CN106185969A - A kind of 2MgO B2o31.5H2the preparation method of O nanometer stub - Google Patents

A kind of 2MgO B2o31.5H2the preparation method of O nanometer stub Download PDF

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CN106185969A
CN106185969A CN201610556120.9A CN201610556120A CN106185969A CN 106185969 A CN106185969 A CN 106185969A CN 201610556120 A CN201610556120 A CN 201610556120A CN 106185969 A CN106185969 A CN 106185969A
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2mgo
preparation
oil phase
aqueous solution
nanometer stub
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CN106185969B (en
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刘志宏
张蕾
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Shaanxi Normal University
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B35/00—Boron; Compounds thereof
    • C01B35/08—Compounds containing boron and nitrogen, phosphorus, oxygen, sulfur, selenium or tellurium
    • C01B35/10—Compounds containing boron and oxygen
    • C01B35/12—Borates
    • C01B35/126—Borates of alkaline-earth metals, beryllium, aluminium or magnesium
    • 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
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    • C01—INORGANIC CHEMISTRY
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    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
    • C01P2002/85—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by XPS, EDX or EDAX data
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
    • C01P2002/88—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by thermal analysis data, e.g. TGA, DTA, DSC
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    • 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
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    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
    • C01P2004/16—Nanowires or nanorods, i.e. solid nanofibres with two nearly equal dimensions between 1-100 nanometer
    • 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
    • C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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    • C01P2004/60—Particles characterised by their size
    • C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer

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Abstract

The invention discloses a kind of 2MgO B2O3·1.5H2The preparation method of O nanometer stub, the method is first by Mg (NO3)2·6H2O and NH4HB4O7·3H2O is scattered in oil phase, forms microemulsion, is then mixed by both microemulsions, uses solvent-thermal method i.e. can obtain the nanometer stub 2MgO B with one-dimensional nano structure2O3·1.5H2O.Preparation method of the present invention is simple, and reaction temperature is relatively low, gained 2MgO B2O3·1.5H2The morphology controllable of O nanometer stub, its diameter is about 20～35nm, length is about 50～110nm, and fire resistance is significantly better than non-nano structure.

Description

A kind of 2MgO B2O3·1.5H2The preparation method of O nanometer stub
Technical field
The invention belongs to the boratory synthesis technical field of magnesium, be specifically related to a kind of 2MgO B2O3·1.5H2O nanometer is short The preparation method of rod.
Background technology
One-dimensional (1D) nano material, such as nanometer rods, nano wire, nanotube and nano belt, because it is in mesoscopic systems and nanometer Technical elements has unique texture and huge using value, so it becomes a hot issue in recent years.Magnesium boric acid Salt is important containing boron substance, owing to it has excellent thermostability, bigger coefficient of elasticity, birefringece crystal structure, preferably Anticorrosion and abrasion resistance, so magnesium borate is widely used.A series of method can be used for synthesizing nanometer boron Acid magnesium.Present stage we known have chemical vapour deposition technique, thermal evaporation method, flow or supercritical methanol technology, this type of method Preparation temperature requires higher, typically could need to prepare under conditions of higher than 800 DEG C.Also have some such as homogeneous precipitation-ol molten Glue method, sol-gel process and phase transformation synthetic method.These methods also have the limitation of himself, and innovative point herein is We use a kind of novel synthetic method, and synthesized that other method can not synthesize at a lower temperature has less chi The nanometer stub that very little, pattern is the most single.Here, we are not only innovated in method, overcome other method in system Standby upper such as growth conditions requires height, produces and controls a series of shortcomings such as more difficult, it is often more important that the nanometer that we are made Stub particle diameter is less, and volume of production is the most considerable, can be widely used in nanotechnology from now on.
Summary of the invention
The technical problem to be solved is to provide a kind of reaction temperature relatively low, has one-dimensional nano structure 2MgO·B2O3·1.5H2The preparation method of O nanometer stub.
Solve the technical scheme that above-mentioned technical problem used to be made up of following step:
1, by Mg (NO3)2·6H2O aqueous solution, oil phase, surfactant mix, and form microemulsion A, by NH4HB4O7· 3H2O aqueous solution, oil phase, surfactant mix, and form microemulsion B, wherein Mg (NO3)2·6H2O aqueous solution and the body of oil phase Long-pending ratio is 1:2～6, NH4HB4O7·3H2O aqueous solution is 1:2～6 with the volume ratio of oil phase, and described oil phase is n-butyl alcohol and ring The volume ratio of hexane is the mixture of 1:6～12.
2, under agitation, microemulsion A is added dropwise in microemulsion B, wherein Mg (NO3)2·6H2O with NH4HB4O7·3H2The mol ratio of O is 1:0.5～3, proceeds in reactor with NaOH aqueous solution regulation pH value to 8～10, Hydro-thermal reaction 24～48 hours at 160～200 DEG C, be down to room temperature, sucking filtration, washs, is dried, and obtains 2MgO B2O3·1.5H2O Nanometer stub.
In above-mentioned steps 1, preferably Mg (NO3)2·6H2O aqueous solution is 1:4～5, NH with the volume ratio of oil phase4HB4O7· 3H2O aqueous solution and volume ratio 1:4～5 of oil phase, wherein said Mg (NO3)2·6H2O aqueous solution and NH4HB4O7·3H2O is water-soluble The mixture that volume ratio is 1:8～10 of the concentration of liquid preferably 1～2mol/L, the preferred n-butyl alcohol of described oil phase and hexamethylene.
In above-mentioned steps 1, described surfactant is PEG20000, Macrogol 4000, cetyl trimethyl Any one in ammonium bromide, dodecyl sodium sulfate, dodecylbenzene sodium sulfonate etc., the matter of preferred surfactant and oil phase Amount-volume ratio is 1g:15～30mL.
In above-mentioned steps 2, preferably Mg (NO3)2·6H2O and NH4HB4O7·3H2The mol ratio of O is 1:1～2.
In above-mentioned steps 2, further preferably hydro-thermal reaction 48 hours at 180 DEG C.
The present invention is first by Mg (NO3)2·6H2O and NH4HB4O7·3H2O is scattered in oil phase, forms microemulsion, then will Both microemulsion mixing, in this system, two kinds of immiscible continuous medias are divided into by surfactant parents' molecule Short space forms microreactor, then uses solvent-thermal method i.e. can obtain the nanometer stub with one-dimensional nano structure 2MgO·B2O3·1.5H2O.Preparation method of the present invention is simple, and reaction temperature is relatively low, gained 2MgO B2O3·1.5H2O nanometer is short The morphology controllable of rod, its diameter is about 20～35nm, length is about 50～110nm, and fire resistance is significantly better than non-nano structure.
Accompanying drawing explanation
Fig. 1 is the 2MgO B of embodiment 1 preparation2O3·1.5H2The EDS figure of O.
Fig. 2 is the 2MgO B of embodiment 1 and 2 preparation2O3·1.5H2The X-ray powder diffraction spectrum of O.
Fig. 3 is the 2MgO B of embodiment 1 and 2 preparation2O3·1.5H2The infrared spectrogram of O.
Fig. 4 is the 2MgO B of embodiment 1 preparation2O3·1.5H2The TG-DTA figure of O.
Fig. 5 is the 2MgO B of embodiment 1 preparation2O3·1.5H2The SEM figure of O.
Fig. 6 is the 2MgO B of embodiment 2 preparation2O3·1.5H2The EDS figure of O.
Fig. 7 is the 2MgO B of embodiment 2 preparation2O3·1.5H2The TG-DTA figure of O.
Fig. 8 is the 2MgO B of embodiment 2 preparation2O3·1.5H2The SEM figure of O.
Fig. 9 is the 2MgO B of embodiment 3 preparation2O3·1.5H2The SEM figure of O.
Figure 10 is the 2MgO B of embodiment 4 preparation2O3·1.5H2The SEM figure of O.
Detailed description of the invention
The present invention is described in more detail with embodiment below in conjunction with the accompanying drawings, but protection scope of the present invention is not limited only to These embodiments.
Embodiment 1
1, by 5mL1.5mol/L Mg (NO3)2·6H2O aqueous solution adds 2mL n-butyl alcohol, 20mL hexamethylene, the poly-second of 1g two In the mixture of alcohol 10000, stir and clarify to solution, form microemulsion A；By 5mL1.5mol/L NH4HB4O7·3H2O is water-soluble Liquid adds in the mixture of 2mL n-butyl alcohol, 20mL hexamethylene, 1g PEG20000, stirs and clarifies to solution, forms microemulsion Liquid B.
2, under agitation, gained microemulsion A is added dropwise in microemulsion B, stirs after dripping, use NaOH Aqueous solution regulation pH value proceeds in reactor after 8, and reactor is placed in baking oven hydro-thermal reaction 48 hours at 180 DEG C, from So being down to room temperature, sucking filtration, products therefrom is successively with after deionized water, absolute ethanol washing, and 65 DEG C are dried 12 hours in an oven, Obtain 2MgO B2O3·1.5H2O nanometer stub.
Gained sample is respectively adopted DX-2700 type X-ray powder diffractometer, Tensor 27 type Fourier transform infrared light Spectrometer, SU8020 type cold field emission scanning electron microscope, Q600 type synchronize TG/DTA thermogravimetric analyzer and characterize respectively, and result is shown in figure 1～5.
From figure 1 it appears that gained sample contains tetra-kinds of elements of Mg, B, O, Au, there is no other element, wherein Au from Sample pretreatment gold-plated.As shown in Figure 2, sample peak shape and peak position and 2MgO B2O3·H2O like, gained sample Principal character d value is 6.294,5.230,3.880,3.232,2.994,2.668,2.428,2.313,2.209,2.083, 1.995、Its feature interplanar distance d value and 2MgO B2O3·H2The JCPDS card (File No.33-0859) of O is consistent.
The peak shape of sample and peak position and 2MgO B in Fig. 32O3·H2The spectrogram of O is basically identical, 3564cm-1Place is strong to be absorbed Peak is the stretching vibration peak of O-H；1273cm-1、1212cm-1Place's absworption peak is the in-plane bending vibration of B-O-H；1012cm-1With 836cm-1Place is the asymmetric and symmetrical stretching vibration peak of four-coordination boron oxygen key B (4)-O；1403cm-1Place's absworption peak is respectively three The antisymmetry of coordination boron oxygen key B (3)-O and symmetrical stretching vibration peak；706cm-1、629cm-1Place's absworption peak is the face of B (3)-O key Outside sweep vibration peak；1486cm-1And 924cm-1Place's absworption peak is respectively the antisymmetry of three-fold coordination boron oxygen key B (3)-O and symmetry is stretched Contracting vibration peak.
From thermal multigraph 4, the TG curve of sample is 30～600 DEG C in temperature a continuous weightless section, total weightlessness It is 15.41%, in the range of error allows, this and 2MgO B2O3·1.5H2O loses 1.5 H2The calculated value of O 15.24% matches；In DTA curve, sample has more weak endothermic peak at about 585.03 DEG C, corresponding to constitution water in sample Or the depigmentation of hydroxyl.
Analysis result in conjunction with Fig. 1～4 understands, and gained sample is 2MgO B2O3·1.5H2O.As seen from Figure 5, gained 2MgO·B2O3·1.5H2The pattern of O is nanometer stub, and they are a diameter of 20～35nm, a length of 50～110nm years old.
Embodiment 2
In the present embodiment, reactor is placed in baking oven hydro-thermal reaction 48 hours at 200 DEG C, other steps and embodiment 1 is identical, obtains 2MgO B2O3·1.5H2O nanometer stub.From the characterization result of Fig. 2,3,6,7, gained sample is 2MgO·B2O3·1.5H2O, as seen from Figure 8,2MgO B2O3·1.5H2The pattern of O is nanometer stub, and its its diameter is about 20 ～35nm, length are about 50～110nm.
Embodiment 3
In the step 1 of embodiment 1, by 5mL 1.5mol/L Mg (NO3)2·6H2O aqueous solution addition 2mL n-butyl alcohol, 20mL hexamethylene, 1g PEG20000 mixture in, stir to solution clarify, formed microemulsion A；By 10mL1.5mol/ L NH4HB4O7·3H2O aqueous solution adds in the mixture of 2mL n-butyl alcohol, 20mL hexamethylene, 1g PEG20000, stirring Clarify to solution, form microemulsion B.Other steps are same as in Example 1, obtain 2MgO B2O3·1.5H2O nanometer stub (see Fig. 9).
Embodiment 4
In the step 1 of embodiment 1, by 10mL 1.5mol/L Mg (NO3)2·6H2O aqueous solution addition 2mL n-butyl alcohol, 16mL hexamethylene, 1g cetyl trimethylammonium bromide mixture in, stir to solution clarify, formed microemulsion A；Will 5mL1.5mol/L NH4HB4O7·3H2O aqueous solution adds 2mL n-butyl alcohol, 16mL hexamethylene, 1g cetyl trimethyl bromination In the mixture of ammonium, stir and clarify to solution, form microemulsion B.Other steps are same as in Example 1, obtain 2MgO B2O3· 1.5H2O nanometer stub (see Figure 10).

Claims (10)

1. a 2MgO B2O3·1.5H2The preparation method of O nanometer stub, it is characterised in that it is made up of following step:
(1) by Mg (NO3)2·6H2O aqueous solution, oil phase, surfactant mix, and form microemulsion A, by NH4HB4O7·3H2O water Solution, oil phase, surfactant mix, and form microemulsion B, wherein Mg (NO3)2·6H2O aqueous solution with the volume ratio of oil phase is 1:2～6, NH4HB4O7·3H2O aqueous solution is 1:2～6 with the volume ratio of oil phase, and described oil phase is n-butyl alcohol and hexamethylene Volume ratio is the mixture of 1:6～12；
(2) under agitation, microemulsion A is added dropwise in microemulsion B, wherein Mg (NO3)2·6H2O and NH4HB4O7· 3H2The mol ratio of O is 1:0.5～3, proceeds in reactor, at 160～200 DEG C with NaOH aqueous solution regulation pH value to 8～10 Lower hydro-thermal reaction 24～48 hours, be down to room temperature, sucking filtration, washs, is dried, and obtains 2MgO B2O3·1.5H2O nanometer stub.
2MgO B the most according to claim 12O3·1.5H2The preparation method of O nanometer stub, it is characterised in that: in step Suddenly in (1), described Mg (NO3)2·6H2O aqueous solution is 1:4～5 with the volume ratio of oil phase.
2MgO B the most according to claim 12O3·1.5H2The preparation method of O nanometer stub, it is characterised in that: described Mg(NO3)2·6H2The concentration of O aqueous solution is 1～2mol/L.
2MgO B the most according to claim 12O3·1.5H2The preparation method of O nanometer stub, it is characterised in that: in step Suddenly in (1), described NH4HB4O7·3H2O aqueous solution is 1:4～5 with the volume ratio of oil phase.
2MgO B the most according to claim 12O3·1.5H2The preparation method of O nanometer stub, it is characterised in that: described NH4HB4O7·3H2The concentration of O aqueous solution is 1～2mol/L.
2MgO B the most according to claim 12O3·1.5H2The preparation method of O nanometer stub, it is characterised in that: in step Suddenly, in (1), described oil phase is the mixture that volume ratio is 1:8～10 of n-butyl alcohol and hexamethylene.
7. according to the 2MgO B described in claim 1～6 any one2O3·1.5H2The preparation method of O nanometer stub, it is special Levying and be: in step (1), described surfactant is PEG20000, Macrogol 4000, cetyl trimethyl Any one in ammonium bromide, dodecyl sodium sulfate, dodecylbenzene sodium sulfonate.
2MgO B the most according to claim 72O3·1.5H2The preparation method of O nanometer stub, it is characterised in that: in step Suddenly, in (1), described surfactant is 1g:15～30mL with the quality-volume ratio of oil phase.
2MgO B the most according to claim 12O3·1.5H2The preparation method of O nanometer stub, it is characterised in that: in step Suddenly in (2), described Mg (NO3)2·6H2O and NH4HB4O7·3H2The mol ratio of O is 1:1～2.
2MgO B the most according to claim 12O3·1.5H2The preparation method of O nanometer stub, it is characterised in that: described In step (2), hydro-thermal reaction 48 hours at 180 DEG C.
CN201610556120.9A 2016-07-14 2016-07-14 A kind of 2MgOB2O3·1.5H2The preparation method of O nanometer stubs Expired - Fee Related CN106185969B (en)

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CN106904627A (en) * 2017-03-16 2017-06-30 陕西师范大学 2MgO·B2O3·1.5H2O/Mg(OH)2Nanometer flame retardent materials and its in-situ preparation method
CN106939166A (en) * 2017-03-16 2017-07-11 陕西师范大学 A kind of 2CaOB2O3·H2O/Mg(OH)2Composite nanometer flame retardant
CN107855096A (en) * 2017-11-20 2018-03-30 陕西师范大学 A kind of double salt inversion of phases prepares multi-stage porous flower ball-shaped nanostructured 7MgO2B2O3·7H2O method

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