CN115744945B - Magnesium hydroxide continuous preparation method with controllable hydrophobicity - Google Patents
Magnesium hydroxide continuous preparation method with controllable hydrophobicity Download PDFInfo
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- CN115744945B CN115744945B CN202211469824.4A CN202211469824A CN115744945B CN 115744945 B CN115744945 B CN 115744945B CN 202211469824 A CN202211469824 A CN 202211469824A CN 115744945 B CN115744945 B CN 115744945B
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- magnesium hydroxide
- flotation
- continuous preparation
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- hydrophobicity
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- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 title claims abstract description 114
- 239000000347 magnesium hydroxide Substances 0.000 title claims abstract description 106
- 229910001862 magnesium hydroxide Inorganic materials 0.000 title claims abstract description 106
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 238000005188 flotation Methods 0.000 claims abstract description 64
- 230000004048 modification Effects 0.000 claims abstract description 34
- 238000012986 modification Methods 0.000 claims abstract description 34
- 230000002209 hydrophobic effect Effects 0.000 claims abstract description 24
- 238000000034 method Methods 0.000 claims abstract description 24
- 230000008569 process Effects 0.000 claims abstract description 23
- 239000004088 foaming agent Substances 0.000 claims abstract description 21
- 239000008396 flotation agent Substances 0.000 claims abstract description 17
- 239000012141 concentrate Substances 0.000 claims abstract description 12
- 239000002002 slurry Substances 0.000 claims abstract description 12
- 238000001914 filtration Methods 0.000 claims abstract description 7
- 239000003607 modifier Substances 0.000 claims abstract description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 16
- 239000002270 dispersing agent Substances 0.000 claims description 8
- 239000002994 raw material Substances 0.000 claims description 7
- 239000007787 solid Substances 0.000 claims description 7
- -1 styryl phosphonate Chemical compound 0.000 claims description 7
- WVYWICLMDOOCFB-UHFFFAOYSA-N 4-methyl-2-pentanol Chemical compound CC(C)CC(C)O WVYWICLMDOOCFB-UHFFFAOYSA-N 0.000 claims description 6
- POULHZVOKOAJMA-UHFFFAOYSA-N dodecanoic acid Chemical compound CCCCCCCCCCCC(O)=O POULHZVOKOAJMA-UHFFFAOYSA-N 0.000 claims description 6
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims description 4
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims description 4
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims description 4
- 239000005642 Oleic acid Substances 0.000 claims description 4
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 4
- BCKXLBQYZLBQEK-KVVVOXFISA-M Sodium oleate Chemical compound [Na+].CCCCCCCC\C=C/CCCCCCCC([O-])=O BCKXLBQYZLBQEK-KVVVOXFISA-M 0.000 claims description 4
- 235000021355 Stearic acid Nutrition 0.000 claims description 4
- IPCSVZSSVZVIGE-UHFFFAOYSA-N hexadecanoic acid Chemical compound CCCCCCCCCCCCCCCC(O)=O IPCSVZSSVZVIGE-UHFFFAOYSA-N 0.000 claims description 4
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 4
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 4
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 4
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 4
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 4
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 4
- 229920000136 polysorbate Polymers 0.000 claims description 4
- 229950008882 polysorbate Drugs 0.000 claims description 4
- 229910052708 sodium Inorganic materials 0.000 claims description 4
- 239000011734 sodium Substances 0.000 claims description 4
- 239000008117 stearic acid Substances 0.000 claims description 4
- 239000005639 Lauric acid Substances 0.000 claims description 3
- SEGLCEQVOFDUPX-UHFFFAOYSA-N di-(2-ethylhexyl)phosphoric acid Chemical compound CCCCC(CC)COP(O)(=O)OCC(CC)CCCC SEGLCEQVOFDUPX-UHFFFAOYSA-N 0.000 claims description 3
- 239000003921 oil Substances 0.000 claims description 3
- OYHQOLUKZRVURQ-NTGFUMLPSA-N (9Z,12Z)-9,10,12,13-tetratritiooctadeca-9,12-dienoic acid Chemical compound C(CCCCCCC\C(=C(/C\C(=C(/CCCCC)\[3H])\[3H])\[3H])\[3H])(=O)O OYHQOLUKZRVURQ-NTGFUMLPSA-N 0.000 claims description 2
- FJLUATLTXUNBOT-UHFFFAOYSA-N 1-Hexadecylamine Chemical compound CCCCCCCCCCCCCCCCN FJLUATLTXUNBOT-UHFFFAOYSA-N 0.000 claims description 2
- FRPZMMHWLSIFAZ-UHFFFAOYSA-N 10-undecenoic acid Chemical compound OC(=O)CCCCCCCCC=C FRPZMMHWLSIFAZ-UHFFFAOYSA-N 0.000 claims description 2
- DSCFFEYYQKSRSV-UHFFFAOYSA-N 1L-O1-methyl-muco-inositol Natural products COC1C(O)C(O)C(O)C(O)C1O DSCFFEYYQKSRSV-UHFFFAOYSA-N 0.000 claims description 2
- HNNQYHFROJDYHQ-UHFFFAOYSA-N 3-(4-ethylcyclohexyl)propanoic acid 3-(3-ethylcyclopentyl)propanoic acid Chemical compound CCC1CCC(CCC(O)=O)C1.CCC1CCC(CCC(O)=O)CC1 HNNQYHFROJDYHQ-UHFFFAOYSA-N 0.000 claims description 2
- VJXUJFAZXQOXMJ-UHFFFAOYSA-N D-1-O-Methyl-muco-inositol Natural products CC12C(OC)(C)OC(C)(C)C2CC(=O)C(C23OC2C(=O)O2)(C)C1CCC3(C)C2C=1C=COC=1 VJXUJFAZXQOXMJ-UHFFFAOYSA-N 0.000 claims description 2
- DSCFFEYYQKSRSV-KLJZZCKASA-N D-pinitol Chemical compound CO[C@@H]1[C@@H](O)[C@@H](O)[C@H](O)[C@H](O)[C@H]1O DSCFFEYYQKSRSV-KLJZZCKASA-N 0.000 claims description 2
- REYJJPSVUYRZGE-UHFFFAOYSA-N Octadecylamine Chemical compound CCCCCCCCCCCCCCCCCCN REYJJPSVUYRZGE-UHFFFAOYSA-N 0.000 claims description 2
- 235000021314 Palmitic acid Nutrition 0.000 claims description 2
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 2
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 2
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 2
- DTOSIQBPPRVQHS-PDBXOOCHSA-N alpha-linolenic acid Chemical compound CC\C=C/C\C=C/C\C=C/CCCCCCCC(O)=O DTOSIQBPPRVQHS-PDBXOOCHSA-N 0.000 claims description 2
- 235000020661 alpha-linolenic acid Nutrition 0.000 claims description 2
- KHAVLLBUVKBTBG-UHFFFAOYSA-N caproleic acid Natural products OC(=O)CCCCCCCC=C KHAVLLBUVKBTBG-UHFFFAOYSA-N 0.000 claims description 2
- 239000004359 castor oil Substances 0.000 claims description 2
- 235000019438 castor oil Nutrition 0.000 claims description 2
- TVACALAUIQMRDF-UHFFFAOYSA-N dodecyl dihydrogen phosphate Chemical compound CCCCCCCCCCCCOP(O)(O)=O TVACALAUIQMRDF-UHFFFAOYSA-N 0.000 claims description 2
- JRBPAEWTRLWTQC-UHFFFAOYSA-N dodecylamine Chemical compound CCCCCCCCCCCCN JRBPAEWTRLWTQC-UHFFFAOYSA-N 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- ZEMPKEQAKRGZGQ-XOQCFJPHSA-N glycerol triricinoleate Natural products CCCCCC[C@@H](O)CC=CCCCCCCCC(=O)OC[C@@H](COC(=O)CCCCCCCC=CC[C@@H](O)CCCCCC)OC(=O)CCCCCCCC=CC[C@H](O)CCCCCC ZEMPKEQAKRGZGQ-XOQCFJPHSA-N 0.000 claims description 2
- ZUVCYFMOHFTGDM-UHFFFAOYSA-N hexadecyl dihydrogen phosphate Chemical compound CCCCCCCCCCCCCCCCOP(O)(O)=O ZUVCYFMOHFTGDM-UHFFFAOYSA-N 0.000 claims description 2
- 229960004488 linolenic acid Drugs 0.000 claims description 2
- KQQKGWQCNNTQJW-UHFFFAOYSA-N linolenic acid Natural products CC=CCCC=CCC=CCCCCCCCC(O)=O KQQKGWQCNNTQJW-UHFFFAOYSA-N 0.000 claims description 2
- WQEPLUUGTLDZJY-UHFFFAOYSA-N n-Pentadecanoic acid Natural products CCCCCCCCCCCCCCC(O)=O WQEPLUUGTLDZJY-UHFFFAOYSA-N 0.000 claims description 2
- 235000021313 oleic acid Nutrition 0.000 claims description 2
- 239000003208 petroleum Substances 0.000 claims description 2
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 2
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 2
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 2
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 2
- 239000000344 soap Substances 0.000 claims description 2
- PNGBYKXZVCIZRN-UHFFFAOYSA-M sodium;hexadecane-1-sulfonate Chemical compound [Na+].CCCCCCCCCCCCCCCCS([O-])(=O)=O PNGBYKXZVCIZRN-UHFFFAOYSA-M 0.000 claims description 2
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 claims description 2
- 239000003784 tall oil Substances 0.000 claims description 2
- TUNFSRHWOTWDNC-HKGQFRNVSA-N tetradecanoic acid Chemical compound CCCCCCCCCCCCC[14C](O)=O TUNFSRHWOTWDNC-HKGQFRNVSA-N 0.000 claims description 2
- 229960002703 undecylenic acid Drugs 0.000 claims description 2
- KBAFDSIZQYCDPK-UHFFFAOYSA-M sodium;octadecane-1-sulfonate Chemical compound [Na+].CCCCCCCCCCCCCCCCCCS([O-])(=O)=O KBAFDSIZQYCDPK-UHFFFAOYSA-M 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 230000033228 biological regulation Effects 0.000 abstract description 3
- 238000005516 engineering process Methods 0.000 abstract description 2
- 238000009776 industrial production Methods 0.000 abstract description 2
- 239000007788 liquid Substances 0.000 abstract 1
- 239000000047 product Substances 0.000 description 39
- 239000003153 chemical reaction reagent Substances 0.000 description 12
- 239000002245 particle Substances 0.000 description 11
- 238000003756 stirring Methods 0.000 description 11
- 238000009826 distribution Methods 0.000 description 9
- 238000011084 recovery Methods 0.000 description 8
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 7
- 239000011777 magnesium Substances 0.000 description 7
- 229910052749 magnesium Inorganic materials 0.000 description 7
- 238000002156 mixing Methods 0.000 description 7
- 239000000203 mixture Substances 0.000 description 6
- 229910019142 PO4 Inorganic materials 0.000 description 5
- 239000002253 acid Substances 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 5
- 239000003795 chemical substances by application Substances 0.000 description 5
- 239000003063 flame retardant Substances 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 235000021317 phosphate Nutrition 0.000 description 5
- 230000035484 reaction time Effects 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- DHRRIBDTHFBPNG-UHFFFAOYSA-L magnesium dichloride hexahydrate Chemical compound O.O.O.O.O.O.[Mg+2].[Cl-].[Cl-] DHRRIBDTHFBPNG-UHFFFAOYSA-L 0.000 description 4
- 125000005600 alkyl phosphonate group Chemical group 0.000 description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- 230000001186 cumulative effect Effects 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000010419 fine particle Substances 0.000 description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 3
- 239000010452 phosphate Substances 0.000 description 3
- 229920002994 synthetic fiber Polymers 0.000 description 3
- 238000001238 wet grinding Methods 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- ABLZXFCXXLZCGV-UHFFFAOYSA-N Phosphorous acid Chemical class OP(O)=O ABLZXFCXXLZCGV-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 239000012065 filter cake Substances 0.000 description 2
- 238000011068 loading method Methods 0.000 description 2
- 239000000395 magnesium oxide Substances 0.000 description 2
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 2
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 2
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 239000000779 smoke Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000004094 surface-active agent Substances 0.000 description 2
- 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 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- PAHWROPPWOVREG-UHFFFAOYSA-N P(=O)(O)(O)O.C(CCCCCCCCCCCCCCC)[K] Chemical group P(=O)(O)(O)O.C(CCCCCCCCCCCCCCC)[K] PAHWROPPWOVREG-UHFFFAOYSA-N 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000006477 desulfuration reaction Methods 0.000 description 1
- 230000023556 desulfurization Effects 0.000 description 1
- YVIGPQSYEAOLAD-UHFFFAOYSA-L disodium;dodecyl phosphate Chemical compound [Na+].[Na+].CCCCCCCCCCCCOP([O-])([O-])=O YVIGPQSYEAOLAD-UHFFFAOYSA-L 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 150000002170 ethers Chemical class 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 159000000003 magnesium salts Chemical class 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- UEZVMMHDMIWARA-UHFFFAOYSA-M phosphonate Chemical compound [O-]P(=O)=O UEZVMMHDMIWARA-UHFFFAOYSA-M 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 description 1
- 229920000053 polysorbate 80 Polymers 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 239000011819 refractory material Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- BTURAGWYSMTVOW-UHFFFAOYSA-M sodium dodecanoate Chemical compound [Na+].CCCCCCCCCCCC([O-])=O BTURAGWYSMTVOW-UHFFFAOYSA-M 0.000 description 1
- 229940082004 sodium laurate Drugs 0.000 description 1
- DAJSVUQLFFJUSX-UHFFFAOYSA-M sodium;dodecane-1-sulfonate Chemical compound [Na+].CCCCCCCCCCCCS([O-])(=O)=O DAJSVUQLFFJUSX-UHFFFAOYSA-M 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000001629 suppression Effects 0.000 description 1
- 210000004243 sweat Anatomy 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 229920006305 unsaturated polyester Polymers 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
Landscapes
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention discloses a continuous preparation process of magnesium hydroxide with controllable hydrophobicity, which comprises the steps of adding magnesium hydroxide into modification equipment for surface modification, and enabling modified slurry to enter a multistage flotation tank. Adding a surface modifier into the modifying equipment, adding a flotation agent and a foaming agent into a flotation tank in steps, filtering the flotation concentrate, and then, feeding the flotation concentrate into a flash dryer to obtain hydrophobic magnesium hydroxide, wherein the tail liquid of the flotation tank returns to the modifying equipment. The process combines the surface modification and the multistage flotation process, effectively regulates the hydrophobicity of the magnesium hydroxide, and continuously prepares the hydrophobic magnesium hydroxide. Solves the problem that the current surface modification technology can not realize the accurate regulation and control of the hydrophobic property of the modified magnesium hydroxide; the prepared magnesium hydroxide has controllable hydrophobicity, stable product quality and high production efficiency, and meets the requirements of industrial production.
Description
Technical Field
The invention relates to a continuous preparation process of magnesium hydroxide with controllable hydrophobicity, and belongs to the technical field of magnesium hydroxide preparation.
Background
Sodium, potassium, magnesium, lithium and other abundant resources exist in Qinghai Bohr sweat salt lake. A large amount of bischofite is produced in the process of developing the salt lake resource of the halhidrosis, and is locally called as 'magnesium hazard'. Magnesium is deposited by ammonia method by Qinghai western magnesium industry Co-Ltd, bischofite is used as raw material to prepare magnesium hydroxide product on a large scale, and the problem of magnesium harm in salt lake is successfully solved.
Magnesium hydroxide has wide application in the chemical industry, and industrial grade magnesium hydroxide is sequentially classified into three grades according to the order of decreasing the purity of magnesium hydroxide. The first grade product is mainly used for flame retardant filler, the second grade product is used as raw material for producing high-purity magnesium oxide and magnesium salt, and the third grade product is mainly used for environmental treatment, such as flue desulfurization, wastewater treatment, soil improvement and the like.
Magnesium hydroxide is a filled flame retardant which releases bound water by thermal decomposition and absorbs a large amount of latent heat to reduce the surface temperature of the synthetic material filled with the magnesium hydroxide in a flame, and has the effects of inhibiting polymer decomposition and cooling the generated combustible gas. Magnesium oxide generated by decomposing magnesium hydroxide is a good refractory material, can also help to improve the fire resistance of the synthetic material, and can also be used as a smoke suppressant by the water vapor emitted by the synthetic material. Therefore, the magnesium hydroxide is an excellent flame retardant with triple functions of flame retardance, smoke suppression and filling in the well-known rubber and plastic industry. Can be widely applied to rubber, chemical industry, building materials, plastics, electronics, unsaturated polyester, paint, coating and other polymer materials. However, magnesium hydroxide generally has a loading of 50% or more, which is comparable to halogen-containing organic flame retardants. Because the magnesium hydroxide surface is naturally hydrophilic, the magnesium hydroxide has poor compatibility with the hydrophobic high polymer base material. Such a high loading of magnesium hydroxide, if not surface-modified, will result in a decrease in the mechanical properties of the composite material after the magnesium hydroxide is loaded into the polymeric material. However, the current surface modification process cannot realize the precise regulation and control of the hydrophobicity of the modified magnesium hydroxide, so that the hydrophobicity of the modified magnesium hydroxide is unstable. Therefore, the preparation of magnesium hydroxide with controllable hydrophobicity is key to the successful application of magnesium hydroxide in the high-end flame retardant industry.
In order to further widen the application range of magnesium hydroxide produced by bischofite in salt lake, a continuous magnesium hydroxide production process with controllable hydrophobicity is researched. The process can accurately and continuously regulate the hydrophobic property of the magnesium hydroxide, improves the product value of magnesium hydroxide produced by bischofite, has great economic benefit, and lays a foundation for realizing diversification, serialization and scale production of high-end magnesium-based compound products in China.
At present, in the field of magnesium hydroxide surface modification and flotation separation, no report is seen on realizing the precise regulation and control of the hydrophobicity of magnesium hydroxide and the continuous preparation of hydrophobic magnesium hydroxide by combining a surface modification and flotation process, and no report is seen on using phosphate, alkyl phosphonate or a mixture of one or more of phosphate agents, esters, ethers and alcohol agents as a magnesium hydroxide flotation agent.
Disclosure of Invention
Aiming at the defect of unstable hydrophobic property of surface modified magnesium hydroxide in the prior art, the invention aims to provide a magnesium hydroxide continuous preparation process with adjustable hydrophobic property. The process combines surface modification and floatation, and accurately and continuously regulates and controls the hydrophobic property of magnesium hydroxide; solves the problem that the modification of magnesium hydroxide produced in the salt lake is unstable at present and the application of magnesium hydroxide in the high-end magnesium material is limited; the prepared magnesium hydroxide product has stable hydrophobicity, high production efficiency and high recovery rate, and meets the industrial production requirement.
The invention discloses a continuous preparation process of magnesium hydroxide with controllable hydrophobicity, which comprises the following steps:
(1) Adding magnesium hydroxide raw material into a modifying device to carry out surface modification by using a surface modifier; the hydrophobicity of the modified magnesium hydroxide is greater than that of the magnesium hydroxide before modification;
(2) The modified magnesium hydroxide slurry enters a flotation tank, and a flotation agent and a foaming agent are respectively added for flotation; the agent used for floatation contains A; the A is at least one selected from phosphate compounds, alkyl phosphates, alkyl phosphonates and phosphonate compounds;
(3) Filtering the flotation concentrate and drying to obtain hydrophobic magnesium hydroxide; the flotation tailings are returned to the modifying apparatus.
The continuous preparation process of the hydrophobic controllable magnesium hydroxide also comprises the following preferable scheme:
Preferably, as in step (1), the magnesium hydroxide raw material has a D50 particle size of 1-60um and a purity of more than 98%.
Preferably, as in step (1), the reaction time is 50-80min.
Preferably, as in step (1), the reaction time temperature is 60-95 ℃.
Preferably, as in step (1), the surface modifier is at least one of silane coupling agent, dodecyl amine, hexadecyl amine, octadecyl amine, sodium dodecyl sulfate, sodium petroleum sulfonate, sodium dodecyl sulfonate, sodium hexadecyl sulfonate, oleic acid, linoleic acid, linolenic acid, lauric acid, myristic acid, palmitic acid, stearic acid, naphthenic acid, tall oil soap, sodium oleate, undecylenic acid.
Preferably, the dispersant used for the modification in the step (1) is at least one selected from ethanol, polyvinylpyrrolidone, polyvinyl alcohol and sulfated castor oil. In industrial applications, both wet and dry modifications are suitable for the present invention.
Wet modification is preferred. In wet modification, the magnesium hydroxide raw material is prepared into slurry with the solid content of 10-65%.
Preferably, as in step (2), the magnesium hydroxide solids content of the slurry entering the flotation tank is 10-65%, preferably 20-60%.
Preferably, the flotation cell is a 1-6 stage flotation cell as in step (2).
Preferably, the flotation pH is in the range 7-12 as in step (2).
Preferably, as in step (2), the flotation reagent is a mixture of one or more of phosphate or phosphonate reagents such as di (2-ethylhexyl) phosphate, alpha styrylphosphonate, dodecyl phosphate, hexadecyl phosphate and one or more of polysorbate, octylphenyl polyoxyethylene ether, monohydric alcohol.
Further preferably, the flotation reagent consists of A and at least one of polysorbate, octyl phenyl polyoxyethylene ether and monohydric alcohol; and the content of A in the flotation reagent is more than or equal to 80wt%.
Preferably, as in step (2), the foaming agent is one of MIBC, pinitol oil, and industrial No. 2 oil.
Preferably, as in step (2), the surface modifying agent: dispersing agent: flotation agent: foaming agent: the mass ratio of the magnesium hydroxide is 1-80:0-20:1-20:1-10:200000.
As a further preference, the flotation agent: foaming agent: the mass ratio of the magnesium hydroxide is 3-19:2-9:200000.
As a further preference, the flotation agent: foaming agent: the mass ratio of the magnesium hydroxide is 4-18:2-8:200000.
As a still further preferred, the amount of flotation agent according to the invention is greater than the amount of frothing agent.
Preferably, as in step (2), the flotation reagent is added first and stirred for 5-10 minutes.
Preferably, the foaming agent is added after the step (2) and stirred for 3 to 5 minutes.
Preferably, the flotation time is 5-8 minutes as in step (2).
Preferably, as in step (3), the magnesium hydroxide concentrate is automatically overflowed and filtered and then enters a flash dryer to obtain hydrophobic magnesium hydroxide.
Preferably, as in step (3), the filtration is performed using a plate filter press.
Preferably, as in step (3), the flotation cell tailings are returned to the modification apparatus. Further preferred are: the tailings of the flotation tank are returned to the modification equipment in the step (1).
The invention firstly proposes that the hydrophobicity of magnesium hydroxide is initially adjusted by modification; at the moment, the condition that the surface modification of part of raw material magnesium hydroxide is uneven is unavoidable; then separating the magnesium hydroxide which is not modified in place and the magnesium hydroxide which is modified by adopting a special flotation agent in the follow-up process; and further obtaining a high-quality product with small fluctuation of the hydrophobicity. The invention adopts the thought of rough adjustment and precise control to realize the preparation of the high-quality magnesium hydroxide with the fluctuation range of the contact angle of the product in the same batch within 16 degrees for the first time.
The invention is characterized in that the products in the same batch are produced; the fluctuation range of the contact angle in air after tabletting is within 16 degrees. Preferably, the temperature can be controlled within 12 degrees. And the recovery rate of the product is more than or equal to 90 percent, and the recovery rate of the optimized product is more than or equal to 95 percent.
Compared with the prior art, the technical scheme of the invention has the beneficial effects that:
1. The invention combines the surface modification and the flotation process in a closed loop, solves the problem of unstable hydrophobic property of the modified product, and utilizes the flotation process to accurately regulate and control the hydrophobic property of the surface modified product.
2. The flotation reagent provided by the invention is a mixture of at least one of phosphate compounds, alkyl phosphates, alkyl phosphonates and phosphonate compounds and one or more of polysorbate, octyl phenyl polyoxyethylene ether and monohydric alcohol, so that the purpose of optimizing the flotation effect is achieved.
3. The invention adopts the flotation technology to dynamically control the hydrophobicity of the modified product, is beneficial to reducing the dosage of the medicament in the surface modification process, achieves the adsorption of the monomolecular layer, and realizes the interaction strengthening effect of the medicament in the flotation process and the surface modification process.
4. The process is closed-loop combined, no waste water and waste residue are discharged, the environment is friendly, and the industrial use requirements are met.
Drawings
FIG. 1 is a process flow diagram of the present invention.
Fig. 2 is a schematic diagram of a multistage flotation cell.
Figure 3 is a plot of the flotation concentrate particle size distribution of example 3.
DETAILED DESCRIPTION OF EMBODIMENT (S) OF INVENTION
The following further description of the present invention is provided in connection with the embodiments, and it should be emphasized that the following description is merely exemplary in nature and is not intended to limit the scope of the invention or its application.
Example 1
Step (1): adding magnesium hydroxide (D50 particle size of 45 um) slurry with solid content of 33% into a modification kettle, and stirring for reaction, wherein a surfactant is oleic acid; the reaction time is 57min, the reaction temperature is 70 ℃, and the mass ratio of oleic acid to magnesium hydroxide is 15:200000; the pH was 7.9.
Step (2): the flotation tank is a 3-level flotation tank, the flotation reagent is hexadecyl potassium phosphate and Tween 80, the mass ratio is 85:15, and the foaming agent is MIBC. Adding the flotation reagent, stirring for 5 minutes, adding the foaming agent, stirring for 3 minutes, and introducing air to perform flotation for 6 minutes. Flotation agent: foaming agent: the mass ratio of the magnesium hydroxide is 7:2:200000.
Step (3): and overflowing the flotation tank to obtain concentrates #1, #2 and #3, mixing, filtering by a plate filter press, and then entering a flash dryer to obtain the hydrophobic magnesium hydroxide. The inlet air temperature of the flash dryer is 240 ℃, the mixing temperature is 110 ℃, and the outlet air temperature is 110 ℃. The tailings of the flotation tank are returned to the modification kettle.
The cumulative recycle, magnesium hydroxide recovery was about 96wt% (the remainder being very fine particles difficult to recover).
7 Samples are randomly taken from the magnesium hydroxide product, the contact angle in air after tabletting is 112 degrees+/-8 degrees, the product hydrophobicity distribution is narrow, the product quality is stable, and the hydrophobicity fluctuation is small.
Example 2
Adding magnesium hydroxide (D50 particle size of 50 um) slurry with solid content of 38% into a modification kettle, wherein a surfactant is stearic acid, and ethanol is a dispersing agent, and stirring for reaction; the reaction time is 65min, the reaction temperature is 75 degrees, and the mass ratio of stearic acid, ethanol and magnesium hydroxide is 18:1:200000.pH 8.
Step (2): the flotation tank is a 2-grade flotation tank, the flotation agent is a mixture of di (2-ethylhexyl) phosphate and monohydric alcohol, the mass ratio is 90:10, and the foaming agent is MIBC. Adding the flotation reagent, stirring for 6 minutes, adding the foaming agent, stirring for 3 minutes, and introducing air to perform flotation for 7 minutes. Flotation agent: foaming agent: the mass ratio of the magnesium hydroxide is 5:2:200000.
Step (3): and overflowing the flotation tank to obtain concentrates #1 and #2, mixing, filtering by a plate filter press, and then entering a flash evaporation dryer to obtain the hydrophobic magnesium hydroxide. The inlet air temperature of the flash dryer is 250 ℃, the mixing temperature is 120 ℃, and the outlet air temperature is 100 ℃. The tailings of the flotation tank are returned to the modification kettle.
The cumulative recycle, magnesium hydroxide recovery was about 97wt% (the remainder being very fine particles difficult to recover).
The purity of the product hydrophobic magnesium hydroxide is 99.7%, 7 samples are randomly taken from the magnesium hydroxide product, the contact angle in air after tabletting is 98 degrees+/-6 degrees, the product hydrophobicity distribution is narrow, the product quality is stable, and the hydrophobicity fluctuation is small.
Example 3
Adding magnesium hydroxide (D50 particle size of 1.5 um) slurry with solid content of 25% into a modification kettle, stirring and reacting; the reaction time is 75min, the reaction temperature is 64 degrees, and the mass ratio of lauric acid to magnesium hydroxide is 40:200000. And pH 9.
Step (2): the flotation tank is a 6-grade flotation tank, the flotation agent is a mixture of sodium dodecyl phosphate and monohydric alcohol, the mass ratio is 90:10, and the foaming agent is MIBC. Adding the flotation reagent, stirring for 10 minutes, adding the foaming agent, stirring for 5 minutes, and introducing air to perform flotation for 8 minutes. Flotation agent: foaming agent: the mass ratio of the magnesium hydroxide is 14:7:200000.
Step (3): the flotation tank overflows to obtain concentrates #1, #2, #3, #4, #5 and #6, and the concentrates are mixed, filtered by a plate filter press and then enter a flash dryer to obtain hydrophobic magnesium hydroxide. The inlet air temperature of the flash dryer is 260 ℃, the mixing temperature is 130 ℃, and the outlet air temperature is 110 ℃. The tailings of the flotation tank are returned to the modification kettle.
The cumulative recycle, magnesium hydroxide recovery was about 95wt% (the remainder being very fine particles difficult to recover).
7 Samples are randomly taken from the magnesium hydroxide product, the contact angle in air after tabletting is 105 degrees+/-5 degrees, the product hydrophobicity distribution is narrow, the product quality is stable, the hydrophobicity fluctuation is small, the particle size distribution diagram is shown in figure 3, and the median particle size is 1.5um.
Comparative example 1
Placing 100 parts by weight of magnesium hydroxide, 2 parts by weight of polycarboxylic acid type dispersing agent, 2 parts by weight of sodium stearyl acid and 100 parts by weight of water into a ball mill; wet milling was carried out for 6 hours with 100 parts by weight of alumina medium having a particle size of 5 mm. After crushing for 2 hours, 2 parts by weight of a polycarboxylic acid type dispersant was added, and after crushing for 4 hours, 2 parts by weight of sodium oleate was added. The obtained slurry was filtered and separated, and the cake was dried at 120℃for 2 hours to obtain a magnesium hydroxide cake. 7 samples are randomly taken from the magnesium hydroxide product, the contact angle in air after tabletting is 90 degrees+/-25 degrees, the product hydrophobicity distribution is wide, and the product hydrophobicity fluctuation is large. The hydrophilic and hydrophobic magnesium hydroxide in the product are not effectively separated.
Comparative example 2
100 Parts by weight of magnesium hydroxide, 4 parts by weight of a polycarboxylic acid type dispersant, 2 parts by weight of sodium laurate and 100 parts by weight of water were put into a ball mill, and wet milling was performed for 6 hours under 100 parts by weight of an alumina medium having a particle diameter of 5 mm. The resulting slurry was filtered off and the filter cake was dried at 120℃for 2 hours to give magnesium hydroxide. 7 samples are randomly taken from the magnesium hydroxide product, the contact angle in air after tabletting is 75 degrees+/-35 degrees, the product hydrophobicity distribution is wide, and the product hydrophobicity fluctuation is large. The hydrophilic and hydrophobic magnesium hydroxide in the product are not effectively separated.
Comparative example 3
100 Parts by weight of magnesium hydroxide, 2 parts by weight of a polycarboxylic acid type dispersant, 2 parts by weight of sodium oleate and 100 parts by weight of water were put into a ball mill, and wet milling was performed for 6 hours under 100 parts by weight of alumina medium having a particle diameter of 5 mm. The resulting slurry was filtered off and the filter cake was dried at 120℃for 2 hours to give magnesium hydroxide. 7 samples are randomly taken from the magnesium hydroxide product, the contact angle in air after tabletting is 80 degrees+/-40 degrees, the product hydrophobicity distribution is wide, and the product hydrophobicity fluctuation is large. The hydrophilic and hydrophobic magnesium hydroxide in the product are not effectively separated.
Comparative example 4
Magnesium hydroxide with 30% of solid content (D50 particle size is 5 um) is added into a 3-grade flotation tank, the flotation reagent is a mixture of alpha styryl phosphonate and monohydric alcohol, the mass ratio is 92:8, the foaming agent is MIBC, and the pH is 8.5. Adding the flotation reagent, stirring for 5 minutes, adding the foaming agent, stirring for 5 minutes, and introducing air to perform flotation for 8 minutes. Flotation agent: foaming agent: the mass ratio of the magnesium hydroxide is 11:5:200000. and overflowing the flotation tank to obtain concentrates #1, #2 and #3, mixing, filtering by a plate filter press, and then entering a flash dryer to obtain the hydrophobic magnesium hydroxide. The inlet air temperature of the flash dryer is 260 ℃, the mixing temperature is 130 ℃, and the outlet air temperature is 110 ℃. The magnesium hydroxide recovery was 52wt%. 7 samples are randomly taken from the magnesium hydroxide product, the contact angle in air after tabletting is 51 DEG + -5 DEG, the hydrophobicity distribution of the product is narrow, but the hydrophobicity and the recovery rate are lower.
The background section of the present invention may contain background information about the problems or environments of the present invention and is not necessarily descriptive of the prior art. Accordingly, inclusion in the background section is not an admission of prior art by the applicant.
The foregoing is a further detailed description of the invention in connection with specific embodiments, and it is not intended that the invention be limited to such description. It will be apparent to those skilled in the art that several alternatives or modifications can be made to the described embodiments without departing from the spirit of the invention, and these alternatives or modifications should be considered to be within the scope of the invention. In the description of the present specification, a description referring to terms "one embodiment," "some embodiments," "examples," "specific examples," or "some examples," etc., means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present invention. In this specification, schematic representations of the above terms are not necessarily directed to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Those skilled in the art may combine and combine the features of the different embodiments or examples described in this specification and of the different embodiments or examples without contradiction. Although embodiments of the present invention and their advantages have been described in detail, it should be understood that various changes, substitutions and alterations can be made herein without departing from the scope of the invention as defined by the appended claims.
Claims (8)
1. A continuous preparation process of magnesium hydroxide with controllable hydrophobicity is characterized in that: comprises the following steps of;
(1) Adding magnesium hydroxide raw material into a modifying device to carry out surface modification by using a surface modifier; the hydrophobicity of the modified magnesium hydroxide is greater than that of the magnesium hydroxide before modification;
(2) The modified magnesium hydroxide slurry enters a flotation tank, and a flotation agent and a foaming agent are respectively added for flotation; the flotation agent consists of A and B; and the content of A in the flotation agent is more than or equal to 80wt%, wherein the A is one or more selected from di (2-ethylhexyl) phosphate, alpha styryl phosphonate, dodecyl phosphate and hexadecyl phosphate; the B is at least one selected from polysorbate, octyl phenyl polyoxyethylene ether and monohydric alcohol;
(3) Filtering the flotation concentrate and drying to obtain hydrophobic magnesium hydroxide; the flotation tailings are returned to the modifying apparatus.
2. The continuous preparation process of magnesium hydroxide with controllable hydrophobicity according to claim 1, wherein the process comprises the following steps: the surface modifier in the step (1) is at least one selected from silane coupling agents, dodecyl amine, hexadecyl amine, octadecyl amine, sodium dodecyl sulfate, sodium petroleum sulfonate, sodium hexadecyl sulfonate, sodium octadecyl sulfonate, oleic acid, linoleic acid, linolenic acid, lauric acid, myristic acid, palmitic acid, stearic acid, naphthenic acid, tall oil soap, sodium oleate and undecylenic acid.
3. The continuous preparation process of magnesium hydroxide with controllable hydrophobicity according to claim 1, wherein the process comprises the following steps: the dispersing agent used in the surface modification process in the step (1) is at least one selected from ethanol, polyvinylpyrrolidone, polyvinyl alcohol and sulfated castor oil.
4. The continuous preparation process of magnesium hydroxide with controllable hydrophobicity according to claim 1, wherein the process comprises the following steps: the solid content of the magnesium hydroxide slurry entering the flotation tank is 10-65%.
5. The continuous preparation process of magnesium hydroxide with controllable hydrophobicity according to claim 1, wherein the process comprises the following steps: in the step (2), the flotation tank is a 1-6-grade flotation tank.
6. The continuous preparation process of magnesium hydroxide with controllable hydrophobicity according to claim 1, wherein the process comprises the following steps: in the step (2), the pH value of the flotation is 7-12.
7. The continuous preparation process of magnesium hydroxide with controllable hydrophobicity according to claim 1, wherein the process comprises the following steps: and (2) the foaming agent is at least one of MIBC and pinitol oil.
8. The continuous preparation process of magnesium hydroxide with controllable hydrophobicity according to claim 1, wherein the process comprises the following steps: in the step (3), the magnesium hydroxide concentrate automatically overflows and filters and then enters a flash dryer to obtain hydrophobic magnesium hydroxide, and tailings in a flotation tank return to the modification equipment.
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