CN103482703A - Preparation method of barium molybdate micro-nano powder having controllable morphology and particle size - Google Patents
Preparation method of barium molybdate micro-nano powder having controllable morphology and particle size Download PDFInfo
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- CN103482703A CN103482703A CN201310470191.3A CN201310470191A CN103482703A CN 103482703 A CN103482703 A CN 103482703A CN 201310470191 A CN201310470191 A CN 201310470191A CN 103482703 A CN103482703 A CN 103482703A
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Abstract
The invention relates to a preparation method of an inorganic functional material, and especially relates to a preparation method of barium molybdate micro-nano powder having a controllable morphology and a particle size. The problems of easy agglomeration in the preparation process, and large particle size, non-uniform particle size distribution and difficult morphology control of prepared BaMoO4 powder of present methods are solved in the invention. The method comprises the following steps: 1, processing barium nitrate and sodium citrate to prepare a mixed solution A; 2, processing sodium molybdate to prepare a solution B; 3, dumping the solution B to the mixed solution A under stirring to obtain a new mixed solution, adjusting the pH value of the new mixed solution, and carrying out a hydrothermal reaction when the new solution is milky in color after a chemical reaction to obtain a white solid-liquid mixture; and 4, centrifuging the white solid-liquid mixture, washing, and drying to obtain barium molybdate micro-nano powder. The obtained powder is spherical in shape, has a particle size of about 500nm, is small and uniform, and can be used for preparing inorganic nonmetal powder materials.
Description
Technical field
The present invention relates to a kind of preparation of inorganic functional material, particularly the preparation method of the controlled barium molybdate micro-nano powder of a kind of pattern particle diameter.
Background technology
Alkali-earth metal oxide hydrochlorate BaSO
4, SrSO
4and BaCrO
4deng being rhombic system at normal temperatures, there is good thermostability, all shown good lubricity in wide temperature range, in the high temperature self-lubricating composite field, receive much concern.Recent study is found, barium molybdate is tetragonal system at normal temperatures, all have huge using value as high temperature self-lubricating composite, luminescent material, fire retardant material etc., the metal barium molybdate that under nanoscale, dispersing property is good possesses significant advantage when preparing high temperature self-lubricating composite material.
But the BaMoO of existing preparation method's gained
4powder mostly is micron order, and particle diameter is 5 μ m~10 μ m, is four rib bipyramid structures or loose spherical.And very easily produce agglomeration in preparation process, make size distribution inhomogeneous, when preparing matrix material, through long mix and blend, still can't make each component of matrix material well disperse, cause the matrix material of preparing to have very large performance deficiency.
Summary of the invention
The present invention easily produces for solving in existing method preparation process the BaMoO that reunites and make
4the problem such as diameter of particle is large, size distribution is inhomogeneous and pattern is wayward, and the preparation method of the controlled barium molybdate micro-nano powder of a kind of pattern particle diameter is provided.
The preparation method of the barium molybdate micro-nano powder that a kind of pattern particle diameter of the present invention is controlled carries out according to the following steps:
One, after nitrate of baryta and Trisodium Citrate are mixed, add deionized water, take stirring velocity as 300r/min~500r/min after to be dissolved, stir 20min~40min, be configured to the mixed solution A that concentration is 0.1mol/L~0.5mol/L; The mass ratio of described nitrate of baryta and Trisodium Citrate is 1:(0.05~0.5); The quality of described nitrate of baryta is 5.23g:(80~120 with the ratio of the volume of deionized water) mL;
Two, add deionized water in Sodium orthomolybdate, to be dissolved after, take stirring velocity as 300r/min~500r/min, stir 0.5h~1h, be configured to the solution B that concentration is 0.1mol/L~0.5mol/L; The mass ratio of the Sodium orthomolybdate described in the nitrate of baryta described in step 1 and step 2 is 1:(0.5~1.5); The quality of the nitrate of baryta described in step 1 is 4.84g:(80~120 with the ratio of the volume of the deionized water described in step 2) mL;
Three, the mixed solution A of step 1 is placed under the constant temperature that temperature is room temperature, take stirring velocity as 300r/min~500r/min, continue to stir, in 10s~60s, the solution B of step 2 is poured in the mixed solution A of step 1, then in 10s~60s, regulator solution pH value is 5~8, reaction 10min~30min, solution becomes oyster white, proceed in the hydrothermal reaction kettle of sealing, and, under the condition that is 80~160 ℃ in temperature by the hydrothermal reaction kettle of sealing, hydro-thermal reaction 8h~18h, obtain white solidliquid mixture;
Four, white solidliquid mixture step 3 obtained carries out centrifugation, then white solid centrifugation gone out is washed, first use absolute ethanol washing 3~5 times, and then with deionized water wash 3~5 times, put into baking oven after washing, under the condition that is 40~60 ℃ in temperature, dry 6h~16h, obtain the barium molybdate micro-nano powder.
Preparation method of the present invention selects Trisodium Citrate as the morphology control agent, using distilled water and alcohol as reaction soln, take Sodium orthomolybdate and nitrate of baryta as reactant, first configure the mixing solutions of nitrate of baryta and Trisodium Citrate, configure again the mixing solutions of Sodium orthomolybdate and alcohol, then the mixing solutions of Sodium orthomolybdate and alcohol is poured in the mixing solutions of the nitrate of baryta of vigorous stirring and Trisodium Citrate, after utilizing ammoniacal liquor and hydrochloric acid to regulate the pH of mixing solutions under the vigorous stirring state, hydro-thermal reaction for some time takes out centrifugal, washing, drying obtains the barium molybdate micro-nano powder, preparation method of the present invention has solved existing method and be inconvenient to control the granular size of product and the difficult problem of granule-morphology in reaction process, reach the pattern of control barium molybdate micro-nano powder and the purpose of particle diameter by add-on and the hydrothermal temperature of controlling Trisodium Citrate, and it is simple that preparation method of the present invention has production technique, production process safety, reaction temperature and safety, with low cost, advantage without complicated additive, the barium molybdate micro-nano powder prepared, be difficult for reuniting, size distribution is even, particle diameter little (500nm left and right), good dispersity, can be widely used in the preparation of inorganic non-metallic powder body material.
The accompanying drawing explanation
Fig. 1 is the electron microscope photo scanning of test one;
Fig. 2 is the X ray diffracting spectrum of test one.
Embodiment
Technical scheme of the present invention is not limited to following embodiment, also comprises the arbitrary combination between each embodiment.
Embodiment one: the preparation method of the barium molybdate micro-nano powder that a kind of pattern particle diameter of present embodiment is controlled carries out according to the following steps:
One, after nitrate of baryta and Trisodium Citrate are mixed, add deionized water, take stirring velocity as 300r/min~500r/min after to be dissolved, stir 20min~40min, be configured to the mixed solution A that concentration is 0.1mol/L~0.5mol/L; The mass ratio of described nitrate of baryta and Trisodium Citrate is 1:(0.05~0.5); The quality of described nitrate of baryta is 5.23g:(80~120 with the ratio of the volume of deionized water) mL;
Two, add deionized water in Sodium orthomolybdate, to be dissolved after, take stirring velocity as 300r/min~500r/min, stir 0.5h~1h, be configured to the solution B that concentration is 0.1mol/L~0.5mol/L; The mass ratio of the Sodium orthomolybdate described in the nitrate of baryta described in step 1 and step 2 is 1:(0.5~1.5); The quality of the nitrate of baryta described in step 1 is 4.84g:(80~120 with the ratio of the volume of the deionized water described in step 2) mL;
Three, the mixed solution A of step 1 is placed under the constant temperature that temperature is room temperature, take stirring velocity as 300r/min~500r/min, continue to stir, in 10s~60s, the solution B of step 2 is poured in the mixed solution A of step 1, then in 10s~60s, regulator solution pH value is 5~8, reaction 10min~30min, solution becomes oyster white, proceed in the hydrothermal reaction kettle of sealing, and, under the condition that is 80~160 ℃ in temperature by the hydrothermal reaction kettle of sealing, hydro-thermal reaction 8h~18h, obtain white solidliquid mixture;
Four, white solidliquid mixture step 3 obtained carries out centrifugation, then white solid centrifugation gone out is washed, first use absolute ethanol washing 3~5 times, and then with deionized water wash 3~5 times, put into baking oven after washing, under the condition that is 40~60 ℃ in temperature, dry 6h~16h, obtain the barium molybdate micro-nano powder.
The preparation method of present embodiment selects Trisodium Citrate as the morphology control agent, using distilled water and alcohol as reaction soln, take Sodium orthomolybdate and nitrate of baryta as reactant, first configure the mixing solutions of nitrate of baryta and Trisodium Citrate, configure again the mixing solutions of Sodium orthomolybdate and alcohol, then the mixing solutions of Sodium orthomolybdate and alcohol is poured in the mixing solutions of the nitrate of baryta of vigorous stirring and Trisodium Citrate, after utilizing ammoniacal liquor and hydrochloric acid to regulate the pH of mixing solutions under the vigorous stirring state, hydro-thermal reaction for some time takes out centrifugal, washing, drying obtains the barium molybdate micro-nano powder, the preparation method of present embodiment has solved existing method and be inconvenient to control the granular size of product and the difficult problem of granule-morphology in reaction process, reach the pattern of control barium molybdate micro-nano powder and the purpose of particle diameter by add-on and the hydrothermal temperature of controlling Trisodium Citrate, and it is simple that the preparation method of present embodiment has production technique, production process safety, reaction temperature and safety, with low cost, advantage without complicated additive, the barium molybdate micro-nano ground rice prepared, be difficult for reuniting, size distribution is even, particle diameter little (500nm left and right), good dispersity, can be widely used in the preparation of inorganic non-metallic powder body material.
Embodiment two: present embodiment is different from embodiment one: the mass ratio of the nitrate of baryta described in step 1 and Trisodium Citrate is 1:0.1.Other step and parameter are identical with embodiment one.
Embodiment three: present embodiment is different from embodiment one or two: the quality of the nitrate of baryta described in step 1 is 5.23g:100mL with the ratio of the volume of deionized water.Other step and parameter are identical with embodiment one or two.
Embodiment four: present embodiment is different from one of embodiment one to three: be configured to the mixed solution A that concentration is 0.2mol/L in step 1.Other step and parameter are identical with one of embodiment one to three.
Embodiment five: present embodiment is different from one of embodiment one to four: the nitrate of baryta in step 2 described in step 1 and the mass ratio of the Sodium orthomolybdate described in step 2 are 1:1.Other step and parameter are identical with one of embodiment one to four.
Embodiment six: present embodiment is different from one of embodiment one to five: the quality of the nitrate of baryta in step 2 described in step 1 is 4.84g:100mL with the ratio of the volume of the deionized water described in step 2.Other step and parameter are identical with one of embodiment one to five.
Embodiment seven: present embodiment is different from one of embodiment one to six: be configured to the solution B that concentration is 0.2mol/L in step 2.Other step and parameter are identical with one of embodiment one to six.
Embodiment eight: present embodiment is different from one of embodiment one to seven: using ammoniacal liquor or hydrochloric acid conditioning solution pH value in step 3 is 7.Other step and parameter are identical with one of embodiment one to seven.
Embodiment nine: present embodiment is different from one of embodiment one to eight: under the condition that is 140 ℃ by the hydrothermal reaction kettle of sealing in temperature in step 3, hydro-thermal reaction 16h, obtain white solidliquid mixture.Other step and parameter are identical with one of embodiment one to eight.
Embodiment ten: present embodiment is different from one of embodiment one to nine: under the condition that is 50 ℃ in temperature in step 4, dry 10h.Other step and parameter are identical with one of embodiment one to nine.
With following verification experimental verification beneficial effect of the present invention:
Test one: the preparation method of the barium molybdate micro-nano powder that a kind of pattern particle diameter is controlled carries out according to the following steps:
One, take 5.23g nitrate of baryta and 0.5g agent Trisodium Citrate, then, by after nitrate of baryta and Trisodium Citrate mixing, add the 100mL deionized water, after to be dissolved, be placed on magnetic stirring apparatus, take stirring velocity as 400r/min, stir 30min, the mixed solution A that the concentration that is configured to 100mL is 0.2mol/L;
Two, take the 4.84g Sodium orthomolybdate, then add the 100mL deionized water, be placed on magnetic stirring apparatus after dissolving to be mixed, take stirring velocity as 400r/min, stir 0.5h, the solution B that the concentration that is configured to 100mL is 0.2mol/L;
Three, mixed solution A is placed under the constant temperature that temperature is room temperature, take stirring velocity as 400r/min, continue to stir, in 60s, solution B is poured in mixed solution A, then in 60s, regulator solution pH value is 7, reaction 10min, and solution becomes oyster white, proceed in the hydrothermal reaction kettle of sealing, and, under the condition that is 140 ℃ in temperature by the hydrothermal reaction kettle of sealing, hydro-thermal reaction 10h, obtain white solidliquid mixture;
Four, on the whizzer that white solidliquid mixture step 4 obtained is 400r/min at rotating speed, carry out centrifugation, then white solid centrifugation gone out is washed, first use absolute ethanol washing 3 times, and then, with deionized water wash 3 times, put into baking oven after washing, under the condition that is 50 ℃ in temperature, dry 10h, obtain the barium molybdate micro-nano powder.
The FIB/SEM focused ion that the model that adopts U.S. FEI Co. to produce is HELIOS NanoLab 600i/micro-Electronic Speculum of electronics two-beam is carried out electron-microscope scanning to testing a barium molybdate micro-nano powder obtained, obtain electron microscope photo scanning as shown in Figure 1, as seen from Figure 1, the test one barium molybdate micro-nano powder obtained has consistent appearance, spherical in shape, particle diameter evenly, be of moderate size, median size is 500nm, the advantages such as good dispersity, can be widely used in the preparation of inorganic non-metallic powder body material.
Adopting Rigaku Co., Ltd. model is that D/max-rB 12KW type X-ray diffraction analysis instrument carries out X-ray diffraction analysis to testing a barium molybdate micro-nano powder obtained, the X ray diffracting spectrum obtained as shown in Figure 2, as seen from Figure 2, reference standard card (JCPDS.card.no29-0193) is found out (112), (004), (006), (200), (211), and (220) (204), (116), (312), (224), (008), (218), (316), (332), (228), (1, 1, 10), (424), etc. (336) the feature diffraction of crystal face is consistent with standard card.Except the diffraction peak of above-mentioned crystal face, and have no other diffraction peaks in diffracting spectrum, prove this experiment gained BaMoO
4the compound inclusion-free, purity is high, good crystallinity, and can find out that from the diffraction peak width product cut size does not significantly increase phenomenon.
Claims (10)
1. the preparation method of the controlled barium molybdate micro-nano powder of a pattern particle diameter is characterized in that the preparation method of the barium molybdate micro-nano powder that a kind of pattern particle diameter is controlled carries out according to the following steps:
One, after nitrate of baryta and Trisodium Citrate are mixed, add deionized water, take stirring velocity as 300r/min~500r/min after to be dissolved, stir 20min~40min, be configured to the mixed solution A that concentration is 0.1mol/L~0.5mol/L; The mass ratio of described nitrate of baryta and Trisodium Citrate is 1:(0.05~0.5); The quality of described nitrate of baryta is 5.23g:(80~120 with the ratio of the volume of deionized water) mL;
Two, add deionized water in Sodium orthomolybdate, to be dissolved after, take stirring velocity as 300r/min~500r/min, stir 0.5h~1h, be configured to the solution B that concentration is 0.1mol/L~0.5mol/L; The mass ratio of the Sodium orthomolybdate described in the nitrate of baryta described in step 1 and step 2 is 1:(0.5~1.5); The quality of the nitrate of baryta described in step 1 is 4.84g:(80~120 with the ratio of the volume of the deionized water described in step 2) mL;
Three, the mixed solution A of step 1 is placed under the constant temperature that temperature is room temperature, take stirring velocity as 300r/min~500r/min, continue to stir, in 10s~60s, the solution B of step 2 is poured in the mixed solution A of step 1, then in 10s~60s, regulator solution pH value is 5~8, reaction 10min~30min, solution becomes oyster white, proceed in the hydrothermal reaction kettle of sealing, and, under the condition that is 80~160 ℃ in temperature by the hydrothermal reaction kettle of sealing, hydro-thermal reaction 8h~18h, obtain white solidliquid mixture;
Four, white solidliquid mixture step 3 obtained carries out centrifugation, then white solid centrifugation gone out is washed, first use absolute ethanol washing 3~5 times, and then with deionized water wash 3~5 times, put into baking oven after washing, under the condition that is 40~60 ℃ in temperature, dry 6h~16h, obtain the barium molybdate micro-nano powder.
2. the preparation method of the controlled barium molybdate micro-nano powder of a kind of pattern particle diameter according to claim 1, the mass ratio that it is characterized in that the nitrate of baryta described in step 1 and Trisodium Citrate is 1:0.1.
3. the preparation method of the controlled barium molybdate micro-nano powder of a kind of pattern particle diameter according to claim 1 and 2, is characterized in that the quality of the nitrate of baryta described in step 1 and the ratio of the volume of deionized water are 5.23g:100mL.
4. the preparation method of the controlled barium molybdate micro-nano powder of a kind of pattern particle diameter according to claim 3, is characterized in that in step 1 being configured to the mixed solution A that concentration is 0.2mol/L.
5. the preparation method of the controlled barium molybdate micro-nano powder of a kind of pattern particle diameter according to claim 3, is characterized in that the mass ratio of the Sodium orthomolybdate described in the nitrate of baryta described in step 1 and step 2 in step 2 is 1:1.
6. the preparation method of the controlled barium molybdate micro-nano powder of a kind of pattern particle diameter according to claim 3, is characterized in that the quality of the nitrate of baryta described in step 1 in step 2 and the ratio of the volume of the deionized water described in step 2 are 4.84g:100mL.
7. the preparation method of the controlled barium molybdate micro-nano powder of a kind of pattern particle diameter according to claim 3, is characterized in that in step 2 being configured to the solution B that concentration is 0.2mol/L.
8. the preparation method of the controlled barium molybdate micro-nano powder of a kind of pattern particle diameter according to claim 3, is characterized in that using ammoniacal liquor or hydrochloric acid conditioning solution pH value in step 3 is 7.
9. the preparation method of the controlled barium molybdate micro-nano powder of a kind of pattern particle diameter according to claim 3, is characterized in that, under the condition that is 140 ℃ by the hydrothermal reaction kettle of sealing in temperature in step 3, hydro-thermal reaction 16h, obtain white solidliquid mixture.
10. the preparation method of the controlled barium molybdate micro-nano powder of a kind of pattern particle diameter according to claim 3, is characterized in that under the condition that is 50 ℃ in temperature in step 4, dries 10h.
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Cited By (4)
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CN106915774A (en) * | 2017-05-04 | 2017-07-04 | 洛阳理工学院 | A kind of preparation method of barium molybdate nano piece self assembly ball |
CN109336179A (en) * | 2018-12-14 | 2019-02-15 | 辽宁星空钠电电池有限公司 | A kind of rapid precipitation prepares one-dimensional BaMoO4Method |
CN109761279A (en) * | 2018-12-14 | 2019-05-17 | 辽宁星空钠电电池有限公司 | A kind of rapid precipitation preparation two dimension BaMoO4Method |
CN112758945A (en) * | 2019-11-04 | 2021-05-07 | 曲阜师范大学 | Barium silicate microsphere and preparation method and application thereof |
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CN101676361A (en) * | 2008-09-16 | 2010-03-24 | 中国科学院福建物质结构研究所 | Europium-ion-doped barium molybdate nano luminescent powder and preparation method thereof |
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106915774A (en) * | 2017-05-04 | 2017-07-04 | 洛阳理工学院 | A kind of preparation method of barium molybdate nano piece self assembly ball |
CN106915774B (en) * | 2017-05-04 | 2018-05-22 | 洛阳理工学院 | A kind of preparation method of barium molybdate nano piece self assembly ball |
CN109336179A (en) * | 2018-12-14 | 2019-02-15 | 辽宁星空钠电电池有限公司 | A kind of rapid precipitation prepares one-dimensional BaMoO4Method |
CN109761279A (en) * | 2018-12-14 | 2019-05-17 | 辽宁星空钠电电池有限公司 | A kind of rapid precipitation preparation two dimension BaMoO4Method |
CN112758945A (en) * | 2019-11-04 | 2021-05-07 | 曲阜师范大学 | Barium silicate microsphere and preparation method and application thereof |
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