CN115259095A - Method for preparing hydrotalcite-type layered hydroxide by utilizing saline-alkali soil and application - Google Patents
Method for preparing hydrotalcite-type layered hydroxide by utilizing saline-alkali soil and application Download PDFInfo
- Publication number
- CN115259095A CN115259095A CN202210826634.7A CN202210826634A CN115259095A CN 115259095 A CN115259095 A CN 115259095A CN 202210826634 A CN202210826634 A CN 202210826634A CN 115259095 A CN115259095 A CN 115259095A
- Authority
- CN
- China
- Prior art keywords
- hydrotalcite
- acid
- hydroxide
- saline
- solution
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000003513 alkali Substances 0.000 title claims abstract description 66
- 239000002689 soil Substances 0.000 title claims abstract description 46
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 title claims abstract description 40
- 238000000034 method Methods 0.000 title claims abstract description 31
- GDVKFRBCXAPAQJ-UHFFFAOYSA-A dialuminum;hexamagnesium;carbonate;hexadecahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Al+3].[Al+3].[O-]C([O-])=O GDVKFRBCXAPAQJ-UHFFFAOYSA-A 0.000 claims abstract description 58
- 229960001545 hydrotalcite Drugs 0.000 claims abstract description 58
- 229910001701 hydrotalcite Inorganic materials 0.000 claims abstract description 58
- 239000000243 solution Substances 0.000 claims abstract description 58
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims abstract description 42
- 239000007787 solid Substances 0.000 claims abstract description 38
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 33
- 238000006243 chemical reaction Methods 0.000 claims abstract description 24
- 238000010438 heat treatment Methods 0.000 claims abstract description 23
- 239000000047 product Substances 0.000 claims abstract description 22
- 239000001103 potassium chloride Substances 0.000 claims abstract description 21
- 235000011164 potassium chloride Nutrition 0.000 claims abstract description 21
- 239000011780 sodium chloride Substances 0.000 claims abstract description 19
- 238000005406 washing Methods 0.000 claims abstract description 17
- 238000001914 filtration Methods 0.000 claims abstract description 11
- 238000002360 preparation method Methods 0.000 claims abstract description 9
- 239000007788 liquid Substances 0.000 claims abstract description 8
- 239000002253 acid Substances 0.000 claims abstract description 7
- 239000012670 alkaline solution Substances 0.000 claims abstract description 7
- 238000005189 flocculation Methods 0.000 claims abstract description 7
- 230000016615 flocculation Effects 0.000 claims abstract description 7
- 239000000706 filtrate Substances 0.000 claims abstract description 6
- 238000005216 hydrothermal crystallization Methods 0.000 claims abstract description 6
- 238000009830 intercalation Methods 0.000 claims abstract description 5
- 230000002687 intercalation Effects 0.000 claims abstract description 5
- 150000004679 hydroxides Chemical class 0.000 claims abstract description 4
- 230000001276 controlling effect Effects 0.000 claims abstract 2
- 230000001105 regulatory effect Effects 0.000 claims abstract 2
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 36
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 claims description 12
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 12
- 239000008367 deionised water Substances 0.000 claims description 10
- 229910021641 deionized water Inorganic materials 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 10
- 239000003960 organic solvent Substances 0.000 claims description 9
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 9
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 8
- 235000017550 sodium carbonate Nutrition 0.000 claims description 8
- QAIPRVGONGVQAS-DUXPYHPUSA-N trans-caffeic acid Chemical compound OC(=O)\C=C\C1=CC=C(O)C(O)=C1 QAIPRVGONGVQAS-DUXPYHPUSA-N 0.000 claims description 8
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 claims description 8
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 7
- 239000008247 solid mixture Substances 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 6
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 6
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 6
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 6
- CHPZKNULDCNCBW-UHFFFAOYSA-N gallium nitrate Chemical compound [Ga+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O CHPZKNULDCNCBW-UHFFFAOYSA-N 0.000 claims description 6
- 150000007522 mineralic acids Chemical class 0.000 claims description 6
- 239000011259 mixed solution Substances 0.000 claims description 6
- 150000007524 organic acids Chemical class 0.000 claims description 6
- OERNJTNJEZOPIA-UHFFFAOYSA-N zirconium nitrate Chemical compound [Zr+4].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O OERNJTNJEZOPIA-UHFFFAOYSA-N 0.000 claims description 6
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 5
- 239000012760 heat stabilizer Substances 0.000 claims description 5
- 229910021645 metal ion Inorganic materials 0.000 claims description 5
- 229910017604 nitric acid Inorganic materials 0.000 claims description 5
- 239000004014 plasticizer Substances 0.000 claims description 5
- 239000000843 powder Substances 0.000 claims description 5
- ACEAELOMUCBPJP-UHFFFAOYSA-N (E)-3,4,5-trihydroxycinnamic acid Natural products OC(=O)C=CC1=CC(O)=C(O)C(O)=C1 ACEAELOMUCBPJP-UHFFFAOYSA-N 0.000 claims description 4
- XXLFLUJXWKXUGS-UHFFFAOYSA-N 6-methoxyquinoline-4-carboxylic acid Chemical compound N1=CC=C(C(O)=O)C2=CC(OC)=CC=C21 XXLFLUJXWKXUGS-UHFFFAOYSA-N 0.000 claims description 4
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 4
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 4
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 claims description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 4
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims description 4
- RQPZNWPYLFFXCP-UHFFFAOYSA-L barium dihydroxide Chemical compound [OH-].[OH-].[Ba+2] RQPZNWPYLFFXCP-UHFFFAOYSA-L 0.000 claims description 4
- 229910001863 barium hydroxide Inorganic materials 0.000 claims description 4
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 claims description 4
- 229940074360 caffeic acid Drugs 0.000 claims description 4
- 235000004883 caffeic acid Nutrition 0.000 claims description 4
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims description 4
- QAIPRVGONGVQAS-UHFFFAOYSA-N cis-caffeic acid Natural products OC(=O)C=CC1=CC=C(O)C(O)=C1 QAIPRVGONGVQAS-UHFFFAOYSA-N 0.000 claims description 4
- 238000002425 crystallisation Methods 0.000 claims description 4
- 230000008025 crystallization Effects 0.000 claims description 4
- 238000001704 evaporation Methods 0.000 claims description 4
- 230000008020 evaporation Effects 0.000 claims description 4
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 4
- YGSDEFSMJLZEOE-UHFFFAOYSA-N salicylic acid Chemical compound OC(=O)C1=CC=CC=C1O YGSDEFSMJLZEOE-UHFFFAOYSA-N 0.000 claims description 4
- 239000000725 suspension Substances 0.000 claims description 4
- QDZRBIRIPNZRSG-UHFFFAOYSA-N titanium nitrate Chemical compound [O-][N+](=O)O[Ti](O[N+]([O-])=O)(O[N+]([O-])=O)O[N+]([O-])=O QDZRBIRIPNZRSG-UHFFFAOYSA-N 0.000 claims description 4
- 239000001110 calcium chloride Substances 0.000 claims description 3
- 229910001628 calcium chloride Inorganic materials 0.000 claims description 3
- 239000000920 calcium hydroxide Substances 0.000 claims description 3
- 229910001861 calcium hydroxide Inorganic materials 0.000 claims description 3
- 235000011116 calcium hydroxide Nutrition 0.000 claims description 3
- 239000006185 dispersion Substances 0.000 claims description 3
- 230000003311 flocculating effect Effects 0.000 claims description 3
- 229940044658 gallium nitrate Drugs 0.000 claims description 3
- 229920006395 saturated elastomer Polymers 0.000 claims description 3
- BJEPYKJPYRNKOW-REOHCLBHSA-N (S)-malic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O BJEPYKJPYRNKOW-REOHCLBHSA-N 0.000 claims description 2
- MIJYXULNPSFWEK-GTOFXWBISA-N 3beta-hydroxyolean-12-en-28-oic acid Chemical compound C1C[C@H](O)C(C)(C)[C@@H]2CC[C@@]3(C)[C@]4(C)CC[C@@]5(C(O)=O)CCC(C)(C)C[C@H]5C4=CC[C@@H]3[C@]21C MIJYXULNPSFWEK-GTOFXWBISA-N 0.000 claims description 2
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 2
- 239000005711 Benzoic acid Substances 0.000 claims description 2
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 claims description 2
- JKLISIRFYWXLQG-UHFFFAOYSA-N Epioleonolsaeure Natural products C1CC(O)C(C)(C)C2CCC3(C)C4(C)CCC5(C(O)=O)CCC(C)(C)CC5C4CCC3C21C JKLISIRFYWXLQG-UHFFFAOYSA-N 0.000 claims description 2
- YBRJHZPWOMJYKQ-UHFFFAOYSA-N Oleanolic acid Natural products CC1(C)CC2C3=CCC4C5(C)CCC(O)C(C)(C)C5CCC4(C)C3(C)CCC2(C1)C(=O)O YBRJHZPWOMJYKQ-UHFFFAOYSA-N 0.000 claims description 2
- MIJYXULNPSFWEK-UHFFFAOYSA-N Oleanolinsaeure Natural products C1CC(O)C(C)(C)C2CCC3(C)C4(C)CCC5(C(O)=O)CCC(C)(C)CC5C4=CCC3C21C MIJYXULNPSFWEK-UHFFFAOYSA-N 0.000 claims description 2
- KDYFGRWQOYBRFD-UHFFFAOYSA-N Succinic acid Natural products OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 claims description 2
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 claims description 2
- 235000011054 acetic acid Nutrition 0.000 claims description 2
- 239000003463 adsorbent Substances 0.000 claims description 2
- BJEPYKJPYRNKOW-UHFFFAOYSA-N alpha-hydroxysuccinic acid Natural products OC(=O)C(O)CC(O)=O BJEPYKJPYRNKOW-UHFFFAOYSA-N 0.000 claims description 2
- ILRRQNADMUWWFW-UHFFFAOYSA-K aluminium phosphate Chemical compound O1[Al]2OP1(=O)O2 ILRRQNADMUWWFW-UHFFFAOYSA-K 0.000 claims description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 2
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 claims description 2
- 239000011668 ascorbic acid Substances 0.000 claims description 2
- 235000010323 ascorbic acid Nutrition 0.000 claims description 2
- 229960005070 ascorbic acid Drugs 0.000 claims description 2
- 235000010233 benzoic acid Nutrition 0.000 claims description 2
- 229960004365 benzoic acid Drugs 0.000 claims description 2
- KDYFGRWQOYBRFD-NUQCWPJISA-N butanedioic acid Chemical compound O[14C](=O)CC[14C](O)=O KDYFGRWQOYBRFD-NUQCWPJISA-N 0.000 claims description 2
- 239000003054 catalyst Substances 0.000 claims description 2
- 235000015165 citric acid Nutrition 0.000 claims description 2
- 239000000084 colloidal system Substances 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- 235000019253 formic acid Nutrition 0.000 claims description 2
- 229910000154 gallium phosphate Inorganic materials 0.000 claims description 2
- 229910000373 gallium sulfate Inorganic materials 0.000 claims description 2
- UPWPDUACHOATKO-UHFFFAOYSA-K gallium trichloride Chemical compound Cl[Ga](Cl)Cl UPWPDUACHOATKO-UHFFFAOYSA-K 0.000 claims description 2
- LWFNJDOYCSNXDO-UHFFFAOYSA-K gallium;phosphate Chemical compound [Ga+3].[O-]P([O-])([O-])=O LWFNJDOYCSNXDO-UHFFFAOYSA-K 0.000 claims description 2
- SBDRYJMIQMDXRH-UHFFFAOYSA-N gallium;sulfuric acid Chemical compound [Ga].OS(O)(=O)=O SBDRYJMIQMDXRH-UHFFFAOYSA-N 0.000 claims description 2
- 239000001630 malic acid Substances 0.000 claims description 2
- 235000011090 malic acid Nutrition 0.000 claims description 2
- 238000001728 nano-filtration Methods 0.000 claims description 2
- 229940100243 oleanolic acid Drugs 0.000 claims description 2
- 235000006408 oxalic acid Nutrition 0.000 claims description 2
- DCKVFVYPWDKYDN-UHFFFAOYSA-L oxygen(2-);titanium(4+);sulfate Chemical compound [O-2].[Ti+4].[O-]S([O-])(=O)=O DCKVFVYPWDKYDN-UHFFFAOYSA-L 0.000 claims description 2
- FJKROLUGYXJWQN-UHFFFAOYSA-N papa-hydroxy-benzoic acid Natural products OC(=O)C1=CC=C(O)C=C1 FJKROLUGYXJWQN-UHFFFAOYSA-N 0.000 claims description 2
- HZLWUYJLOIAQFC-UHFFFAOYSA-N prosapogenin PS-A Natural products C12CC(C)(C)CCC2(C(O)=O)CCC(C2(CCC3C4(C)C)C)(C)C1=CCC2C3(C)CCC4OC1OCC(O)C(O)C1O HZLWUYJLOIAQFC-UHFFFAOYSA-N 0.000 claims description 2
- 238000001223 reverse osmosis Methods 0.000 claims description 2
- 229960004889 salicylic acid Drugs 0.000 claims description 2
- 239000011975 tartaric acid Substances 0.000 claims description 2
- 235000002906 tartaric acid Nutrition 0.000 claims description 2
- 229910000348 titanium sulfate Inorganic materials 0.000 claims description 2
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 claims description 2
- JUWGUJSXVOBPHP-UHFFFAOYSA-B titanium(4+);tetraphosphate Chemical compound [Ti+4].[Ti+4].[Ti+4].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O JUWGUJSXVOBPHP-UHFFFAOYSA-B 0.000 claims description 2
- 238000000108 ultra-filtration Methods 0.000 claims description 2
- 229910000166 zirconium phosphate Inorganic materials 0.000 claims description 2
- DUNKXUFBGCUVQW-UHFFFAOYSA-J zirconium tetrachloride Chemical compound Cl[Zr](Cl)(Cl)Cl DUNKXUFBGCUVQW-UHFFFAOYSA-J 0.000 claims description 2
- ZXAUZSQITFJWPS-UHFFFAOYSA-J zirconium(4+);disulfate Chemical compound [Zr+4].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O ZXAUZSQITFJWPS-UHFFFAOYSA-J 0.000 claims description 2
- LEHFSLREWWMLPU-UHFFFAOYSA-B zirconium(4+);tetraphosphate Chemical compound [Zr+4].[Zr+4].[Zr+4].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O LEHFSLREWWMLPU-UHFFFAOYSA-B 0.000 claims description 2
- 238000000926 separation method Methods 0.000 abstract description 13
- 230000004888 barrier function Effects 0.000 abstract description 5
- 239000000654 additive Substances 0.000 abstract description 2
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- 150000001768 cations Chemical class 0.000 abstract 1
- 230000001502 supplementing effect Effects 0.000 abstract 1
- 235000002639 sodium chloride Nutrition 0.000 description 27
- 239000000463 material Substances 0.000 description 16
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 15
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- 238000012360 testing method Methods 0.000 description 9
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- IEECXTSVVFWGSE-UHFFFAOYSA-M iron(3+);oxygen(2-);hydroxide Chemical compound [OH-].[O-2].[Fe+3] IEECXTSVVFWGSE-UHFFFAOYSA-M 0.000 description 8
- BJQHLKABXJIVAM-UHFFFAOYSA-N bis(2-ethylhexyl) phthalate Chemical group CCCCC(CC)COC(=O)C1=CC=CC=C1C(=O)OCC(CC)CCCC BJQHLKABXJIVAM-UHFFFAOYSA-N 0.000 description 7
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- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
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- 238000002441 X-ray diffraction Methods 0.000 description 1
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- 238000006555 catalytic reaction Methods 0.000 description 1
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- 238000011978 dissolution method Methods 0.000 description 1
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- 150000002500 ions Chemical class 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
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- 229910000021 magnesium carbonate Inorganic materials 0.000 description 1
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- 239000002105 nanoparticle Substances 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000000618 nitrogen fertilizer Substances 0.000 description 1
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 1
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 1
- 239000003895 organic fertilizer Substances 0.000 description 1
- 239000002686 phosphate fertilizer Substances 0.000 description 1
- 229910001414 potassium ion Inorganic materials 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000000750 progressive effect Effects 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 235000017557 sodium bicarbonate Nutrition 0.000 description 1
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 1
- 229910001415 sodium ion Inorganic materials 0.000 description 1
- 239000002881 soil fertilizer Substances 0.000 description 1
- 239000012265 solid product Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000008117 stearic acid Substances 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
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- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B13/00—Oxygen; Ozone; Oxides or hydroxides in general
- C01B13/14—Methods for preparing oxides or hydroxides in general
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F11/00—Compounds of calcium, strontium, or barium
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/78—Compounds containing aluminium and two or more other elements, with the exception of oxygen and hydrogen
- C01F7/784—Layered double hydroxide, e.g. comprising nitrate, sulfate or carbonate ions as intercalating anions
- C01F7/785—Hydrotalcite
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- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
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Abstract
The invention discloses a method for preparing hydrotalcite type layered hydroxide by utilizing saline-alkali soil and application thereof, wherein the method comprises the steps of adding acid into the saline-alkali soil, heating for dissolving, filtering and washing to obtain a solution for later use; then adjusting the pH value with an alkaline solution, heating for flocculation, filtering, supplementing a certain amount of trivalent metal cations into the filtrate, and regulating and controlling the intercalation elements; then reacting with an alkaline solution, and centrifuging after the reaction is finished to obtain a solid and a clear liquid; and dispersing and centrifugally washing the obtained solid, then carrying out hydrothermal crystallization, and carrying out centrifugal separation to obtain hydrotalcite-like layered hydroxides with various intercalation structures and functions. The hydrotalcite type layered hydroxide prepared by the invention is used for preparing plasticized products such as PVC products and the like, is used as an additive, improves the performances such as mechanics and gas barrier and the like, and simultaneously obtains sodium chloride and potassium chloride byproducts. The preparation process is simple, is suitable for industrial application, and realizes the full and effective utilization of saline-alkali soil.
Description
Technical Field
The invention relates to the technical field of material preparation, in particular to a method for preparing hydrotalcite-type layered hydroxide by utilizing saline-alkali soil and application of the prepared hydrotalcite.
Background
At present, the treatment method for saline-alkali soil mainly comprises a solar salt treatment method and a water washing salt pressing method, but salt impurities obtained through solar salt treatment are many, the utilization value is low, a large amount of manpower and material resources are wasted, the water washing salt pressing method is easy to repeat, saline and alkali cannot be radically treated, and the application range of the method is severely limited.
Hydrotalcite materials are short for Layered Double Hydroxides (LDHs), and are anionic clays comprising Hydrotalcite (Hydrotalcite) materials and Hydrotalcite-like (Hydrotalcite-like) materials. The LDHs material generally consists of a host laminate and an interlayer guest, wherein the host laminate consists of binary or multi-element metal hydroxide, generally hydroxide of divalent or trivalent metal ions is formed by covalent bonds, and the laminate is positively charged; the LDHs laminates are arranged between the anions, and negative charges carried by the anions are balanced with positive charges carried by the laminates through electrostatic force and are orderly arranged, so that an electrically neutral LDH two-dimensional crystalline structure is formed.
The LDHs material has the most remarkable characteristic that a main body layer plate metal element and interlayer anions can be adjusted in a large range, so that a large class of LDHs materials with different compositions and properties can be formed; meanwhile, the LDHs material also has excellent properties such as memory effect, acid-base duality, thermal stability and the like. The LDHs material has the characteristics of adjustable chemical composition of a host laminate, adjustable charge density and distribution of the laminate, adjustable types and quantity of anions of an interlayer guest, adjustable elastic space in a layer, adjustable grain size distribution and mesoscopic appearance, adjustable interaction between the host and the guest and the like, has been rapidly and deeply developed in the fields of catalysis, medicine, photochemistry, electrochemistry, magnetic materials, selective adsorption and the like due to the particularity of the composition and the structure of the LDHs material, and in recent years, the LDHs material arouses high attention and wide interest of researchers in the fields of supermolecular structural materials and functional materials in China and China.
Therefore, how to provide a method for preparing hydrotalcite-type layered hydroxide by using saline-alkali soil is a problem that needs to be solved urgently by those skilled in the art.
Disclosure of Invention
In view of the above, the invention provides a method for preparing hydrotalcite-type layered hydroxide by using saline-alkali soil, the method adopts the saline-alkali soil as a main raw material to synthesize the hydrotalcite, the process is simple, the popularization is easy, the effective utilization of the saline-alkali soil is realized, and the significance of promoting the treatment and the effective utilization of the saline-alkali soil is realized.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for preparing hydrotalcite type layered hydroxide by utilizing saline-alkali soil comprises the following steps:
(1) Pretreating saline-alkali soil: adding acid into saline-alkali soil, heating for dissolving, dissolving out inorganic salt ions, removing carbonate ions, filtering, and washing to obtain a solution for later use;
(2) Adjusting the pH value of the solution obtained in the step (1) to 3-5 by using an alkaline solution, heating, flocculating, filtering, obtaining a ferric hydroxide by-product from a solid, and adding a certain amount of metal ions into the filtrate;
(3) Preparing an alkali solution, mixing the alkali solution and the solution finally obtained in the step (2) under ultrasonic stirring for reaction, and performing centrifugal operation after the reaction is finished to obtain a solid and a clear solution;
(4) And (4) dispersing the solid obtained in the step (3) in water, centrifugally washing for 3-5 times, dispersing the solid in deionized water, adding the dispersed solid into a hydrothermal kettle, putting the kettle into a heater for hydrothermal crystallization, and centrifugally separating after crystallization reaction is finished to obtain the hydrotalcite-type layered hydroxide.
The beneficial effects of the above technical scheme are: the method has the advantages that the salt and alkali are extracted by an acid dissolution method, the separation of iron ions is realized by utilizing different precipitation equilibrium constants, the hydrotalcite product widely applied in industry is prepared by a hydrothermal method, and finally, sodium ions and potassium ions in the waste liquid are extracted and separated to prepare potassium chloride and sodium chloride products.
Preferably, in the above method for preparing hydrotalcite-type layered hydroxide using saline-alkali soil, in the step (1), 1 to 60 vol% of an inorganic acid or an organic acid is added to the saline-alkali soil, and the mixture is heated at 25 to 105 ℃ for 1 to 48 hours to dissolve the inorganic acid or the organic acid; (ii) a The inorganic acid is selected from nitric acid, phosphoric acid or sulfuric acid; the organic acid is selected from citric acid, malic acid, tartaric acid, acetic acid, succinic acid, oxalic acid, corrosive acid, formic acid, pyroligneous acid, ascorbic acid, benzoic acid, salicylic acid, caffeic acid, quininic acid, caffeic acid or oleanolic acid.
The beneficial effects of the above technical scheme are: the inorganic acid can remove carbonate ions in the saline-alkali soil, the content of nitrogen fertilizer or phosphate fertilizer in the soil is increased, the organic acid can increase the fertilizer efficiency of organic fertilizer in the soil, the nitric acid is used for dissolving the saline-alkali soil compared with other acid solutions, a hydrotalcite product with a better crystal form can be obtained, and the preparation process is simpler and easier.
Preferably, the temperature of the heating flocculation in the step (2) is 60-210 ℃, the stirring speed is 0.1-1000rpm, and the time is 0.1-48h, and the alkaline solution is selected from: potassium hydroxide, sodium hydroxide, lithium hydroxide, barium hydroxide, calcium hydroxide, sodium carbonate, sodium bicarbonate and ammonia water. More preferably, the alkaline solution is selected from ammonia water, and can improve the nitrogen content in soil and the soil fertilizer efficiency. The metal ion is selected from aluminum chloride, aluminum nitrate, aluminum sulfate, aluminum phosphate, titanium chloride, titanium sulfate, titanium nitrate, titanium phosphate, zirconium nitrate, zirconium chloride, zirconium sulfate, zirconium phosphate, calcium chloride, zinc nitrate, gallium chloride, gallium sulfate, gallium nitrate or gallium phosphate.
The beneficial effects of the above technical scheme are: if the temperature and time of heating flocculation are lower than the set values, hydrotalcite-type layered hydroxide cannot be prepared, and if the temperature and time of heating flocculation are higher than the set values, the crystal form of the prepared hydrotalcite product is poor, and the product quality is poor.
Preferably, the alkali solution in step (3) is selected from: the volume ratio of 2:1 is mixed solution of sodium hydroxide and sodium carbonate or 1mol/L sodium carbonate, sodium bicarbonate, ammonia water solution or 0.1mol/L solution of sodium hydroxide, potassium hydroxide, lithium hydroxide, barium hydroxide and calcium hydroxide; and (3) carrying out mixing reaction on the alkali solution and the solution finally obtained in the step (2) according to the volume ratio of 4:1 under ultrasonic stirring.
The beneficial effects of the above technical scheme are: and adding sodium carbonate to prepare the carbonate intercalated hydrotalcite.
Preferably, the clear liquid obtained in the step (3) is subjected to ultrafiltration and nanofiltration reverse osmosis or reduced pressure concentration or solar evaporation and saturated crystallization to obtain thick colloid, sodium chloride products are obtained by filtration, and the filtered liquid is concentrated or separated out by solar evaporation to obtain potassium chloride products.
Further, the clear liquid is crystallized under the reduced pressure of 0.05Mpa at room temperature, and is filtered when the solid-to-liquid ratio of the concentrated saturated crystals is 1, so as to obtain sodium chloride crystals and a potassium chloride solution, and the potassium chloride solution is concentrated to obtain a potassium chloride solid product.
The beneficial effects of the above technical scheme are: the invention realizes the productization of saline-alkali by preparing potassium chloride and sodium chloride products through the solubility difference, and has important theoretical and practical significance.
Preferably, in the step (4), the temperature of the hydrothermal kettle is set to be 90-200 ℃, the hydrothermal crystallization time is 6-64h, and the heating mode of the heater comprises the following steps: electrical heating, microwave and infrared heating.
The beneficial effects of the above technical scheme are: if the crystal form of the hydrotalcite-like layered hydroxide is lower than the set value, the hydrotalcite-like layered hydroxide cannot be prepared, and if the crystal form of the hydrotalcite-like layered hydroxide is higher than the set value, the crystal form of the prepared hydrotalcite product is poor, and the product quality is poor.
Preferably, in the above method for preparing hydrotalcite-type layered hydroxide using saline-alkali soil, the step (4) centrifuges the solid before washing at a rotation speed of 100 to 500000rpm for 1 to 360min.
The beneficial effects of the above technical scheme are: the growth of hydrotalcite in the hydrothermal process is controlled by separating out salt ions in the solution, hydrotalcite with nano particle size can be obtained, and incomplete separation is easy to occur if the rotating speed is low and the time is short, so that the loss of materials is caused.
The invention also discloses application of the hydrotalcite-like layered hydroxide obtained by the preparation method, and the hydrotalcite-like layered hydroxide is used for preparing plastic products or adsorbents or catalysts.
Preferably, the hydrotalcite layered hydroxide is used for preparing a heat stabilizer of a PVC product as an additive to improve mechanical and gas barrier properties, and the preparation method of the PVC product comprises the following steps:
(5) Adding hydrotalcite type layered hydroxide into an organic solvent, centrifuging, dispersing and washing for 3-5 times;
(6) After washing, adding an organic solvent for dispersion, and then adding PVC powder to obtain a uniform suspension;
(7) Carrying out centrifugal separation on the suspension to obtain a solid hydrotalcite and PVC solid mixture, and drying to obtain a uniform solid hydrotalcite and PVC solid mixture;
(8) And (4) adding a plasticizer into the solid hydrotalcite and PVC solid mixture obtained in the step (3) to obtain a PVC product.
Further, the organic solvent is ethanol or acetone or methanol, the organic solvent is added in the step (1) to wash excessive moisture in the hydrotalcite, and the organic solvent is added in the step (2) to disperse the hydrotalcite, so that high dispersion of the hydrotalcite and the PVC powder is realized.
Further, the ratio of the PCV powder to the organic solvent is 1:5-20, preferably 1.
Preferably, in the above application of the hydrotalcite-like layered hydroxide, the hydrotalcite accounts for 3 to 20% by mass of the total substance, and further the hydrotalcite accounts for 6 to 9% by mass of the total substance.
The beneficial effects of the above technical scheme are: if the mass percentage of the hydrotalcite in the total substance is higher or lower than a set value, the thermal stability of the hydrotalcite is poor, and if the adding amount of the hydrotalcite is too much, the material waste is caused.
Preferably, in the application of the hydrotalcite-type layered hydroxide, the mass ratio of the PVC compound, the plasticizer and the solid hydrotalcite is 1.
The beneficial effects of the above technical scheme are: if the set value is higher or lower than the above ratio, the hydrotalcite may have poor thermal stability.
Preferably, in the above use of one of the hydrotalcite-type layered hydroxides, the steps (1) and (2) are carried out under ultrasound-assisted stirring conditions.
Preferably, in the above application of one hydrotalcite-type layered hydroxide, the plasticizer is dioctyl phthalate.
The saline-alkali soil in Xinjiang mainly contains sodium chloride, sodium carbonate, sodium bicarbonate, calcium carbonate, magnesium carbonate, ferric hydroxide and the like, and the saline-alkali soil in Xinjiang is wide and high in calcium and magnesium content. According to the technical scheme, compared with the prior art, the invention discloses a method for preparing hydrotalcite-type layered hydroxide by utilizing saline-alkali soil, which achieves the following technical effects:
(1) According to the invention, alkali liquor is extracted from Xinjiang saline-alkali soil, iron ions are obtained by extraction, then MgCaAl hydrotalcite products are prepared by a hydrothermal method, and rock salt (sodium chloride and potassium chloride products) is prepared by using the residual alkali liquor, so that the saline-alkali soil is fully and effectively utilized;
(2) The invention avoids the repeated use of saline-alkali while utilizing the saline-alkali soil, and can fundamentally treat the saline-alkali while popularizing the technology for preparing hydrotalcite by using the saline-alkali soil;
(3) The preparation method is simple in preparation process, easy to popularize and obvious in economic value.
Drawings
FIG. 1 is an XRD pattern of hydrotalcite prepared with different elements added from salt and alkali prepared according to the present invention 1-3 and comparative examples 1-2;
FIG. 2 is an infrared image of hydrotalcites prepared from salts and alkalis with different elements added according to the present invention 1-3 and comparative examples 1-2; wherein a-e are respectively: example 3, example 2, example 1, comparative example 2.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention.
The embodiment of the invention discloses a method for preparing hydrotalcite type layered hydroxide, which adopts saline-alkali soil as a main raw material to synthesize hydrotalcite, has simple process and easy popularization, and realizes the effective utilization of the saline-alkali soil.
Example 1
(1) Dissolving 500g of saline-alkali soil in 10% nitric acid at 100 ℃, and filtering to obtain a solution for later use;
(2) Adjusting pH to 3 with 15% ammonia water solution to obtain brick red ferric hydroxide precipitate, heating at 100 deg.C for flocculation for 10 hr, centrifuging to remove brick red solid ferric hydroxide to obtain filtrate, and adding 2g aluminum nitrate;
(3) Preparing 400ml of mixed solution of sodium hydroxide and sodium carbonate, carrying out ultrasonic high-speed stirring mixing reaction with 100ml of reaction solution obtained in the step (2), carrying out centrifugal separation after the reaction is finished to obtain a solid, adding 500ml of deionized water, washing and dispersing, carrying out centrifugal separation on the obtained colloidal solution, and repeating for 5 times; finally, the cleaned solid is dispersed in 400ml of deionized water, placed in a hydrothermal kettle, electrically heated and crystallized for 24 hours at 120 ℃, and centrifugally separated after the reaction is finished, so that the hydrotalcite-type layered hydroxide is obtained.
(4) And (3) carrying out centrifugal separation on the reaction mixed solution obtained in the step (2) to obtain a solution, carrying out reduced pressure concentration to obtain a concentrated solution, separating to obtain solid sodium chloride and a potassium chloride solution through the solubility difference of potassium chloride and sodium chloride, and removing moisture from the potassium chloride solution to obtain solid potassium chloride.
(5) Adding the obtained hydrotalcite into a methanol solution, wherein the volume ratio of the hydrotalcite to methanol is 1.
(6) Adding dioctyl phthalate into the mixture of hydrotalcite and PVC solid, wherein the mass ratio of PVC to DOP is 1:1, and heating and plasticizing at 185 ℃ for 5 minutes to prepare a PVC sample.
And (3) putting the prepared PVC sample into a heat aging oven at 180 ℃ for static heat aging experiment, taking the PVC sample once every 10min, and testing the whiteness of the PVC test piece according to GB/T2913-1982 standard, wherein the PVC test piece containing the saline-alkali hydrotalcite heat stabilizer can be kept for 320 min without aging. Compared with PVC without the saline alkali talcum, the mechanical property is improved by 18.1 percent, and the gas barrier property is improved by 6.3 percent.
From XRD of fig. 1, characteristic peaks of hydrotalcite 003, 006, 009, 110 appear, indicating successful preparation of hydrotalcite functional material from saline-alkali soil.
Example 2
Example 1 was repeated except that "2g of aluminum nitrate" in the step (2) in example 1 was replaced with "0.6g of zinc nitrate".
Example 3
Example 1 was repeated except that "2g of aluminum nitrate" in the step (2) in example 1 was replaced with "0.6g of anhydrous calcium chloride".
Comparative example 1
Example 1 was repeated except that "0.6g of aluminum nitrate" in the step (2) in example 1 was replaced with "0.6g of stearic acid".
Comparative example 2
The "addition of a certain amount of 0.6g of aluminum nitrate" in the step (2) in example 1 was deleted; the rest is the same as example 1.
As can be seen from fig. 1 and fig. 2, the hydrotalcite prepared by salt and alkali can be used to construct hydrotalcite with various structures and applications by intercalation method, and construct novel functional materials.
Example 4
(1) Dissolving 500g of saline-alkali soil with 8% hydrochloric acid at 100 ℃, and filtering to obtain a solution for later use;
(2) Adjusting pH to 3 with 10% sodium hydroxide solution to obtain red ferric hydroxide precipitate, heating at 100 deg.C for flocculation for 24 hr, centrifuging to remove brick red solid ferric hydroxide to obtain filtrate, and adding a certain amount of 1.5g calcium chloride and 0.2g zirconium nitrate;
(3) Preparing 400ml of 0.001mol/L sodium hydroxide solution, carrying out ultrasonic high-speed stirring mixing reaction with 100ml of the reaction solution obtained in the step (2), carrying out centrifugal separation after the reaction is finished to obtain a solid, adding 500ml of deionized water, washing and dispersing, carrying out centrifugal separation on the obtained colloidal solution, and repeating for 5 times; and finally, dispersing the cleaned solid into 400ml of deionized water, placing the deionized water into a hydrothermal kettle, electrically heating and crystallizing the mixture at the temperature of 110 ℃ for 20 hours, and carrying out centrifugal separation after the reaction is finished to obtain the hydrotalcite-type layered hydroxide.
And (3) centrifugally separating the reaction mixed solution obtained in the step (2) to obtain a solution, carrying out reduced pressure concentration to obtain a concentrated solution, separating to obtain solid sodium chloride and a potassium chloride solution through the solubility difference of potassium chloride and sodium chloride, and removing moisture from the potassium chloride solution to obtain solid potassium chloride.
(4) Adding the obtained hydrotalcite into an acetone solution, wherein the volume ratio of the hydrotalcite to acetone is 1.
(5) Adding dioctyl phthalate into the mixture of hydrotalcite and PVC solid, wherein the mass ratio of PVC to DOP is 1:1, and heating and plasticizing at 185 ℃ for 5 minutes to prepare a PVC sample.
And (3) putting the prepared PVC sample into a heat aging oven at 180 ℃ for static heat aging experiment, taking the PVC sample once every 10min, and testing the whiteness of the PVC test piece according to GB/T2913-1982 standard, wherein the PVC test piece containing the saline-alkali hydrotalcite heat stabilizer can be kept for 300 min without aging. Compared with PVC without the saline alkali talcum, the mechanical property is improved by 16.5 percent, and the gas barrier property is improved by 5.7 percent.
Example 5
(1) Dissolving 500g of saline-alkali soil in 10% nitric acid at 100 ℃, and filtering to obtain a solution for later use;
(2) Firstly, adjusting the pH value of the solution to 2 by using a 20% NaOH solution, then adjusting the pH value to 3 by using a 5% NaOH solution, heating and flocculating for 6 hours at 80 ℃ to obtain brick red ferric hydroxide precipitate, centrifugally separating to remove brick red solid ferric hydroxide to obtain filtrate, and adding a certain amount of 2g of zinc nitrate and 0.1g of gallium nitrate;
(3) Preparing 400ml of 0.1mol/L sodium hydroxide solution, carrying out ultrasonic high-speed stirring mixing reaction with 100ml of the reaction solution obtained in the step (2), carrying out centrifugal separation after the reaction is finished to obtain a solid, adding 500ml of deionized water, washing and dispersing, carrying out centrifugal separation on the obtained colloidal solution, and repeating for 5 times; and finally, dispersing the cleaned solid into 400ml of deionized water, placing the deionized water into a hydrothermal kettle, carrying out microwave hydrothermal crystallization at 120 ℃ for 12 hours, and carrying out centrifugal separation after the reaction is finished to obtain the hydrotalcite-type layered hydroxide.
And (3) centrifugally separating the reaction mixed solution obtained in the step (2) to obtain a solution, carrying out reduced pressure concentration to obtain a concentrated solution, separating to obtain solid sodium chloride and a potassium chloride solution through the solubility difference of potassium chloride and sodium chloride, and removing moisture from the potassium chloride solution to obtain solid potassium chloride.
(4) Adding the obtained hydrotalcite into a methanol solution, wherein the volume ratio of the hydrotalcite to methanol is 1.
(5) Adding dioctyl phthalate into the solid mixture of hydrotalcite and PVC, wherein the mass ratio of PVC to DOP is 1:1, and heating and plasticizing at 185 ℃ for 5 minutes to prepare a PVC sample.
And (3) putting the prepared PVC sample into a heat aging oven at 180 ℃ for static heat aging experiment, taking the PVC sample once every 10min, and testing the whiteness of the PVC test piece according to GB/T2913-1982 standard, wherein the PVC test piece containing the saline-alkali hydrotalcite heat stabilizer can be kept for 320 min without aging. Compared with PVC without the saline alkali talcum, the mechanical property is improved by 18.1 percent, and the gas barrier property is improved by 6.3 percent.
In the present specification, the embodiments are described in a progressive manner, each embodiment focuses on differences from other embodiments, and the same and similar parts among the embodiments are referred to each other. The device disclosed by the embodiment corresponds to the method disclosed by the embodiment, so that the description is simple, and the relevant points can be referred to the method part for description.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (10)
1. A method for preparing hydrotalcite-type layered hydroxide by utilizing saline-alkali soil is characterized by comprising the following steps:
(1) Pretreating saline-alkali soil: adding acid into saline-alkali soil, heating for dissolving, filtering and washing to obtain a solution for later use;
(2) Adjusting the pH value of the solution obtained in the step (1) to 3-5 by using an alkaline solution, heating, flocculating, filtering, adding a certain amount of metal ions into the filtrate, and regulating and controlling the intercalation elements;
(3) Preparing a certain amount of alkali solution, mixing the alkali solution with the solution finally obtained in the step (2) under ultrasonic stirring for reaction, and performing centrifugal operation after the reaction is finished to obtain a solid and a clear liquid;
(4) And (4) dispersing the solid obtained in the step (3) in water, centrifugally washing for 3-5 times, dispersing the solid in deionized water, adding the dispersed solid into a hydrothermal kettle, putting the kettle into a heater for hydrothermal crystallization, and centrifugally separating after crystallization reaction is finished to obtain hydrotalcite-type layered hydroxides with various intercalation structures and functions.
2. The method for preparing hydrotalcite-type layered hydroxide using saline-alkali soil according to claim 1, wherein in the step (1), inorganic acid or organic acid with a volume concentration of 1-60% is added to the saline-alkali soil, and the mixture is heated at 25-105 ℃ for 1-48 hours to dissolve the mixture; the inorganic acid is selected from nitric acid, phosphoric acid or sulfuric acid; the organic acid is selected from citric acid, malic acid, tartaric acid, acetic acid, succinic acid, oxalic acid, corrosive acid, formic acid, pyroligneous acid, ascorbic acid, benzoic acid, salicylic acid, caffeic acid, quininic acid, caffeic acid or oleanolic acid.
3. The method for preparing hydrotalcite-type layered hydroxide using saline-alkali soil according to claim 1, wherein the temperature of the heating flocculation in step (2) is 60-210 ℃, the stirring speed is 0.1-1000rpm, and the time is 0.1-48h, and the alkaline solution is selected from: potassium hydroxide, sodium hydroxide, lithium hydroxide, barium hydroxide, calcium hydroxide, sodium carbonate, sodium bicarbonate, and ammonia water; the metal ion is selected from aluminum chloride, aluminum nitrate, aluminum sulfate, aluminum phosphate, titanium chloride, titanium sulfate, titanium nitrate, titanium phosphate, zirconium nitrate, zirconium chloride, zirconium sulfate, zirconium phosphate, calcium chloride, zinc nitrate, gallium chloride, gallium sulfate, gallium nitrate or gallium phosphate.
4. The method for preparing hydrotalcite-like layered hydroxide using saline-alkali soil according to claim 1, wherein the alkali solution in step (3) is selected from: the volume ratio is 2:1, the mixed solution of sodium hydroxide and sodium carbonate or 0.1-1mol/L sodium carbonate, sodium bicarbonate, ammonia water solution or 0.1-1mol/L sodium hydroxide, potassium hydroxide, lithium hydroxide, barium hydroxide, calcium hydroxide solution; and (3) carrying out mixing reaction on the alkali solution and the solution finally obtained in the step (2) according to the volume ratio of 4:1 under ultrasonic stirring.
5. The method for preparing hydrotalcite-type layered hydroxide from saline-alkali soil according to claim 1, wherein the clear solution obtained in step (3) is subjected to ultrafiltration and nanofiltration reverse osmosis, reduced pressure concentration, solar evaporation and saturated crystallization to obtain a thick colloid, sodium chloride products are obtained by filtration, and the filtered liquid is concentrated or separated by solar evaporation to obtain potassium chloride products.
6. The method for preparing hydrotalcite-like layered hydroxide using saline-alkali soil according to claim 1, wherein in the step (4), the temperature of the hydrothermal reactor is set to 90-200 ℃, the hydrothermal crystallization time is 6-64h, and the heating manner of the heater comprises: electrical heating, microwave and infrared heating.
7. The method for preparing hydrotalcite-type layered hydroxide from saline-alkali soil according to claim 1, wherein step (4) comprises centrifuging the solid at a speed of 100-500000rpm/min for 1-360min before washing.
8. Use of the hydrotalcite-like layered hydroxide prepared by the method according to any one of claims 1 to 7 for the preparation of plastic articles or adsorbents or catalysts;
the method for preparing the PVC product heat stabilizer from the hydrotalcite layered hydroxide comprises the following steps:
(1) Adding hydrotalcite type layered hydroxide into an organic solvent, centrifuging, dispersing and washing for 3-5 times;
(2) After washing, adding an organic solvent for dispersion, and then adding PVC powder to obtain a uniform suspension;
(3) Centrifugally separating the suspension to obtain a solid hydrotalcite and PVC solid mixture, and drying to obtain a uniform solid hydrotalcite and PVC solid mixture;
(4) And (4) adding a plasticizer into the solid hydrotalcite and PVC solid mixture obtained in the step (3) to obtain a PVC product.
9. The use of the hydrotalcite-type layered hydroxide according to claim 8,
the ratio of the PCV powder to the organic solvent is 1:5-20.
10. The use of the hydrotalcite-like layered hydroxide according to claim 8, wherein the hydrotalcite is present in an amount of 3 to 20% by mass of the total mass; the mass ratio of the PVC mixture, the plasticizer and the solid hydrotalcite is 1.
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