CN102815728A - Method for preparing nano-sized magnesium hydroxide and nano-silica by utilization of boron mud - Google Patents
Method for preparing nano-sized magnesium hydroxide and nano-silica by utilization of boron mud Download PDFInfo
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- CN102815728A CN102815728A CN2012101975103A CN201210197510A CN102815728A CN 102815728 A CN102815728 A CN 102815728A CN 2012101975103 A CN2012101975103 A CN 2012101975103A CN 201210197510 A CN201210197510 A CN 201210197510A CN 102815728 A CN102815728 A CN 102815728A
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- boron mud
- sized magnesium
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- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 title claims abstract description 30
- 229910052796 boron Inorganic materials 0.000 title claims abstract description 30
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 title claims abstract description 20
- 239000000347 magnesium hydroxide Substances 0.000 title claims abstract description 18
- 229910001862 magnesium hydroxide Inorganic materials 0.000 title claims abstract description 18
- 238000000034 method Methods 0.000 title claims abstract description 14
- 239000002105 nanoparticle Substances 0.000 title claims abstract description 13
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title abstract description 17
- 239000000377 silicon dioxide Substances 0.000 title abstract description 5
- HEMHJVSKTPXQMS-UHFFFAOYSA-M sodium hydroxide Substances [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 22
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000001914 filtration Methods 0.000 claims abstract description 15
- 239000002245 particle Substances 0.000 claims abstract description 15
- 239000003513 alkali Substances 0.000 claims abstract description 10
- 238000000926 separation method Methods 0.000 claims abstract description 7
- 239000003607 modifier Substances 0.000 claims abstract description 6
- 239000002893 slag Substances 0.000 claims abstract description 6
- 239000000706 filtrate Substances 0.000 claims abstract 5
- 238000006243 chemical reaction Methods 0.000 claims description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- 229910021392 nanocarbon Inorganic materials 0.000 claims description 11
- 238000001035 drying Methods 0.000 claims description 10
- 239000011734 sodium Substances 0.000 claims description 9
- 238000005406 washing Methods 0.000 claims description 9
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 8
- 238000007254 oxidation reaction Methods 0.000 claims description 8
- 239000010802 sludge Substances 0.000 claims description 8
- 239000002002 slurry Substances 0.000 claims description 8
- 238000001354 calcination Methods 0.000 claims description 7
- -1 titanic acid ester Chemical class 0.000 claims description 7
- 239000012754 barrier agent Substances 0.000 claims description 6
- 239000007822 coupling agent Substances 0.000 claims description 6
- 239000007787 solid Substances 0.000 claims description 6
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 5
- 229910052708 sodium Inorganic materials 0.000 claims description 5
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 4
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 4
- 150000004645 aluminates Chemical class 0.000 claims description 4
- 239000007795 chemical reaction product Substances 0.000 claims description 4
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 4
- 230000003647 oxidation Effects 0.000 claims description 4
- 150000002978 peroxides Chemical class 0.000 claims description 4
- 229910000077 silane Inorganic materials 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 3
- 239000001117 sulphuric acid Substances 0.000 claims description 3
- 235000011149 sulphuric acid Nutrition 0.000 claims description 3
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 2
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims 2
- 238000009388 chemical precipitation Methods 0.000 claims 1
- 239000005543 nano-size silicon particle Substances 0.000 claims 1
- 239000000047 product Substances 0.000 abstract description 12
- 239000006229 carbon black Substances 0.000 abstract description 10
- 239000002253 acid Substances 0.000 abstract description 7
- 239000007788 liquid Substances 0.000 abstract description 6
- 239000000395 magnesium oxide Substances 0.000 abstract description 3
- 238000005516 engineering process Methods 0.000 abstract description 2
- 238000003912 environmental pollution Methods 0.000 abstract description 2
- 238000010494 dissociation reaction Methods 0.000 abstract 2
- 230000005593 dissociations Effects 0.000 abstract 2
- 238000002386 leaching Methods 0.000 abstract 2
- 238000004090 dissolution Methods 0.000 abstract 1
- 235000014413 iron hydroxide Nutrition 0.000 abstract 1
- NCNCGGDMXMBVIA-UHFFFAOYSA-L iron(ii) hydroxide Chemical compound [OH-].[OH-].[Fe+2] NCNCGGDMXMBVIA-UHFFFAOYSA-L 0.000 abstract 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 abstract 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 abstract 1
- 239000002075 main ingredient Substances 0.000 abstract 1
- 230000001590 oxidative effect Effects 0.000 abstract 1
- 235000021110 pickles Nutrition 0.000 abstract 1
- 238000001556 precipitation Methods 0.000 abstract 1
- 230000032683 aging Effects 0.000 description 11
- 238000003483 aging Methods 0.000 description 11
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 10
- 235000011121 sodium hydroxide Nutrition 0.000 description 6
- 229910004298 SiO 2 Inorganic materials 0.000 description 4
- 239000011777 magnesium Substances 0.000 description 4
- 239000002244 precipitate Substances 0.000 description 4
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 4
- 230000008021 deposition Effects 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- 235000019353 potassium silicate Nutrition 0.000 description 3
- 230000001376 precipitating effect Effects 0.000 description 3
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 2
- 229910021538 borax Inorganic materials 0.000 description 2
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 2
- 239000004327 boric acid Substances 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 229910052749 magnesium Inorganic materials 0.000 description 2
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 description 2
- 239000011268 mixed slurry Substances 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000004328 sodium tetraborate Substances 0.000 description 2
- 235000010339 sodium tetraborate Nutrition 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 244000025254 Cannabis sativa Species 0.000 description 1
- 229910019440 Mg(OH) Inorganic materials 0.000 description 1
- 239000004115 Sodium Silicate Substances 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 230000029087 digestion Effects 0.000 description 1
- 229960004887 ferric hydroxide Drugs 0.000 description 1
- 239000011790 ferrous sulphate Substances 0.000 description 1
- 235000003891 ferrous sulphate Nutrition 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 description 1
- RUTXIHLAWFEWGM-UHFFFAOYSA-H iron(3+) sulfate Chemical compound [Fe+3].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O RUTXIHLAWFEWGM-UHFFFAOYSA-H 0.000 description 1
- IEECXTSVVFWGSE-UHFFFAOYSA-M iron(3+);oxygen(2-);hydroxide Chemical compound [OH-].[O-2].[Fe+3] IEECXTSVVFWGSE-UHFFFAOYSA-M 0.000 description 1
- 229910000359 iron(II) sulfate Inorganic materials 0.000 description 1
- 229910000360 iron(III) sulfate Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 235000010755 mineral Nutrition 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000011175 product filtration Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 239000011435 rock Substances 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 229910052911 sodium silicate Inorganic materials 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000002910 solid waste Substances 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000008399 tap water Substances 0.000 description 1
- 235000020679 tap water Nutrition 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Images
Abstract
The invention relates to a method for preparing nano-sized magnesium hydroxide and nano-silica by the utilization of boron mud, comprising the following steps of: adding calcined boron mud into concentrated sulfuric acid for acid leaching and dissociation; carrying out solid-liquid separation on a pickle liquor which has undergone acid leaching and dissociation; oxidizing a filtrate which has undergone solid-liquid separation and using alkali lye for precipitation separation of iron hydroxide; adding the iron-removed filtrate into a particle surface modifier and alkali lye to prepare nano-sized magnesium hydroxide; carrying out alkali dissolution by the use of acid slag obtained after solid-liquid separation, filtering, and adding a particle blocker and an acid solution into a filtrate to prepare nano-silica. According to the technology, main ingredients of magnesium oxide and silica in boron mud can be highly efficiently and comprehensively utilized to prepare the product with high added value, and the environmental pollution problem of boron mud can be solved. The magnesium hydroxide prepared in the invention is sheet-shaped nanometer magnesium hydroxide. White carbon black is spherical nanometer white carbon black.
Description
Technical field
The present invention relates to a kind of method of utilizing boric sludge to be equipped with nano-sized magnesium hydroxide and Nano carbon white, belong to mineral processing and utilize technical field with solid waste.
Background technology
Boron mud is the waste residue that produces when producing product such as boric acid, borax.Boron mud is light red, and particle is thin, becomes loose shape, and its major ingredient is MgO and SiO
2, and contain a spot of Fe
2O
3, Al
2O
3, CaO, B
2O
3Deng.Because the apparent alkalescence of boron mud, its alkali lye can be added in the underground water, makes the farmland underproduction on every side, can cause the farm crop total crop failure when serious, and tap water is on every side produced pollution.Therefore, it is land occupation not only, and to around the arable land cause severe contamination, the institute's part soil that discharges exhaustion, not even a blade of grass grows.Along with socioeconomic continuous development, the demand of borax, boric acid is increased year by year, the output of boron mud also will increase year by year.The processing of a large amount of boron mud has become one of difficult problem that boron development of resources and boron rock processing industry need to be resolved hurrily at present.
Contain valuable elements such as magnesium, silicon in the boron mud, have higher utility value.Therefore, develop this secondary resource, produce high-quality Marinco H and WHITE CARBON BLACK, all significant to reducing environmental pollution, promote resource recovery and improving the business economic benefit.
The present invention is directed to the present situation of present boron mud pollution on the environment and comprehensive utilization, propose a kind of method of efficiently utilizing Natural manganese dioxide and silica component in the boron mud to prepare nano-sized magnesium hydroxide and Nano carbon white.
Summary of the invention
Boron mud and sulphuric acid soln are leached reaction; With reacted dope filtration, washing to separate the solid-liquid component; In gained filtrating, add suitable oxygenant oxidation Fe wherein
2+After add the iron component in the alkali solution precipitate filtrating; After removing by filter throw outs such as ironic hydroxide, add alkali reaction, add an amount of particle surface modifier simultaneously; Carry out ageing, filtration, washing, drying and the depolymerization of reaction system after the reaction, obtaining simple granularity is that nano level, particle shape are flaky Marinco H powder; Residue behind boron mud and the sulfuric acid reaction and sodium hydroxide are carried out hydro-thermal reaction under the situation of heating, after the reaction product is filtered, filtrating is added add a certain amount of particle barrier agent after water is adjusted to certain concentration, carry out precipitating with acid; With obtaining ball shaped nano level WHITE CARBON BLACK after the ageing of precipitating product, filtration, washing, the drying.
Its process step and principle are following:
(1) boron mud is calcined 0.5~1.5h down for 300~700 ℃ in calcining temperature;
(2) will calcine that back boron mud adds water and sulfuric acid reacts, and obtain the mixed slurry of compositions such as sulfur acid magnesium, Tai-Ace S 150, ferrous sulfate and ferric sulfate, its reaction formula is:
MgO+H
2SO
4→MgSO
4+H
2O
Al
2O
3+3H
2SO
4→Al
2(SO
4)
3+3H
2O
Fe
2O
3+3H
2SO
4→2Fe
2(SO
4)
3+3H
2O
FeO+H
2SO
4→FeSO
4+H
2O
(3) above-mentioned mixed slurry is filtered, transfers to suitable concentration after removing solid residue, add ydrogen peroxide 50 and add alkali reaction to slurry pH value 4~7 after to oxidation of divalent iron ion 15~45min, its reaction formula is following:
H
2O
2+2FeSO
4+H
2SO
4=Fe
2(SO
4)
3+2H
2O
Fe
2(SO
4)
3+6NaOH=2Fe(OH)
3↓+3Na
2SO
4
(4) with after above-mentioned oxidation reaction product filtration, removing ferric hydroxide precipitate, add the particle surface modifier, add alkali reaction to slurry pH value 10~13, get magnesium hydrate precipitate.Its reaction formula is following:
MgSO
4+2NaOH=Mg(OH)
2↓+Na
2SO
4
(5) will contain slurries ageing, filtration, washing, the drying of magnesium hydrate precipitate thing, depolymerization promptly obtains flake nano level magnesium hydroxide products.
(6) solid residue that leaches in the step (2) and caustic soda are reacted under heating condition, generate the slurries that contain water glass, its reaction formula is:
SiO
2·nH
2O+2NaOH=Na
2O·mSiO
2+(n+1)H
2O
(7) with the above-mentioned dope filtration that contains water glass, remove solid residue and add water move to 10~30 ° of solution degree Beaume; Descend and flow to add sour precipitating to slurry pH value 3~7 at 30~90 ℃; Simultaneously under agitation add the particle barrier agent, obtain the hydrated SiO 2 deposition, its reaction formula is following:
Na
2O·mSiO
2+H
2SO
4+nH
2O→mSiO
2·nH
2O
↓+Na
2SO
4
This reaction product ageing, filtration, washing, drying, depolymerization are promptly got ball shaped nano level WHITE CARBON BLACK product.
Boron mud described in the step (1), its granularity are 50~500 orders.
Particle surface modifier described in the step (4) is one of titanic acid ester, silane, aluminate coupling agent, organosilicon or the combination between them.
Particle barrier agent described in the step (7) is one of polyoxyethylene glycol, aluminate coupling agent, titanate coupling agent, silane coupling agent, organosilicon, OP-10 or the combination between them.
Below be prescription of the present invention and processing condition:
(1) acid is dissolved: calcining boron mud: 96% sulfuric acid: water (mass ratio)=100: 80~160: 120~240,90~120 ℃ of temperature of reaction, reaction times 0.5~3h;
(2) iron removal by oxidation: 30%H
2O
2Consumption be 1%~10% of calcining boron shale amount, 30~80 ℃ of temperature of reaction, ageing 30~60min;
(3) deposition Mg (OH)
2: 30~90 ℃ of temperature of reaction, digestion time 15~60min; The coating materials consumption is 0.3%~5% of a Marinco H quality;
(4) sour molten slag alkali dissolves: sour molten slag: NaOH: water=100: 20~80: 200~400,90~120 ℃ of temperature of reaction, reaction times 1~4h;
(5) hydrated SiO 2 deposition: particle barrier agent consumption is 0.5%~6% of a Nano carbon white quality.
Use the Marinco H of the present invention's preparation to be flake nano level Marinco H, and (the BET specific surface area is less than 70m to have less specific surface area
2/ g), higher degree (Mg (OH)
2Content>98%), dispersiveness and good surface activity; The WHITE CARBON BLACK product is a ball shaped nano level WHITE CARBON BLACK product, and (the BET specific surface area is greater than 200m greatly to have specific surface area and pore volume
2/ g and pore volume are greater than 1.0cm
3/ g), the high (SiO of purity
2Content>98%), the light (bulk density≤0.15g/cm of unit weight
3), characteristic such as dispersiveness and good surface activity.
The accompanying drawing content
Accompanying drawing 1 is technical process of the present invention, and accompanying drawing 2 is the flake nano level Marinco H of embodiment of the invention preparation and the scanning electron microscope analysis result of ball shaped nano level WHITE CARBON BLACK.
Embodiment
Embodiment one:
200g boron mud is calcined 1h down at 600 ℃; Get calcining boron mud 100g, add water 180g, concentration is 96% sulfuric acid 120g, reacts 1.5h down at 95 ℃; Filter the back and separate the solid-liquid component; Adding 5.0g mass concentration is 30% ydrogen peroxide 50 in leach liquor, reacts 15min down at 60 ℃; The pH value of hydro-oxidation sodium solution regulation system is 6.5, ageing 30min; Behind the filtering separation throw out, the degree Beaume of regulator solution is 20 °, adds polyoxyethylene glycol 0.12g, is 13 in the pH value of 80 ℃ of following dropping sodium solution to systems, can obtain flake nano level magnesium hydroxide products after ageing 50min after-filtration, washing, the drying.
Get dry sour lixiviation slag 40g; Add water 120g, solid sodium hydroxide 13g,, remove by filter residue at 95 ℃ of following stirring reaction 1h; Add water the degree Beaume of filtrating is adjusted to 20 °; Add 1.2g silane, 70 ℃ down and drips to add degree Beaume be that 20 ° water glass solution and mass concentration is that 20% sulphuric acid soln reacts, reaction system final pH value is 3.5; Ageing 50min in reaction back filters then, washs, drying and depolymerization promptly get ball shaped nano level WHITE CARBON BLACK product.
Embodiment two:
500kg boron mud is calcined 1h down at 600 ℃; Get calcining boron mud 200kg, add water 360kg, concentration is 96% sulfuric acid 240kg, reacts 1.5h down at 100 ± 5 ℃; Filter the back and separate the solid-liquid component; Adding 10kg mass concentration is 30% ydrogen peroxide 50 in leach liquor, reacts 15min down at 60 ℃; The pH value of hydro-oxidation sodium solution regulation system is 6.5, ageing 30min; Behind the filtering separation throw out, the degree Beaume of regulator solution is 20 °, adds polyoxyethylene glycol 0.24kg, is 13 in the pH value of 80 ℃ of following dropping sodium solution to systems, can obtain flake nano level magnesium hydroxide products after ageing 50min after-filtration, washing, the drying.
Get dry sour lixiviation slag 80kg; Add water 220kg, solid sodium hydroxide 26kg,, remove by filter residue at 100 ± 5 ℃ of following stirring reaction 1h; Add water the degree Beaume of filtrating is adjusted to 20 °; Add 2.4kg silane, 70 ℃ down and drips to add degree Beaume be that 20 ° sodium silicate solution and mass concentration is that 20% sulfuric acid reacts, the last pH value of reaction system is 3.5; Ageing 50min in reaction back filters then, washs, drying and depolymerization promptly get ball shaped nano level WHITE CARBON BLACK product.
Table 1 is embodiment products obtained therefrom physicochemical property detected results.
The check and analysis result of table 1 embodiment sample
Claims (6)
1. method of utilizing boric sludge to be equipped with nano-sized magnesium hydroxide and Nano carbon white is characterized in that its process step is:
(1) boron mud is calcined 1h down at 600 ℃;
(2) will calcine that back boron mud adds water and sulphuric acid soln reacts;
(3) reaction product is filtered separating solid residue;
(4) will filtrate and under 30~80 ℃, add hydrogen peroxide oxidation and alkaline chemical precipitation ironic hydroxide to slurries pH=4~7, and the filtering separation ironic hydroxide;
(5) filtrating after the deironing is added the particle surface modifier, and under 30~90 ℃ of temperature of reaction, add alkali reaction to slurries pH=10~13, after-filtration, washing, drying, depolymerization are accomplished in reaction, nano-sized magnesium hydroxide;
(6) step (3) filter residue hydro-oxidation sodium and water are reacted 1~4h down at 90~120 ℃, and to dope filtration;
(7) will filtrate with sulfuric acid 30~90 ℃ down and stream react to slurries pH=3~7, add the particle barrier agent simultaneously, after-filtration, washing, drying, depolymerization are accomplished in reaction, obtain nano silicon.
2. a kind of method of utilizing boric sludge to be equipped with nano-sized magnesium hydroxide and Nano carbon white according to claim 1; The batching mass ratio that it is characterized in that step (2) is calcining boron mud: 96% sulfuric acid: water (mass ratio)=100: 80~160: 120~240; 90~120 ℃ of temperature of reaction, reaction times 0.5~3h.
3. a kind of method of utilizing boric sludge to be equipped with nano-sized magnesium hydroxide and Nano carbon white according to claim 1 is characterized in that the consumption of ydrogen peroxide 50 is 1%~10% of calcining boron shale amount.
4. a kind of method of utilizing boric sludge to be equipped with nano-sized magnesium hydroxide and Nano carbon white according to claim 1; The particle surface modifier that it is characterized in that step (5) is one of titanic acid ester, silane, aluminate coupling agent, organosilicon or the combination between them, and consumption is 0.3%~5% of a Marinco H quality.
5. a kind of method of utilizing boric sludge to be equipped with nano-sized magnesium hydroxide and Nano carbon white according to claim 1, the batching mass ratio that it is characterized in that step (6) is sour molten slag: NaOH: water=100: 20~80: 200~400.
6. a kind of method of utilizing boric sludge to be equipped with nano-sized magnesium hydroxide and Nano carbon white according to claim 1; The particle barrier agent that it is characterized in that step (7) is one of polyoxyethylene glycol, aluminate coupling agent, titanate coupling agent, silane coupling agent, organosilicon, OP-10 or the combination between them, and consumption is 0.5%~6% of a Nano carbon white quality.
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Cited By (6)
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CN104446598A (en) * | 2014-06-30 | 2015-03-25 | 中国地质大学(北京) | Flame-retarding heat-insulating material based on boric sludgeand preparation method of flame-retarding heat-insulating material |
CN104671262A (en) * | 2015-01-30 | 2015-06-03 | 李广凡 | Light magnesium carbonate prepared by boric sludge acidification method as well as production method and application thereof |
CN112316910A (en) * | 2020-10-28 | 2021-02-05 | 东北大学 | Method for preparing adsorbent by graft modification of waste boric sludge sulfonic acid group |
CN112574504A (en) * | 2020-11-20 | 2021-03-30 | 应急管理部沈阳消防研究所 | Aerogel prepared by boron mud waste, flame retardant and modification application of aerogel |
CN116282096A (en) * | 2023-05-12 | 2023-06-23 | 中科镁基(北京)科技有限公司 | Comprehensive utilization method of boric sludge |
Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101161591A (en) * | 2006-10-09 | 2008-04-16 | 中国矿业大学(北京) | A method for preparing schistose nanometer magnesium hydroxide and sphericity nanometer white carbon black using zillerite gangue |
CN101323452A (en) * | 2007-06-11 | 2008-12-17 | 肖莹 | Method for preparing precipitated silica with boron sludge |
CN102030349A (en) * | 2010-11-29 | 2011-04-27 | 沈阳工业大学 | Method for extracting magnesium hydroxide by using boric sludge and treating dye wastewater |
-
2012
- 2012-08-31 CN CN2012101975103A patent/CN102815728A/en active Pending
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101161591A (en) * | 2006-10-09 | 2008-04-16 | 中国矿业大学(北京) | A method for preparing schistose nanometer magnesium hydroxide and sphericity nanometer white carbon black using zillerite gangue |
CN101323452A (en) * | 2007-06-11 | 2008-12-17 | 肖莹 | Method for preparing precipitated silica with boron sludge |
CN102030349A (en) * | 2010-11-29 | 2011-04-27 | 沈阳工业大学 | Method for extracting magnesium hydroxide by using boric sludge and treating dye wastewater |
Non-Patent Citations (2)
Title |
---|
宁志强等: "利用硼泥制备氢氧化镁", 《矿冶工程》, vol. 28, no. 2, 30 April 2008 (2008-04-30) * |
葛旭东: "硼泥的综合回收及氧化镁的制备", 《中国优秀硕士学位论文全文数据库工程科技I辑》, no. 3, 20 August 2007 (2007-08-20) * |
Cited By (10)
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CN103923379A (en) * | 2013-01-14 | 2014-07-16 | 中国地质大学(北京) | Method for preparing fire retardation polymer composite material by using boron mud |
CN103923379B (en) * | 2013-01-14 | 2016-08-10 | 中国地质大学(北京) | A kind of utilize boric sludge for the method for flame-retardant high-molecular composite |
CN104446598A (en) * | 2014-06-30 | 2015-03-25 | 中国地质大学(北京) | Flame-retarding heat-insulating material based on boric sludgeand preparation method of flame-retarding heat-insulating material |
CN104446598B (en) * | 2014-06-30 | 2016-09-07 | 中国地质大学(北京) | A kind of fire-retardant fireproof insulation material based on boron mud and preparation method thereof |
CN104671262A (en) * | 2015-01-30 | 2015-06-03 | 李广凡 | Light magnesium carbonate prepared by boric sludge acidification method as well as production method and application thereof |
CN104671262B (en) * | 2015-01-30 | 2017-11-03 | 吴细霞 | Light magnesium carbonate and its production method and purposes made from a kind of boron mud acidization |
CN112316910A (en) * | 2020-10-28 | 2021-02-05 | 东北大学 | Method for preparing adsorbent by graft modification of waste boric sludge sulfonic acid group |
CN112316910B (en) * | 2020-10-28 | 2021-11-05 | 东北大学 | Method for preparing adsorbent by graft modification of waste boric sludge sulfonic acid group |
CN112574504A (en) * | 2020-11-20 | 2021-03-30 | 应急管理部沈阳消防研究所 | Aerogel prepared by boron mud waste, flame retardant and modification application of aerogel |
CN116282096A (en) * | 2023-05-12 | 2023-06-23 | 中科镁基(北京)科技有限公司 | Comprehensive utilization method of boric sludge |
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