CN114591360A - 有机硅浆渣的分离处理***及回收利用技术 - Google Patents
有机硅浆渣的分离处理***及回收利用技术 Download PDFInfo
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- CN114591360A CN114591360A CN202011298588.5A CN202011298588A CN114591360A CN 114591360 A CN114591360 A CN 114591360A CN 202011298588 A CN202011298588 A CN 202011298588A CN 114591360 A CN114591360 A CN 114591360A
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- silicon
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- solid
- separation
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- 239000002002 slurry Substances 0.000 title claims abstract description 59
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 28
- 239000010703 silicon Substances 0.000 title claims abstract description 27
- 238000004064 recycling Methods 0.000 title claims abstract description 5
- 238000000926 separation method Methods 0.000 title claims description 24
- 238000005516 engineering process Methods 0.000 title claims description 5
- 238000000034 method Methods 0.000 claims abstract description 52
- 239000007787 solid Substances 0.000 claims abstract description 35
- 239000007788 liquid Substances 0.000 claims abstract description 34
- 238000009835 boiling Methods 0.000 claims abstract description 27
- 239000002904 solvent Substances 0.000 claims abstract description 17
- 239000000126 substance Substances 0.000 claims abstract description 15
- 238000005406 washing Methods 0.000 claims abstract description 15
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910052802 copper Inorganic materials 0.000 claims abstract description 12
- 239000010949 copper Substances 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229910052581 Si3N4 Inorganic materials 0.000 claims abstract description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000000605 extraction Methods 0.000 claims abstract description 5
- 230000005484 gravity Effects 0.000 claims abstract description 5
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims abstract description 5
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229910010271 silicon carbide Inorganic materials 0.000 claims abstract description 4
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract 5
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical compound [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 claims abstract 4
- 229910052759 nickel Inorganic materials 0.000 claims abstract 3
- 229910052742 iron Inorganic materials 0.000 claims abstract 2
- 239000000377 silicon dioxide Substances 0.000 claims abstract 2
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract 2
- 230000007062 hydrolysis Effects 0.000 claims description 37
- 238000006460 hydrolysis reaction Methods 0.000 claims description 37
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 26
- 230000008569 process Effects 0.000 claims description 18
- 239000002699 waste material Substances 0.000 claims description 17
- 238000006243 chemical reaction Methods 0.000 claims description 11
- 229910000041 hydrogen chloride Inorganic materials 0.000 claims description 10
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 9
- 239000000178 monomer Substances 0.000 claims description 9
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 8
- 150000001875 compounds Chemical class 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 7
- 229910052801 chlorine Inorganic materials 0.000 claims description 6
- -1 amine halides Chemical class 0.000 claims description 5
- 239000000460 chlorine Substances 0.000 claims description 5
- 239000007789 gas Substances 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 5
- 238000000108 ultra-filtration Methods 0.000 claims description 5
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 4
- 239000003054 catalyst Substances 0.000 claims description 4
- 238000005336 cracking Methods 0.000 claims description 4
- 239000007791 liquid phase Substances 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 4
- 150000003839 salts Chemical class 0.000 claims description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 3
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 3
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical class Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims description 3
- 238000004523 catalytic cracking Methods 0.000 claims description 3
- 238000005119 centrifugation Methods 0.000 claims description 3
- 230000000694 effects Effects 0.000 claims description 3
- 229920001296 polysiloxane Polymers 0.000 claims description 3
- ZDHXKXAHOVTTAH-UHFFFAOYSA-N trichlorosilane Chemical compound Cl[SiH](Cl)Cl ZDHXKXAHOVTTAH-UHFFFAOYSA-N 0.000 claims description 3
- 239000005052 trichlorosilane Substances 0.000 claims description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical class [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 2
- 230000015572 biosynthetic process Effects 0.000 claims description 2
- 125000001309 chloro group Chemical group Cl* 0.000 claims description 2
- 239000002131 composite material Chemical class 0.000 claims description 2
- 229910052739 hydrogen Inorganic materials 0.000 claims description 2
- 239000001257 hydrogen Substances 0.000 claims description 2
- 229920002635 polyurethane Polymers 0.000 claims description 2
- 239000004814 polyurethane Substances 0.000 claims description 2
- 238000003786 synthesis reaction Methods 0.000 claims description 2
- 239000010457 zeolite Substances 0.000 claims 5
- 239000012013 faujasite Substances 0.000 claims 2
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 claims 1
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims 1
- JLTDJTHDQAWBAV-UHFFFAOYSA-N N,N-dimethylaniline Chemical compound CN(C)C1=CC=CC=C1 JLTDJTHDQAWBAV-UHFFFAOYSA-N 0.000 claims 1
- 229910021118 PdCo Inorganic materials 0.000 claims 1
- 229920001774 Perfluoroether Polymers 0.000 claims 1
- XYFCBTPGUUZFHI-UHFFFAOYSA-N Phosphine Natural products P XYFCBTPGUUZFHI-UHFFFAOYSA-N 0.000 claims 1
- 230000002378 acidificating effect Effects 0.000 claims 1
- 229910052783 alkali metal Inorganic materials 0.000 claims 1
- 150000001340 alkali metals Chemical class 0.000 claims 1
- 150000004996 alkyl benzenes Chemical class 0.000 claims 1
- 125000000217 alkyl group Chemical group 0.000 claims 1
- JYIBXUUINYLWLR-UHFFFAOYSA-N aluminum;calcium;potassium;silicon;sodium;trihydrate Chemical compound O.O.O.[Na].[Al].[Si].[K].[Ca] JYIBXUUINYLWLR-UHFFFAOYSA-N 0.000 claims 1
- 150000001412 amines Chemical class 0.000 claims 1
- 229910052794 bromium Inorganic materials 0.000 claims 1
- UNYSKUBLZGJSLV-UHFFFAOYSA-L calcium;1,3,5,2,4,6$l^{2}-trioxadisilaluminane 2,4-dioxide;dihydroxide;hexahydrate Chemical compound O.O.O.O.O.O.[OH-].[OH-].[Ca+2].O=[Si]1O[Al]O[Si](=O)O1.O=[Si]1O[Al]O[Si](=O)O1 UNYSKUBLZGJSLV-UHFFFAOYSA-L 0.000 claims 1
- 125000004432 carbon atom Chemical group C* 0.000 claims 1
- 229910052676 chabazite Inorganic materials 0.000 claims 1
- 150000008280 chlorinated hydrocarbons Chemical group 0.000 claims 1
- 150000001805 chlorine compounds Chemical class 0.000 claims 1
- 229910001603 clinoptilolite Inorganic materials 0.000 claims 1
- PZPGRFITIJYNEJ-UHFFFAOYSA-N disilane Chemical class [SiH3][SiH3] PZPGRFITIJYNEJ-UHFFFAOYSA-N 0.000 claims 1
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 claims 1
- 238000001035 drying Methods 0.000 claims 1
- 229910052675 erionite Inorganic materials 0.000 claims 1
- 229910052731 fluorine Inorganic materials 0.000 claims 1
- 229910052736 halogen Inorganic materials 0.000 claims 1
- 150000002367 halogens Chemical group 0.000 claims 1
- 231100001261 hazardous Toxicity 0.000 claims 1
- 150000002431 hydrogen Chemical class 0.000 claims 1
- 239000012535 impurity Substances 0.000 claims 1
- 239000011261 inert gas Substances 0.000 claims 1
- 239000012442 inert solvent Substances 0.000 claims 1
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical class [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 claims 1
- 229910052744 lithium Inorganic materials 0.000 claims 1
- 239000002808 molecular sieve Substances 0.000 claims 1
- 150000004767 nitrides Chemical class 0.000 claims 1
- 229910052763 palladium Inorganic materials 0.000 claims 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims 1
- 229910000073 phosphorus hydride Inorganic materials 0.000 claims 1
- 229910052697 platinum Inorganic materials 0.000 claims 1
- 229920000548 poly(silane) polymer Polymers 0.000 claims 1
- 229920001709 polysilazane Polymers 0.000 claims 1
- 229910052700 potassium Inorganic materials 0.000 claims 1
- 229910002093 potassium tetrachloropalladate(II) Inorganic materials 0.000 claims 1
- 239000002243 precursor Substances 0.000 claims 1
- 229910052703 rhodium Inorganic materials 0.000 claims 1
- 229910052707 ruthenium Inorganic materials 0.000 claims 1
- 239000010802 sludge Substances 0.000 claims 1
- 229910052708 sodium Inorganic materials 0.000 claims 1
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims 1
- 239000002910 solid waste Substances 0.000 claims 1
- 150000003512 tertiary amines Chemical class 0.000 claims 1
- 229910052723 transition metal Inorganic materials 0.000 claims 1
- 150000003624 transition metals Chemical class 0.000 claims 1
- RIOQSEWOXXDEQQ-UHFFFAOYSA-N triphenylphosphine Chemical compound C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1 RIOQSEWOXXDEQQ-UHFFFAOYSA-N 0.000 claims 1
- 239000002893 slag Substances 0.000 abstract description 18
- 238000011084 recovery Methods 0.000 abstract description 13
- 239000000243 solution Substances 0.000 abstract description 8
- 239000011863 silicon-based powder Substances 0.000 abstract description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 abstract description 4
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 abstract description 2
- 239000007864 aqueous solution Substances 0.000 abstract description 2
- 239000011575 calcium Substances 0.000 abstract description 2
- 229910052791 calcium Inorganic materials 0.000 abstract description 2
- 229910052751 metal Inorganic materials 0.000 abstract description 2
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 abstract 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 abstract 1
- 238000005342 ion exchange Methods 0.000 abstract 1
- 229910052718 tin Inorganic materials 0.000 abstract 1
- 239000011135 tin Substances 0.000 abstract 1
- 239000000413 hydrolysate Substances 0.000 description 12
- 238000001704 evaporation Methods 0.000 description 9
- 238000001914 filtration Methods 0.000 description 8
- 239000005046 Chlorosilane Substances 0.000 description 5
- KOPOQZFJUQMUML-UHFFFAOYSA-N chlorosilane Chemical compound Cl[SiH3] KOPOQZFJUQMUML-UHFFFAOYSA-N 0.000 description 5
- 230000008020 evaporation Effects 0.000 description 5
- 239000002609 medium Substances 0.000 description 5
- 239000012071 phase Substances 0.000 description 5
- 230000009467 reduction Effects 0.000 description 5
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 4
- 239000002253 acid Substances 0.000 description 4
- 230000007613 environmental effect Effects 0.000 description 4
- 239000000706 filtrate Substances 0.000 description 4
- 238000001556 precipitation Methods 0.000 description 4
- 239000004094 surface-active agent Substances 0.000 description 4
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 3
- 108010009736 Protein Hydrolysates Proteins 0.000 description 3
- 125000003545 alkoxy group Chemical group 0.000 description 3
- 238000005576 amination reaction Methods 0.000 description 3
- 239000006227 byproduct Substances 0.000 description 3
- 238000004140 cleaning Methods 0.000 description 3
- 230000003301 hydrolyzing effect Effects 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- LXEXBJXDGVGRAR-UHFFFAOYSA-N trichloro(trichlorosilyl)silane Chemical compound Cl[Si](Cl)(Cl)[Si](Cl)(Cl)Cl LXEXBJXDGVGRAR-UHFFFAOYSA-N 0.000 description 3
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 2
- 238000009825 accumulation Methods 0.000 description 2
- 239000012736 aqueous medium Substances 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 229910000019 calcium carbonate Inorganic materials 0.000 description 2
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 2
- 239000000920 calcium hydroxide Substances 0.000 description 2
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 2
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 2
- 239000000292 calcium oxide Substances 0.000 description 2
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 2
- YGZSVWMBUCGDCV-UHFFFAOYSA-N chloro(methyl)silane Chemical class C[SiH2]Cl YGZSVWMBUCGDCV-UHFFFAOYSA-N 0.000 description 2
- IJOOHPMOJXWVHK-UHFFFAOYSA-N chlorotrimethylsilane Chemical compound C[Si](C)(C)Cl IJOOHPMOJXWVHK-UHFFFAOYSA-N 0.000 description 2
- 238000009833 condensation Methods 0.000 description 2
- 230000005494 condensation Effects 0.000 description 2
- 239000006184 cosolvent Substances 0.000 description 2
- VEYJKODKHGEDMC-UHFFFAOYSA-N dichloro(trichlorosilyl)silicon Chemical compound Cl[Si](Cl)[Si](Cl)(Cl)Cl VEYJKODKHGEDMC-UHFFFAOYSA-N 0.000 description 2
- 238000004821 distillation Methods 0.000 description 2
- 239000010408 film Substances 0.000 description 2
- 239000003292 glue Substances 0.000 description 2
- JLUFWMXJHAVVNN-UHFFFAOYSA-N methyltrichlorosilane Chemical compound C[Si](Cl)(Cl)Cl JLUFWMXJHAVVNN-UHFFFAOYSA-N 0.000 description 2
- 239000002480 mineral oil Substances 0.000 description 2
- 235000010446 mineral oil Nutrition 0.000 description 2
- 239000012046 mixed solvent Substances 0.000 description 2
- 238000006386 neutralization reaction Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 230000002194 synthesizing effect Effects 0.000 description 2
- VYFXMIAQVGXIIN-UHFFFAOYSA-N trichloro(chlorosilyl)silane Chemical compound Cl[SiH2][Si](Cl)(Cl)Cl VYFXMIAQVGXIIN-UHFFFAOYSA-N 0.000 description 2
- 229910002808 Si–O–Si Inorganic materials 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000001464 adherent effect Effects 0.000 description 1
- 229920000615 alginic acid Polymers 0.000 description 1
- 239000000783 alginic acid Substances 0.000 description 1
- 229960001126 alginic acid Drugs 0.000 description 1
- 235000010443 alginic acid Nutrition 0.000 description 1
- 150000004781 alginic acids Chemical class 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 229920003180 amino resin Polymers 0.000 description 1
- 125000000129 anionic group Chemical group 0.000 description 1
- 239000003945 anionic surfactant Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- SRSXLGNVWSONIS-UHFFFAOYSA-M benzenesulfonate Chemical compound [O-]S(=O)(=O)C1=CC=CC=C1 SRSXLGNVWSONIS-UHFFFAOYSA-M 0.000 description 1
- 229940077388 benzenesulfonate Drugs 0.000 description 1
- 239000001110 calcium chloride Substances 0.000 description 1
- 229910001628 calcium chloride Inorganic materials 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 239000012700 ceramic precursor Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- QABCGOSYZHCPGN-UHFFFAOYSA-N chloro(dimethyl)silicon Chemical compound C[Si](C)Cl QABCGOSYZHCPGN-UHFFFAOYSA-N 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 229910000365 copper sulfate Inorganic materials 0.000 description 1
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- KTQYJQFGNYHXMB-UHFFFAOYSA-N dichloro(methyl)silicon Chemical compound C[Si](Cl)Cl KTQYJQFGNYHXMB-UHFFFAOYSA-N 0.000 description 1
- FXOCTISBMXDWGP-UHFFFAOYSA-N dichloro(silyl)silane Chemical compound [SiH3][SiH](Cl)Cl FXOCTISBMXDWGP-UHFFFAOYSA-N 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- LIKFHECYJZWXFJ-UHFFFAOYSA-N dimethyldichlorosilane Chemical compound C[Si](C)(Cl)Cl LIKFHECYJZWXFJ-UHFFFAOYSA-N 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 239000010791 domestic waste Substances 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 239000005010 epoxy-amino resin Substances 0.000 description 1
- 238000007667 floating Methods 0.000 description 1
- 238000005188 flotation Methods 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 229910001504 inorganic chloride Inorganic materials 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000005055 methyl trichlorosilane Substances 0.000 description 1
- 239000005048 methyldichlorosilane Substances 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 239000003607 modifier Substances 0.000 description 1
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 1
- 239000002736 nonionic surfactant Substances 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 150000001367 organochlorosilanes Chemical class 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 150000004760 silicates Chemical class 0.000 description 1
- 239000011856 silicon-based particle Substances 0.000 description 1
- 229920002379 silicone rubber Chemical group 0.000 description 1
- CZDYPVPMEAXLPK-UHFFFAOYSA-N tetramethylsilane Chemical compound C[Si](C)(C)C CZDYPVPMEAXLPK-UHFFFAOYSA-N 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 239000005051 trimethylchlorosilane Substances 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic Table
- C07F7/02—Silicon compounds
- C07F7/08—Compounds having one or more C—Si linkages
- C07F7/12—Organo silicon halides
- C07F7/121—Preparation or treatment not provided for in C07F7/14, C07F7/16 or C07F7/20
- C07F7/126—Preparation or treatment not provided for in C07F7/14, C07F7/16 or C07F7/20 by reactions involving the formation of Si-Y linkages, where Y is not a carbon or halogen atom
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/02—Silicon
- C01B33/037—Purification
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic Table
- C07F7/02—Silicon compounds
- C07F7/08—Compounds having one or more C—Si linkages
- C07F7/12—Organo silicon halides
- C07F7/121—Preparation or treatment not provided for in C07F7/14, C07F7/16 or C07F7/20
- C07F7/123—Preparation or treatment not provided for in C07F7/14, C07F7/16 or C07F7/20 by reactions involving the formation of Si-halogen linkages
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic Table
- C07F7/02—Silicon compounds
- C07F7/08—Compounds having one or more C—Si linkages
- C07F7/20—Purification, separation
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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Abstract
本发明主要包括：1.通过选择特殊溶剂萃取，特殊离心重力沉降方法，完全分离出浆渣的液体浆料高沸物并回收利用，消除了液体浆料中安全隐患。2.液体浆渣回收利用方法特殊，包括直接蒸馏低沸点可以直接利用成分，通过溶液中直接转化可利用成分。3.固体渣浆通过特殊水洗、溶解得到的固体物易于过滤分离出得纯净固体单质硅粉含量为95％以上，其可用来用来生产二氧化硅、氧化亚硅、碳化硅、氮化硅等硅类物质。4.固体渣浆通过特殊水洗得到的液体中不含还原性铜、铝、锡、铁、钙、镍等金属元素，而以硫酸盐或者氯化物的形式富集在水溶液中，可以采用离子交换富集，并还原被回收，其中铜的回收率达到90％以上。
Description
技术领域
本发明专利涉及一种有机硅浆渣分离回收利用技术，属于有机硅浆渣综合利用领域。
背景技术
有机硅浆渣是有机硅单体合成过程中所产生的废弃物，其主要由大量的高沸物和少量流化床带出的未反应的硅粉和铜粉组成，如果暴露在空气中，就会燃烧或形成强酸雾或强酸液体，因此如果直接排放会对环境造成严重污染，所以必须进行无公害化处理有机硅合成产物经过旋分分离和精馅分离后的浆渣固含量约为25％左右，其组分主要为硅、铜、锌、碳，还有微量铝、钙以及镣等；液相中的主要组成为(CH3)4Cl2Si2、(CH3)2Cl4Si2、其他沸点较低的单硅烷和Si-O-Si等高沸物，其中，(CH3)4Cl2Si2和(O)2Cl4Si2的量总计约占整个浆渣的50-70％。国内对有机硅浆渣减量化处理及水解均没有成熟的工艺。减量化处理基本采用原始的沉淀分离，有的采用闪蒸槽蒸发分离工艺，但效果均不好，沉淀分离及闪蒸槽蒸发分离回收的高沸物少，且分离后的浆渣中仍然有大量高沸物，使水解***的负荷较大。浆渣水解工艺更是多种多样，各厂一般是根据技术人员的经验进行建设，但仍会存在水解不完全，因剩余高沸物较多及水解控制条件的差异，水解过程中产生的水解胶链物较多，容易出现胶链结死现象，并产生大量的氯化氢气体，易发生安全事故，而且易对环境造成污染，不环保。所以，传统的废渣浆处理方法操作繁杂，并且还不能彻底的处理干净废弃物，还极易造成环境污染等问题；若采用堆积的方法处理，污染严重，且存在安全隐患。而国内在废渣浆处理技术方面还是一个空白，目前只能积压堵库或简单的回收铜，没有从根本上解决环保问题且造成氯的浪费。
US Pat 4 221 691提供了一种处理废渣浆的方法：向渣浆中加入少量的矿物油以改善水解物的处理特性。但该方法的缺点在于：渣浆与水解介质接触不充分，水解的速度比较缓慢，得到的水解物为粘稠状态，难以从体系中分离；另外，该方法要求在渣浆的有机硅单体分子中，每个硅原子上连接的氯基团不少于3个，但是大多数渣浆中的单体不满足它的要求，因此不能使用该方法处理大多数渣浆；而且在水解过程中加入矿物油将增加废料处理费用，并增加了新的污染源，不符合环保要求。
US 4 408 030提供了一种含氯硅烷的多物流的废料处理工艺，包括如下步骤：(A)测定物流的平均SICL官能度；(B)混合至少两种物流以使混合物流的SICL官能度大于或等于2.8； (C)在50℃及水解介质沸点之间，用水解介质混合物流使其水解，并(D)分离水解介质，得到胶粒，该胶粒在后续处理过程中易处理，方便运输和进一步处理操作。其中的水解介质选自水、氯化钙溶液、及浓盐酸溶液。水解温度优选60-90℃。可回收水解过程中产生的HCL。该方法中的胶粒可用水洗，以进一步减少胶粒中的氯含量。若水解溶液最初仅含水，则随着水解的进行，形成盐酸，当水中的盐酸饱和时，氯化氢就解析出来。水解介质中可加入盐酸和无机氯化物使水解溶液达到饱和，这样氯化氢在水解开始阶段就解析出来。水解物通过过滤或离心与液体分离，所得固体水解物颗粒不粘附，易于处理，方便运输和进一步处理操作，水解物还可用水一次或多次冲洗，进一步降低水解物中氯的含量。该方法存在的缺点如下，其一，以水、氯化钙溶液、或浓盐酸溶液作水解介质，水解颗粒细小，不易于从反应釜中采出；其二，水解物表面所吸附的氯根离子浓度达到10％以上，若想降至较低浓度，需要大量水冲洗，废酸液排放量大。
EP 867442A2介绍了一种甲基氯硅烷副产物的水解工艺，该工艺得到至少两相，包括在副产物中加入水介质进行水解，水介质中可含有表面活性剂，PH至少为7左右，温度高于0℃。其中的一相为隋性固体，第二相为水溶液，基本上不含金属，可经处理或不经处理直接排放。可用过滤、沉淀、浮选或离心技术分离固体，及分离水介质以回收盐、硅酸盐或排至废水处理装置。表面活性剂为阴离子或非离子表面活性剂，优选非表面活性剂。该工艺的优点在于：其一，该方法减少了水解液中的重金属浓度，解决了废物处理的难题，水解工艺得到的产品为惰性，高闪点，无气体析出，不粘稠、无尘易流动，易于处理和运输。其二，铜被富集在固体水解物中，可以充分回收。缺点在于：反应产物之一的氯化氢被水解介质中的碱中和成为盐，白白浪费了一部分资源；此外固体水解物中含有的还原性的铜在受热、太阳光长时间照射或堆积的情况下容易发生自燃，是一个重要的安全隐患。
DE4116925 A1介绍了一种甲基氯硅烷副产物的水解工艺，通过对由氯-和/或有机氯硅烷的直接混合物组成的残液进行制备，在温度从20℃升到100℃时(主要是在35℃～60℃间)，与浓度为20％
70％(主要是40％～60％浓度)的硫酸混合，并且与分离出的水解物-氢氧化钙、氧化钙、碳酸钙或其混合物进行中和反应，直到产生一种主要由聚硅氧烷或藻酸组成的浮动固体为止。通过与氢氧化钙、氧化钙、碳酸钙或其混合物混合后，会从原来的湿水解物中产生一种干燥的悬浮固体。这个固体包括最多5％wt的剩余氯化物以及少量的20％wt水，废弃物比重总计0.5
1克/毫升。分离后的液态阶段会再次水解或用于洗涤和干燥那些转化反应物、气态氯化氢。该工艺的主要缺点是把渣浆液相完全水解掉，造成了浪费。
CN106220666 A公开了一种有机硅浆渣的处理***与处理方法，包括有机硅浆渣源、加热蒸发装置以及冷凝回收装置，其中，加热蒸发装置的入口与有机硅浆渣源连接，加热蒸发装置提供低压环境，并对有机硅浆渣进行加热；冷凝回收装置的入口与加热蒸发装置的上端出口连接，对有机硅浆渣加热蒸发出来的气相物料进行冷凝回收。该方法虽然通过减压蒸馏方法可以回收部分高沸点难处理的有机硅浆料，但是由于由于浆渣成分复杂，实际沸点差异比较小，因此根本没有办法解决回收后馏分纯度，因此整体液体浆料回收率比较低。
CN1618840A介绍一种有机硅单体合成过程中的废渣浆的处理方法。该发明通过离心重力沉降分离回收大部分的高沸物，并且对剩余的渣浆水解得到的水解物易采出，且不含还原性铜，消除了安全隐患；渣浆中的铜以硫酸铜的形式富集在水解溶液中，可以通过还原的方法被回收，铜的回收率达到95％以上；固体水解物基本达到环保要求，但是该方法对液体浆料回收率非常低，实际只是解决固体渣料中铜的回收率问题。
CN106170325B发明公开了从反应残余物回收氢卤硅烷的方法。使无机卤硅烷浆料穿过薄膜干燥器以移除卤硅烷并且形成包含硅颗粒的固体残余物，所述无机卤硅烷浆料包含(i)四卤硅烷、三卤硅烷、二卤硅烷、或它们的任何组合在浆料穿过薄膜干燥器时移除重物质。该方法目的实际是减少液体减料与固体渣料粘结性，扩大蒸馏挥发速度，但是由于薄膜蒸发器面积及浆渣对薄膜蒸发器污染影响传热效率限制，因此该发明根本无法满足大规模浆渣处理量的要求。
发明内容
针对现有技术中存在的不足，本发明公开了一种有机硅浆渣的分离处理***和回收技术方法。为了解决以上技术问题，本发明的技术方案为：
1.一种有机硅浆渣的萃取洗涤处理***，包括有机硅浆渣源、特殊溶剂、助溶剂、空气隔绝密闭搅拌釜、离心过滤装置、超滤装置以及滤液回收装置，其中，搅拌釜与有机硅浆渣源、混合溶剂储存釜、离心过滤、超滤装置进出口等采用密闭管道连接，根据浆渣固体含量、粘度，离心过滤罐的要求把浆渣源与混合溶剂按照一定比例混合，导入到离心过滤机里，经过多次萃取过滤，得固体滤渣和液体浆料，并汇聚一临时储液罐，再进行超滤，以彻底除去液体中固体颗粒，得液体供进一步利用，而离心机中固体直接进入固体清洗釜，经过多次清洗过滤得干净固体硅粉和进一步处理的滤液。
优选的，所述分离处理***还包括溶剂与助溶剂混合装置、硅浆渣和溶剂计量装置、粗离心分离装置、次离心分离装置、精离心分离装置、离心浆渣溶剂再萃取溶解搅拌、固体浆渣再水洗、过滤及滤液处理***。
进一步优选的，所述分离处理***中液体浆料与固体浆渣分离、液体浆料的超滤阶段所有物料传输、混合、分离都是在密闭环境中完成，所有装置材料都应该耐腐蚀尤其是氯化氢、特殊溶剂腐蚀。
更进一步优选的，所述浆渣水洗装置中可加热、可添加苯磺酸盐类洗涤增效剂和盐酸或者硫酸，以提高洗涤效果和溶解铜粉，其中温度为25～55℃，溶液酸度控制在PH为1以下，而水洗后的固体硅粉可以在线实现烘干包装。
2.本发明方案中浆渣进行固液分离后，液体浆料与特殊溶剂一起回收采用分级精馏方式进行，其中低沸点单硅烷如四甲基硅烷、三甲基氯硅烷、二甲基二氯硅烷、三氯甲基硅烷等，低沸点全氯二硅烷如三氯二硅烷、四氯二硅烷、五氯二硅烷、六氯二硅烷等沸点确定且与溶剂沸点差异较大均可以直接回收利用，而沸点与溶剂沸点差异较小，根据实际应用，通过通入干燥氨气、烷基胺转化为氨基化产物化，进行分离。对于高沸点化合物超过150C一般为寡聚氯硅烷或者多烷基化预聚物，通过氨基化或者烷氧基直接转化为超支链化物，作为特殊功能材料。
优先的，液体浆料中三氯二硅烷、四氯二硅烷、五氯二硅烷、六氯二硅烷进一步提纯，转化为满足电子级的氮化硅、和单晶硅镀膜材料，二氯二硅烷转化为氮化硅陶瓷前驱体材料，用于生产碳化硅陶瓷材料。
进一步优选的高沸点无法裂解和分离的成分，通过氨基化或者烷氧基直接转化为超支链化物，而该超支链化物可以进一步与丙烯酸、、硅橡胶原料、聚氨酯、环氧树脂或者氨基树脂改性，成为特殊复合材料，用于特殊功能材料中。
更进一步优选的高沸点无法裂解和分离的成分，通过氨基化或者烷氧基直接转化为高分子功能表面活性剂，直接应用于油田化学品或者建筑水泥添加剂和改性剂。
本发明的有益效果：
本发明可以将难处理的有机硅浆渣真正实现变废为宝，通过溶剂稀释萃取方法，避免了常规水解方法水解物难分离、液体成分回收利用率低，固体成分清洗不彻底的，同时通过分级精馏，对每级馏分进行采用不同回收利用方法，催化剂使用效率高，催化裂化转化率高，因此可分别生产各种沸点不同应用和使用价值的氯硅烷、高分子聚合物，使浆渣中有用的液体基本能够实现完全得以回收利用，实现有机硅浆渣的减量化处理，提高浆渣中有用物料的利用效率，降低了浆渣处理费用，从而降低了生产成本。年生产量为40万吨的氯硅烷装置，每年8000吨固体浆渣可回收利用液体成分达可到5000吨，具有较好的经济效益。
本发明的***和方法不但可以对有机硅浆渣进行减量化生产，回收其中的大部分的氯硅烷，对剩余的残渣进行水解中和反应，由于残渣中的氯硅烷已经被回收，所以降低了残渣的水解难度，提高了残渣中的废液的水解程度，并且避免了水解过程中容易胶链结死现象，还会大大减少氯化氢气体的产生；此外，水解产生的清液还可以用于氯化钙的生产或循环回水解中和过程进行反应，减少了废液的排放，提高了有机硅浆渣处理的程度，同时能够实现节能、环保、创收。进行反应，减少了废液的排放，提高了有机硅浆渣处理的程度，同时节能、环保、创收。
具体实施方式
结合实施例对本发明作进一步的说明，下述说明仅是为了解释本发明，并不对其内容进行限定。
实施例1
从浆渣原料缓冲罐中取500公斤浆渣输入到离心过滤器中，通过离心过滤得液体浆料300 公斤及固体滤渣200公斤，再把滤渣用溶剂洗涤过滤，重复多次，汇聚所有滤液1500公斤，然后蒸发溶剂1200公斤，再精馏得可再裂解的有机硅成分A 225公斤和不能够裂解高沸点的成分 B 135公斤；对于固体渣料，用酸溶解洗涤三次得硅粉C 180公斤，铁粉还原回收铜7公斤，回收率为95％。
将225公斤可裂解有机硅A重新注入釜中以三氯化铝、氯化氢、氢气作催化剂，在245度条件下进行裂解，重新得甲基二氯硅烷150公斤，甲基三氯硅烷50公斤，二甲基氯硅烷20公斤。
以上所述仅为本发明的一种实施方式，不是全部或唯一的实施方式，本领域普通技术人员通过阅读本发明说明书而对本发明技术方案采取的任何等效的变换，均为本发明的权利要求所涵盖。
Claims (8)
1.一种有机硅单体合成过程中的废渣浆的分离处理***及利用技术，包括如下步骤：
A有机硅单体合成中的废渣浆经过特殊溶剂多次洗涤，离心重力沉降离心机分离出液体浆料98％以上的混合物，用于精馏、裂解和转化其他用途物质；
B离心后的固体的废渣在特殊水解釜中进行水洗涤，水解介质为PH为1到2的酸性硫酸或者盐酸溶液，并添加了相关洗涤增效剂；少量含有硅氧烷的氯化氢气体从液相中析出；
C水洗物经液固分离，固体烘干回收利用，液相经后续处理回收铜、铁、铝、镍。
2.根据权利要求1中A所述的方法，其特征在于特殊溶剂为氯代烃类或者氟醚类，其中溶剂沸点为40到70℃之间、不易燃而对有机硅单体和低聚物有比较好的溶解性能、低沸点、化学性能稳定、加热不分解的惰性溶剂，溶剂可以长期循化重复使用。
3.根据权利要求1中A所述的方法，其特征溶剂多次洗涤后液体混合经过超滤后无固体杂质，而且溶剂可以不分离而直接与有机硅单体或者预聚物长时间稳定储存存，并一起于精馏、裂解和转化其他用途物质的生产过程。
4.根据权利要求1中A所述的方法，其特征浆渣萃取分离出液体回收利用方法采用精馏方法和直接转化其他物质两方法处理，其中蒸馏出的馏分纯度比较高的成分直接回收，而沸点相差比较小、纯度不高馏分，通过添加其他物质转化不同物质再分离出相关物质；对于氯原子数目小于3个的多氯二硅烷和三硅烷类采用催化裂解转化小分子单体，沸点超过150℃高沸点混合物直接添加其他物质采用转化其他混合物利用。
5.根据权利要求1中A所述的方法，其特征离心重力沉降分离和液体超滤过程分离过程在密闭惰性气体保护下进行分离，以保护液体浆料避免吸收空气水。
6.根据权利要求4中所述的方法，其特征液体浆料成分转化过程采用催化裂解方法时催化剂为氯化铁、氯化铝、氯化氢、氢气、、复合盐MAlX4(M为碱金属Na、K、Li；X为卤素Cl、Br、F等、有机胺及其盐(叔胺、N，N-二甲基苯胺、N，N-二甲基甲酰胺、N，N-二乙基甲酰胺、季胺卤化物和季膦卤化物等)、过渡金属Pd、Pt、Rh、Ru和Ni及其化合物氯化物如K2PdCl4、(R3P)2PdCl2、(R3P)2PtCl2、(R3P)2NiCl2、、(R为1-6个碳原子的烷基和苯基)、(Ph3P)2NiCl2、(Me2PllP)2PdCl2、(Ph3P)4PdCO等、活性炭、分子筛包括天然沸石如菱沸石、发光沸石、八面沸石、斜发沸石、毛沸石以及人工合成沸石ZSM-5、ZSM-1l等，尤以LZ-Y-64、LZ-Y-74、LZ-M-8为佳，并辅以一定量的氢气、氯气或氯化氢为裂解气等其中1种、2种或者多种组合作催化剂；在非催化裂解转化中转化物包括含氮化物和含氧化物、或者自缩合、聚合物成的有机硅高分物质，且这些化物可能为硅基碳化硅、氮化硅前驱体、聚硅氧烷、聚硅氮烷、聚硅烷、及其他丙烯酸、聚氨酯类接枝化物。
7.根据权利要求1中B所述的方法，其特征在于固液分离后滤渣在可以在常温或者加温条件下快速进行水洗，其中可以添加盐酸、或者硫酸、烷基苯磺酸类洗涤增效剂，提高洗涤速度和效果。。
8.根据权利要求1中C所述的方法，其特征在于洗涤后固体单质硅颗粒含量高，无任何危险杂质成分，可以满足普通化学品相关流通要求，纯度可以满足生产二氧化硅、氧化亚硅、碳化硅、氮化硅等产品质量标准要求。
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| TWI831510B (zh) * | 2022-12-09 | 2024-02-01 | 中聯資源股份有限公司 | 富含金屬回收料之回收方法(二) |
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| TWI831510B (zh) * | 2022-12-09 | 2024-02-01 | 中聯資源股份有限公司 | 富含金屬回收料之回收方法(二) |
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