CN101165227A - Method for synthesizing magnesium borate whisker by using bittern - Google Patents
Method for synthesizing magnesium borate whisker by using bittern Download PDFInfo
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- CN101165227A CN101165227A CNA2007100589726A CN200710058972A CN101165227A CN 101165227 A CN101165227 A CN 101165227A CN A2007100589726 A CNA2007100589726 A CN A2007100589726A CN 200710058972 A CN200710058972 A CN 200710058972A CN 101165227 A CN101165227 A CN 101165227A
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- Prior art keywords
- bittern
- magnesium borate
- whisker
- magnesium
- utilizing
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Links
- NFMWFGXCDDYTEG-UHFFFAOYSA-N trimagnesium;diborate Chemical compound [Mg+2].[Mg+2].[Mg+2].[O-]B([O-])[O-].[O-]B([O-])[O-] NFMWFGXCDDYTEG-UHFFFAOYSA-N 0.000 title claims abstract description 43
- 241001131796 Botaurus stellaris Species 0.000 title claims abstract description 36
- 238000000034 method Methods 0.000 title claims abstract description 22
- 230000002194 synthesizing effect Effects 0.000 title claims description 16
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 30
- 239000013078 crystal Substances 0.000 claims abstract description 27
- 238000006243 chemical reaction Methods 0.000 claims abstract description 22
- 239000000843 powder Substances 0.000 claims abstract description 22
- 238000001035 drying Methods 0.000 claims abstract description 16
- 238000005406 washing Methods 0.000 claims abstract description 15
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000004327 boric acid Substances 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910001868 water Inorganic materials 0.000 claims abstract description 8
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 7
- 239000000725 suspension Substances 0.000 claims abstract description 6
- 239000011780 sodium chloride Substances 0.000 claims abstract description 4
- 239000011777 magnesium Substances 0.000 claims description 16
- 238000003756 stirring Methods 0.000 claims description 14
- DPDMMXDBJGCCQC-UHFFFAOYSA-N [Na].[Cl] Chemical compound [Na].[Cl] DPDMMXDBJGCCQC-UHFFFAOYSA-N 0.000 claims description 11
- 239000000706 filtrate Substances 0.000 claims description 10
- 238000005507 spraying Methods 0.000 claims description 10
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 9
- 238000001914 filtration Methods 0.000 claims description 9
- 229910052749 magnesium Inorganic materials 0.000 claims description 9
- 239000012065 filter cake Substances 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 5
- 238000002203 pretreatment Methods 0.000 claims description 5
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 claims description 5
- 230000003252 repetitive effect Effects 0.000 claims description 3
- 238000005201 scrubbing Methods 0.000 claims description 3
- 238000005245 sintering Methods 0.000 claims description 3
- 241000370738 Chlorion Species 0.000 claims description 2
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 2
- 239000003814 drug Substances 0.000 claims description 2
- 239000000047 product Substances 0.000 claims description 2
- 238000002386 leaching Methods 0.000 claims 1
- 238000010438 heat treatment Methods 0.000 abstract description 6
- 238000001816 cooling Methods 0.000 abstract description 2
- 238000013329 compounding Methods 0.000 abstract 1
- 238000001694 spray drying Methods 0.000 abstract 1
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 description 12
- 239000002994 raw material Substances 0.000 description 7
- 238000004458 analytical method Methods 0.000 description 6
- 230000015572 biosynthetic process Effects 0.000 description 6
- 229910001629 magnesium chloride Inorganic materials 0.000 description 6
- 239000012071 phase Substances 0.000 description 6
- 238000003786 synthesis reaction Methods 0.000 description 6
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 5
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 5
- 229910052796 boron Inorganic materials 0.000 description 5
- 239000006227 byproduct Substances 0.000 description 5
- 235000002639 sodium chloride Nutrition 0.000 description 5
- 239000007788 liquid Substances 0.000 description 4
- 238000010532 solid phase synthesis reaction Methods 0.000 description 4
- 241000272875 Ardeidae Species 0.000 description 3
- 239000003513 alkali Substances 0.000 description 3
- -1 alkali metal salt Chemical class 0.000 description 3
- 229910021538 borax Inorganic materials 0.000 description 3
- 238000007654 immersion Methods 0.000 description 3
- 239000000395 magnesium oxide Substances 0.000 description 3
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 3
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 3
- 238000000643 oven drying Methods 0.000 description 3
- 239000004328 sodium tetraborate Substances 0.000 description 3
- 235000010339 sodium tetraborate Nutrition 0.000 description 3
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 2
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- 239000002585 base Substances 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- UQGFMSUEHSUPRD-UHFFFAOYSA-N disodium;3,7-dioxido-2,4,6,8,9-pentaoxa-1,3,5,7-tetraborabicyclo[3.3.1]nonane Chemical compound [Na+].[Na+].O1B([O-])OB2OB([O-])OB1O2 UQGFMSUEHSUPRD-UHFFFAOYSA-N 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 description 2
- 239000001095 magnesium carbonate Substances 0.000 description 2
- 235000014380 magnesium carbonate Nutrition 0.000 description 2
- 229960001708 magnesium carbonate Drugs 0.000 description 2
- 229910000021 magnesium carbonate Inorganic materials 0.000 description 2
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 description 2
- 239000000347 magnesium hydroxide Substances 0.000 description 2
- 229910001862 magnesium hydroxide Inorganic materials 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910052700 potassium Inorganic materials 0.000 description 2
- 239000011591 potassium Substances 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 229910052938 sodium sulfate Inorganic materials 0.000 description 2
- 235000011152 sodium sulphate Nutrition 0.000 description 2
- 239000007790 solid phase Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000010189 synthetic method Methods 0.000 description 2
- 239000012745 toughening agent Substances 0.000 description 2
- 238000010792 warming Methods 0.000 description 2
- GDTSJMKGXGJFGQ-UHFFFAOYSA-N 3,7-dioxido-2,4,6,8,9-pentaoxa-1,3,5,7-tetraborabicyclo[3.3.1]nonane Chemical compound O1B([O-])OB2OB([O-])OB1O2 GDTSJMKGXGJFGQ-UHFFFAOYSA-N 0.000 description 1
- 206010016654 Fibrosis Diseases 0.000 description 1
- JLVVSXFLKOJNIY-UHFFFAOYSA-N Magnesium ion Chemical compound [Mg+2] JLVVSXFLKOJNIY-UHFFFAOYSA-N 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052810 boron oxide Inorganic materials 0.000 description 1
- YMEKEHSRPZAOGO-UHFFFAOYSA-N boron triiodide Chemical compound IB(I)I YMEKEHSRPZAOGO-UHFFFAOYSA-N 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000004761 fibrosis Effects 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- OTCKOJUMXQWKQG-UHFFFAOYSA-L magnesium bromide Chemical compound [Mg+2].[Br-].[Br-] OTCKOJUMXQWKQG-UHFFFAOYSA-L 0.000 description 1
- 229910001623 magnesium bromide Inorganic materials 0.000 description 1
- 229910001425 magnesium ion Inorganic materials 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- VGTPKLINSHNZRD-UHFFFAOYSA-N oxoborinic acid Chemical compound OB=O VGTPKLINSHNZRD-UHFFFAOYSA-N 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000005060 rubber Substances 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- NVIFVTYDZMXWGX-UHFFFAOYSA-N sodium metaborate Chemical compound [Na+].[O-]B=O NVIFVTYDZMXWGX-UHFFFAOYSA-N 0.000 description 1
- KEAYESYHFKHZAL-BJUDXGSMSA-N sodium-22 Chemical compound [22Na] KEAYESYHFKHZAL-BJUDXGSMSA-N 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
Landscapes
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The process of preparing magnesium borate crystal whisker with bittern includes the following steps: pre-treating bittern; compounding bittern with boric acid, sodium chloride, water, sodium hydroxide and crystal seed, and reaction to form suspension; spray drying the suspension to obtain powder; heating to 800-850 deg.c and reaction at the temperature for 2-3 hr; cooling, washing and drying to obtain magnesium borate crystal whisker. The process has the main components in bittern utilized, lowered magnesium borate crystal whisker producing cost, and wide industrial application foreground.
Description
Technical field
The present invention relates to magnesium borate (Mg
2B
2O
5) synthetic method of whisker, particularly relate to the method for bittern of utilizing for the raw material synthesizing magnesium borate whisker.
Background technology
Magnesium borate (Mg
2B
2O
5) whisker is fibrous single crystal, have high strength, high-modulus, high-wearing feature, lightweight and advantages such as corrosion-resistant and Heat stability is good, can be used as the type material toughener and be applied in the goods of light metal material and plastics, rubber, ceramic and other composite material, can be widely used in fields such as automobile, electric, electronics, machinery, chemical industry.
The magnesium borate crystal whisker synthetic method of prior art comprises: 1) High Temperature Gas phase synthesi; 2) process for solid-phase microwave synthesis; 3) hydro-thermal-high-temperature synthesis; 4) high-temperature dry solid-phase synthesis; 5) high temperature wet solid-phase synthesis.
The High Temperature Gas phase synthesi is a catalyzer with molybdenum/palladium, and by magnesium oxide, boron iodide and boric acid synthesizing magnesium borate whisker under the high temperature gas phase condition, the material cost of this method is too high and be not suitable for suitability for industrialized production.
Process for solid-phase microwave synthesis is to be raw material with magnesium chloride and borax, is the heating medium synthesizing magnesium borate whisker with zinc oxide under microwave radiation, and this method energy consumption is huge and be not suitable for suitability for industrialized production.
Hydro-thermal-high-temperature synthesis is the boron source with boric acid or borax, with magnesium hydroxide, magnesiumcarbonate or magnesium oxide as the magnesium source, boron source and magnesium source are added the water mixing, be put in the autoclave and obtain alkali formula magnesium borate slurries with 100～400 ℃ of heating, again after filtration, washing, drying obtain alkali formula magnesium borate, then alkali formula magnesium borate obtained magnesium borate crystal whisker 660～1100 ℃ of heating.This method is under high pressure carried out, conversion unit is required high, not easy to operate, and strengthen the property difference and be difficult to practical application of synthetic whisker.
The high-temperature dry solid-phase synthesis with magnesium oxide, magnesium hydroxide, alkaline magnesium carbonate, sal epsom, magnesium chloride or magnesium bromide as the magnesium source, with boron oxide, boric acid, metaboric acid or corresponding alkali metal salt such as Sodium Tetraborate, sodium pyroborate, potassium pyroborate, sodium metaborate etc. as the boron source, with sodium halide or potassium halide as fusing assistant.The fusing assistant of magnesium source, boron source and interpolation is mixed the back in 600～1000 ℃ temperature range internal heating reaction, and then cooling, washing, drying obtain magnesium borate crystal whisker.This method synthetic magnesium borate crystal whisker fibrosis is not remarkable, fusion between the fiber and form tangible reunion, the whisker yardstick has a very wide distribution, the thickness fiber hybrid together, it is relatively poor to strengthen the property when using as toughener, therefore influences its practical application.
The high temperature wet solid-phase synthesis is a raw material with boric acid, magnesium chloride, sodium hydroxide, sodium-chlor or Repone K are fusing assistant, obtain powder after the mixed spray dried, powder 750～950 ℃ of reacting by heating, is separated obtaining magnesium borate crystal whisker again behind the cool to room temperature.This method synthetic whisker fibreization is remarkable, and length-to-diameter ratio is greater than 10, is used to strengthen aluminium base and magnesium base composite material is obtained effect preferably.But the sodium-chlor that this method adopted, Repone K, magnesium chloride raw material all need chemical pure or top grade industrial goods, have the raw materials cost problem of higher, influence its industrialization and produce.
Summary of the invention
At the problem that above-mentioned prior art exists, the present invention has released the method for utilizing bittern to produce magnesium borate crystal whisker.Bittern is the by product of salt industry, and is with low cost, contains magnesium chloride, sal epsom, sodium-chlor and the Repone K of high density.Utilize magnesium ion in the bittern as the magnesium source of synthesizing magnesium borate whisker, the sodium sulfate of the Repone K in the bittern, sodium-chlor and building-up reactions by-product is as fusing assistant, and the boric acid that adds can realize utilizing low-cost raw material synthesizing magnesium borate whisker as the boron source.
The method of utilizing the bittern synthesizing magnesium borate whisker involved in the present invention comprises: processing steps such as bittern pre-treatment, batching reaction, spraying drying, sintered molten, washing and drying.
(1) bittern pre-treatment
In bittern, add an amount of clorox medicament, stir after-filtration, impurity such as organism in the removal bittern and colloid, the bittern that is purified.Clorox and bittern blended volume ratio are 1: 1000.
(2) batching reaction
Pretreated bittern, boric acid, sodium-chlor are at room temperature added sodium hydroxide behind the stirring and evenly mixing, and restir obtains suspension.Above-mentioned batching mass ratio is: than (magnesium in the bittern): H
3BO
3: NaCl: NaOH=1: 3.05～3.31: 12.5 7: 3.38.
For the reaction of above-mentioned batching, add a small amount of magnesium borate crystal whisker crystal seed when can after mixing bittern, boric acid, sodium-chlor, add sodium hydroxide, stirring obtains suspension then.Magnesium borate crystal whisker crystal seed add-on is 10% of synthetic whisker theoretical amount.
(3) spraying drying
The suspension that above-mentioned batching reaction is obtained carries out spraying drying, obtains powder.
(4) sintered molten
The resulting powder of above-mentioned spraying drying is placed crucible, again the crucible of built-in powder is put into temperature programming stove sintering, be warming up to 800～850 ℃ with 10 ℃/minute speed, this temperature range reaction 2～3 hours, then the sintered molten thing is cooled to room temperature, obtains the mixture of magnesium borate crystal whisker and fusing assistant.
(5) washing
The magnesium borate crystal whisker that sintering is obtained and the mixture of fusing assistant are dissolved in the water, and stir 10～30 minutes after-filtration, obtain filter cake.With clear water repetitive scrubbing filter cake, in filtrate, do not contain till chlorion and the sulfate ion.
(6) drying
The filter cake that above-mentioned repetitive scrubbing obtains is dry under 100～120 ℃ of temperature, promptly obtain the magnesium borate crystal whisker product.
The method of synthesizing magnesium borate whisker involved in the present invention has been utilized the by product bittern of salt industry, has solved the raw materials cost problem of higher that exists in the existing method.China's sea salt output has reached more than 2,200 ten thousand tons/year, and corresponding by-product bittern total amount reaches 1800 ten thousand steres, makes bittern become the liquid resource with low cost of not only abundant but also Sustainable Development and Utilization.Make full use of the main component in the bittern in this preparation method, the magnesium chloride of high density, sal epsom are as the magnesium source of synthesizing magnesium borate whisker, with the sodium sulfate of Repone K, sodium-chlor and reaction by-product fusing assistant as sintered molten, reduce the cost of synthesizing magnesium borate whisker, had wide industrial prospect.
Embodiment
1, embodiment 1
Get 6 milliliters of clorox and place 6 liters of bitterns, stir and stop after 10 minutes, filter, analyze consisting of of filtrate: Mg
2+, 52g/l; Cl
-, 177g/l; SO
4 2-, 64g/l; Na
+, 40g/1; K
+, 13g/l.915 gram sodium-chlor, 222 gram boric acid, 1.4 are gone up and stated filtrate and place reactor, add 6 premium on currency simultaneously, open stirrer, add 246 gram sodium hydroxide in the time of stirring, stir and stop after 20 minutes, carry out spraying drying, obtain powder.Prepared powder is placed in the crucible, places the temperature programming stove to be warmed up to 800 ℃, react 2 hours postcooling, obtain reaction and finish thing with 10 ℃ of/minute clock rate.The thing taking-up is finished in reaction put into the water immersion, blend, through repeatedly washing, filtering, in filtrate, do not contain Cl again
-And SO
4 2-Till.The filter cake that obtains is put into the baking oven drying and is obtained white powder 200 grams.It is higher that washing for the first time contains liquid fusing assistant concentration, preserves when this filtrate is synthesized whisker as next time and use.The above-mentioned white powder of X diffraction phase analysis is triclinic system magnesium borate (Mg
2B
2O
5) single crystal, its diameter of scanning electron microscope morphology analysis is 0.1～0.2 μ m, length is 2～4 μ m.
2, embodiment 2
Get among the embodiment 14 liters of the washingss among 1.4 liters of filtering bitterns, the embodiment 1, mix the back and add 100 gram sodium-chlor, 231 gram boric acid and 2 premium on currency, open and stir, add 246 gram sodium hydroxide when stirring, stir and stop after 20 minutes, carry out spraying drying, obtain powder.Prepared powder is placed in the crucible, prepared powder is placed in the crucible, place the temperature programming stove to be warmed up to 800 ℃, reacted 2.5 hours, be cooled to room temperature and obtain reaction and finish thing with 10 ℃ of/minute clock rate.The thing taking-up is finished in reaction put into the water immersion, blend, through repeatedly washing, filtering, in filtrate, do not contain Cl again
-And S0
4 2-Till.The filter cake that obtains is put into the baking oven drying and is obtained white powder 208 grams.It is higher that washing for the first time contains liquid fusing assistant concentration, preserves when this filtrate is synthesized whisker as next time and use.The above-mentioned white powder of X diffraction phase analysis is triclinic system magnesium borate (Mg
2B
2O
5) single crystal, its diameter of scanning electron microscope morphology analysis is 0.2～0.4 μ m, length is 3～6 μ m.
3, embodiment 3
Get among the embodiment 14 liters of the washingss among 1.4 liters of filtering bitterns, the embodiment 2, mix the back and add 100 gram sodium-chlor, 241 gram boric acid and 2 premium on currency, open and stir, add 246 gram sodium hydroxide and 22 gram magnesium borate crystal seeds when stirring, stir and stop after 20 minutes, carry out spraying drying, obtain powder.Prepared powder is placed in the crucible, prepared powder is placed in the crucible, place the temperature programming stove to be warming up to 850 ℃, reacted 3 hours, be cooled to room temperature and obtain reaction and finish thing with 10 ℃ of/minute clock rate.The thing taking-up is finished in reaction put into the water immersion, blend, again through repeatedly washing, filtering, not conforming in filtrate has Cl
-And SO
4 2-Till.The filter cake that obtains is put into the baking oven drying and is obtained white powder 222 grams.It is higher that washing for the first time contains liquid fusing assistant concentration, preserves when this filtrate is synthesized whisker as next time and use.The above-mentioned white powder of X diffraction phase analysis is triclinic system magnesium borate (Mg
2B
2O
5) single crystal, its diameter of scanning electron microscope morphology analysis is 0.5～1.8 μ m, length is 6～20 μ m.
Claims (5)
1. a method of utilizing the bittern synthesizing magnesium borate whisker is characterized in that: comprise processing steps such as bittern pre-treatment, batching reaction, spraying drying, sintered molten, washing and drying; The bittern pre-treatment is to add the clorox medicament in bittern; Batching reaction is to add sodium hydroxide with behind the bittern of pre-treatment after and boric acid, the sodium-chlor stirring and evenly mixing, and the mass ratio of preparing burden is: Mg (magnesium in the bittern): H
3B0
3: NaCl: NaOH=1: 3.05～3.31: 12.57: 3.38; The reaction suspension of will preparing burden carries out spraying drying, obtains powder; The resulting powder of spraying drying is placed the crucible sintered molten, 800～850 ℃ of frit reactions 2～3 hours; The magnesium borate crystal whisker that sintering is obtained and the mixture of fusing assistant are dissolved in the water, and washing obtains filter cake; The filtration cakes torrefaction that washing is obtained obtains magnesium borate crystal whisker.
2. the method for utilizing the bittern synthesizing magnesium borate whisker according to claim 1 is characterized in that clorox and bittern blended volume ratio are 1: 1000.
3. the method for utilizing the bittern synthesizing magnesium borate whisker according to claim 1 adds the magnesium borate crystal whisker crystal seed when it is characterized in that batching reaction batch mixing, and add-on is 10% of synthetic whisker theoretical amount.
4. the method for utilizing the bittern synthesizing magnesium borate whisker according to claim 1 is characterized in that washing leaching cake is to carry out repeatedly, does not contain till chlorion and the sulfate ion in filtrate.
5. the method for utilizing the bittern synthesizing magnesium borate whisker according to claim 1 is characterized in that the filter cake that repetitive scrubbing is obtained is dry under 100～120 ℃ of temperature, to obtain the magnesium borate crystal whisker product.
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|---|---|---|---|
| CNB2007100589726A CN100500952C (en) | 2007-08-20 | 2007-08-20 | Method for synthesizing magnesium borate whisker by using bittern |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007100589726A CN100500952C (en) | 2007-08-20 | 2007-08-20 | Method for synthesizing magnesium borate whisker by using bittern |
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|---|---|
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| CN100500952C CN100500952C (en) | 2009-06-17 |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102002751A (en) * | 2010-10-11 | 2011-04-06 | 国家海洋局天津海水淡化与综合利用研究所 | Method for directly synthesizing basic magnesium sulfate whiskers by brine |
| CN102181933A (en) * | 2011-04-13 | 2011-09-14 | 国家海洋局天津海水淡化与综合利用研究所 | Method for synthesizing one-dimensional nano magnesium borate crystal whisker by using concentrated seawater |
| CN102206860A (en) * | 2011-05-23 | 2011-10-05 | 华东理工大学 | Method for preparing magnesium borate whisker with high length-to-diameter ratio by pelletization |
| CN101709509B (en) * | 2009-12-10 | 2011-12-07 | 太原理工大学 | Method for preparing magnesium borate whisker |
| CN107287651A (en) * | 2017-07-31 | 2017-10-24 | 岭南师范学院 | A kind of method for preparing alkali formula magnesium borate crystal whisker |
| CN108073788A (en) * | 2017-12-25 | 2018-05-25 | 岭南师范学院 | A kind of method that alkali formula magnesium borate crystal whisker is prepared using bittern in salt lake |
| CN112239360A (en) * | 2020-09-23 | 2021-01-19 | 华南理工大学 | Boron oxide, magnesium oxide and reaction product thereof synergistically toughened tungsten carbide composite material and preparation thereof |
-
2007
- 2007-08-20 CN CNB2007100589726A patent/CN100500952C/en active Active
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101709509B (en) * | 2009-12-10 | 2011-12-07 | 太原理工大学 | Method for preparing magnesium borate whisker |
| CN102002751A (en) * | 2010-10-11 | 2011-04-06 | 国家海洋局天津海水淡化与综合利用研究所 | Method for directly synthesizing basic magnesium sulfate whiskers by brine |
| CN102181933A (en) * | 2011-04-13 | 2011-09-14 | 国家海洋局天津海水淡化与综合利用研究所 | Method for synthesizing one-dimensional nano magnesium borate crystal whisker by using concentrated seawater |
| CN102206860A (en) * | 2011-05-23 | 2011-10-05 | 华东理工大学 | Method for preparing magnesium borate whisker with high length-to-diameter ratio by pelletization |
| CN102206860B (en) * | 2011-05-23 | 2013-07-10 | 华东理工大学 | Method for preparing magnesium borate whisker with high length-to-diameter ratio by pelletization |
| CN107287651A (en) * | 2017-07-31 | 2017-10-24 | 岭南师范学院 | A kind of method for preparing alkali formula magnesium borate crystal whisker |
| CN108073788A (en) * | 2017-12-25 | 2018-05-25 | 岭南师范学院 | A kind of method that alkali formula magnesium borate crystal whisker is prepared using bittern in salt lake |
| CN112239360A (en) * | 2020-09-23 | 2021-01-19 | 华南理工大学 | Boron oxide, magnesium oxide and reaction product thereof synergistically toughened tungsten carbide composite material and preparation thereof |
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| CN100500952C (en) | 2009-06-17 |
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