CN1288078A - Method for synthesis of well-dispersed and super fine anion laminated material - Google Patents
Method for synthesis of well-dispersed and super fine anion laminated material Download PDFInfo
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- CN1288078A CN1288078A CN 99119385 CN99119385A CN1288078A CN 1288078 A CN1288078 A CN 1288078A CN 99119385 CN99119385 CN 99119385 CN 99119385 A CN99119385 A CN 99119385A CN 1288078 A CN1288078 A CN 1288078A
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Abstract
A nucleating/crystallizing isolation process for synthesizing uniformly dispersed superfine laminated anionic materical is disclosed. An instantaneous nucleating technique is used to generate a lot of nucleuses instantaneously is reaction system to prevent nucleation in crystallizing procedure. A dynamic crystallizing technique with program controlled temp. it used to promote uniform distribution of crystal grains and shorten crystallizing time. Its advantages include: better crystal phase, uniform granularities, simple process, less investment, short production period and no environmental pollution.
Description
The present invention relates to a kind of novel synthesis that all disperses anion layer shape super-fine material (LDHs), nucleation/crystallization isolation method has overcome that nucleation and crystallization make crystal grain shortcoming pockety synchronously in the crystal growing process.
Anion laminated material is the important inorganic non-metallic crystalline material that a class has the special rules structure, and its chemical constitution is [M
2+ 1-xM
3+ x(OH)
2] A
N- X/nMH
2O, wherein:
M
2+=Mg
2+Zn
2+Cu
2+Ni
2+Fe
2+Mn
2+Ca
2+……，
M
3+=Al
3+Cr
3+Fe
3+V
3=Co
3+Ga
3+Ti
3+……，
A
n-=F
-Cl
-Br
-I
-CO
3 2-SO
4 2-NO
3 -ClO
3 -OH
-H
2PO
4 -WO
4 3-……，
Because the adjustable sex change of its special The Nomenclature Composition and Structure of Complexes is widely used in the industries such as chemical industry, medicine, agricultural it.The synthetic method of existing comparative maturity is a coprecipitation method, but because coprecipitation method exists nucleation and crystallization is carried out synchronously, make sintetics have shortcomings such as crystalline phase is bad, grain size is inhomogeneous, the difficult control of grain-size, generated time length, limited the suitability for industrialized production of this inorganic non-metallic crystalline material and its widespread use.
The present invention considers from the crystal generative process, the isolated synthetic method of nucleation/crystallization has been proposed, avoided the contradiction that nucleation and crystallization are carried out synchronously in the crystal growing process, full back-mixing explosive type moment one-tenth nuclear technique and temperature programmed control dynamic crystallization technology have been adopted simultaneously, can make the specific composition of preparing all disperse anion layer shape super-fine material to have better crystalline phase and uniform size distribution, and can simplify preparation technology, reduce facility investment, shorten the production time greatly, cut down the consumption of energy and non-environmental-pollution.Purpose of the present invention: a kind of novel synthesis that all disperses anion layer shape super-fine material (LDHs) is provided, make in the building-up process of negatively charged ion stratiform super-fine material (LDHs), shortcomings such as avoided the crystalline phase of negatively charged ion stratiform super-fine material (LDHs) bad, grain size is inhomogeneous, the difficult control of grain-size, generated time are long have simultaneously and simplify preparation technology, reduce facility investment, shorten the production time, cut down the consumption of energy and avoid the purpose of environmental pollution.
Main points of the present invention: the invention provides a kind of novel synthesis that all disperses anion layer shape super-fine material.The irregular and unequal shortcoming of size distribution of crystalline phase at product in the existing anion laminated material synthetic method, the present invention is with nucleation/crystallization isolation method, all dispersions anion layer shape super-fine material that utilizes full back-mixing explosive type moment nucleation and temperature programmed control dynamic crystallization technology to prepare to have specific composition.Compare with traditional preparation method, method therefor of the present invention can make anion laminated material have better crystalline phase and uniform size distribution, has simultaneously that preparation technology simplifies, reduces facility investment, shortens the production time, energy efficient, non-environmental-pollution, an advantage such as applied widely.
The present invention adopts following technical essential:
1), nucleation/crystallization partition method.According to the crystallography principle, overcome the shortcoming that nucleation and crystallization are carried out synchronously in the crystal growing process with nucleation/crystallization partition method.
2), full back-mixing explosive type moment one-tenth nuclear technique.Utilize full back-mixing explosive type moment one-tenth nuclear technique to make reaction system, and then stop the generation of nucleation in crystallization process in a large amount of nucleation of moment.Full back-mixing explosive type moment becomes the nuclear reaction device self-control, nucleation reaction times 2-10 second.
3), temperature programmed control dynamic crystallization technology.Utilize temperature programmed control dynamic crystallization technology to impel crystal grain to be evenly distributed, shortened crystallization time simultaneously greatly.The self-control of temperature programmed control dynamic crystallization reaction unit, 30-100 ℃ of dynamic crystallization temperature of reaction.Crystallization time 1-10 hour.
Technology provided by the invention is applicable to following building-up reactions:
1, the negatively charged ion stratiform super-fine material of different cation compositions is synthetic.
2, anionic negatively charged ion stratiform super-fine material is synthetic between different layers.
3, the negatively charged ion stratiform super-fine material of different cationic proportions is synthetic.
4, the negatively charged ion stratiform super-fine material of interlayer different anions is synthetic.
5, the above-mentioned different super-fine material of forming different size of particles synthesizes.
Technology provided by the invention is with different material (M (NO
3)
x, MCl
x, M
x(SO
4)
Y, KOH, NaOH, Na
2CO
3, K
2CO
3) the synthetic of anion laminated material of difference composition shown: utilize nucleation/crystallization partition method, become nuclear technique and temperature programmed control dynamic crystallization technology synthetic anion laminated material to have the good and characteristics of size distribution and grain size controlled amount uniformly of crystalline phase with full back-mixing explosive type moment, have preparation technology simultaneously and simplify, reduce facility investment, shortening production time, energy efficient, non-environmental-pollution, advantage such as applied widely.
The invention will be further described below in conjunction with embodiment:
Embodiment 1: different magnaliums are than all disperseing the synthetic of anion layer shape super-fine material
Choosing a certain amount of magnesium salts and aluminium salt, is 2 (adjustable between 2-4) by the mol ratio of magnesium salts and aluminium salt, is made into the solution of certain volume, gets a certain amount of NaOH and Na
2CO
3Be made into the solution of certain volume, press the volumetric molar concentration 1.6M (adjustable between 0.4-2.0M) of magnesium salts, become in the nuclear reaction device two solution short mix, 5 seconds reaction times, mixed serum pH=10.5 (9-12 all can) in full back-mixing explosive type moment.Mixed serum is moved to temperature programmed control dynamic crystallization reaction unit, 30-100 ℃ of dynamic crystallization temperature of reaction, 6 hours dynamic crystallization time (variable in 2-10 hour).
The synthetic product yield is greater than 99%, and the product crystal phase structure is good, particle diameter 0.3 μ (0.05-0.4 μ is controlled), and particle distribution (particle diameter=0.3 μ) is greater than 99%.
Embodiment 2: the Different Zinc aluminum ratio all disperses the synthetic of anion layer shape super-fine material
Choosing a certain amount of zinc salt and aluminium salt, is 2 (adjustable between 2-4) by the mol ratio of zinc salt and aluminium salt, is made into the solution of certain volume, gets a certain amount of NaOH and Na
2CO
3Be made into the solution of certain volume, press the volumetric molar concentration 1 of zinc salt: 6M (adjustable between 0.4-2.0M), become in the nuclear reaction device with two solution short mix 5 seconds reaction times, mixed serum pH=11 in full back-mixing explosive type moment.0 (9-12 all can).Mixed serum is moved to temperature programmed control dynamic crystallization reaction unit, 30-100 ℃ of dynamic crystallization temperature of reaction, 4 hours dynamic crystallization time (variable in 2-10 hour).
The synthetic product yield is greater than 99%, and the product crystal phase structure is good, particle diameter 0.2 μ (0.05-0.4 μ is controlled), and particle distribution (particle diameter=0.2 μ) is greater than 99%.
Embodiment 3: different cobalt aluminum ratios all disperse the synthetic of anion layer shape super-fine material
Choosing a certain amount of cobalt salt and aluminium salt, is 2 (adjustable between 2-4) by the mol ratio of cobalt salt and aluminium salt, is made into the solution of certain volume, gets a certain amount of NaOH and Na
2CO
3Be made into the solution of certain volume, press the volumetric molar concentration 0.8M (adjustable between 0.4-2.0M) of cobalt salt, become in the nuclear reaction device two solution short mix, 5 seconds reaction times, mixed serum pH=9.5 (9-11 all can) in full back-mixing explosive type moment.Mixed serum is moved to temperature programmed control dynamic crystallization reaction unit, 30-100 ℃ of dynamic crystallization temperature of reaction, 8 hours dynamic crystallization time (variable in 2-10 hour).
The synthetic product yield is greater than 96%, and the product crystal phase structure is good, particle diameter 0.3 μ (0.05-0.4 μ is controlled), and particle distribution (particle diameter=0.3 μ) is greater than 99%.
Embodiment 4: different nickel aluminum ratios all disperse the synthetic of anion layer shape super-fine material
Choosing a certain amount of nickel salt and aluminium salt, is 2 (adjustable between 2-4) by the mol ratio of nickel salt and aluminium salt, is made into the solution of certain volume, gets a certain amount of NaOH and Na
2CO
3Be made into the solution of certain volume, press the volumetric molar concentration 1.2M (adjustable between 0.4-2.0M) of nickel salt, become in the nuclear reaction device two solution short mix, 5 seconds reaction times, mixed serum pH=9 (9-10 all can) in full back-mixing explosive type moment.Mixed serum is moved to temperature programmed control dynamic crystallization reaction unit, 30-100 ℃ of dynamic crystallization temperature of reaction, 6 hours dynamic crystallization time (variable in 2-10 hour).
The synthetic product yield is greater than 97%, and the product crystal phase structure is good, particle diameter 0.2 μ (0.05-0.4 μ is controlled), and particle distribution (particle diameter=0.2 μ) is greater than 99%.
Embodiment 5: different manganese aluminum ratios all disperse the synthetic of anion layer shape super-fine material
Choosing a certain amount of manganese salt and aluminium salt, is 2 (adjustable between 2-4) by the mol ratio of manganese salt and aluminium salt, is made into the solution of certain volume, gets a certain amount of NaOH and Na
2CO
3Be made into the solution of certain volume, press the volumetric molar concentration 0.6M (adjustable between 0.4-2.0M) of manganese salt, become in the nuclear reaction device two solution short mix, 5 seconds reaction times, mixed serum pH=10 (9-11 all can) in full back-mixing explosive type moment.Mixed serum is moved to temperature programmed control dynamic crystallization reaction unit, 30-100 ℃ of dynamic crystallization temperature of reaction, 8 hours dynamic crystallization time (variable in 2-10 hour).
The synthetic product yield is greater than 95%, and the product crystal phase structure is good, particle diameter 0.2 μ (0.05-0.4 μ is controlled), and particle distribution (particle diameter=0.2 μ) is greater than 99%.
Embodiment 6: zinc-magnesium aluminium all disperses the synthetic of anion layer shape super-fine material
Choosing a certain amount of magnesium salts and zinc salt (composition of magnesium and zinc can at 0-100% scope modulation) and aluminium salt, is 2 (adjustable between 2-4) by the mol ratio of magnesium salts and zinc salt total amount and aluminium salt, is made into the solution of certain volume, gets a certain amount of NaOH and Na
2CO
3Be made into the solution of certain volume, press the volumetric molar concentration 1.6M (adjustable between 0.4-2.0M) of magnesium salts and zinc salt total amount, become in the nuclear reaction device two solution short mix, 5 seconds reaction times, mixed serum pH=10.5 (9-12 all can) in full back-mixing explosive type moment.Mixed serum is moved to temperature programmed control dynamic crystallization reaction unit, 30-100 ℃ of dynamic crystallization temperature of reaction, 6 hours dynamic crystallization time (variable in 2-10 hour).
The synthetic product yield is greater than 99%, and the product crystal phase structure is good, particle diameter 0.3 μ (0.05-0.4 μ is controlled), and particle distribution (particle diameter=0.3 μ) is greater than 99%.
Claims (3)
1. novel synthesis that all disperses super fine anion laminated material, nucleation/crystallization isolation method, make reaction system in a large amount of nucleation of moment with full back-mixing explosive type moment one-tenth nuclear technique, and then the generation of prevention nucleation in crystallization process, utilize temperature programmed control dynamic crystallization technology to impel crystal grain to be more evenly distributed, and can shorten crystallization time greatly.
2. full back-mixing explosive type according to claim 1 moment becomes nuclear technique, it is characterized in that: reaction raw materials is in high-speed stirring a large amount of nucleation of following moment, nucleation reaction times 2-10 second.
3. temperature programmed control dynamic crystallization technology according to claim 1 is characterized in that: the slurries after the homogeneous nucleation are the continuous flow crystallization between controlled crystallization temperature 30-100 ℃, crystallization time 1-10 hour
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|---|---|---|---|---|
| WO2004000757A1 (en) * | 2002-06-24 | 2003-12-31 | Beijing University Of Chemical Technology | A package method of anion supermolecule intercalation structured material |
| WO2004054361A1 (en) * | 2002-12-13 | 2004-07-01 | Beijing University Of Chemical Technology | A slow-released glyphosate formulation with supermolecular structure and the preparation method thereof |
| WO2005067975A1 (en) * | 2004-01-07 | 2005-07-28 | Beijing University Of Chemical Technology | Title: a sustained release captopril formulation having a supermolecular intercalation structure and the preparation process thereof |
| WO2007073639A1 (en) * | 2005-12-29 | 2007-07-05 | Beijing University Of Chemical Technology | Preparation method for highly orientated transparent thin film of double-layered-hydroxides |
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| WO2008083563A1 (en) * | 2007-01-12 | 2008-07-17 | Beijing University Of Chemical Technology | A microsphere of layered double hydroxide and method for preparing the same |
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| CN102180614A (en) * | 2011-03-21 | 2011-09-14 | 北京化工大学 | Magnelium base layer-shaped double-hydroxide ultraviolet barrier material used in anti-aging asphalt |
| CN102205981A (en) * | 2011-04-28 | 2011-10-05 | 北京化工大学 | Preparation method of layered compound metal hydroxide for controlling surface defects and surface potentials |
| CN101531766B (en) * | 2009-04-10 | 2012-04-11 | 北京化工大学 | Method for preparing bovine serum albumin hybridized membrane |
| CN102898849A (en) * | 2012-11-09 | 2013-01-30 | 北京化工大学 | Zinc-base doped layered double-hydroxide ultraviolet barrier material for ageing-resistant asphalt |
| CN103962157A (en) * | 2014-05-19 | 2014-08-06 | 北京化工大学 | Nano-structure CoSx/C cathode electro-catalytic material and preparation method thereof |
| CN104087243A (en) * | 2013-04-01 | 2014-10-08 | 上海杰事杰新材料(集团)股份有限公司 | Hydrotalcite-like ultraviolet absorbent and preparation method thereof |
| CN107814415A (en) * | 2016-09-13 | 2018-03-20 | 同济大学 | The establishment of the hydro-thermal supported liquid membrane synthetic method of nano material |
| CN115873008A (en) * | 2023-03-01 | 2023-03-31 | 中化学科学技术研究有限公司 | Method for purifying isosorbide and purified isosorbide |
-
1999
- 1999-09-14 CN CN 99119385 patent/CN1288078A/en active Pending
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| WO2004000757A1 (en) * | 2002-06-24 | 2003-12-31 | Beijing University Of Chemical Technology | A package method of anion supermolecule intercalation structured material |
| WO2004054361A1 (en) * | 2002-12-13 | 2004-07-01 | Beijing University Of Chemical Technology | A slow-released glyphosate formulation with supermolecular structure and the preparation method thereof |
| WO2005067975A1 (en) * | 2004-01-07 | 2005-07-28 | Beijing University Of Chemical Technology | Title: a sustained release captopril formulation having a supermolecular intercalation structure and the preparation process thereof |
| WO2007073639A1 (en) * | 2005-12-29 | 2007-07-05 | Beijing University Of Chemical Technology | Preparation method for highly orientated transparent thin film of double-layered-hydroxides |
| CN100383197C (en) * | 2006-06-09 | 2008-04-23 | 北京化工大学 | Sulfosalicylic with super molecular inserting layer structure, its preparation process and use |
| WO2008083563A1 (en) * | 2007-01-12 | 2008-07-17 | Beijing University Of Chemical Technology | A microsphere of layered double hydroxide and method for preparing the same |
| CN101140257B (en) * | 2007-10-18 | 2010-04-21 | 北京化工大学 | Biologic sensor enzyme functional susceptivity film containing nickel and aluminum hydrotalcite nano piece and method of producing the same |
| WO2010111849A1 (en) * | 2009-04-02 | 2010-10-07 | 北京化工大学 | Solid basic catalyst for synthesizing alkanolamide compounds and preparation method thereof |
| CN101531766B (en) * | 2009-04-10 | 2012-04-11 | 北京化工大学 | Method for preparing bovine serum albumin hybridized membrane |
| CN102180614A (en) * | 2011-03-21 | 2011-09-14 | 北京化工大学 | Magnelium base layer-shaped double-hydroxide ultraviolet barrier material used in anti-aging asphalt |
| CN102180614B (en) * | 2011-03-21 | 2012-08-01 | 北京化工大学 | Magnelium base layer-shaped double-hydroxide ultraviolet barrier material used in anti-aging asphalt |
| CN102205981A (en) * | 2011-04-28 | 2011-10-05 | 北京化工大学 | Preparation method of layered compound metal hydroxide for controlling surface defects and surface potentials |
| CN102205981B (en) * | 2011-04-28 | 2012-12-12 | 北京化工大学 | Preparation method of layered compound metal hydroxide for controlling surface defects and surface potentials |
| CN102898849A (en) * | 2012-11-09 | 2013-01-30 | 北京化工大学 | Zinc-base doped layered double-hydroxide ultraviolet barrier material for ageing-resistant asphalt |
| CN102898849B (en) * | 2012-11-09 | 2015-04-15 | 北京化工大学 | Zinc-base doped layered double-hydroxide ultraviolet barrier material for ageing-resistant asphalt |
| CN104087243A (en) * | 2013-04-01 | 2014-10-08 | 上海杰事杰新材料(集团)股份有限公司 | Hydrotalcite-like ultraviolet absorbent and preparation method thereof |
| CN103962157A (en) * | 2014-05-19 | 2014-08-06 | 北京化工大学 | Nano-structure CoSx/C cathode electro-catalytic material and preparation method thereof |
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