CN115259220A - Preparation method of antimony tristannate - Google Patents
Preparation method of antimony tristannate Download PDFInfo
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- CN115259220A CN115259220A CN202210876738.9A CN202210876738A CN115259220A CN 115259220 A CN115259220 A CN 115259220A CN 202210876738 A CN202210876738 A CN 202210876738A CN 115259220 A CN115259220 A CN 115259220A
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- antimony
- tristannate
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- sodium stannate
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- 229910052787 antimony Inorganic materials 0.000 title claims abstract description 43
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 title claims abstract description 43
- 238000002360 preparation method Methods 0.000 title claims abstract description 7
- TVQLLNFANZSCGY-UHFFFAOYSA-N disodium;dioxido(oxo)tin Chemical compound [Na+].[Na+].[O-][Sn]([O-])=O TVQLLNFANZSCGY-UHFFFAOYSA-N 0.000 claims abstract description 32
- 229940079864 sodium stannate Drugs 0.000 claims abstract description 32
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 30
- GUNJVIDCYZYFGV-UHFFFAOYSA-K Antimony trifluoride Inorganic materials F[Sb](F)F GUNJVIDCYZYFGV-UHFFFAOYSA-K 0.000 claims abstract description 29
- ODNBVEIAQAZNNM-UHFFFAOYSA-N 1-(6-chloroimidazo[1,2-b]pyridazin-3-yl)ethanone Chemical compound C1=CC(Cl)=NN2C(C(=O)C)=CN=C21 ODNBVEIAQAZNNM-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000000243 solution Substances 0.000 claims abstract description 26
- 238000003756 stirring Methods 0.000 claims abstract description 24
- 238000005406 washing Methods 0.000 claims abstract description 15
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims abstract description 12
- 238000006243 chemical reaction Methods 0.000 claims abstract description 11
- 238000001914 filtration Methods 0.000 claims abstract description 11
- 239000012071 phase Substances 0.000 claims abstract description 10
- 239000012267 brine Substances 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims abstract description 9
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 claims abstract description 9
- 239000007790 solid phase Substances 0.000 claims abstract description 9
- 238000005191 phase separation Methods 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims description 12
- GVFOJDIFWSDNOY-UHFFFAOYSA-N antimony tin Chemical compound [Sn].[Sb] GVFOJDIFWSDNOY-UHFFFAOYSA-N 0.000 abstract description 3
- 239000000047 product Substances 0.000 description 22
- 239000010865 sewage Substances 0.000 description 15
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 11
- 239000003063 flame retardant Substances 0.000 description 11
- 238000007599 discharging Methods 0.000 description 10
- 239000002253 acid Substances 0.000 description 6
- ADCOVFLJGNWWNZ-UHFFFAOYSA-N antimony trioxide Chemical compound O=[Sb]O[Sb]=O ADCOVFLJGNWWNZ-UHFFFAOYSA-N 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- 238000003860 storage Methods 0.000 description 6
- 239000007864 aqueous solution Substances 0.000 description 5
- 239000012065 filter cake Substances 0.000 description 5
- 239000000706 filtrate Substances 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- 238000005086 pumping Methods 0.000 description 5
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 4
- 239000002270 dispersing agent Substances 0.000 description 3
- 239000013589 supplement Substances 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 239000000779 smoke Substances 0.000 description 2
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 description 2
- 230000001629 suppression Effects 0.000 description 2
- BHSXLOMVDSFFHO-UHFFFAOYSA-N (3-ethylsulfanylphenyl)methanamine Chemical compound CCSC1=CC=CC(CN)=C1 BHSXLOMVDSFFHO-UHFFFAOYSA-N 0.000 description 1
- 239000008346 aqueous phase Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 235000013024 sodium fluoride Nutrition 0.000 description 1
- 239000011775 sodium fluoride Substances 0.000 description 1
- RCIVOBGSMSSVTR-UHFFFAOYSA-L stannous sulfate Chemical compound [SnH2+2].[O-]S([O-])(=O)=O RCIVOBGSMSSVTR-UHFFFAOYSA-L 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 229910000375 tin(II) sulfate Inorganic materials 0.000 description 1
- BNEMLSQAJOPTGK-UHFFFAOYSA-N zinc;dioxido(oxo)tin Chemical compound [Zn+2].[O-][Sn]([O-])=O BNEMLSQAJOPTGK-UHFFFAOYSA-N 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G30/00—Compounds of antimony
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
-
- 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
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
A preparation method of antimony tristannate comprises the steps of firstly preparing an antimony trifluoride solution with a molar concentration of 0.5-1 moL/L and a sodium stannate solution with a molar concentration of 0.5-1 moL/L, wherein the molar ratio of antimony trifluoride to sodium stannate is 2; then adding sodium dodecyl benzene sulfonate into the sodium stannate solution, slowly dropwise adding the antimony trifluoride solution, and stirring and reacting for 3-5 h at the constant temperature of 60-80 ℃; and standing for phase separation after the reaction is finished, removing a brine phase, washing the solid phase with water, filtering and drying to obtain a yellow antimony tristannate product. The invention can prepare antimony tristannate with fine and uniform grain diameter to obtain a new tin-antimony compound, thereby meeting the requirements of technical development and market.
Description
Technical Field
The invention relates to the technical field of inorganic tin product production, in particular to a preparation method of antimony tristannate.
Background
The lead-acid storage battery is added with stannous sulfate and antimony trioxide independently or simultaneously, so that the capacity life of the battery can be prolonged, the performance of the lead-acid storage battery can be improved by adding the tin antimony compound, and theoretically, the antimony tristannate can be applied to the formula addition of the lead-acid storage battery. Meanwhile, in the flame retardant market, antimony trioxide is matched with halogen substances, so that the flame retardant effect is good, the antimony trioxide is widely used, and the antimony-containing compound is fully proved to have flame retardancy. With the appearance of flame retardants such as zinc stannate and magnesium stannate in recent years, the tin-based flame retardants have better performances in the aspects of smoke suppression, flame retardance and the like, and the tin-based flame retardants also have certain advantages in the aspect of flame retardance. Antimony tristannate contains antimony and tin base, and theoretically has better flame retardant and smoke suppression effects. Antimony tristannate currently belongs to the product blank in the market, and relevant literature data such as product synthesis process, appearance, physicochemical properties and the like are not reported. The preparation of antimony tristannate can enrich the variety of inorganic tin products and fill up the blank of the products; secondly, the formula of the lead-acid storage battery can be researched, so that the performance of the lead-acid storage battery is improved; and thirdly, the flame retardant can be applied to the addition of flame retardants such as plastics, wall materials and the like, can enrich the product market of antimony-containing flame retardants or tin-based flame retardants, and has good market application prospect.
Disclosure of Invention
The invention aims to provide a method for preparing antimony tristannate with fine and uniform particle size, and a novel tin-antimony compound is prepared, so that the requirements of technical development and market are met.
The technical scheme adopted by the invention is as follows:
a method for preparing antimony tristannate comprises the following steps:
(1) Preparing an antimony trifluoride solution with a molar concentration of 0.5-1 moL/L and a sodium stannate solution with a molar concentration of 0.5-1 moL/L, wherein the molar ratio of antimony fluoride to sodium stannate is 2;
(2) Adding sodium dodecyl benzene sulfonate into the sodium stannate solution, then slowly dropwise adding the antimony trifluoride solution, and stirring and reacting for 3-5 h at the constant temperature of 60-80 ℃;
(3) And after the reaction is finished, stopping stirring, standing for phase separation, removing a brine phase, washing the solid phase with water, filtering and drying to obtain a yellow antimony tristannate product.
Furthermore, the addition amount of the sodium dodecyl benzene sulfonate is 1-2% of the mass of the sodium stannate.
Further, the solid phase is washed for 3 to 5 times by water, and the water consumption is 1 to 2 times of that of the solid phase.
The method adopts sodium stannate, antimony trifluoride and a dispersing agent as raw materials, directly synthesizes and prepares the antimony tristannate, and has the advantages of simple and safe process method, less equipment investment, easily controlled production conditions, high production efficiency, high product yield and stable quality.
The antimony tristannate has strong hydrophilic property, and the method adds the sodium dodecyl benzene sulfonate serving as the dispersant in the synthetic reaction, so that the hydrophilicity of the antimony tristannate is reduced, the hydrophobicity is improved, the antimony tristannate is fully separated from a water phase, the solid-liquid separation can be accelerated, the filtration and the washing are easier, the filtration time is reduced, and a product with uniform and fine particle size is obtained.
Drawings
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
The invention is further illustrated by the following examples in conjunction with the drawings. The examples listed are only some examples of the present invention and do not limit the scope of the present invention.
A preparation method of antimony tristannate is shown in figure 1, and comprises the following specific steps:
(1) Adding deionized water into sodium stannate to prepare a sodium stannate solution with a molar concentration of 0.5-1 moL/L, and adding deionized water into antimony trifluoride to prepare an antimony trifluoride solution with a molar concentration of 0.5-1 moL/L; controlling the molar ratio of antimony trifluoride to sodium stannate to be 2;
(2) Firstly, adding sodium dodecyl benzene sulfonate which is a dispersant and accounts for 1-2% of the mass of sodium stannate into a sodium stannate solution to improve the hydrophobicity of antimony tristannate, then slowly dropwise adding antimony trifluoride, stirring and reacting for 3-5 h at a constant temperature of 60-80 ℃ to obtain solid phase antimony tristannate and aqueous phase sodium fluoride, wherein the chemical reaction formula is as follows:
2SbF3+3Na2SnO3＝Sb2(SnO3)3+6NaF
(3) After the reaction, the stirring was stopped, the mixture was allowed to stand for phase separation, and the brine phase was removed. And washing the solid phase with water, filtering and drying to obtain a yellow antimony tristannate product.
Example 1
853.2kg of sodium stannate with tin content of 41.5 percent is added into 300L of water and stirred to be dissolved, so as to obtain sodium stannate solution with molar concentration of 1moL L/L; 364.8kg of antimony trifluoride was added to 400L of water and dissolved by stirring to obtain an antimony trifluoride solution having a molar concentration of 0.5 moL/L. Pumping the dissolved sodium stannate solution into a reaction kettle, adding 8.5kg of sodium dodecyl benzene sulfonate, starting heat conduction oil to reach the temperature of 80 ℃, starting stirring, introducing an antimony trifluoride aqueous solution at the speed of 5kg/min, and reacting for 3 hours at the constant temperature of 80 ℃. Stopping stirring, standing for layering, and discharging the brine phase into a sewage system. Supplement 1m3Water is stirred and washed for 15min, standing and layering are carried out, washing water is discharged into a sewage system, and washing is carried out for three times. And opening a discharge valve, introducing all materials into a bag filter for filtering, discharging filtrate into a sewage system, and drying a filter cake to obtain 732.8Kg of yellow antimony tristannate product. The antimony content in the product is 32.58 percent, and the direct yield of antimony is 98.05 percent.
Example 2
Adding 838kg of sodium stannate with tin content of 42.5% into 300L of water, stirring and dissolving to obtain a sodium stannate solution with molar concentration of 1moL L/L; 364.8kg of antimony trifluoride was added to 400L of water and dissolved by stirring to obtain an antimony trifluoride solution having a molar concentration of 0.5 moL/L. Pumping the dissolved sodium stannate into a reaction kettle, adding 12kg of sodium dodecyl benzene sulfonate, starting heat conduction oil to 80 ℃, starting stirring, introducing an antimony trifluoride aqueous solution at the speed of 5kg/min, and reacting for 4 hours at the constant temperature of 80 ℃. Stopping stirring, standing for layering, and discharging the brine phase into a sewage system. Supplement 1m3Water is stirred and washed for 15min, standing and layering are carried out, washing water is discharged into a sewage system, and washing is carried out for four times repeatedly. And opening a discharge valve, introducing all the materials into a bag type filter for filtering, discharging the filtrate into a sewage system, and drying a filter cake to obtain 733.2kg of yellow antimony tristannate product. The antimony content in the product is 32.61%, and the direct yield of antimony is 98.19%.
Example 3
Adding 828kg of sodium stannate with tin content of 43% into 600L of water, stirring and dissolving to obtain sodium stannate solution with molar concentration of 0.5moL L/L; 364.8kg of antimony trifluoride was added to 200L of water and dissolved by stirring to obtain an antimony trifluoride solution having a molar concentration of 1 moL/L. Pumping the dissolved sodium stannate into a reaction kettle, adding 16kg of sodium dodecyl benzene sulfonate, starting heat conduction oil to 70 ℃, starting stirring, introducing an antimony trifluoride aqueous solution at the speed of 5kg/min, and reacting for 5 hours at the constant temperature of 70 ℃. Stopping stirring, standing for layering, and discharging the brine phase into a sewage system. Supplement 1m3Water is stirred and washed for 15min, standing and layering are carried out, washing water is discharged into a sewage system, and washing is carried out for five times repeatedly. And opening a discharge valve, introducing all the materials into a bag type filter for filtering, discharging the filtrate into a sewage system, and drying a filter cake to obtain 732.1kg of yellow antimony tristannate product. The antimony content in the product is 32.55%, and the direct yield of antimony is 97.86%.
Example 4
1676kg of sodium stannate with tin content of 42.5 percent is added with water and stirred to be dissolved, and sodium stannate solution with the molar concentration of 0.8moL/L is obtained; 729.6kg of antimony trifluoride was dissolved in water under stirring to obtain an antimony trifluoride solution having a molar concentration of 0.6 moL/L. Pumping the dissolved sodium stannate into a reaction kettle, adding 17kg of sodium dodecyl benzene sulfonate, starting heat conduction oil to 60 ℃, starting stirring, introducing an antimony trifluoride aqueous solution at the speed of 10kg/min, and reacting for 3 hours at the constant temperature of 60 ℃. Stopping stirring, standing for layering, and discharging the brine phase into a sewage system. Supplemented by 2m3Water is stirred and washed for 15min, standing and layering are carried out, washing water is discharged into a sewage system, and washing is carried out for three times. And opening a discharge valve, introducing all the materials into a bag type filter for filtering, discharging the filtrate into a sewage system, and drying a filter cake to obtain 1465kg of yellow antimony tristannate products. The antimony content in the product is 32.57%, and the direct yield of antimony is 97.98%.
Example 5
1676kg of sodium stannate with tin content of 42.5 percent is added with water and stirred to be dissolved, and sodium stannate solution with the molar concentration of 0.6moL L/L is obtained; 729.6kg of antimony trifluoride was dissolved in water under stirring to obtain an antimony trifluoride solution having a molar concentration of 0.7 moL/L. Pumping the dissolved sodium stannate into a reaction kettle, adding 33kg of sodium dodecyl benzene sulfonate, starting heat conduction oil to 80 ℃, starting stirring, introducing an antimony trifluoride aqueous solution at the speed of 10kg/min, and reacting for 4 hours at the constant temperature of 80 ℃. Stopping stirring, standing for layering, and discharging the brine phase into a sewage system. Supplemented by 2m3Water is stirred and washed for 15min, standing and layering are carried out, washing water is discharged into a sewage system, and washing is carried out for four times repeatedly. And opening a discharge valve, introducing all materials into a bag type filter for filtering, discharging filtrate into a sewage system, and drying a filter cake to obtain 1458kg of yellow antimony tristannate products. The antimony content in the product is 32.63 percent, and the direct yield of antimony is 97.69 percent.
The method has the advantages of simple equipment, easy control of process conditions, high production efficiency, high yield, low manufacturing cost, stable product quality and the like, and the prepared antimony tristannate product has high purity and can meet the application requirements of industries such as lead-acid storage batteries or flame retardants.
Claims (3)
1. The preparation method of the antimony tristannate is characterized by comprising the following steps of:
(1) Preparing an antimony trifluoride solution with a molar concentration of 0.5-1 moL/L and a sodium stannate solution with a molar concentration of 0.5-1 moL/L, wherein the molar ratio of antimony trifluoride to sodium stannate is 2;
(2) Adding sodium dodecyl benzene sulfonate into the sodium stannate solution, then slowly dropwise adding the antimony trifluoride solution, and stirring and reacting for 3-5 h at the constant temperature of 60-80 ℃;
(3) And after the reaction is finished, stopping stirring, standing for phase separation, removing a brine phase, washing a solid phase with water, filtering and drying to obtain a yellow antimony tristannate product.
2. The method for preparing antimony tristannate according to claim 1, wherein the amount of sodium dodecylbenzene sulfonate added is 1-2% of the mass of sodium stannate.
3. The method of claim 1, wherein the solid phase is washed with water 3-5 times in an amount of 1-2 times the amount of the solid phase.
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2022
- 2022-07-25 CN CN202210876738.9A patent/CN115259220A/en active Pending
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