X-ray diffractogram of the basic magnesium carbonate three-dimensional nanostructure prepared of the present invention.
Fig. 2 is the sem photograph of the basic magnesium carbonate three-dimensional nanostructure prepared of the present invention.
Embodiment
Embodiment
(1) 73.2g magnesium chloride hexahydrate, 109.1g urea and 250mL water are put into the there-necked flask of 500mL, added the Triton X-100 of 1g simultaneously, heating in water bath to 95 ℃ reacted 5 hours, and ageing 2 hours obtains throw out;
(2) with throw out repeatedly suction filtration, be washed to the inclusion-free ion, obtain filter cake;
(3) filter cake is placed baking oven, drying is 3 hours under 100 ℃, obtains the basic magnesium carbonate three-dimensional nanostructure that petal thickness is about 100nm.
Claims (4)
1. a method for preparing basic magnesium carbonate three-dimensional nanostructure is characterized in that, this method may further comprise the steps:
(1) magnesium chloride hexahydrate and urea are mixed with the aqueous solution that magnesium ion concentration is 0.5～3mol/L for 1:1～1:4 in molar ratio, the dispersion agent that adds magnesium chloride hexahydrate quality 1～3% again, heating in water bath to 80～99 ℃, stirring reaction 3～8 hours, ageing 1～3 hour obtains throw out;
(2) with throw out repeatedly suction filtration, be washed to the inclusion-free ion, obtain filter cake;
(3) filter cake is placed baking oven, drying is 3 hours under 100 ℃, obtains the basic magnesium carbonate three-dimensional nanostructure that petal thickness is about 100nm.
2. a kind of method for preparing basic magnesium carbonate three-dimensional nanostructure according to claim 1 is characterized in that described dispersion agent is a polyoxyethylene glycol-1000.
3. a kind of method for preparing basic magnesium carbonate three-dimensional nanostructure according to claim 1 is characterized in that described dispersion agent is a polyoxyethylene glycol-6000.
4. a kind of method for preparing basic magnesium carbonate three-dimensional nanostructure according to claim 1 is characterized in that described dispersion agent is a Triton X-100.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007100114727A CN100506696C (en) | 2007-05-26 | 2007-05-26 | Method of preparing basic magnesium carbonate three-dimensional nanostructure |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007100114727A CN100506696C (en) | 2007-05-26 | 2007-05-26 | Method of preparing basic magnesium carbonate three-dimensional nanostructure |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101058430A CN101058430A (en) | 2007-10-24 |
| CN100506696C true CN100506696C (en) | 2009-07-01 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2007100114727A Expired - Fee Related CN100506696C (en) | 2007-05-26 | 2007-05-26 | Method of preparing basic magnesium carbonate three-dimensional nanostructure |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN100506696C (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2018130876A1 (en) * | 2017-01-10 | 2018-07-19 | Dukebox Sp. Z O. O. | A method of manufacturing a suspension of nanoparticles of potassium salt or magnesium salt |
Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102069003A (en) * | 2009-11-23 | 2011-05-25 | 中国科学院福建物质结构研究所 | Novel carbonate optical catalyst and preparation method thereof |
| CN102153115B (en) * | 2011-05-23 | 2013-11-13 | 大连交通大学 | Method for preparing anhydrous magnesium carbonate powder |
| CN105047421B (en) * | 2015-06-15 | 2017-11-10 | 昆明理工大学 | A kind of preparation method of graphene/subcarbonate nano composite material |
| CN105347369A (en) * | 2015-12-14 | 2016-02-24 | 苏州市泽镁新材料科技有限公司 | Preparation method of high-purity magnesium carbonate |
| CN105347368A (en) * | 2015-12-14 | 2016-02-24 | 苏州市泽镁新材料科技有限公司 | Preparing method of high purity magnesium carbonate |
| CN105668596B (en) * | 2016-01-05 | 2018-06-26 | 武汉工程大学 | The method that template-mediated/precipitation from homogeneous solution prepares en plaque basic magnesium carbonate |
| CN112029913B (en) * | 2019-06-04 | 2024-01-30 | 广西科技大学 | Sugar juice clarifying and decoloring agent and application thereof |
-
2007
- 2007-05-26 CN CNB2007100114727A patent/CN100506696C/en not_active Expired - Fee Related
Non-Patent Citations (4)
| Title |
|---|
| 不同溶剂置换法制备纳米氧化镁粉体的研究. 张伟等.无机盐工业，第37卷第2期. 2005 |
| 不同溶剂置换法制备纳米氧化镁粉体的研究. 张伟等.无机盐工业，第37卷第2期. 2005 * |
| 均匀沉淀法制备纳米氧化镁粉体的试验研究. 张伟等.河南化工，第23卷第7期. 2006 |
| 均匀沉淀法制备纳米氧化镁粉体的试验研究. 张伟等.河南化工，第23卷第7期. 2006 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2018130876A1 (en) * | 2017-01-10 | 2018-07-19 | Dukebox Sp. Z O. O. | A method of manufacturing a suspension of nanoparticles of potassium salt or magnesium salt |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101058430A (en) | 2007-10-24 |
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Granted publication date: 20090701 Termination date: 20120526 |