CN106185969B - A kind of 2MgOB2O3·1.5H2The preparation method of O nanometer stubs - Google Patents

A kind of 2MgOB2O3·1.5H2The preparation method of O nanometer stubs Download PDF

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CN106185969B
CN106185969B CN201610556120.9A CN201610556120A CN106185969B CN 106185969 B CN106185969 B CN 106185969B CN 201610556120 A CN201610556120 A CN 201610556120A CN 106185969 B CN106185969 B CN 106185969B
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2mgob
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stubs
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oil phase
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CN106185969A (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
    • 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
    • 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
    • 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
    • C01P2004/10—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
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer

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  • Organic Chemistry (AREA)
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Abstract

The invention discloses a kind of 2MgOB2O3·1.5H2The preparation method of O nanometer stubs, this method is first by Mg (NO3)2·6H2O and NH4HB4O7·3H2O is scattered in oil phase, forms microemulsion, then mixes both microemulsions, is the nanometer stub 2MgOB that can obtain having one-dimensional nano structure using solvent-thermal method2O3·1.5H2O.Preparation method of the present invention is simple, and reaction temperature is relatively low, gained 2MgOB2O3·1.5H2The morphology controllable of O nanometer stubs, 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 2MgOB2O3·1.5H2The preparation method of O nanometer stubs
Technical field
The invention belongs to the synthesis technical field of magnesium borate, and in particular to a kind of 2MgOB2O3·1.5H2O nanometers are short The preparation method of rod.
Background technology
One-dimensional (1D) nano material, such as nanometer rods, nano wire, nanotube and nanobelt, because it is in mesoscopic systems and nanometer Technical elements have unique texture and huge application value, so it turns into a hot issue in recent years.Magnesium boric acid Salt be it is important contain boron substance, because it has excellent heat resistance, larger 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 synthesis nanometer boron Sour magnesium.There are chemical vapour deposition technique, thermal evaporation method, flow or supercritical methanol technology known to us at this stage, such method Preparation temperature requires higher, need to could typically be prepared under conditions of higher than 800 DEG C.More such as homogeneous precipitation -ol is molten Glue method, sol-gel process and phase transformation synthetic method.These methods also have the limitation of its own, and this paper innovative point is We use a kind of new synthetic method, and synthesized that other methods can not synthesize at a lower temperature has smaller chi Very little, the uniform single nanometer stub of pattern.Here, we are not only innovated in method, overcome other methods and making Standby upper such as growth conditions requires high, a series of shortcomings such as production control is more difficult, it is often more important that our made nanometers Stub particle diameter is smaller, and output is also more considerable, can be widely used in nanometer technology from now on.
The content of the invention
The technical problems to be solved by the invention are to provide that a kind of reaction temperature is relatively low, have one-dimensional nano structure 2MgO·B2O3·1.5H2The preparation method of O nanometer stubs.
Technical scheme is made up of following step used by solving above-mentioned technical problem：
1st, by Mg (NO3)2·6H2The O aqueous solution, oil phase, surfactant mixing, form microemulsion A, by NH4HB4O7· 3H2The O aqueous solution, oil phase, surfactant mixing, form microemulsion B, wherein Mg (NO3)2·6H2The body of the O aqueous solution and oil phase Product is than being 1:2~6, NH4HB4O7·3H2The volume ratio of the O aqueous solution and oil phase is 1:2~6, described oil phase is n-butanol and ring The volume ratio of hexane is 1:6~12 mixture.
2nd, under agitation, microemulsion A is added dropwise in microemulsion B, wherein Mg (NO3)2·6H2O with NH4HB4O7·3H2O mol ratio is 1:0.5~3, pH value is adjusted to being transferred in reactor after 8~10 with the NaOH aqueous solution, Hydro-thermal reaction 24~48 hours at 160~200 DEG C, room temperature is down to, filters, wash, dry, obtain 2MgOB2O3·1.5H2O Nanometer stub.
In above-mentioned steps 1, preferably Mg (NO3)2·6H2The volume ratio of the O aqueous solution and oil phase is 1:4~5, NH4HB4O7· 3H2The volume ratio 1 of the O aqueous solution and oil phase:4~5, wherein the Mg (NO3)2·6H2The O aqueous solution and NH4HB4O7·3H2O is water-soluble The volume ratio of the concentration of liquid preferably 1~2mol/L, the preferred n-butanol of the oil phase and hexamethylene is 1:8~10 mixture.
In above-mentioned steps 1, the surfactant is PEG20000, Macrogol 4000, cetyl trimethyl Any one in ammonium bromide, dodecyl sodium sulfate, neopelex 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 NH4HB4O7·3H2O mol ratio is 1:1~2.
In above-mentioned steps 2, hydro-thermal reaction 48 hours further preferably 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, is then the nanometer stub that can obtain having one-dimensional nano structure using solvent-thermal method 2MgO·B2O3·1.5H2O.Preparation method of the present invention is simple, and reaction temperature is relatively low, gained 2MgOB2O3·1.5H2O nanometers are 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 knot Structure.
Brief description of the drawings
Fig. 1 is 2MgOB prepared by embodiment 12O3·1.5H2O EDS figures.
Fig. 2 is 2MgOB prepared by Examples 1 and 22O3·1.5H2O X-ray powder diffractions spectrum.
Fig. 3 is 2MgOB prepared by Examples 1 and 22O3·1.5H2O infrared spectrogram.
Fig. 4 is 2MgOB prepared by embodiment 12O3·1.5H2O TG-DTA figures.
Fig. 5 is 2MgOB prepared by embodiment 12O3·1.5H2O SEM figures.
Fig. 6 is 2MgOB prepared by embodiment 22O3·1.5H2O EDS figures.
Fig. 7 is 2MgOB prepared by embodiment 22O3·1.5H2O TG-DTA figures.
Fig. 8 is 2MgOB prepared by embodiment 22O3·1.5H2O SEM figures.
Fig. 9 is 2MgOB prepared by embodiment 32O3·1.5H2O SEM figures.
Figure 10 is 2MgOB prepared by embodiment 42O3·1.5H2O SEM figures.
Embodiment
The present invention is described in more detail with reference to the accompanying drawings and examples, but protection scope of the present invention is not limited only to These embodiments.
Embodiment 1
1st, by 5mL1.5mol/L Mg (NO3)2·6H2The O aqueous solution adds 2mL n-butanols, 20mL hexamethylenes, the poly- second two of 1g In the mixture of alcohol 10000, stir to solution and clarify, form microemulsion A；By 5mL1.5mol/L NH4HB4O7·3H2O is water-soluble Liquid is added in the mixture of 2mL n-butanols, 20mL hexamethylenes, 1g PEG20000s, is stirred to solution and is clarified, and forms micro emulsion Liquid B.
2nd, under agitation, gained microemulsion A is added dropwise in microemulsion B, is stirred after dripping, use NaOH The aqueous solution adjusts pH value to being transferred in reactor after 8, and reactor is placed in baking oven into hydro-thermal reaction 48 hours at 180 DEG C, from Room temperature so is down to, is filtered, after products therefrom is washed with deionized water, absolute ethyl alcohol successively, 65 DEG C of dryings 12 hours in an oven, Obtain 2MgOB2O3·1.5H2O nanometer stubs.
DX-2700 type X-ray powder diffractions instrument, the type Fourier transform infrared light of Tensor 27 is respectively adopted in gained sample Spectrometer, SU8020 type cold field emissions ESEM, Q600 type synchronization TG/DTA thermogravimetric analyzers are characterized respectively, as a result see figure 1~5.
From figure 1 it appears that gained sample contains tetra- kinds of elements of Mg, B, O, Au, without other elements, wherein Au comes from Sample pretreatment it is gold-plated.As shown in Figure 2, sample peak shape and peak position and 2MgOB2O3·H2O is like gained sample Principal character d values be 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 2MgOB2O3·H2O JCPDS cards (File No.33-0859) are consistent.
The peak shape of sample and peak position and 2MgOB in Fig. 32O3·H2O spectrogram is basically identical, 3564cm-1Place is strong to be absorbed Peak is O-H stretching vibration peak；1273cm-1、1212cm-1Locate the in-plane bending vibration that absworption peak is B-O-H；1012cm-1With 836cm-1Place is four-coordination boron oxygen key B (4)-O asymmetry and symmetrical stretching vibration peak；1403cm-1It is respectively three to locate absworption peak It is coordinated boron oxygen key B (3)-O antisymmetry and symmetrical stretching vibration peak； 706cm-1、629cm-1Place's absworption peak is B (3)-O keys Out-of-plane bending vibration peak；1486cm-1And 924cm-1Place's absworption peak is respectively three-fold coordination boron oxygen key B (3)-O antisymmetry and symmetrical Stretching vibration peak.
From thermal multigraph 4, the TG curves of sample are 30~600 DEG C in temperature a continuous weightless section, total weightlessness For 15.41%, in the range of error permission, this and 2MgOB2O3·1.5H2O loses 1.5 H2O calculated value 15.24% matches；In DTA curve, sample has weaker endothermic peak at 585.03 DEG C or so, corresponding to constitution water in sample Or the depigmentation of hydroxyl.
Understand that gained sample is 2MgOB with reference to the analysis result of Fig. 1~42O3·1.5H2O.As seen from Figure 5, gained 2MgO·B2O3·1.5H2O pattern is nanometer stub, and its a diameter of 20~35nm, length are 50~110nm.
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 2MgOB2O3·1.5H2O nanometer stubs.From the characterization result of Fig. 2,3,6,7, gained sample is 2MgO·B2O3·1.5H2O, as seen from Figure 8,2MgOB2O3·1.5H2O pattern 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-butanols, 20mL hexamethylenes, 1g PEG20000s mixture in, stir to solution and clarify, form microemulsion A；By 10mL1.5mol/ L NH4HB4O7·3H2The O aqueous solution is added in the mixture of 2mL n-butanols, 20mL hexamethylenes, 1g PEG20000s, stirring Clarified to solution, form microemulsion B.Other steps are same as Example 1, obtain 2MgOB2O3·1.5H2O nanometers 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-butanols, 16mL hexamethylenes, 1g cetyl trimethylammonium bromides mixture in, stir to solution and clarify, form microemulsion A；Will 5mL1.5mol/L NH4HB4O7·3H2The O aqueous solution adds 2mL n-butanols, 16mL hexamethylenes, 1g cetyl trimethyl brominations In the mixture of ammonium, stir to solution and clarify, form microemulsion B.Other steps are same as Example 1, obtain 2MgOB2O3· 1.5H2O nanometers stub (see Figure 10).

Claims (9)

  1. A kind of 1. 2MgOB2O3·1.5H2The preparation method of O nanometer stubs, it is characterised in that it is made up of following step：
    (1) by Mg (NO3)2·6H2The O aqueous solution, oil phase, surfactant mixing, form microemulsion A, by NH4HB4O7·3H2O water Solution, oil phase, surfactant mixing, form microemulsion B, wherein Mg (NO3)2·6H2The volume ratio of the O aqueous solution and oil phase is 1:2~6, NH4HB4O7·3H2The volume ratio of the O aqueous solution and oil phase is 1:2~6, described oil phase is n-butanol and hexamethylene Volume ratio is 1:6~12 mixture, the surfactant are PEG20000, Macrogol 4000, cetyl three Any one in methyl bromide ammonium, dodecyl sodium sulfate, neopelex；
    (2) under agitation, microemulsion A is added dropwise in microemulsion B, wherein Mg (NO3)2·6H2O and NH4HB4O7· 3H2O mol ratio is 1:0.5~3, with being transferred to after NaOH aqueous solution regulation pH value to 8~10 in reactor, at 160~200 DEG C Lower hydro-thermal reaction 24~48 hours, room temperature is down to, filters, wash, dry, obtain 2MgOB2O3·1.5H2O nanometer stubs.
  2. 2. 2MgOB according to claim 12O3·1.5H2The preparation method of O nanometer stubs, it is characterised in that：In step Suddenly in (1), the Mg (NO3)2·6H2The volume ratio of the O aqueous solution and oil phase is 1:4~5.
  3. 3. 2MgOB according to claim 12O3·1.5H2The preparation method of O nanometer stubs, it is characterised in that：It is described Mg(NO3)2·6H2The concentration of the O aqueous solution is 1~2mol/L.
  4. 4. 2MgOB according to claim 12O3·1.5H2The preparation method of O nanometer stubs, it is characterised in that：In step Suddenly in (1), the NH4HB4O7·3H2The volume ratio of the O aqueous solution and oil phase is 1:4~5.
  5. 5. 2MgOB according to claim 12O3·1.5H2The preparation method of O nanometer stubs, it is characterised in that：It is described NH4HB4O7·3H2The concentration of the O aqueous solution is 1~2mol/L.
  6. 6. 2MgOB according to claim 12O3·1.5H2The preparation method of O nanometer stubs, it is characterised in that：In step Suddenly in (1), the oil phase is that the volume ratio of n-butanol and hexamethylene is 1:8~10 mixture.
  7. 7. 2MgOB according to claim 12O3·1.5H2The preparation method of O nanometer stubs, it is characterised in that：In step Suddenly in (1), quality-volume ratio of described surfactant and oil phase is 1g:15~30mL.
  8. 8. 2MgOB according to claim 12O3·1.5H2The preparation method of O nanometer stubs, it is characterised in that：In step Suddenly in (2), the Mg (NO3)2·6H2O and NH4HB4O7·3H2O mol ratio is 1:1~2.
  9. 9. 2MgOB according to claim 12O3·1.5H2The preparation method of O nanometer stubs, it is characterised in that：It is 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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CN106939166B (en) * 2017-03-16 2018-07-10 陕西师范大学 A kind of 2CaOB2O3·H2O/Mg(OH)2Composite nanometer flame retardant
CN106904627B (en) * 2017-03-16 2019-03-05 陕西师范大学 2MgO·B2O3·1.5H2O/Mg(OH)2Nanometer flame retardent materials and its in-situ preparation method
CN107855096B (en) * 2017-11-20 2020-07-28 陕西师范大学 Preparation of hierarchical porous flower spherical nanostructure 7 MgO.2B by double salt phase inversion2O3·7H2Method of O

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