CN103193236B - Method of preparing silica by using diatomite - Google Patents
Method of preparing silica by using diatomite Download PDFInfo
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- CN103193236B CN103193236B CN201310070008.0A CN201310070008A CN103193236B CN 103193236 B CN103193236 B CN 103193236B CN 201310070008 A CN201310070008 A CN 201310070008A CN 103193236 B CN103193236 B CN 103193236B
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- hydrochloric acid
- diatomite
- substance
- fluorine
- sio
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 109
- 239000000377 silicon dioxide Substances 0.000 title claims abstract description 30
- 238000000034 method Methods 0.000 title claims abstract description 24
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 96
- 238000006243 chemical reaction Methods 0.000 claims abstract description 39
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims abstract description 34
- 229910052731 fluorine Inorganic materials 0.000 claims abstract description 34
- 239000011737 fluorine Substances 0.000 claims abstract description 34
- 235000012538 ammonium bicarbonate Nutrition 0.000 claims abstract description 22
- 239000000706 filtrate Substances 0.000 claims abstract description 19
- 230000020477 pH reduction Effects 0.000 claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000002253 acid Substances 0.000 claims abstract description 11
- 239000012065 filter cake Substances 0.000 claims abstract description 6
- 239000000126 substance Substances 0.000 claims description 28
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 25
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 25
- 150000004649 carbonic acid derivatives Chemical class 0.000 claims description 25
- 229910052739 hydrogen Inorganic materials 0.000 claims description 25
- 239000001257 hydrogen Substances 0.000 claims description 25
- 239000012295 chemical reaction liquid Substances 0.000 claims description 24
- 235000012239 silicon dioxide Nutrition 0.000 claims description 22
- 229960001866 silicon dioxide Drugs 0.000 claims description 21
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 12
- 238000000967 suction filtration Methods 0.000 claims description 9
- 238000010907 mechanical stirring Methods 0.000 claims description 7
- 238000004821 distillation Methods 0.000 claims description 5
- 238000013019 agitation Methods 0.000 claims description 4
- 235000021050 feed intake Nutrition 0.000 claims description 4
- 229920006395 saturated elastomer Polymers 0.000 abstract description 12
- 238000004176 ammonification Methods 0.000 abstract description 8
- 239000002699 waste material Substances 0.000 abstract description 8
- 239000006227 byproduct Substances 0.000 abstract description 6
- 238000005516 engineering process Methods 0.000 abstract description 5
- 238000003756 stirring Methods 0.000 abstract description 5
- 239000012141 concentrate Substances 0.000 abstract 2
- 238000001914 filtration Methods 0.000 abstract 2
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 abstract 1
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 abstract 1
- 239000001099 ammonium carbonate Substances 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- 238000005086 pumping Methods 0.000 abstract 1
- 238000005406 washing Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 19
- 239000007864 aqueous solution Substances 0.000 description 10
- 239000000047 product Substances 0.000 description 10
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical compound [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 7
- 230000006837 decompression Effects 0.000 description 5
- 239000007787 solid Substances 0.000 description 5
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 4
- 230000009466 transformation Effects 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 2
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 2
- 229910000040 hydrogen fluoride Inorganic materials 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 229910000519 Ferrosilicon Inorganic materials 0.000 description 1
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 1
- 239000006004 Quartz sand Substances 0.000 description 1
- 239000003082 abrasive agent Substances 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000035 biogenic effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 210000003298 dental enamel Anatomy 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000006052 feed supplement Substances 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 230000003311 flocculating effect Effects 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000000873 masking effect Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000003110 molding sand Substances 0.000 description 1
- 235000019353 potassium silicate Nutrition 0.000 description 1
- 239000011241 protective layer Substances 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 239000011819 refractory material Substances 0.000 description 1
- 239000011435 rock Substances 0.000 description 1
- 239000013049 sediment Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- -1 there is lightweight Substances 0.000 description 1
- 239000012745 toughening agent Substances 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
Landscapes
- Silicon Compounds (AREA)
Abstract
The invention discloses a method of preparing silica by using diatomite. The method comprises dropwise adding fluorine-containing hydrochloric acid into the diatomite with stirring, acidifying under a temperature of 30-50 DEG C, after the acidification, filtering the acidification reaction solution through pumping to obtain a filtrate, that is, a hydrochloric acid solution of fluosilicic acid, distilling the hydrochloric acid solution of the fluosilicic acid under a reduced pressure to obtain a concentrate, adding a saturated aqueous ammonium bicarbonate into the concentrate, carrying out an ammonification reaction under a temperature of 10-90 DEG C, after completing the ammonification reaction, filtering the ammonification reaction solution, washing filter cakes with water, and drying to obtain the silica. The method uses the secondary diatomite and the by-product fluorine-containing hydrochloric acid, is easy to operate, high in conversion rate, and convenient to process, takes full use of resources, can turn wastes into treasures, and is a green and environmental-protective technology of continuously-developed circular economy.
Description
(1) technical field
The present invention relates to prepare the method for silicon-dioxide, particularly a kind of is raw material by long white secondary diatomite, utilizes fluorine chemical industry by-product hydrogen fluoride and hydrogen chloride solution to prepare the method for high-purity silicon dioxide.
(2) background technology
Diatomite is comprised of the remains of the very high diatom of silicon oxide-containing, radiolarians or sponge, to take diatom (housing) as main a kind of biogenic sediment rock, there is lightweight, chemical stability is good, porosity is high, sound insulation, wear-resisting, acidproof, heat-resisting, adsorptivity are strong, fusing point high, has been widely used in each industrial sector as flocculating aids, filling agent, support of the catalyst, abrasive material toughener and animal-feed supplement etc.The diatomaceous developing history of China is shorter, and product mostly is primary products.Autonomous county of the Chang Bai Korean nationality diatomite reserves in Changbai mountain, Jilin southern foot and source, the Yalu River are Fias, the diatomite resource base that grade is the highest, approximately 200,000,000 tons of geologic reserve.Wherein first grade ore deposit accounts for 1/3rd of workable reserve.But to one-level soil index, operation easier is large by low-grade purifying secondary diatomite, yield is low, and the cycle is long.In order to make full use of resource, improve the diatomaceous utilization ratio of secondary, be necessary the research that carries on technical development in product transformation upgrading.
Silicon-dioxide claims again silica.Very wide in distributed in nature, as quartz, quartz sand etc.White or colourless, density 2.2～2.66, fusing point 1670 ℃ of (tridymite), 1710 ℃ (cristobalites), 2230 ℃ of boiling points, relative permittivity is 3.9.Water insoluble, be slightly soluble in general acid, but be dissolved in hydrofluoric acid and hot strong phosphoric acid, energy and melting bases work.Be used for glass processed, water glass, pottery, enamel, refractory materials, ferrosilicon, molding sand, elemental silicon.In transistor and unicircuit, make masking film and the protective layer of diffusion of contaminants, make silicon dioxide film and make integrated circuit (IC)-components.
Along with the high speed development of fluorine chemical industry, at fluorine chemical enterprise fluorine-containing hydrochloric acid, be the large-tonnage by product that fluorine chemical enterprise all faces.In fluorine-containing hydrochloric acid, the existence of fluorion directly has influence on its use range and safety in utilization, also easily causes in addition the fluoride pollution of surrounding enviroment.The market of facing fluorine-containing hydrochloric acid is tending towards saturated severe situation day by day, and the scope of application how to expand fluorine-containing hydrochloric acid has become the matter of utmost importance that fluorine chemical enterprise development faces.Therefore, utilizing fluorine-containing hydrochloric acid to process secondary diatomite, prepare highly purified silicon-dioxide, is important green synthesis techniques and the developing direction of product transformation upgrading.
(3) summary of the invention
The object of the invention is to provide a kind of by product fluorine-containing hydrochloric acid that utilizes fluorine chemical industry and long white secondary diatomite is raw material, through acidifying, filter and alkalization decomposition reaction technology is prepared the method for high-purity silicon dioxide, it is cheap and easy to get that the method has used reaction raw materials, it is performance resources advantage, turn waste into wealth, a novelty production technology of the Sustainable development of product transformation upgrading.
The technical solution used in the present invention is:
The invention provides a kind of method of utilizing diatomite to prepare silicon-dioxide, described method is: under agitation fluorine-containing hydrochloric acid is added drop-wise in diatomite, at 30～50 ℃, carry out acidification reaction, after acidification reaction is complete, by acidification reaction liquid suction filtration, obtaining filtrate is the hydrochloric acid soln of silicofluoric acid, then hydrochloric acid soln underpressure distillation to the absence of liquid of silicofluoric acid is flowed out to remove hydrochloric acid, obtains concentrated solution; Then in concentrated solution, add unsaturated carbonate hydrogen aqueous ammonium, carry out aminating reaction at 10～90 ℃, after aminating reaction is complete, aminating reaction liquid is filtered, filter cake washes with water rear dry, obtains described silicon-dioxide; Described diatomite quality consumption is with SiO
2amount of substance meter, described fluorine-containing hydrochloric acid quality consumption is in HF amount of substance, the SiO in described diatomite
2with the feed intake ratio of amount of substance of HF in fluorine-containing hydrochloric acid be 1:6～7, the SiO in described diatomite
2with the ratio of bicarbonate of ammonia amount of substance in unsaturated carbonate hydrogen aqueous ammonium be 1:6～7.
Further, SiO in described diatomite
2mass content is 40～55%, preferably the secondary diatomite in Ba Daogou town, the white county of Jilin governor.
Further, in described fluorine-containing hydrochloric acid, HF mass content is 10～15%, preferred fluorinated industrial and commercial bank industry by-product hydrogen fluoride and hydrogen chloride solution mixed solution.
Further, described acidification reaction is to react 1～5h at 30～50 ℃.
Further, described aminating reaction carries out as follows: first in concentrated solution, add unsaturated carbonate hydrogen aqueous ammonium a at 15～20 ℃ of aminating reaction 3～4h, obtain aminating reaction liquid a, aminating reaction liquid a is filtered, in filtrate, add unsaturated carbonate hydrogen aqueous ammonium b at 80～85 ℃ of aminating reaction 1～2h, obtain aminating reaction liquid b, aminating reaction liquid b is filtered, filter cake washes with water rear dry, obtains described silicon-dioxide; The total amount of substance of bicarbonate of ammonia and SiO in described unsaturated carbonate hydrogen aqueous ammonium a and unsaturated carbonate hydrogen aqueous ammonium b
2the ratio of amount of substance is 6～7:1, unsaturated carbonate hydrogen aqueous ammonium a, and unsaturated carbonate hydrogen aqueous ammonium b consumption is separately on not impact of the present invention.
Further, of the present inventionly utilize the method that diatomite prepares silicon-dioxide to recommend to carry out as follows: in the there-necked flask that mechanical stirring, prolong, dropping funnel are housed, to add diatomite, under agitation fluorine-containing hydrochloric acid is added drop-wise in there-necked flask, at 35～40 ℃, carry out acidification reaction 2～4h, after acidification reaction is complete, by acidification reaction liquid suction filtration, obtaining filtrate is the hydrochloric acid soln of silicofluoric acid, again the hydrochloric acid soln underpressure distillation of silicofluoric acid is removed to hydrochloric acid, obtain concentrated solution; In concentrated solution, add unsaturated carbonate hydrogen aqueous ammonium a at 15～20 ℃ of aminating reaction 3～4h, obtain aminating reaction liquid a, aminating reaction liquid a is filtered, in filtrate, add unsaturated carbonate hydrogen aqueous ammonium b at 80～85 ℃ of aminating reaction 1～2h, obtain aminating reaction liquid b, aminating reaction liquid b is filtered, and filter cake washes with water rear dry, obtains described silicon-dioxide; SiO in described diatomite
2mass content is 40～55%, and in described fluorine-containing hydrochloric acid, HF mass content is 10～15%; Described diatomite quality consumption is with SiO
2amount of substance meter, described fluorine-containing hydrochloric acid quality consumption is in HF amount of substance, described SiO
2with the feed intake ratio of amount of substance of HF be 1:6～7, the total amount of substance of bicarbonate of ammonia and SiO in described unsaturated carbonate hydrogen aqueous ammonium a and unsaturated carbonate hydrogen aqueous ammonium b
2the ratio of amount of substance is 6～7:1, and unsaturated carbonate hydrogen aqueous ammonium a and unsaturated carbonate hydrogen aqueous ammonium b consumption are separately how many on not impact of the present invention.
The reaction formula that utilizes diatomite to prepare silicon-dioxide of the present invention is as follows:
SiO
2+HF→H
2SiF
6
H
2SiF
6+NH
4HCO
3→(NH
4)
2SiF
6
(NH
4)
2SiF
6→SiO
2↓+NH
4F+CO2↑+H
2O
Unsaturated carbonate hydrogen aqueous ammonium a of the present invention and unsaturated carbonate hydrogen aqueous ammonium b are unsaturated carbonate hydrogen aqueous ammonium, for ease of distinguishing different step institute consumption difference, name, aminating reaction liquid a and aminating reaction liquid b are aminating reaction liquid, for ease of distinguishing the reaction solution difference of different step acquisition, name, letter itself does not have implication.
After testing, purity reaches more than 95.0% the prepared silicon-dioxide of the present invention.
Compared with prior art, its beneficial effect is embodied in the present invention: the present invention uses secondary diatomite and by-product fluorine-containing hydrochloric acid, and technology is easy to operate, transformation efficiency is high, and it is convenient to process, and resource makes full use of, and can turn waste into wealth, be the recycling economy green environmental protection technique of Sustainable development.
(4) embodiment
Below in conjunction with specific embodiment, the present invention is described further, but protection scope of the present invention is not limited in this:
The diatomite using in the embodiment of the present invention is the secondary diatomite in Ba Daogou town, the white county of Jilin governor.
Embodiment 1
Secondary diatomite (the SiO that adds the white county of Jilin governor Ba Daogou town diatomite company to produce in the 5000mL there-necked flask of mechanical stirring, prolong, dropping funnel is housed
2content 40wt%) 150g (1mol), stir lower fluorine-containing hydrochloric acid (the HF content 10wt%) 1200g (6mol) that drips, 35 ℃ of acidification reactions 2 hours, react complete, suction filtration is removed after waste residue, getting filtrate decompression is concentrated into absence of liquid and spills out except remaining hydrochloric acid, obtain concentrated solution, at 15 ℃ to saturated aqueous solution (the bicarbonate of ammonia 160g that slowly adds bicarbonate of ammonia in concentrated solution, 2mol) carry out ammonification 3 hours, filter, filtrate adds saturated aqueous solution (the bicarbonate of ammonia 316g of 316g bicarbonate of ammonia again, 4mol) 80 ℃ of reactions of heating are 2 hours, filter, solid washes with water rear dry, obtain silica product 58g, yield 97%, purity 98%.
Embodiment 2
In being housed, the 5000mL there-necked flask of mechanical stirring, prolong, dropping funnel adds long Bai Badao ditch secondary diatomite (SiO
2content 50wt%) 120g (1mol), stirred lower fluorine-containing hydrochloric acid (the HF content 15wt%) 930g (7mol) that drips, 40 ℃ of acidification reactions 4 hours, react complete, suction filtration is removed after waste residue, gets filtrate decompression distillation and removes remaining hydrochloric acid, obtains concentrated solution.At 20 ℃ to saturated aqueous solution (the bicarbonate of ammonia 160g slowly adding in concentrated solution,) carry out ammonification 5 hours, filter, 85 ℃ of reactions of the saturated aqueous solution that filtrate adds again (bicarbonate of ammonia 316g, 4mol) heating 1 hour, filter, solid washes with water dry, obtain silica product 59g, yield 98%, purity 98%.
Embodiment 3
In being housed, the 5000mL there-necked flask of mechanical stirring, prolong, dropping funnel adds long Bai Badao ditch secondary diatomite (SiO
2content 50wt%) 120g (1mol), drips fluorine-containing hydrochloric acid (HF content 15wt%) 930g (7mol) under stirring, and 40 ℃ of reactions 5 hours, reacts complete, and suction filtration is removed after waste residue, gets concentrated remaining hydrochloric acid, the acquisition concentrated solution removed of filtrate decompression.At 20 ℃ to saturated aqueous solution (the bicarbonate of ammonia 160g that slowly adds bicarbonate of ammonia in concentrated solution, 2mol) carry out ammonification 5 hours, filter, filtrate adds the saturated aqueous solution (bicarbonate of ammonia 395g, 5mol) of bicarbonate of ammonia to heat 85 ℃ of reactions 2 hours again, filters, solid washes with water dry, obtain silica product 59g, yield 98%, purity 98%.
Embodiment 4
In being housed, the 5000mL there-necked flask of mechanical stirring, prolong, dropping funnel adds long Bai Badao ditch secondary diatomite (SiO
2content 45wt%) 810g (6mol), drips fluorine-containing hydrochloric acid (HF content 10wt%) 1400g (7mol) under stirring, and 40 ℃ of reactions 5 hours, reacts complete, and suction filtration is removed after waste residue, gets concentrated remaining hydrochloric acid, the acquisition concentrated solution removed of filtrate decompression.At 20 ℃, in concentrated solution, slowly add saturated aqueous solution to carry out ammonification 5 hours, filter, filtrate adds saturated aqueous solution (the bicarbonate of ammonia 395g of bicarbonate of ammonia again, 5mol) 85 ℃ of reactions of heating are 2 hours, filter, solid washes with water dry, obtains silica product 59g, yield 98%, purity 98%.
Embodiment 5
In being housed, the 5000mL there-necked flask of mechanical stirring, prolong, dropping funnel adds long Bai Badao ditch secondary diatomite (SiO
2content 55wt%) 110g (1mol), drips fluorine-containing hydrochloric acid (HF content 15wt%) 800g (6mol) under stirring, and 40 ℃ of reactions 5 hours, reacts complete, and suction filtration is removed after waste residue, gets concentrated remaining hydrochloric acid, the acquisition concentrated solution removed of filtrate decompression.At 20 ℃ to saturated aqueous solution (the bicarbonate of ammonia 160g that slowly adds bicarbonate of ammonia in concentrated solution, 2mol) carry out ammonification 5 hours, filter, filtrate adds the saturated aqueous solution (bicarbonate of ammonia 395g, 5mol) of bicarbonate of ammonia to heat 85 ℃ of reactions 2 hours again, filters, solid washes with water dry, obtain silica product 59g, yield 98%, purity 98%.
Claims (5)
1. a method of utilizing diatomite to prepare silicon-dioxide, it is characterized in that described method is: under agitation fluorine-containing hydrochloric acid is added drop-wise in diatomite, at 30～50 ℃, carry out acidification reaction, after acidification reaction is complete, by acidification reaction liquid suction filtration, obtaining filtrate is the hydrochloric acid soln of silicofluoric acid, then the hydrochloric acid soln underpressure distillation of silicofluoric acid is removed to hydrochloric acid, obtains concentrated solution; In concentrated solution, add unsaturated carbonate hydrogen aqueous ammonium a at 15～20 ℃ of aminating reaction 3～4h, obtain aminating reaction liquid a, aminating reaction liquid a is filtered, in filtrate, add unsaturated carbonate hydrogen aqueous ammonium b at 80～85 ℃ of aminating reaction 1～2h, obtain aminating reaction liquid b, aminating reaction liquid b is filtered, and filter cake washes with water rear dry, obtains described silicon-dioxide; Described diatomite quality consumption is with SiO
2amount of substance meter, described fluorine-containing hydrochloric acid quality consumption is in HF amount of substance, the SiO in described diatomite
2with the feed intake ratio of amount of substance of HF in fluorine-containing hydrochloric acid be 1:6～7, the total amount of substance of bicarbonate of ammonia and SiO in described unsaturated carbonate hydrogen aqueous ammonium a and unsaturated carbonate hydrogen aqueous ammonium b
2the ratio of amount of substance is 6～7:1.
2. utilize as claimed in claim 1 diatomite to prepare the method for silicon-dioxide, it is characterized in that SiO in described diatomite
2mass content is 40～55%.
3. utilize as claimed in claim 1 diatomite to prepare the method for silicon-dioxide, it is characterized in that in described fluorine-containing hydrochloric acid, HF mass content is 10～15%.
4. utilize as claimed in claim 1 diatomite to prepare the method for silicon-dioxide, it is characterized in that described acidification reaction is to react 1～5h at 30～50 ℃.
5. utilize as claimed in claim 1 diatomite to prepare the method for silicon-dioxide, it is characterized in that described method carries out as follows: in the there-necked flask that mechanical stirring, prolong, dropping funnel are housed, add diatomite, under agitation fluorine-containing hydrochloric acid is added drop-wise in there-necked flask, at 35～40 ℃, carry out acidification reaction 2～4h, after acidification reaction is complete, by acidification reaction liquid suction filtration, obtaining filtrate is the hydrochloric acid soln of silicofluoric acid, again the hydrochloric acid soln underpressure distillation of silicofluoric acid is removed to hydrochloric acid, obtain concentrated solution; In concentrated solution, add unsaturated carbonate hydrogen aqueous ammonium a at 15～20 ℃ of aminating reaction 3～4h, obtain aminating reaction liquid a, aminating reaction liquid a is filtered, in filtrate, add unsaturated carbonate hydrogen aqueous ammonium b at 80～85 ℃ of aminating reaction 1～2h, obtain aminating reaction liquid b, aminating reaction liquid b is filtered, and filter cake washes with water rear dry, obtains described silicon-dioxide; SiO in described diatomite
2mass content is 40～55%, and in described fluorine-containing hydrochloric acid, HF mass content is 10～15%; Described diatomite quality consumption is with SiO
2amount of substance meter, described fluorine-containing hydrochloric acid quality consumption is in HF amount of substance, described SiO
2with the feed intake ratio of amount of substance of HF be 1:6～7, the total amount of substance of bicarbonate of ammonia and SiO in described unsaturated carbonate hydrogen aqueous ammonium a and unsaturated carbonate hydrogen aqueous ammonium b
2the ratio of amount of substance is 6～7:1.
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| CN201310070008.0A CN103193236B (en) | 2013-03-05 | 2013-03-05 | Method of preparing silica by using diatomite |
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| CN104291341B (en) * | 2014-04-23 | 2016-06-29 | 多氟多化工股份有限公司 | A kind of preparation method of tire level white carbon |
| CN113120910A (en) * | 2020-01-15 | 2021-07-16 | 北京化工大学 | Method for preparing silicon dioxide by using silicon-containing minerals and application thereof |
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| CN1069245A (en) * | 1992-08-17 | 1993-02-24 | 陈汉长 | The soda acid dissolving working system of hydrated SiO 2 |
| CN1055296C (en) * | 1995-03-17 | 2000-08-09 | 武汉工业大学北京研究生部 | Prepn of silica white with opal and diatomite |
| US6930219B2 (en) * | 1999-09-07 | 2005-08-16 | Abb Lummus Global Inc. | Mesoporous material with active metals |
| CN1212267C (en) * | 2002-12-18 | 2005-07-27 | 中国矿业大学（北京校区） | Method for preparing nano silicon dioxide using diatomaceous earth |
| CN100567146C (en) * | 2008-03-20 | 2009-12-09 | 绍兴纳诺气凝胶新材料研发中心有限公司 | Diatomite is the method for feedstock production aerosil |
| CN101913595B (en) * | 2010-08-04 | 2012-02-22 | 中国科学院广州地球化学研究所 | Method for preparing porous carbon and white carbon black by using diatomite |
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