CN106006721B - A kind of magnesium hydroxide cladding powdered zinc hydroxytannate and preparation method thereof - Google Patents
A kind of magnesium hydroxide cladding powdered zinc hydroxytannate and preparation method thereof Download PDFInfo
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- CN106006721B CN106006721B CN201610444579.XA CN201610444579A CN106006721B CN 106006721 B CN106006721 B CN 106006721B CN 201610444579 A CN201610444579 A CN 201610444579A CN 106006721 B CN106006721 B CN 106006721B
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- Prior art keywords
- zinc
- magnesium hydroxide
- stannate
- hydroxytannate
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- 229910052725 zinc Inorganic materials 0.000 title claims abstract description 107
- 239000011701 zinc Substances 0.000 title claims abstract description 107
- 229910001862 magnesium hydroxide Inorganic materials 0.000 title claims abstract description 87
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 title claims abstract description 85
- 239000000347 magnesium hydroxide Substances 0.000 title claims abstract description 85
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 title claims abstract description 57
- 238000005253 cladding Methods 0.000 title claims abstract description 46
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 229940071182 stannate Drugs 0.000 claims abstract description 87
- 238000006243 chemical reaction Methods 0.000 claims abstract description 26
- 239000000843 powder Substances 0.000 claims abstract description 13
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 20
- 238000003756 stirring Methods 0.000 claims description 19
- YVZATJAPAZIWIL-UHFFFAOYSA-M [Zn]O Chemical compound [Zn]O YVZATJAPAZIWIL-UHFFFAOYSA-M 0.000 claims description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
- 239000002253 acid Substances 0.000 claims description 12
- 125000005402 stannate group Chemical group 0.000 claims description 12
- 159000000003 magnesium salts Chemical class 0.000 claims description 11
- 239000007864 aqueous solution Substances 0.000 claims description 10
- 239000011787 zinc oxide Substances 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 9
- TVQLLNFANZSCGY-UHFFFAOYSA-N disodium;dioxido(oxo)tin Chemical compound [Na+].[Na+].[O-][Sn]([O-])=O TVQLLNFANZSCGY-UHFFFAOYSA-N 0.000 claims description 8
- 229940079864 sodium stannate Drugs 0.000 claims description 8
- 239000000706 filtrate Substances 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 7
- 239000011268 mixed slurry Substances 0.000 claims description 6
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 5
- 238000013019 agitation Methods 0.000 claims description 5
- 241000370738 Chlorion Species 0.000 claims description 4
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 claims description 4
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 claims description 4
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims description 4
- 150000002500 ions Chemical class 0.000 claims description 4
- YIXJRHPUWRPCBB-UHFFFAOYSA-N magnesium nitrate Chemical compound [Mg+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O YIXJRHPUWRPCBB-UHFFFAOYSA-N 0.000 claims description 4
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- VSKDLKJOZFLQQZ-UHFFFAOYSA-M O[Sn] Chemical compound O[Sn] VSKDLKJOZFLQQZ-UHFFFAOYSA-M 0.000 claims description 2
- IOUCSUBTZWXKTA-UHFFFAOYSA-N dipotassium;dioxido(oxo)tin Chemical compound [K+].[K+].[O-][Sn]([O-])=O IOUCSUBTZWXKTA-UHFFFAOYSA-N 0.000 claims description 2
- 229910001629 magnesium chloride Inorganic materials 0.000 claims description 2
- 229910052943 magnesium sulfate Inorganic materials 0.000 claims description 2
- 235000019341 magnesium sulphate Nutrition 0.000 claims description 2
- 238000005516 engineering process Methods 0.000 abstract description 6
- 238000000354 decomposition reaction Methods 0.000 abstract description 5
- 239000011248 coating agent Substances 0.000 abstract description 4
- 238000000576 coating method Methods 0.000 abstract description 4
- 239000011258 core-shell material Substances 0.000 abstract description 3
- 239000002245 particle Substances 0.000 abstract description 3
- 239000007788 liquid Substances 0.000 abstract 1
- 239000007791 liquid phase Substances 0.000 abstract 1
- 239000002002 slurry Substances 0.000 description 23
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 21
- 239000000243 solution Substances 0.000 description 10
- BNEMLSQAJOPTGK-UHFFFAOYSA-N zinc;dioxido(oxo)tin Chemical compound [Zn+2].[O-][Sn]([O-])=O BNEMLSQAJOPTGK-UHFFFAOYSA-N 0.000 description 10
- 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 9
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 9
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 9
- 239000011734 sodium Substances 0.000 description 9
- 229910052708 sodium Inorganic materials 0.000 description 9
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 8
- 239000003063 flame retardant Substances 0.000 description 8
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 5
- 239000011777 magnesium Substances 0.000 description 5
- 229910052749 magnesium Inorganic materials 0.000 description 5
- 239000002994 raw material Substances 0.000 description 5
- 229910000019 calcium carbonate Inorganic materials 0.000 description 4
- 239000000779 smoke Substances 0.000 description 4
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 description 4
- 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 group 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 3
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 3
- 239000005864 Sulphur Substances 0.000 description 3
- 239000008187 granular material Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 238000001556 precipitation Methods 0.000 description 3
- 150000003606 tin compounds Chemical class 0.000 description 3
- 150000003751 zinc Chemical class 0.000 description 3
- 229920001661 Chitosan Polymers 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 2
- 229910007694 ZnSnO3 Inorganic materials 0.000 description 2
- 230000033228 biological regulation Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- 125000002057 carboxymethyl group Chemical group [H]OC(=O)C([H])([H])[*] 0.000 description 2
- 239000000460 chlorine Substances 0.000 description 2
- 229910052801 chlorine Inorganic materials 0.000 description 2
- 239000004927 clay Substances 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000004079 fireproofing Methods 0.000 description 2
- ZSIAUFGUXNUGDI-UHFFFAOYSA-N hexan-1-ol Chemical compound CCCCCCO ZSIAUFGUXNUGDI-UHFFFAOYSA-N 0.000 description 2
- 239000004530 micro-emulsion Substances 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- 239000011591 potassium Substances 0.000 description 2
- 229910052700 potassium Inorganic materials 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 208000016261 weight loss Diseases 0.000 description 2
- 230000004580 weight loss Effects 0.000 description 2
- 239000011592 zinc chloride Substances 0.000 description 2
- 235000005074 zinc chloride Nutrition 0.000 description 2
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 description 2
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 description 2
- 229960001763 zinc sulfate Drugs 0.000 description 2
- 229910000368 zinc sulfate Inorganic materials 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- 206010013786 Dry skin Diseases 0.000 description 1
- 241000165940 Houjia Species 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 241000276489 Merlangius merlangus Species 0.000 description 1
- 229910021627 Tin(IV) chloride Inorganic materials 0.000 description 1
- PTFCDOFLOPIGGS-UHFFFAOYSA-N Zinc dication Chemical compound [Zn+2] PTFCDOFLOPIGGS-UHFFFAOYSA-N 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 1
- 229910021502 aluminium hydroxide Inorganic materials 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 230000002421 anti-septic effect Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000031709 bromination Effects 0.000 description 1
- 238000005893 bromination reaction Methods 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 239000000920 calcium hydroxide Substances 0.000 description 1
- 235000011116 calcium hydroxide Nutrition 0.000 description 1
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 1
- 239000000292 calcium oxide Substances 0.000 description 1
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 125000004836 hexamethylene group Chemical group [H]C([H])([*:2])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[*:1] 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 230000003137 locomotive effect Effects 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910000000 metal hydroxide Inorganic materials 0.000 description 1
- 150000004692 metal hydroxides Chemical class 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 125000000913 palmityl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 229910052625 palygorskite Inorganic materials 0.000 description 1
- UOURRHZRLGCVDA-UHFFFAOYSA-D pentazinc;dicarbonate;hexahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Zn+2].[Zn+2].[Zn+2].[Zn+2].[Zn+2].[O-]C([O-])=O.[O-]C([O-])=O UOURRHZRLGCVDA-UHFFFAOYSA-D 0.000 description 1
- 229920001495 poly(sodium acrylate) polymer Polymers 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- NNMHYFLPFNGQFZ-UHFFFAOYSA-M sodium polyacrylate Chemical compound [Na+].[O-]C(=O)C=C NNMHYFLPFNGQFZ-UHFFFAOYSA-M 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 230000001629 suppression Effects 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 229910001432 tin ion Inorganic materials 0.000 description 1
- HPGGPRDJHPYFRM-UHFFFAOYSA-J tin(iv) chloride Chemical compound Cl[Sn](Cl)(Cl)Cl HPGGPRDJHPYFRM-UHFFFAOYSA-J 0.000 description 1
- 238000009941 weaving Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- 150000003752 zinc compounds Chemical class 0.000 description 1
- UGZADUVQMDAIAO-UHFFFAOYSA-L zinc hydroxide Chemical compound [OH-].[OH-].[Zn+2] UGZADUVQMDAIAO-UHFFFAOYSA-L 0.000 description 1
- 229910021511 zinc hydroxide Inorganic materials 0.000 description 1
- 229940007718 zinc hydroxide Drugs 0.000 description 1
- CHSMNMOHKSNOKO-UHFFFAOYSA-L zinc;dichloride;hydrate Chemical compound O.[Cl-].[Cl-].[Zn+2] CHSMNMOHKSNOKO-UHFFFAOYSA-L 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G19/00—Compounds of tin
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/10—Encapsulated ingredients
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Inorganic Chemistry (AREA)
- Cosmetics (AREA)
Abstract
The present invention disclose a kind of magnesium hydroxide cladding powdered zinc hydroxytannate, and in described powder, zinc hydroxyl stannate is core, and magnesium hydroxide is that shell wraps zinc hydroxyl stannate, and described zinc hydroxyl stannate mass fraction is 83%~99.5%, and remaining is magnesium hydroxide.Invention additionally discloses a kind of preparation method of magnesium hydroxide cladding powdered zinc hydroxytannate, including solid-liquid reaction generation zinc hydroxyl stannate and liquid phase coating to prepare magnesium hydroxide cladding powdered zinc hydroxytannate.The present invention uses coating technology, one layer of magnesium hydroxide is wrapped up on the surface of zinc hydroxyl stannate, form the magnesium hydroxide cladding powdered zinc hydroxytannate of core shell structure, due to the iris action of magnesium hydroxide shell, the shipwreck that zinc hydroxyl stannate thermally decomposes to generate is spread out with being coated from magnesium hydroxide in powdered zinc hydroxytannate particle, so that steam partial pressure raises in shell, so as to improve the heat decomposition temperature of zinc hydroxyl stannate.
Description
Technical field
The invention belongs to the preparing technical field of tin-based composites powder, specially a kind of magnesium hydroxide cladding hydroxyl stannate
Zinc powder body and preparation method thereof.
Background technology
In order to prevent fire and reduce fire damage, strict laws and regulations have all been formulated in countries in the world, in necessary neck
Domain（Such as：Electric, building, vehicles etc.）Pressure uses fire proofing.With the development of the society, people are to fire-retardant material
The requirement of material also more and more higher, from it is single it is fire-retardant develop into have concurrently it is fire-retardant, eliminate smoke, low toxicity, with environmental compatible and to the mankind
Health is harmless.It is flame retardant plastics that current industrial fire proofing, which has 80% or so, and its maximum user is electric, accurate
Machinery, building materials, transport（Aircraft, express locomotive, automobile etc.）, furniture, the industry such as weaving.Fire retardant is added, due to its operation side
Just it is, applied widely, cost is cheap, it has also become the flame-retardant modified major way of high polymer material.
Last century the eighties, International Tin Research Institute develop novel green fire-proof smoke suppressor zinc hydroxyl stannate（ZHS）, it
Than the flame retardancy and smoke suppression more excellent performance of single tin compound or zinc compound.Nowadays, ZHS is registered in REACH,
They have the following advantages that：It is 1. nontoxic（The mg/kg of LD50 ＞ 5000）, safety；2. have fire-retardant, smoke elimination concurrently and reduce CO growing amounts
Effect；3. addition is few；4. with flame retardant filler（Aluminium hydroxide, magnesium hydroxide）And there is good association between halogen flame
Same effect；5. white, easily toning.
But ZHS heat endurance is not high, easily decomposed at a temperature of higher than 180 DEG C and discharge hydrone.Institute
Can only be used in the plastics less than 180 DEG C of operations, which greatly limits it to use field.Unfinished its heat endurance of raising,
The present invention uses coating technology, wraps up one layer of magnesium hydroxide on the surface of zinc hydroxyl stannate, forms the hydroxyl stannate of nucleocapsid structure
Zinc@magnesium hydroxide composite granules.Due to the iris action of magnesium hydroxide shell, shipwreck that zinc hydroxyl stannate thermally decomposes to generate is with from hydroxyl
Spread out in base zinc stannate@magnesium hydroxide particles, cause steam partial pressure in shell to raise, the heat decomposition temperature of zinc hydroxyl stannate
Also improve therewith to more than 180 DEG C, its amplitude improved is determined by the thickness and consistency of magnesium hydroxide shell.Theoretically examine
Consider, because the temperature that magnesium hydroxide shell thermally decomposes is 340 DEG C, so magnesium hydroxide coats zinc hydroxyl stannate core-shell type powder
The heat decomposition temperature of body is between 180 DEG C~340 DEG C.
Preparation on zinc hydroxyl stannate：Domestic patent No.00119199.3（2000）Zinc solution is slowly added to
The synthesis of hydroxy zinc stannate into sodium stannate solution, zinc salt used are zinc chloride and zinc nitrate；Domestic patent
No.200510017855.6（2005）Using cheap tin compound as raw material, hydroxyl stannate of the particle diameter in 2~100 nm is made
Zinc, then nano-zinc stannate is obtained after high temperature sintering；Domestic article " ZnSnO3Microwave synthesis and characterize ",（《Nanosecond science and technology》,
In June, 2009, the 3rd phase of volume 6）Using sodium stannate and cheap zinc sulfate as raw material, synthesized using the microwave technology of fast energy-saving
ZnSnO3Micron ball and nano cubic block, but its X-ray diffractogram is shown as zinc hydroxyl stannate, synthetic reaction is in the solution
Carry out, and heated with microwave；Domestic patent No. 201110404724.9（2011）With three chloride hydrate zinc, stannic chloride and slope
Thread stone clay is raw material, and zinc hydroxyl stannate/palygorskite clay compound is prepared using coprecipitation；Domestic patent
No.201310502881.2（2013）Nano zinc hydroxyl stannate is prepared for by raw material of cheap tin compound, then through calcining
Obtain 5~100 nm zinc stannate；Domestic patent No. 201310223238.6（2013）With cetyl trimethyl bromination
Ammonium, n-hexyl alcohol, hexamethylene and deionized water composition microemulsion, using zinc sulfate and sodium stannate as reactant, are prepared containing sulphur respectively
The microemulsion of sour zinc and sodium stannate, then by both hybrid reactions, obtain sub-micron zinc hydroxyl stannate cubic granules；It is domestic special
Sharp No. 201310749354.1（2013）Zinc salt, stannate, carboxymethyl chitosan are added to the water stirring reaction, then mistake
Filter, be drying to obtain zinc hydroxyl stannate/carboxymethyl chitosan hydridization antiseptic；Domestic patent No. 201310192742.4（2013
Year）Natural whiting ore deposit is sintered into calcium oxide, then plus water digests, is refining to obtain milk of lime, then obtains calcium carbonate after being carbonized
Slurry, it is transferred in cladding kettle, adds and be dissolved in tetravalence pink salt among dilute acid soln, zinc salt and the salt with catalytic metal
Class, alkaline solution being added dropwise, regulation solution pH value is 9~11 or so, then heats up and reacts a period of time, progress press filtration,
Dry, crush, classification, obtaining final metal-doped zinc hydroxyl stannate microencapsulation calcium carbonate；BP No.2230255
（Nineteen ninety）Zinc hydroxyl stannate has been made as raw material using sodium stannate, zinc chloride, Sodium Polyacrylate, then has been calcined through traditional heating mode
Obtain zinc stannate；European patent No.0537479（1993）Acid tin ion solution, zinc ion solution and ammoniacal liquor are mixed,
Zinc hydroxyl stannate precipitation is generated in the range of final pH=5~9, then filtering, dry, calcining obtains zinc stannate, is molded for manufacturing
Material；United States Patent (USP) No.5209911（1993）With solid metal oxide, metal hydroxides and metal carbonate and hydroxyl
Base sodium stannate prepares metal stannate；World patent No.97/00909（1997）On the surface of calcium carbonate or magnesium hydroxide
Deposited hydroxyl zinc stannate, it is prepared for the calcium carbonate or magnesium hydroxide of zinc stannate parcel；European patent No.0483266（1999
Year）Respectively by zinc oxide, zinc hydroxide or basic zinc carbonate and hydroxyl stannate sodium reaction generation zinc hydroxyl stannate.
Above patent focuses on the preparation of the powder of hydroxyl zinc stannate, the heat without putting forth effort raising zinc hydroxyl stannate
Stability, that is, improve its heat decomposition temperature.
The content of the invention
In view of the above-mentioned problems, the present invention provides a kind of magnesium hydroxide cladding powdered zinc hydroxytannate and preparation method thereof,
One layer of magnesium hydroxide is wrapped up on the surface of zinc hydroxyl stannate, forms nucleocapsid structure, and the water for preventing zinc hydroxyl stannate from thermally decomposing to generate expands
Shed, so as to improve the heat decomposition temperature of zinc hydroxyl stannate.
For achieving the above object, technical scheme is as follows：
Described magnesium hydroxide cladding powdered zinc hydroxytannate, zinc hydroxyl stannate are core, and magnesium hydroxide is that shell wraps hydroxyl
Base zinc stannate, described zinc hydroxyl stannate mass fraction are 83%~99.5%, and remaining is magnesium hydroxide.
Described magnesium hydroxide cladding powdered zinc hydroxytannate, its preparation method comprise the following steps：
A, soluble stannate is dissolved in water and is configured to stannic acid saline solution, zinc oxide is added thereto, disperseed, Ran Houjia
The mixed slurry of thermal agitation, reaction generation hydroxyl zinc stannate and hydroxide；
B, by the mixed slurry in step A and the aqueous solution of soluble magnesium salt hybrid reaction under agitation, then it is aged, mistake
Filter, washing, free from admixture ion in filtrate is examined, and after pH value is 7~8, is dried and depolymerization, obtains magnesium hydroxide cladding hydroxyl
Base zinc stannate powder.
Soluble stannate in described step A is sodium stannate or potassium stannate；
In described step B, soluble magnesium salt be magnesium chloride, magnesium sulfate or magnesium nitrate in one kind, foreign ion phase
It should be one kind in chlorion, sulfate ion or nitrate ion.
The mol ratio of soluble stannate and zinc oxide in described step A is 1:1；Described stannic acid saline solution
Molar concentration is in 0.5 molL-1~2.0 molL-1Between.
Scattered in described step A refers to, is 200 rmin in rotating speed-1~3000 rmin-1Lower stirring 5~
30min, temperature are not higher than 40 DEG C.
Heating stirring in described step A refers to, is 200rmin in rotating speed-1~1400 rmin-1Lower stirring
0.5~4 hour, temperature was 40 DEG C~100 DEG C.
Soluble magnesium salt and the mol ratio of soluble stannate are 0.1~1 in described step B:1, soluble magnesium salt
Molar concentration is 0.1 molL-1~1.0 molL-1。
Hybrid reaction refers under agitation for mixed slurry and the aqueous solution of soluble magnesium salt in described step B, keeps stirring
Mix rotating speed is 100 rmin-1~500 rmin-1, the time is 0.5~2 hour, and temperature is 20 DEG C~90 DEG C.
In described step B ageing refer to after the completion of stirring lower hybrid reaction, temperature be 20 DEG C~90 DEG C at stand 1~
4 hours.
Drying temperature in described step B is 80 DEG C~220 DEG C.
The present invention is divided into two steps to realize the preparation of powder：The first step stannic acid saline solution and zinc oxide reaction generation hydroxyl
The slurry of base zinc stannate and hydroxide, zinc hydroxyl stannate is solid not soluble in water in the slurry, and hydrogen is used as in second step
Nucleus in magnesium oxide precipitation reaction；And hydroxide is dissolved in water, precipitating reagent is used as in second step, in zinc hydroxyl stannate nucleus
Induction under with soluble magnesium salt occur precipitation reaction generation magnesium hydroxide, magnesium hydroxide one generation i.e. is wrapped in zinc hydroxyl stannate
The core-shell type powder of the Surface Creation magnesium hydroxide cladding zinc hydroxyl stannate of nucleus.
The present invention effective result be：
The present invention uses coating technology, wraps up one layer of magnesium hydroxide on the surface of zinc hydroxyl stannate, forms nucleocapsid structure
Powder, due to the iris action of magnesium hydroxide shell, shipwreck that zinc hydroxyl stannate thermally decomposes to generate from magnesium hydroxide to coat hydroxyl
Spread out in zinc stannate powder granule, so that steam partial pressure raises in shell, so as to improve the thermal decomposition temperature of zinc hydroxyl stannate
Degree, and then improve the heat endurance of zinc hydroxyl stannate.
Embodiment
Below by specific embodiment, the present invention is described in detail.
Embodiment 1
The magnesium hydroxide cladding powdered zinc hydroxytannate of the present invention, zinc hydroxyl stannate is core, and magnesium hydroxide wraps for shell
Zinc hydroxyl stannate, wherein, the mass fraction of zinc hydroxyl stannate is 83%, and the mass fraction of magnesium hydroxide is 17%.
Described magnesium hydroxide cladding powdered zinc hydroxytannate, its preparation method comprise the following steps：
A, it is 0.5 molL to be dissolved in water to be configured to concentration by 0.5 mol sodium stannates-1Stannic acid sodium water solution, by 0.5
Mol zinc oxide is added thereto, in 40 DEG C, 200 rmin-1Rotating speed under disperse 5min, then in 40 DEG C, 200rmin-1's
Stirred under rotating speed, the slurry of reaction generation hydroxyl zinc stannate and sodium hydroxide；
B, it is 0.1 molL by the hydroxyl zinc stannate in step A and the slurry of sodium hydroxide and 500 mL concentration-1Chlorine
Change the aqueous solution of magnesium in 20 DEG C, 100 rmin-1Rotating speed under, stir 0.5 hour, be allowed to hybrid reaction, 1 be aged at 20 DEG C
Hour, the slurry of generation magnesium hydroxide cladding powdered zinc hydroxytannate；
C, by step B magnesium hydroxide coat powdered zinc hydroxytannate slurry it is filtered, washing, examine filtrate in nothing
Chlorion, it is 7 to survey its pH value, is dried and depolymerization, drying temperature are 80 DEG C, obtain magnesium hydroxide cladding hydroxyl stannate zinc powder
Body.
Embodiment 2
The magnesium hydroxide cladding powdered zinc hydroxytannate of the present invention, zinc hydroxyl stannate is core, and magnesium hydroxide wraps for shell
Zinc hydroxyl stannate, wherein, the mass fraction of zinc hydroxyl stannate is 85%, and the mass fraction of magnesium hydroxide is 15%.
Described magnesium hydroxide cladding powdered zinc hydroxytannate, its preparation method comprise the following steps：
A, it is 0.8 molL to be dissolved in water to be configured to concentration by 0.8 mol potassium stannates-1Stannic acid aqueous solutions of potassium, by 0.8
Mol zinc oxide is added thereto, in 30 DEG C, 800 rmin-1Rotating speed under disperse 10min, then in 50 DEG C, 500rmin-1
Rotating speed under stir, reaction generation hydroxyl zinc stannate and sodium hydroxide slurry；
B, it is 0.5molL by the hydroxyl zinc stannate in step A and the slurry of potassium hydroxide and 1000 mL concentration-1Chlorine
Change the aqueous solution of magnesium in 35 DEG C, 200 rmin-1Rotating speed under, stir 0.8 hour, be allowed to hybrid reaction, 2 be aged at 30 DEG C
Hour, the slurry of generation magnesium hydroxide cladding powdered zinc hydroxytannate；
C, by step B magnesium hydroxide coat powdered zinc hydroxytannate slurry it is filtered, washing, examine filtrate in nothing
Chlorion, it is 7.2 to survey its pH value, is dried and depolymerization, drying temperature are 100 DEG C, obtain magnesium hydroxide cladding hydroxyl stannate
Zinc powder body.
Embodiment 3
The magnesium hydroxide cladding powdered zinc hydroxytannate of the present invention, zinc hydroxyl stannate is core, and magnesium hydroxide wraps for shell
Zinc hydroxyl stannate, wherein, the mass fraction of zinc hydroxyl stannate is 92%, and the mass fraction of magnesium hydroxide is 8%.
Described magnesium hydroxide cladding powdered zinc hydroxytannate, its preparation method comprise the following steps：
A, it is 1.0 molL to be dissolved in water to be configured to concentration by 1.0 mol sodium stannates-1Stannic acid sodium water solution, by 1.0
Mol zinc oxide is added thereto, in 30 DEG C, 1500 rmin-1Rotating speed under disperse 20min, then in 60 DEG C, 800rmin-1
Rotating speed under stir, reaction generation hydroxyl zinc stannate and sodium hydroxide slurry；
B, it is 0.8molL by the hydroxyl zinc stannate in step A and the slurry of sodium hydroxide and 1000 mL concentration-1Sulphur
The aqueous solution of sour magnesium is in 50 DEG C, 300 rmin-1Rotating speed under, stir 1.2 hours, be allowed to hybrid reaction, 3 be aged at 50 DEG C
Hour, the slurry of generation magnesium hydroxide cladding powdered zinc hydroxytannate；
C, by step B magnesium hydroxide coat powdered zinc hydroxytannate slurry it is filtered, washing, examine filtrate in nothing
Sulfate ion, it is 7.5 to survey its pH value, is dried and depolymerization, drying temperature are 150 DEG C, obtain magnesium hydroxide cladding hydroxyl
Zinc stannate powder.
Embodiment 4
The magnesium hydroxide cladding powdered zinc hydroxytannate of the present invention, zinc hydroxyl stannate is core, and magnesium hydroxide wraps for shell
Zinc hydroxyl stannate, wherein, the mass fraction of zinc hydroxyl stannate is 95%, and the mass fraction of magnesium hydroxide is 5%.
Described magnesium hydroxide cladding powdered zinc hydroxytannate, its preparation method comprise the following steps：
A, it is 1.5molL to be dissolved in water to be configured to concentration by 1.5mol sodium stannates-1Stannic acid sodium water solution, by 1.5mol oxygen
Change zinc to be added thereto, in 25 DEG C, 2000 rmin-1Rotating speed under disperse 25min, then in 80 DEG C, 1200rmin-1Turn
Speed is lower to be stirred, the slurry of reaction generation hydroxyl zinc stannate and sodium hydroxide；
B, it is 1.0molL by the hydroxyl zinc stannate in step A and the slurry of potassium hydroxide and 1500 mL concentration-1Nitre
The aqueous solution of sour magnesium is in 70 DEG C, 400 rmin-1Rotating speed under, stir 1.5 hours, be allowed to hybrid reaction, be aged at 70 DEG C
3.5 hours, the slurry of generation magnesium hydroxide cladding powdered zinc hydroxytannate；
C, by step B magnesium hydroxide coat powdered zinc hydroxytannate slurry it is filtered, washing, examine filtrate in nothing
Nitrate ion, it is 7.8 to survey its pH value, is dried and depolymerization, drying temperature are 200 DEG C, obtain magnesium hydroxide cladding hydroxyl
Zinc stannate powder.
Embodiment 5
The magnesium hydroxide cladding powdered zinc hydroxytannate of the present invention, zinc hydroxyl stannate is core, and magnesium hydroxide wraps for shell
Zinc hydroxyl stannate, wherein, the mass fraction of zinc hydroxyl stannate is 99.5%, and the mass fraction of magnesium hydroxide is 0.5%.
Described magnesium hydroxide cladding powdered zinc hydroxytannate, its preparation method comprise the following steps：
A, it is 2.0molL to be dissolved in water to be configured to concentration by 2.0mol sodium stannates-1Stannic acid sodium water solution, by 2.0mol
Zinc oxide is added thereto, in 20 DEG C, 3000 rmin-1Rotating speed under disperse 30min, then in 100 DEG C, 1400rmin-1
Rotating speed under stir, reaction generation hydroxyl zinc stannate and sodium hydroxide slurry；
B, it is 0.75molL by the hydroxyl zinc stannate in step A and the slurry of potassium hydroxide and 2000mL concentration-1Sulphur
The aqueous solution of sour magnesium is in 90 DEG C, 500 rmin-1Rotating speed under, stir 2 hours, be allowed to hybrid reaction, be aged at 90 DEG C 4 small
When, the slurry of generation magnesium hydroxide cladding powdered zinc hydroxytannate；
C, by step B magnesium hydroxide coat powdered zinc hydroxytannate slurry it is filtered, washing, examine filtrate in nothing
Sulfate ion, it is 8 to survey its pH value, is dried and depolymerization, drying temperature are 220 DEG C, obtain magnesium hydroxide cladding hydroxyl tin
Sour zinc powder body.
The magnesium hydroxide of embodiment 6 coats the heat stabilization test of powdered zinc hydroxytannate and powdered zinc hydroxytannate
A certain amount of magnesium hydroxide cladding powdered zinc hydroxytannate is dried to constant weight at 120 DEG C, after being cooled to room temperature,
The accurate magnesium hydroxide cladding powdered zinc hydroxytannate for weighing 2 g dryings, is calcined 4 at 210 DEG C, 220 DEG C and 230 DEG C respectively
Hour, measure its weight-loss ratio.With same method, powdered zinc hydroxytannate is measured respectively at 210 DEG C, 220 DEG C and 230 DEG C
Weight-loss ratio.As a result it is as shown in table 1.
The magnesium hydroxide of table 1 coats powdered zinc hydroxytannate and the heat endurance of powdered zinc hydroxytannate contrasts
As it can be seen from table 1 the heat endurance of the magnesium hydroxide cladding powdered zinc hydroxytannate of the present invention is far better than hydroxyl
Base zinc stannate powder, when below 220 DEG C, it have dropped more than 100 times by thermolytic rate, under 230 DEG C of critical-temperature, its
Resolution ratio also far better than powdered zinc hydroxytannate, has very prominent heat endurance.
Claims (9)
- A kind of 1. preparation method of magnesium hydroxide cladding powdered zinc hydroxytannate, it is characterised in thatComprise the following steps：A, soluble stannate is dissolved in water and is configured to stannic acid saline solution, zinc oxide is added thereto, disperseed, then heating is stirred Mix, the mixed slurry of reaction generation hydroxyl zinc stannate and hydroxide；B, by the mixed slurry in step A and the aqueous solution of soluble magnesium salt hybrid reaction under agitation, then it is aged, filtering, Washing, free from admixture ion in filtrate is examined, and after pH value is 7 ~ 8, is dried and depolymerization, obtains magnesium hydroxide cladding hydroxyl tin Sour zinc powder body；In described powder, zinc hydroxyl stannate is core, and magnesium hydroxide is that shell wraps zinc hydroxyl stannate, described zinc hydroxyl stannate Mass fraction is 83%~99.5%, and remaining is magnesium hydroxide.
- 2. the preparation method of magnesium hydroxide cladding powdered zinc hydroxytannate according to claim 1, it is characterised in that：It is described Step A in soluble stannate be sodium stannate or potassium stannate；In described step B, soluble magnesium salt is one kind in magnesium chloride, magnesium sulfate or magnesium nitrate, and foreign ion mutually should be One kind in chlorion, sulfate ion or nitrate ion.
- 3. the preparation method of magnesium hydroxide cladding powdered zinc hydroxytannate according to claim 1, it is characterised in that：It is described Step A in soluble stannate and zinc oxide mol ratio be 1:1；The molar concentration of described stannic acid saline solution exists 0.5 mol·L-1~2.0 molL-1Between.
- 4. the preparation method of magnesium hydroxide cladding zinc hydroxyl stannate according to claim 1, it is characterised in that：Described step Scattered in rapid A refers to, is 200 rmin in rotating speed-1~3000 r·min-15 ~ 30min of lower stirring, temperature are not higher than 40 ℃。
- 5. the preparation method of magnesium hydroxide cladding powdered zinc hydroxytannate according to claim 1, it is characterised in that：It is described Step A in heating stirring refer to, be 200rmin in rotating speed-1~1400 r·min-1Lower stirring 0.5 ~ 4 hour, temperature For 40 DEG C ~ 100 DEG C.
- 6. the preparation method of magnesium hydroxide cladding powdered zinc hydroxytannate according to claim 1, it is characterised in that：It is described Step B in the mol ratio of soluble magnesium salt and soluble stannate be 0.1 ~ 1:1, the molar concentration of soluble magnesium salt is 0.1 mol·L-1~1.0 mol·L-1。
- 7. the preparation method of magnesium hydroxide cladding powdered zinc hydroxytannate according to claim 1, it is characterised in that：It is described Step B in mixed slurry and the aqueous solution of soluble magnesium salt hybrid reaction refers under agitation, be kept stirring for rotating speed as 100 r·min-1~500 r·min-1, the time is 0.5 ~ 2 hour, and temperature is 20 DEG C ~ 90 DEG C.
- 8. the preparation method of magnesium hydroxide cladding powdered zinc hydroxytannate according to claim 1, it is characterised in that：It is described Step B in be aged and refer to after the completion of stirring lower hybrid reaction, stand 1 ~ 4 hour at being 20 DEG C ~ 90 DEG C in temperature.
- 9. the preparation method of magnesium hydroxide cladding powdered zinc hydroxytannate according to claim 1, it is characterised in that：It is described Step B in drying temperature be 80 DEG C ~ 220 DEG C.
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