CN114315196A - Method for recovering silicon-phosphorus thermal insulation material from alkaline vanadium-containing liquid - Google Patents
Method for recovering silicon-phosphorus thermal insulation material from alkaline vanadium-containing liquid Download PDFInfo
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- CN114315196A CN114315196A CN202111396050.2A CN202111396050A CN114315196A CN 114315196 A CN114315196 A CN 114315196A CN 202111396050 A CN202111396050 A CN 202111396050A CN 114315196 A CN114315196 A CN 114315196A
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- vanadium
- containing liquid
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- alkaline
- magnesium oxide
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- 229910052720 vanadium Inorganic materials 0.000 title claims abstract description 86
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 title claims abstract description 83
- 239000007788 liquid Substances 0.000 title claims abstract description 48
- 238000000034 method Methods 0.000 title claims abstract description 46
- HIVGXUNKSAJJDN-UHFFFAOYSA-N [Si].[P] Chemical compound [Si].[P] HIVGXUNKSAJJDN-UHFFFAOYSA-N 0.000 title claims abstract description 7
- 239000012774 insulation material Substances 0.000 title description 10
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 68
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims abstract description 44
- 239000000395 magnesium oxide Substances 0.000 claims abstract description 37
- 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 claims abstract description 34
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims abstract description 31
- 238000001035 drying Methods 0.000 claims abstract description 22
- 239000000843 powder Substances 0.000 claims abstract description 20
- 238000001914 filtration Methods 0.000 claims abstract description 16
- 239000011810 insulating material Substances 0.000 claims abstract description 12
- 238000006243 chemical reaction Methods 0.000 claims abstract description 11
- 239000012065 filter cake Substances 0.000 claims abstract description 11
- 238000000227 grinding Methods 0.000 claims abstract description 8
- 238000005406 washing Methods 0.000 claims abstract description 8
- 238000003756 stirring Methods 0.000 claims abstract description 4
- KKCBUQHMOMHUOY-UHFFFAOYSA-N Na2O Inorganic materials [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 claims description 15
- 239000002245 particle Substances 0.000 claims description 10
- 230000035484 reaction time Effects 0.000 claims description 6
- 239000012535 impurity Substances 0.000 abstract description 31
- 239000000126 substance Substances 0.000 abstract description 4
- 229910052710 silicon Inorganic materials 0.000 description 35
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 34
- 239000010703 silicon Substances 0.000 description 34
- 229910052698 phosphorus Inorganic materials 0.000 description 25
- 239000011574 phosphorus Substances 0.000 description 24
- 239000002893 slag Substances 0.000 description 24
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 23
- YKTSYUJCYHOUJP-UHFFFAOYSA-N [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] Chemical compound [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] YKTSYUJCYHOUJP-UHFFFAOYSA-N 0.000 description 23
- 230000000694 effects Effects 0.000 description 18
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 17
- 239000011734 sodium Substances 0.000 description 17
- 229910052708 sodium Inorganic materials 0.000 description 17
- 239000000203 mixture Substances 0.000 description 15
- ODINCKMPIJJUCX-UHFFFAOYSA-N Calcium oxide Chemical compound [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 14
- 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 description 14
- 230000000052 comparative effect Effects 0.000 description 9
- 238000001556 precipitation Methods 0.000 description 9
- 239000000292 calcium oxide Substances 0.000 description 7
- 235000012255 calcium oxide Nutrition 0.000 description 7
- 238000004321 preservation Methods 0.000 description 7
- 239000000047 product Substances 0.000 description 7
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 6
- 239000003795 chemical substances by application Substances 0.000 description 6
- GNTDGMZSJNCJKK-UHFFFAOYSA-N divanadium pentaoxide Chemical compound O=[V](=O)O[V](=O)=O GNTDGMZSJNCJKK-UHFFFAOYSA-N 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 229910020489 SiO3 Inorganic materials 0.000 description 5
- 239000002131 composite material Substances 0.000 description 5
- 239000002244 precipitate Substances 0.000 description 5
- 239000002699 waste material Substances 0.000 description 5
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 4
- 238000009413 insulation Methods 0.000 description 4
- 239000011777 magnesium Substances 0.000 description 4
- 229910052749 magnesium Inorganic materials 0.000 description 4
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 description 4
- 239000000347 magnesium hydroxide Substances 0.000 description 4
- 229910001862 magnesium hydroxide Inorganic materials 0.000 description 4
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 3
- 229920000742 Cotton Polymers 0.000 description 3
- 239000004115 Sodium Silicate Substances 0.000 description 3
- 125000003158 alcohol group Chemical group 0.000 description 3
- 239000011575 calcium Substances 0.000 description 3
- 229910052791 calcium Inorganic materials 0.000 description 3
- 238000000605 extraction Methods 0.000 description 3
- BHEPBYXIRTUNPN-UHFFFAOYSA-N hydridophosphorus(.) (triplet) Chemical compound [PH] BHEPBYXIRTUNPN-UHFFFAOYSA-N 0.000 description 3
- 238000002386 leaching Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 3
- 229910052911 sodium silicate Inorganic materials 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 239000000654 additive Substances 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 2
- NWJKPSLXLQLUTC-UHFFFAOYSA-N ethane-1,2-diol;sodium Chemical compound [Na].OCCO NWJKPSLXLQLUTC-UHFFFAOYSA-N 0.000 description 2
- 125000003827 glycol group Chemical group 0.000 description 2
- GVALZJMUIHGIMD-UHFFFAOYSA-H magnesium phosphate Chemical compound [Mg+2].[Mg+2].[Mg+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O GVALZJMUIHGIMD-UHFFFAOYSA-H 0.000 description 2
- 239000004137 magnesium phosphate Substances 0.000 description 2
- 229960002261 magnesium phosphate Drugs 0.000 description 2
- 229910000157 magnesium phosphate Inorganic materials 0.000 description 2
- 235000010994 magnesium phosphates Nutrition 0.000 description 2
- 239000007769 metal material Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000011819 refractory material Substances 0.000 description 2
- CMZUMMUJMWNLFH-UHFFFAOYSA-N sodium metavanadate Chemical compound [Na+].[O-][V](=O)=O CMZUMMUJMWNLFH-UHFFFAOYSA-N 0.000 description 2
- 159000000000 sodium salts Chemical class 0.000 description 2
- 229910000166 zirconium phosphate Inorganic materials 0.000 description 2
- 239000004113 Sepiolite Substances 0.000 description 1
- 229940115440 aluminum sodium silicate Drugs 0.000 description 1
- 239000000440 bentonite Substances 0.000 description 1
- 229910000278 bentonite Inorganic materials 0.000 description 1
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000003365 glass fiber Substances 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- -1 phosphorus ions Chemical class 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 239000013049 sediment Substances 0.000 description 1
- 229910052624 sepiolite Inorganic materials 0.000 description 1
- 235000019355 sepiolite Nutrition 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- 210000002268 wool Anatomy 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention relates to the technical field of chemical industry, and discloses a method for recovering a silicon-phosphorus heat-insulating material from an alkaline vanadium-containing liquid. The method comprises the following steps: (1) adding aluminum sulfate and magnesium oxide into an ethylene glycol solution for reaction, then filtering, and drying and grinding a filter cake; (2) adding the fine powder obtained in the step (1) into an alkaline vanadium-containing liquid, stirring, reacting at 80-90 ℃, adjusting the pH value, standing, filtering, washing filter residues, and drying. The method has the advantages of high impurity removal rate and low vanadium loss, and the recovered heat-insulating material is high-temperature heat-insulating, has good heat-insulating performance and good fire resistance.
Description
Technical Field
The invention relates to the technical field of chemical industry, in particular to a method for recovering a silicon-phosphorus heat-insulating material from an alkaline vanadium-containing liquid.
Background
At present, the vanadium slag sodium salt roasting-water leaching vanadium process adopts sodium salt as roasting additive, roasting is carried out under high temperature and aerobic condition to generate sodium vanadate dissolved in water, sodium vanadate solution is obtained after water leaching, vanadium is further precipitated to obtain vanadium product, but the vanadium slag contains a large amount of silicon, sodium silicate is formed with sodium and enters the solution together, and the quality of vanadium precipitation and vanadium product is influenced if the sodium silicate is not removed from the vanadium solution. A plurality of common silicon removal methods are generally used, and the research of the salt-free roasting leachate deep impurity removal process researches that quicklime is firstly added for removing phosphorus, a silicon removal agent selects aluminum hydroxide, and impurity elements meet the national standard. A large amount of documents and patents are left in the pure silicon and phosphorus removal, and the impurity removal slag needs secondary vanadium extraction or direct stacking with the slag to be used as waste.
The literature of 'research on the deep impurity removal process of salt-free roasting leachate', experiments are carried out by selecting an impurity removal agent, selecting the impurity removal agent, adding conditions and other factors, the concentration of Si and P in vanadium liquid is reduced to be below 20ppm and 10ppm, and the product grade of the obtained vanadium pentoxide is over 99.5%. Adding quicklime for dephosphorization, selecting aluminum hydroxide as a desiliconization agent, controlling the desiliconization pH to be 8, controlling the temperature to be 60-80 ℃, controlling the adding amount to be 12.5 percent of the mass of the converted vanadium pentoxide, controlling the grade of the obtained vanadium pentoxide to be more than 99.5 percent, and enabling impurity elements to meet the national standard requirements.
CN110510930A discloses a heat insulation material with a heat insulation effect, which comprises the following raw materials in parts by mass: 20-75 parts of vitrified micro bubbles; 10-45 parts of sepiolite wool; 1-30 parts of aluminum silicate cotton; 5-20 parts of bentonite; 0.5-10 parts of glass fiber; 1-10 parts of a penetrating agent. The material has excellent long-term heat preservation performance, simultaneously covers the heat insulation temperature range from low temperature to high temperature, has lower volume weight when the material is used with the same thickness as aluminum silicate cotton, can reduce the thickness by more than 50 percent when the surface temperature is the same as that of the aluminum silicate cotton, and has obvious energy-saving effect because the heat dissipation area is greatly reduced. The insulation in this patent consists of a wide variety of different refractory materials.
In view of this, the invention provides a method for recovering heat insulating materials from alkaline vanadium liquid.
Disclosure of Invention
The invention aims to solve the problems that in the prior art, only silicon and phosphorus are simply removed from vanadium extraction leachate, impurities are not further utilized, and a heat insulation material in the prior art consists of a plurality of different refractory materials, and provides a method for recovering a silicon and phosphorus heat insulation material from an alkaline vanadium-containing liquid.
In order to achieve the aim, the invention provides a method for recovering silicon-phosphorus heat-insulating material from alkaline vanadium-containing liquid, which comprises the following steps:
(1) adding aluminum sulfate and magnesium oxide into an ethylene glycol solution for reaction, then filtering, and drying and grinding a filter cake;
(2) adding the fine powder obtained in the step (1) into an alkaline vanadium-containing liquid, stirring, reacting at 80-90 ℃, adjusting the pH value, standing, filtering, washing filter residues, and drying.
Preferably, the pH value of the alkaline vanadium-containing liquid is 9.5-10.
Preferably, the alkaline vanadium-containing liquid contains 35-40 g/L of V and 50-52 g/L of Na2O, 1.3-2 g/L Si and 0.01-0.1 g/L P.
Preferably, in the step (1), the mass ratio of the aluminum sulfate to the magnesium oxide is 48-50: 1.
Preferably, in the step (1), the solid-to-liquid ratio of the mass sum of aluminum sulfate and magnesium oxide to the glycol solution is 1: 0.5-1 g/L; the concentration of the ethylene glycol solution is 0.4-0.6 g/L.
Preferably, in the step (1), the drying temperature is 80-105 ℃.
Preferably, in the step (1), the reaction time is 60-120 min.
Preferably, in step (1), the particles are ground to a particle size of 74 microns or less.
Preferably, in the step (2), the solid-to-liquid ratio of the ground fine powder to the alkaline vanadium-containing liquid is 3-5 g/L.
Preferably, in the step (2), the reaction time is 30-40 min.
Preferably, in the step (2), the pH value is adjusted to 8.5-9.0.
Preferably, in the step (2), standing for 30-40 min.
Preferably, in the step (2), the drying temperature is 200-300 ℃.
Compared with the prior art, the invention has the following advantages:
1) silicon in the alkaline vanadium-containing liquid is used as an impurity, the vanadium precipitation rate and the vanadium precipitation product quality are influenced, and silicon is removed from the alkaline vanadium-containing liquid, so that the vanadium precipitation rate and the vanadium product quality are favorably improved.
2) In the prior art, the desiliconized substance of the alkaline vanadium-containing liquid has high impurity content, low reutilization rate, more wrapped vanadium products and larger vanadium loss, and some silicon-removing slag needs to be treated as waste slag together with the residue after secondary vanadium recovery. The method disclosed by the invention can remove silicon and phosphorus impurities from the alkaline vanadium-containing liquid, the impurity removal efficiency is high, the recovered silicon and phosphorus-removed slag has high-temperature heat insulation performance and can be used as a heat insulation material to recycle wastes, vanadium is hardly lost in the impurity removal process, and the influence of other elements in the alkaline vanadium-containing liquid is small.
3) In the invention, after the aluminum sulfate and the magnesium oxide are treated by the glycol, the remained alcohol group has higher affinity to sodium, is combined with the sodium in the process of removing silicon and phosphorus, has higher solubility, is separated from the precipitate and enters the solution, thus leading to less sodium carried in the precipitated slag, and the sodium content in the recycled silicon and phosphorus removing slag is less than 0.03 percent, therefore, the performance of the mixed silicon and phosphorus removing agent of the aluminum sulfate and the magnesium oxide after the glycol treatment is obviously superior to that of the aluminum sulfate and the magnesium oxide without the glycol treatment.
4) The heat insulation material provided by the invention mainly takes aluminum silicate as a main component, the aluminum silicate in the recycled silicon-removed phosphorus slag accounts for more than 98.5%, the recycled silicon-removed phosphorus slag can be independently used as a heat insulation material and also can be used as an additive of other heat insulation materials, the waste resource utilization is realized, and the recycled silicon-removed phosphorus slag contains a small amount of magnesium and has good fire resistance. .
5) The invention is mainly characterized in that: the silicon-removing phosphorus slag obtained by the invention has high aluminum silicate content and good heat preservation performance, and compared with the existing silicon removing method, the silicon removing method has good silicon removing effect and more importantly, the obtained aluminum silicate has high content.
Detailed Description
The following describes in detail specific embodiments of the present invention. It should be understood that the detailed description and specific examples, while indicating the present invention, are given by way of illustration and explanation only, not limitation.
The endpoints of the ranges and any values disclosed herein are not limited to the precise range or value, and such ranges or values should be understood to encompass values close to those ranges or values. For ranges of values, one or more new ranges of values may be obtained from combinations of values between the endpoints of each range, the endpoints of each range and the individual values, and the individual values of the points, and these ranges of values should be considered as specifically disclosed herein.
The invention provides a method for recovering a silicon-phosphorus heat-insulating material from an alkaline vanadium-containing liquid, which comprises the following steps:
(1) adding aluminum sulfate and magnesium oxide into an ethylene glycol solution for reaction, then filtering, and drying and grinding a filter cake;
(2) adding the fine powder obtained in the step (1) into an alkaline vanadium-containing liquid, stirring, reacting at 80-90 ℃, adjusting the pH value, standing, filtering, washing filter residues, and drying.
The method is simple to operate, and the heat-insulating material with good high-temperature heat-insulating performance and good fire resistance can be obtained by adding aluminum sulfate and magnesium oxide into an ethylene glycol solution for reaction, filtering, drying, grinding, adding the ground fine powder into an alkaline vanadium-containing liquid for reaction at a certain temperature, adjusting the pH value, standing, filtering, washing and drying. Specifically, the method comprises the following steps: in the step (1), the surface tension of the mixture of aluminum sulfate and magnesium oxide is reduced by the glycol, and the surfaces of the formed hydrated aluminum sulfate and magnesium hydroxide are covered by glycol groups, so that the effect of reducing the surface tension is achieved, the combination of aluminum sulfate and magnesium hydroxide with silicon and phosphorus in the subsequent silicon and phosphorus removal process is facilitated, the silicon and phosphorus removal efficiency is improved, meanwhile, after the aluminum sulfate and the magnesium oxide are treated by the glycol, the remaining alcohol groups have higher affinity to sodium, the solubility is higher after the alcohol groups are combined with the sodium in the silicon and phosphorus removal process, and the precipitate is separated and enters the solution, so that the sodium carried in filter residues is less, and the sodium in the recovered silicon and phosphorus removal residue is less. In the step (2), aluminum sulfate and sodium silicate in the alkaline vanadium-containing liquid generate aluminum silicate suspended particles, magnesium hydroxide is combined with phosphorus in the alkaline vanadium-containing liquid to generate magnesium phosphate, ethylene glycol groups are combined with sodium in the alkaline vanadium-containing liquid to generate ethylene glycol sodium, the ethylene glycol sodium enters the solution, and the obtained filter residue contains a large amount of aluminum silicate (with a heat preservation effect), a small amount of magnesium phosphate (with a high temperature resistance effect) and a small amount of sodium (without an effect on the heat preservation effect).
In the method, the alkaline vanadium solution is an alkaline vanadium extraction leaching solution which is conventionally obtained in the field.
In a preferred embodiment, the pH of the alkaline vanadium-containing solution used in the present invention is 9.5 to 10, and may be 9.5, 9.6, 9.7, 9.8, 9.9 or 10, for example.
In a preferred embodiment, the alkaline vanadium-containing solution contains 35-40 g/L of V and 50-52 g/L of Na2O, 1.3-2 g/L Si and 0.01-0.1 g/L P. For example, the alkaline vanadium-containing solution contains 38.5g/L of V and 51.0g/L of Na2O, 1.65g/L Si and 0.076g/L P.
In the method of the invention, in order to achieve better silicon and phosphorus removal effect without excessive entrainment of other ions and influence on the quality of the sediment (filter residue) as a heat preservation material, the dosage ratio of the aluminum sulfate to the magnesium oxide needs to be controlled within a proper range. In the present invention, the aluminum sulfate and the magnesium oxide are both analytically pure.
In a specific embodiment, in step (1), the mass ratio of the aluminum sulfate to the magnesium oxide may be 48 to 50:1, for example, 48:1, 48.5:1, 49:1, 49.5:1 or 50:1, preferably 49: 1.
In the method of the invention, in order to make aluminum sulfate and magnesium oxide form magnesium hydroxide in the glycol solution, and cover a layer of glycol group on the surface of the mixture, so as to reduce the surface tension of the mixture, and not to make excessive glycol enter into the alkaline vanadium solution, the ratio of the total dosage of the aluminum sulfate and the magnesium oxide to the dosage of the glycol solution needs to be controlled within a proper range.
In a specific embodiment, in the step (1), the concentration of the ethylene glycol solution is 0.4-0.6 g/L, such as 0.4g/L, 0.45g/L, 0.5g/L, 0.55g/L or 0.6 g/L; the solid-to-liquid ratio of the sum of the mass of the aluminum sulfate and the mass of the magnesium oxide to the glycol solution is 1: 0.5-1 g/L, such as 1:0.5g/L, 1:0.6g/L, 1:0.7g/L, 1:0.8g/L, 1:0.9g/L or 1:1 g/L.
In a specific embodiment, in the step (1), the reaction time may be 60 to 120min, for example, 60min, 70min, 80min, 90min, 100min, 110min or 120min, and preferably 100 to 120 min.
In a specific embodiment, in the step (1), the drying temperature may be 80 to 105 ℃, for example, 80 ℃, 85 ℃, 90 ℃, 95 ℃, 100 ℃ or 105 ℃.
In the method, the filter cake in the step (1) is ground, so that the surface area is increased when silicon and phosphorus are removed, and silicon and phosphorus ions are captured. In a specific embodiment, in step (1), the particles are ground to a particle size of 74 microns or less.
In a specific embodiment, in the step (2), the solid-to-liquid ratio of the ground fine powder to the alkaline vanadium-containing liquid is 3-5 g/L. The ratio of the fine powder to the alkaline vanadium-containing liquid is controlled within the range, so that silicon and phosphorus can be sufficiently removed without excessive precipitation of other substances.
In the method, the reaction temperature of the fine powder ground in the step (2) and the alkaline vanadium-containing liquid is controlled to be 80-90 ℃, the fine powder is easy to precipitate in the temperature range, aluminum silicate precipitate is favorably formed, and the formed precipitate can suspend and is difficult to precipitate when the temperature is too low. And (3) reacting the fine powder with an alkaline vanadium-containing liquid until the silicon content in the upper layer liquid is less than or equal to 0.015 g/L.
In specific embodiments, the reaction temperature in step (2) may be 80 ℃, 82 ℃, 84 ℃, 85 ℃, 86 ℃, 88 ℃ or 90 ℃.
In a preferred embodiment, in step (2), the reaction time is 30 to 40min, such as 30min, 32min, 34min, 35min, 36min, 38min or 40 min.
In the method, in order to improve the precipitation effect, the pH value of the fine powder ground in the step (2) needs to be adjusted after the fine powder reacts with the alkaline vanadium-containing liquid.
In a particular embodiment, in step (2), the pH is adjusted to a value of 8.5 to 9.0, such as 8.5, 8.6, 8.7, 8.8, 8.9 or 9.0. In the step (2), the ground powder reacts with the alkaline vanadium-containing liquid, and the pH value is adjusted to be in the range, so that the formed aluminum silicate gel-like precipitate chain is long and easy to precipitate.
In a specific embodiment, in step (2), the solution is allowed to stand for 30-40 min, for example, 30min, 32min, 34min, 35min, 36min, 38min or 40min, for complete precipitation after the pH is adjusted.
In a specific embodiment, in the step (2), the drying temperature may be 200 to 300 ℃, for example, 200 ℃, 220 ℃, 240 ℃, 250 ℃, 260 ℃, 280 ℃ or 300 ℃.
The method can remove the silicon and phosphorus impurities in the alkaline vanadium-containing liquid, avoids the impurities from influencing the subsequent vanadium precipitation rate and the quality of vanadium precipitation products, has high silicon impurity removal rate, can use the obtained silicon and phosphorus-removed slag as a heat insulation material, recycles waste, and hardly loses vanadium in the impurity removal process.
The present invention will be described in detail by way of examples, but the scope of the present invention is not limited thereto.
The basic vanadium-containing liquids used in the examples and comparative examples had the main components shown in table 1.
TABLE 1 basic vanadium-containing liquor principal ingredients g/L (pH 9.7)
| V | Na2O | Si | P | Ca | Fe | Mg |
| 38.5 | 51.0 | 1.65 | 0.076 | 0.09 | 0.056 | 0.06 |
Example 1
0.98g of aluminum sulfate and 0.02g of magnesium oxide mixture (the mass of the aluminum sulfate: the mass of the magnesium oxide is 49: 1) are added into 0.5L and 0.5g/L of glycol solution for reaction, and the solid-to-liquid ratio of the aluminum sulfate to the magnesium oxide mixture to the glycol solution is 1:0.5, reacting for 110 min; filtering, and drying a filter cake at 90 ℃; grinding the filter cake to be less than 74 micrometers (passing through a 200-mesh sieve); adding 0.6g of ground particles into 200mL of alkaline vanadium-containing solution, reacting at 80 ℃ for 30min, then adjusting the pH value to 8.5 with sulfuric acid, standing for half an hour, filtering, washing filter residues and drying at 200 ℃.
And (3) testing the components of filter residue: al (Al)2(SiO3)396.50%, MgO 0.80%, CaO 0.60%, P0.40%, TFe 0.30%, Na2O is 0.03%. The components of the vanadium solution after impurity removal are shown in table 2.
TABLE 2 example 1 vanadium solution composition g/L after impurity removal
| V | Na2O | Si | P |
| 38.49 | 50.96 | 0.015 | 0.036 |
As can be seen from Table 2, in example 1, the removal rate of Si was as high as 99%, the removal rate of P was 52.6%, and V, Na% was found in the vanadium solution before and after impurity removal2The content of O hardly changes.
It can be seen that the silicon removal effect in example 1 is good, and the obtained silicon-removing phosphorous slag mainly comprises aluminum silicate and a small amount of calcium and magnesium, so that the heat-insulating material with the aluminum silicate content as high as 96.50% is obtained, and the heat-insulating effect is excellent.
Example 2
Adding 9.8g of aluminum sulfate and 0.2g of magnesium oxide mixture (the mass of the aluminum sulfate: the mass of the magnesium oxide is 49: 1) into 7L of 0.5g/L of glycol solution for reaction, wherein the solid-to-liquid ratio of the aluminum sulfate to the magnesium oxide mixture to the glycol solution is 1:0.7, reacting for 100 min; filtering, and drying a filter cake at 90 ℃; grinding the filter cake to below 74 microns (200 mesh); adding 3.2g of ground particles into 800mL of alkaline vanadium-containing solution, reacting at 85 ℃ for 35min, then adjusting the pH value to 8.8 with sulfuric acid, standing for half an hour, filtering, washing filter residue and drying at 280 ℃.
And (3) testing the components of filter residue: al (Al)2(SiO3)397.30% of MgO, 0.85% of MgO, 0.61% of CaO, 0.40% of P, 0.30% of TFe and Na2O is 0.028%. Vanadium after impurity removalThe liquid composition is shown in Table 3.
TABLE 3 example 2 vanadium solution composition g/L after impurity removal
| V | Na2O | Si | P |
| 38.51 | 50.98 | 0.011 | 0.018 |
As can be seen from Table 3, in example 2, the removal rate of Si was as high as 99.3% or more, the removal rate of P was 76.3%, and V, Na% was present in the vanadium solution before and after impurity removal2The content of O hardly changes.
It can be seen that the silicon removal effect in example 2 is good, and the obtained silicon-removing phosphorous slag mainly comprises aluminum silicate and a small amount of calcium and magnesium, so that the heat-insulating material with the aluminum silicate content as high as 97.30% is obtained, and the heat-insulating effect is excellent.
Example 3
Adding 19.6g of aluminum sulfate and 0.4g of magnesium oxide mixture (the mass of the aluminum sulfate: the mass of the magnesium oxide is 49: 1) into 20L of 0.5g/L of glycol solution for reaction, wherein the solid-to-liquid ratio of the aluminum sulfate to the magnesium oxide mixture to the glycol solution is 1:1, reacting for 120 min; filtering, and drying a filter cake at 105 ℃; grinding the filter cake to be less than 74 micrometers (passing through a 200-mesh sieve); adding 5g of ground particles into 1000mL of alkaline vanadium-containing solution, reacting at 90 ℃ for 40min, then adjusting the pH value to 9.0 with sulfuric acid, standing for half an hour, filtering, washing filter residue and drying at 300 ℃.
And (3) testing the components of filter residue: al (Al)2(SiO3)398.30%, MgO 0.79%, CaO 0.58%, P0.48%, TFe 0.31%, Na2O is 0.018%. The components of the vanadium solution after impurity removal are shown in Table 4.
TABLE 4 example 3 vanadium solution composition g/L after impurity removal
| V | Na2O | Si | P |
| 38.50 | 51.02 | <0.01 | <0.01 |
As can be seen from Table 4, in example 3, the removal rate of Si was as high as 99% or more, the removal rate of P was as high as 99% or more, and V, Na was found in the vanadium solution before and after impurity removal2The content of O hardly changes.
It can be seen that the silicon removal effect in example 3 is good, and the obtained silicon-removing phosphorous slag mainly comprises aluminum silicate and a small amount of calcium and magnesium, so that the heat-insulating material with the aluminum silicate content as high as 98.30% is obtained, and the heat-insulating effect is excellent.
Comparative example 1
The procedure of example 3 was followed except that only magnesium oxide and no aluminum sulfate were added to the ethylene glycol solution.
And (3) testing the components of filter residue: al (Al)2(SiO3)345.50%, MgO 51.67%, CaO 0.48%, P0.47%, TFe 0.28%, Na2O is 1.50%. The components of the vanadium solution after impurity removal are shown in Table 5.
TABLE 5 composition g/L of vanadium solution after impurity removal in comparative example 1
| V | Na2O | Si | P |
| 38.44 | 49.65 | 1.20 | <0.01 |
As can be seen from table 5, the removal rate of silicon in comparative example 1 is not high. The content of aluminum silicate in the obtained silicon-phosphorus-removing slag is only 45.50 percent, and the heat preservation effect is not good.
Comparative example 2
The procedure of example 3 was followed except that aluminum sulfate and magnesium oxide were added without glycol treatment.
And (3) testing the components of filter residue: al (Al)2(SiO3)388.93% of MgO, 0.58% of MgO, 0.37% of CaO, 0.36% of P, 0.29% of TFe and Na2O is 9.43%. The components of the vanadium solution after impurity removal are shown in table 6.
TABLE 6 composition g/L of vanadium solution after impurity removal in comparative example 2
| V | Na2O | Si | P |
| 37.88 | 46.80 | 0.36 | 0.046 |
As can be seen from Table 6, the comparative example 2 has reduced silicon and phosphorus removal effect and also has a small vanadium loss because no ethylene glycol is used for treatment, the impurity-removed slag obtained in the comparative example 2 has high sodium content and cannot be used as a heat-insulating material, sodium is volatile at high temperature, and metal materials in contact with the sodium are easy to corrode other metal materials,
test example
Respectively preparing 2kg of the aluminum silicate slag removing composite powder according to the methods of the examples 1-3 and the comparative examples 1-2, weighing 1kg of the aluminum silicate slag removing composite powder, spreading the aluminum silicate slag removing composite powder in a ceramic tray to a thickness of 3mm, taking out a muffle furnace at 500 ℃, and directly placing a roasting crucible on the muffle furnace; the crucible was taken out of the muffle furnace at 500 ℃ and directly placed on the floor tile, and the results are shown in Table 7.
TABLE 7
As can be seen from Table 7, the 500 ℃ baked crucible is basically cooled to be directly held after being placed on the floor tile for half an hour, but the crucible placed on the aluminum silicate slag removing composite powder prepared by the method is slowly cooled, which indicates that the aluminum silicate slag removing composite powder prepared by the method has good heat preservation performance.
The preferred embodiments of the present invention have been described above in detail, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, many simple modifications can be made to the technical solution of the invention, including combinations of various technical features in any other suitable way, and these simple modifications and combinations should also be regarded as the disclosure of the invention, and all fall within the scope of the invention.
Claims (10)
1. A method for recovering silicon-phosphorus heat-insulating material from alkaline vanadium-containing liquid is characterized by comprising the following steps:
(1) adding aluminum sulfate and magnesium oxide into an ethylene glycol solution for reaction, then filtering, and drying and grinding a filter cake;
(2) adding the fine powder obtained in the step (1) into an alkaline vanadium-containing liquid, stirring, reacting at 80-90 ℃, adjusting the pH value, standing, filtering, washing filter residues, and drying.
2. The method according to claim 1, wherein the pH of the alkaline vanadium-containing liquid is 9.5-10;
preferably, the alkaline vanadium-containing liquid contains 35-40 g/L of V and 50-52 g/L of Na2O, 1.3-2 g/L Si and 0.01-0.1 g/L P.
3. The method according to claim 1, wherein in the step (1), the mass ratio of the aluminum sulfate to the magnesium oxide is 48-50: 1;
preferably, in the step (1), the solid-to-liquid ratio of the mass sum of aluminum sulfate and magnesium oxide to the ethylene glycol solution is 1: 0.5-1 g/L; the concentration of the ethylene glycol solution is 0.4-0.6 g/L.
4. The method according to claim 1 or 3, wherein in the step (1), the reaction time is 60 to 120 min.
5. The method according to claim 1, wherein the drying temperature in step (1) is 80 to 105 ℃.
6. The method of claim 1, wherein in step (1), the particles are ground to a particle size of 74 μm or less.
7. The method according to claim 1, wherein in the step (2), the solid-to-liquid ratio of the ground powder to the alkaline vanadium-containing liquid is 3-5 g/L.
8. The method according to claim 1, wherein in the step (2), the reaction time is 30 to 40 min.
9. The method according to claim 1, wherein in the step (2), the pH value is adjusted to 8.5-9.0;
preferably, in the step (2), standing for 30-40 min.
10. The method according to claim 1, wherein in the step (2), the drying temperature is 200 to 300 ℃.
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