CN107128956B - A kind of preparation method of soilless sticking ordered nano magnesium oxide material - Google Patents
A kind of preparation method of soilless sticking ordered nano magnesium oxide material Download PDFInfo
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- CN107128956B CN107128956B CN201710482070.9A CN201710482070A CN107128956B CN 107128956 B CN107128956 B CN 107128956B CN 201710482070 A CN201710482070 A CN 201710482070A CN 107128956 B CN107128956 B CN 107128956B
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- 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
- C01F5/02—Magnesia
- C01F5/06—Magnesia by thermal decomposition of magnesium compounds
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- 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
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
Abstract
The present invention relates to a kind of preparation methods of soilless sticking ordered nano magnesium oxide material, secondary nucleation and agglomeration easily occurs in an aqueous medium present invention aim to address nano magnesia presoma present in existing nano oxidized magnesium material preparation process so that crystal is unordered uncontrollable, adsorbs the technical issues of being greatly reduced with degerming performance so as to cause the magnesia finished product of subsequent roasting.The technical scheme is that a kind of preparation method of soilless sticking ordered nano magnesium oxide material, it is using magnesium chloride hexahydrate as magnesium source, ammonium carbonate is precipitating reagent, imidazolium ionic liquid is as dispersing agent and structure directing agent, presoma magnesium carbonate trihydrate is synthesized using nucleation/crystallization isolation method, then roasts to obtain soilless sticking ordered nano magnesium oxide material.The present invention has the characteristics that strong operability, reproducible, non-environmental-pollution, ionic liquid can be recycled, are suitable for mass production;Carrying out at normal temperature in the present invention at nuclear reaction, reduces energy consumption.
Description
Technical field
The invention belongs to field of inorganic material preparing technology, and in particular to a kind of preparation of soilless sticking ordered nano magnesium oxide material
Method.
Background technique
The micro- pollution of heavy metal is always that huge obstinate type pollution is endangered in drinking water.Nanometer magnesium salts oxide has been found
It is one of high performance drinking water micro heavy ion removing medium, there is low molten damage, overbasic excellent speciality, because that can solve
Separate out O2 -Ion and possess splendid antibiotic property, and since isoelectric point up to 12.4 shows unique electrostatic to cation
Capturing ability.Usually by Roasting Decomposition, its carbonate precursor obtains nano magnesia.In recent years, nucleation/crystallization isolation method
Appearance solves the technical problem that nano material is difficult to industrialized production.It separately carries out crystal nucleation and crystallization, utilizes height
Fast colloid mill mechanical agitation during rotation, while fixed tooth and turning generated hydraulic cutter active force between tooth,
So that forming a large amount of tiny nucleus in initial reaction stage explosion type, receiving for uniform particle diameter is then prepared by the hydrothermal crystallizing in later period
Meter level material.The method meets chemical coprecipitation principle, has many advantages, such as that reaction is uniform, temperature is low, speed is fast, high-efficient.Cause
This, first prepares the carbonate precursor of nano magnesia using nucleation/crystallization isolation method, can be obtained and receives using simple roasting
Rice magnesia.
But nano magnesia presoma is because easily occurring secondary nucleation and reuniting existing when being prepared in an aqueous medium
As being greatly reduced so as to cause the magnesia finished product absorption of subsequent roasting and degerming performance so that crystal is unordered uncontrollable, therefore late
Fail to be promoted in practice late, becomes the technical bottleneck that the material of this great potential is hovered always except practical application
One of.According to classical surface chemistry theory analysis, the reason of nanometer Mg salt precursor body is reunited may be very much that surface is negatively charged greatly
Active Mg in the nanometer Mg salt precursor body particle easily adsorbent solution of lotus2+Nucleating growth is carried out on its surface.If wanting to reduce
The appearance of reunion seeks to reduce or eliminate nanometer Mg salt precursor body particle to active Mg after all2+Absorption.Usually side
Method is that dispersing agent, surfactant such as polyethylene glycol, ammonium polymethacrylate, poly- hydroxy acid ammonium etc. are added in the reaction system to receiving
Rice grain is wrapped up, and then removes them by the method for subsequent heat treatment.But additive is organic matter mostly, and it is water-soluble
The intermiscibility of liquid is poor, and the nanoparticle growth that can only leave after being added, process are difficult to control, these disadvantages result in this method
Limitation.
Summary of the invention
Present invention aim to address nano magnesia forerunners present in existing nano oxidized magnesium material preparation process
Easily generation secondary nucleation and agglomeration is unordered uncontrollable down to crystal in an aqueous medium for body, so as to cause receiving for subsequent roasting
The technical issues of absorption of rice magnesia finished product and degerming performance are greatly reduced, provides a kind of soilless sticking ordered nano magnesium oxide material
Preparation method.
In order to solve the above technical problems, the technical solution adopted by the present invention is that: a kind of soilless sticking ordered nano magnesia material
The preparation method of material is using magnesium chloride hexahydrate as magnesium source, and ammonium carbonate is precipitating reagent, and imidazolium ionic liquid is as dispersing agent and knot
Structure directed agents synthesize presoma magnesium carbonate trihydrate using nucleation/crystallization isolation method, then roast to obtain the oxidation of soilless sticking ordered nano
Magnesium material.
Further, a kind of preparation method of soilless sticking ordered nano magnesium oxide material, specific preparation process is as follows:
1) compound concentration is 0.01~1.5molL under room temperature-1Magnesium chloride solution and concentration be 0.01~
1.5mol·L-1Sal volatile, the preparation solute of the magnesium chloride solution is magnesium chloride hexahydrate;
2) by prepared magnesium chloride solution and sal volatile by volume 1:1 with peristaltic pump by setting flow simultaneously add
In the rotating liquid-film reactor for entering to have preset revolving speed and shear gap, while imidazolium ionic liquid is added, and be added
The volume of imidazolium ionic liquid is the 1/10 of the magnesium chloride solution volume being added, carries out into nuclear reaction at normal temperature, has reacted
Collection suspension in Bi Houcong rotating liquid-film reactor outlet is stand-by, and the Recycling Mother Solution containing imidazolium ionic liquid is used as raw material;
3) suspension being collected into is subjected to crystallization, then filters and is washed repeatedly with deionized water filter cake 3~5 times, then
Filter cake is placed in in 50 DEG C of baking oven dry 12h presoma magnesium carbonate trihydrate derived above;
4) the presoma magnesium carbonate trihydrate after drying is placed in Muffle furnace, in 600~800 DEG C of roasting temperature 2h,
Obtain soilless sticking ordered nano magnesium oxide material.
Further, step 2) peristaltic pump sets flow as 1.39~25mLmin-1。
Further, in step 2) rotating liquid-film reactor revolving speed be 1000~5000rpm, shear gap be 0.1~
0.5mm。
Further, imidazolium ionic liquid used is chlorination 1 in step 2), 2- dimethyl -3- butyl imidazole, bromination 1,
In 2- dimethyl -3- butyl imidazole, chlorination 1- cetyl -3- methylimidazole or 1- octyl -3- methyl imidazolium tetrafluoroborate
Any one.
Further, the crystallization temperature in step 3) is 15~30 DEG C, and crystallization time is 1~4h.
Further, the partial size that soilless sticking ordered nano magnesium oxide material is obtained in step 4) is 15~30nm.
The beneficial effects of the present invention are:
1) imidazolium ionic liquid is used for the synthesis of nano magnesia presoma by the present invention, in magnesium source MgCl2·6H2O
(magnesium chloride hexahydrate) and precipitating reagent (NH4)2CO3In nucleation/crystallization isolation method synthetic system that (ammonium carbonate) is constituted, imidazoles is played
The regulation characteristic of base ionic liquid finally obtains favorable dispersibility, crystalline order nano magnesia.
2) imidazole radicals of a certain amount is added when nucleation/crystallization isolation method prepares nano magnesia presoma in the present invention
Ionic liquid, the cation A in ionic liquid ABn+It can have an effect with nano magnesia granular precursor and possess biggish position
Resistance, can prevent active Mg2+In particle surface nucleating growth, particle agglomeration phenomenon is substantially reduced.So, by controllable
Adjust the length of cationic substituent position either side chain substituents to adjust the intensity of itself and particle surface active force, in turn
The degree of scatter of gained nano magnesia granular precursor can be controlled;In addition, imidazolium ionic liquid is easy to make by hydrogen bond
Grow up to orderly self-assembled structures with spontaneously forming, is capable of providing good structure-directing effect;
3) there is strong operability, reproducible, non-environmental-pollution, ionic liquid can be recycled, be suitble to criticize by the present invention
The features such as amount production;Carrying out at normal temperature in the present invention at nuclear reaction, reduces energy consumption, is prepared into nano magnesia and is drinking
There is bright application prospect in the fields such as water sterilization and micro heavy ionic adsorption.
4) present invention not only with high purity, the good dispersion that is prepared into nano oxidized magnesium material, and pattern is orderly, and size is equal
One, the partial size of the nano oxidized magnesium granules of gained is 15~30nm.
Specific embodiment
Below with reference to embodiment, the invention will be further described.
The preparation method of one of the present embodiment soilless sticking ordered nano magnesium oxide material, is using magnesium chloride hexahydrate as magnesium
Source, ammonium carbonate are precipitating reagent, and imidazolium ionic liquid is closed as dispersing agent and structure directing agent using nucleation/crystallization isolation method
At presoma magnesium carbonate trihydrate, then roast to obtain soilless sticking ordered nano magnesium oxide material.
Specific preparation process is as follows:
1) compound concentration is 0.01~1.5molL under room temperature-1Magnesium chloride solution and concentration be 0.01~
1.5mol·L-1Sal volatile, the preparation solute of the magnesium chloride solution is magnesium chloride hexahydrate;
2) by prepared magnesium chloride solution and sal volatile by volume 1:1 with peristaltic pump by setting flow simultaneously add
In the rotating liquid-film reactor for entering to have preset revolving speed and shear gap, the peristaltic pump set flow as 1.39~
25mL·min-1, the revolving speed of the rotating liquid-film reactor is 1000~5000rpm, and shear gap is 0.1~0.5mm;Simultaneously
Imidazolium ionic liquid is added, and the volume for the imidazolium ionic liquid being added is the 1/10 of the magnesium chloride solution volume being added,
Nuclear reaction is carried out at normal temperature, it is stand-by from rotating liquid-film reactor outlet collection suspension after completion of the reaction, imidazole radicals will be contained
The Recycling Mother Solution of ionic liquid is used as raw material;
3) suspension being collected into is subjected to crystallization, crystallization temperature is 15~30 DEG C, and crystallization time is 1~4h, then mistake
It filters and is washed repeatedly with deionized water filter cake 3~5 times, then filter cake is placed in dry 12h forerunner derived above in 50 DEG C of baking oven
Body magnesium carbonate trihydrate;
4) the presoma magnesium carbonate trihydrate after drying is placed in Muffle furnace, in 600~800 DEG C of roasting temperature 2h,
Obtain the soilless sticking ordered nano magnesium oxide material that partial size is 15~30nm.
The imidazolium ionic liquid is chlorination 1,2- dimethyl -3- butyl imidazole, bromination 1,2- dimethyl -3- butyl miaow
Any one in azoles, chlorination 1- cetyl -3- methylimidazole or 1- octyl -3- methyl imidazolium tetrafluoroborate.
Embodiment 1
The preparation method of one of the present embodiment soilless sticking ordered nano magnesium oxide material, is using magnesium chloride hexahydrate as magnesium
Source, ammonium carbonate are precipitating reagent, and imidazolium ionic liquid is closed as dispersing agent and structure directing agent using nucleation/crystallization isolation method
At presoma magnesium carbonate trihydrate, then roast to obtain soilless sticking ordered nano magnesium oxide material.
Specific preparation process is as follows:
1) compound concentration is 0.01molL under room temperature-1Magnesium chloride solution and concentration be 0.01molL-1Carbon
Each 250ml of acid ammonium solution, the preparation solute of the magnesium chloride solution are magnesium chloride hexahydrate;
2) by prepared magnesium chloride solution and sal volatile by volume 1:1 with peristaltic pump by setting flow simultaneously add
In the rotating liquid-film reactor for entering to have preset revolving speed and shear gap, the peristaltic pump sets flow as 15mLmin-1, the revolving speed of the rotating liquid-film reactor is 1000rpm, shear gap 0.3mm;25ml chlorination 1,2- diformazan is added simultaneously
Base -3- butyl imidazole, carries out into nuclear reaction at normal temperature, exports collection suspension from rotating liquid-film reactor after completion of the reaction and waits for
With by the Recycling Mother Solution containing imidazolium ionic liquid as raw material;
3) suspension being collected into is subjected to crystallization, crystallization temperature is 20 DEG C, then crystallization time 1h is filtered and spent
Ionized water washs filter cake 3~5 times repeatedly, then filter cake is placed in dry 12h three water carbon of presoma derived above in 50 DEG C of baking oven
Sour magnesium;
4) the presoma magnesium carbonate trihydrate after drying is placed in Muffle furnace, in 600~800 DEG C of roasting temperature 2h,
Obtain the soilless sticking ordered nano magnesium oxide material that partial size is 15~30nm.
Embodiment 2
The preparation method of one of the present embodiment soilless sticking ordered nano magnesium oxide material, is using magnesium chloride hexahydrate as magnesium
Source, ammonium carbonate are precipitating reagent, and imidazolium ionic liquid is closed as dispersing agent and structure directing agent using nucleation/crystallization isolation method
At presoma magnesium carbonate trihydrate, then roast to obtain soilless sticking ordered nano magnesium oxide material.
Specific preparation process is as follows:
1) compound concentration is 0.8molL under room temperature-1Magnesium chloride solution and concentration be 0.8molL-1Carbonic acid
Each 250ml of ammonium salt solution, the preparation solute of the magnesium chloride solution are magnesium chloride hexahydrate;
2) by prepared magnesium chloride solution and sal volatile by volume 1:1 with peristaltic pump by setting flow simultaneously add
In the rotating liquid-film reactor for entering to have preset revolving speed and shear gap, the peristaltic pump sets flow as 1.39mL
min-1, the revolving speed of the rotating liquid-film reactor is 3000rpm, shear gap 0.1mm;25ml chlorination 1,2- bis- is added simultaneously
Methyl -3- butyl imidazole, carries out into nuclear reaction at normal temperature, exports from rotating liquid-film reactor collect suspension after completion of the reaction
For use, the Recycling Mother Solution containing imidazolium ionic liquid is used as raw material;
3) suspension being collected into is subjected to crystallization, crystallization temperature is 15 DEG C, then crystallization time 4h is filtered and spent
Ionized water washs filter cake 3~5 times repeatedly, then filter cake is placed in dry 12h three water carbon of presoma derived above in 50 DEG C of baking oven
Sour magnesium;
4) the presoma magnesium carbonate trihydrate after drying is placed in Muffle furnace, in 600~800 DEG C of roasting temperature 2h,
Obtain the soilless sticking ordered nano magnesium oxide material that partial size is 15~30nm.
Embodiment 3
The preparation method of one of the present embodiment soilless sticking ordered nano magnesium oxide material, is using magnesium chloride hexahydrate as magnesium
Source, ammonium carbonate are precipitating reagent, and imidazolium ionic liquid is closed as dispersing agent and structure directing agent using nucleation/crystallization isolation method
At presoma magnesium carbonate trihydrate, then roast to obtain soilless sticking ordered nano magnesium oxide material.
Specific preparation process is as follows:
1) compound concentration is 1.5molL under room temperature-1Magnesium chloride solution and concentration be 1.5molL-1Carbonic acid
Each 250ml of ammonium salt solution, the preparation solute of the magnesium chloride solution are magnesium chloride hexahydrate;
2) by prepared magnesium chloride solution and sal volatile by volume 1:1 with peristaltic pump by setting flow simultaneously add
In the rotating liquid-film reactor for entering to have preset revolving speed and shear gap, the peristaltic pump sets flow as 25mLmin-1, the revolving speed of the rotating liquid-film reactor is 5000rpm, shear gap 0.5mm;25ml chlorination 1,2- diformazan is added simultaneously
Base -3- butyl imidazole, carries out into nuclear reaction at normal temperature, exports collection suspension from rotating liquid-film reactor after completion of the reaction and waits for
With by the Recycling Mother Solution containing imidazolium ionic liquid as raw material;
3) suspension being collected into is subjected to crystallization, crystallization temperature is 30 DEG C, then crystallization time 2h is filtered and spent
Ionized water washs filter cake 3~5 times repeatedly, then filter cake is placed in dry 12h three water carbon of presoma derived above in 50 DEG C of baking oven
Sour magnesium;
4) the presoma magnesium carbonate trihydrate after drying is placed in Muffle furnace, in 600~800 DEG C of roasting temperature 2h,
Obtain the soilless sticking ordered nano magnesium oxide material that partial size is 15~30nm.
Imidazolium ionic liquid chlorination 1,2- dimethyl -3- butyl imidazole in above-described embodiment can use bromination 1,2- diformazan
Base -3- butyl imidazole, chlorination 1- cetyl -3- methylimidazole or 1- octyl -3- methyl imidazolium tetrafluoroborate replace;And institute
It is that analysis is pure with imidazolium ionic liquid, concentration is greater than 99%.
Claims (7)
1. a kind of preparation method of soilless sticking ordered nano magnesium oxide material, it is characterised in that: be using magnesium chloride hexahydrate as magnesium source,
Ammonium carbonate is precipitating reagent, and imidazolium ionic liquid is as dispersing agent and structure directing agent, using nucleation/crystallization isolation method synthesis three
Aqueous carbonate magnesium, then roast to obtain soilless sticking ordered nano magnesium oxide material.
2. a kind of preparation method of soilless sticking ordered nano magnesium oxide material according to claim 1, which is characterized in that tool
Preparation step is as follows:
1) compound concentration is 0.01~1.5molL under room temperature-1Magnesium chloride solution and concentration be 0.01~1.5mol
L-1Sal volatile, the preparation solute of the magnesium chloride solution is magnesium chloride hexahydrate;
2) by prepared magnesium chloride solution and sal volatile, by setting flow, addition is pre- simultaneously with peristaltic pump by 1:1 by volume
The imidazoles in the rotating liquid-film reactor for first setting revolving speed and shear gap, while imidazolium ionic liquid being added, and being added
The volume of base ionic liquid is the 1/10 of the magnesium chloride solution volume being added, carries out into nuclear reaction at normal temperature, after completion of the reaction
It is stand-by from rotating liquid-film reactor outlet collection suspension, the Recycling Mother Solution containing imidazolium ionic liquid is used as raw material;
3) suspension being collected into is subjected to crystallization, then filters and is washed repeatedly with deionized water filter cake 3~5 times, then will filter
Cake is placed in 50 DEG C of baking oven dry 12h presoma magnesium carbonate trihydrate derived above;
4) the presoma magnesium carbonate trihydrate after drying is placed in Muffle furnace, 600~800 DEG C of roasting temperature 2h to get
To soilless sticking ordered nano magnesium oxide material.
3. a kind of preparation method of soilless sticking ordered nano magnesium oxide material according to claim 2, it is characterised in that: step
Rapid 2) peristaltic pump sets flow as 1.39~25mLmin-1。
4. a kind of preparation method of soilless sticking ordered nano magnesium oxide material according to claim 2, it is characterised in that: step
It is rapid 2) in rotating liquid-film reactor revolving speed be 1000~5000rpm, shear gap be 0.1~0.5mm.
5. a kind of preparation method of soilless sticking ordered nano magnesium oxide material according to claim 2, it is characterised in that: step
It is rapid 2) in imidazolium ionic liquid used be chlorination 1,2- dimethyl -3- butyl imidazole, bromination 1,2- dimethyl -3- butyl miaow
Any one in azoles, chlorination 1- cetyl -3- methylimidazole or 1- octyl -3- methyl imidazolium tetrafluoroborate.
6. a kind of preparation method of soilless sticking ordered nano magnesium oxide material according to claim 2, it is characterised in that: step
It is rapid 3) in crystallization temperature be 15~30 DEG C, crystallization time be 1~4h.
7. a kind of preparation method of soilless sticking ordered nano magnesium oxide material according to claim 2, it is characterised in that: step
It is rapid 4) in obtain soilless sticking ordered nano magnesium oxide material partial size be 15~30nm.
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CN1361062A (en) * | 2000-12-28 | 2002-07-31 | 北京化工大学 | Prepn of nanometer-sized magnesium hydroxide |
CN101523168A (en) * | 2006-10-02 | 2009-09-02 | 新加坡纳米材料科技公司 | Process for making nano-sized and micro-sized precipitate particles |
CN102145910A (en) * | 2011-02-24 | 2011-08-10 | 四川大学 | Method for preparing calcium carbonate of different morphologies from ionic liquid |
CN102491396A (en) * | 2011-11-30 | 2012-06-13 | 厦门大学 | Method for preparing nanometer calcium carbonate |
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