CN111073351A - 一种高耐候、高分散塑料色母二氧化钛颜料的制备方法 - Google Patents
一种高耐候、高分散塑料色母二氧化钛颜料的制备方法 Download PDFInfo
- Publication number
- CN111073351A CN111073351A CN201911242911.4A CN201911242911A CN111073351A CN 111073351 A CN111073351 A CN 111073351A CN 201911242911 A CN201911242911 A CN 201911242911A CN 111073351 A CN111073351 A CN 111073351A
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- Prior art keywords
- titanium dioxide
- solution
- color master
- master batch
- slurry
- 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.)
- Pending
Links
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 273
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 127
- 239000000049 pigment Substances 0.000 title claims abstract description 42
- 239000004595 color masterbatch Substances 0.000 title claims abstract description 38
- 239000004033 plastic Substances 0.000 title claims abstract description 36
- 229920003023 plastic Polymers 0.000 title claims abstract description 36
- 239000006185 dispersion Substances 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000002002 slurry Substances 0.000 claims abstract description 56
- 239000002245 particle Substances 0.000 claims abstract description 47
- 238000000034 method Methods 0.000 claims abstract description 38
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 35
- -1 aluminate compound Chemical class 0.000 claims abstract description 33
- 229920001296 polysiloxane Polymers 0.000 claims abstract description 29
- 238000000227 grinding Methods 0.000 claims abstract description 22
- 239000008367 deionised water Substances 0.000 claims abstract description 19
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 19
- 239000007788 liquid Substances 0.000 claims abstract description 18
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 16
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000010410 layer Substances 0.000 claims abstract description 14
- 239000000843 powder Substances 0.000 claims abstract description 14
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 14
- 239000010703 silicon Substances 0.000 claims abstract description 14
- 239000007888 film coating Substances 0.000 claims abstract description 13
- 238000009501 film coating Methods 0.000 claims abstract description 13
- 230000002378 acidificating effect Effects 0.000 claims abstract description 12
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 11
- 239000003513 alkali Substances 0.000 claims abstract description 10
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000001035 drying Methods 0.000 claims abstract description 10
- 238000010438 heat treatment Methods 0.000 claims abstract description 10
- 238000005406 washing Methods 0.000 claims abstract description 10
- 150000007522 mineralic acids Chemical class 0.000 claims abstract description 9
- KRKNYBCHXYNGOX-UHFFFAOYSA-K Citrate Chemical compound [O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O KRKNYBCHXYNGOX-UHFFFAOYSA-K 0.000 claims abstract description 6
- 239000000243 solution Substances 0.000 claims description 82
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 42
- 239000000047 product Substances 0.000 claims description 31
- ZFOZVQLOBQUTQQ-UHFFFAOYSA-N Tributyl citrate Chemical group CCCCOC(=O)CC(O)(C(=O)OCCCC)CC(=O)OCCCC ZFOZVQLOBQUTQQ-UHFFFAOYSA-N 0.000 claims description 24
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 24
- 238000000576 coating method Methods 0.000 claims description 22
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 19
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 claims description 16
- 239000012266 salt solution Substances 0.000 claims description 16
- 229910052593 corundum Inorganic materials 0.000 claims description 14
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 14
- 239000002270 dispersing agent Substances 0.000 claims description 13
- 239000012065 filter cake Substances 0.000 claims description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 8
- 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 claims description 8
- 229910052799 carbon Inorganic materials 0.000 claims description 8
- 229910052708 sodium Inorganic materials 0.000 claims description 8
- 239000011734 sodium Substances 0.000 claims description 8
- 239000007787 solid Substances 0.000 claims description 8
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims description 7
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 6
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 5
- QZCLKYGREBVARF-UHFFFAOYSA-N Acetyl tributyl citrate Chemical compound CCCCOC(=O)CC(C(=O)OCCCC)(OC(C)=O)CC(=O)OCCCC QZCLKYGREBVARF-UHFFFAOYSA-N 0.000 claims description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 4
- 150000004645 aluminates Chemical class 0.000 claims description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 3
- 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 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 2
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical group [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 claims description 2
- 229910019142 PO4 Inorganic materials 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
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims description 2
- WPUINVXKIPAAHK-UHFFFAOYSA-N aluminum;potassium;oxygen(2-) Chemical compound [O-2].[O-2].[Al+3].[K+] WPUINVXKIPAAHK-UHFFFAOYSA-N 0.000 claims description 2
- 229910017604 nitric acid Inorganic materials 0.000 claims description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 2
- 239000010452 phosphate Substances 0.000 claims description 2
- 238000005660 chlorination reaction Methods 0.000 abstract description 7
- 239000000428 dust Substances 0.000 abstract description 7
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 229920000098 polyolefin Polymers 0.000 abstract description 3
- 229920006351 engineering plastic Polymers 0.000 abstract description 2
- 238000001914 filtration Methods 0.000 abstract 1
- 238000004537 pulping Methods 0.000 abstract 1
- 239000004115 Sodium Silicate Substances 0.000 description 21
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 21
- 229910052911 sodium silicate Inorganic materials 0.000 description 21
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 17
- 229910052681 coesite Inorganic materials 0.000 description 16
- 229910052906 cristobalite Inorganic materials 0.000 description 16
- 239000000377 silicon dioxide Substances 0.000 description 16
- 229910052682 stishovite Inorganic materials 0.000 description 16
- 229910052905 tridymite Inorganic materials 0.000 description 16
- 239000011248 coating agent Substances 0.000 description 13
- 230000000052 comparative effect Effects 0.000 description 9
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 8
- 238000012545 processing Methods 0.000 description 6
- 239000011247 coating layer Substances 0.000 description 5
- 239000011347 resin Substances 0.000 description 5
- 229920005989 resin Polymers 0.000 description 5
- 238000004383 yellowing Methods 0.000 description 5
- 229910000329 aluminium sulfate Inorganic materials 0.000 description 4
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Natural products OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
- 230000015556 catabolic process Effects 0.000 description 3
- 239000012141 concentrate Substances 0.000 description 3
- 238000006731 degradation reaction Methods 0.000 description 3
- 238000002845 discoloration Methods 0.000 description 3
- 239000007791 liquid phase Substances 0.000 description 3
- 239000012071 phase Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000012808 vapor phase Substances 0.000 description 2
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 1
- 239000004594 Masterbatch (MB) Substances 0.000 description 1
- 241000519995 Stachys sylvatica Species 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 229910001882 dioxygen Inorganic materials 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 230000005660 hydrophilic surface Effects 0.000 description 1
- 230000005661 hydrophobic surface Effects 0.000 description 1
- 238000001746 injection moulding Methods 0.000 description 1
- 150000002632 lipids Chemical class 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 239000000088 plastic resin Substances 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- XOFYZVNMUHMLCC-ZPOLXVRWSA-N prednisone Chemical compound O=C1C=C[C@]2(C)[C@H]3C(=O)C[C@](C)([C@@](CC4)(O)C(=O)CO)[C@@H]4[C@@H]3CCC2=C1 XOFYZVNMUHMLCC-ZPOLXVRWSA-N 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 229920006268 silicone film Polymers 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 239000001038 titanium pigment Substances 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/36—Compounds of titanium
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
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- C—CHEMISTRY; METALLURGY
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
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- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/36—Compounds of titanium
- C09C1/3607—Titanium dioxide
- C09C1/3615—Physical treatment, e.g. grinding, treatment with ultrasonic vibrations
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- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/36—Compounds of titanium
- C09C1/3607—Titanium dioxide
- C09C1/3615—Physical treatment, e.g. grinding, treatment with ultrasonic vibrations
- C09C1/3623—Grinding
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- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/36—Compounds of titanium
- C09C1/3607—Titanium dioxide
- C09C1/3615—Physical treatment, e.g. grinding, treatment with ultrasonic vibrations
- C09C1/363—Drying, calcination
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- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/36—Compounds of titanium
- C09C1/3607—Titanium dioxide
- C09C1/3653—Treatment with inorganic compounds
- C09C1/3661—Coating
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- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/36—Compounds of titanium
- C09C1/3607—Titanium dioxide
- C09C1/3669—Treatment with low-molecular organic compounds
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- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/36—Compounds of titanium
- C09C1/3607—Titanium dioxide
- C09C1/3676—Treatment with macro-molecular organic compounds
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- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/36—Compounds of titanium
- C09C1/3607—Titanium dioxide
- C09C1/3684—Treatment with organo-silicon compounds
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- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/36—Compounds of titanium
- C09C1/3692—Combinations of treatments provided for in groups C09C1/3615 - C09C1/3684
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/003—Flushing
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/006—Combinations of treatments provided for in groups C09C3/04 - C09C3/12
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/04—Physical treatment, e.g. grinding, treatment with ultrasonic vibrations
- C09C3/041—Grinding
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/04—Physical treatment, e.g. grinding, treatment with ultrasonic vibrations
- C09C3/043—Drying, calcination
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Abstract
一种高耐候、高分散塑料色母二氧化钛颜料的制备方法，采用氯化法工艺生产二氧化钛初品，在脱盐水中打浆，配制成浆料，采用无机酸或碱调pH值，进行分散、研磨处理；对浆料加热升温，加入碱性铝酸盐化合物，同时用无机酸或酸性铝化合物维持pH值恒定，在二氧化钛粒子表面形成无机铝膜包覆层；采用无机碱溶液调pH值，加入含有活性基团聚硅氧烷液体，形成有机硅膜包覆层；用脱离子水过滤、洗涤、干燥；在汽粉工序加入柠檬酸酯类有机处理剂，汽粉处理后获得二氧化钛成品。优点是：该方法制备的二氧化钛颜料具有高耐候性、高白度、高遮盖力及优异的分散加工性能，在生产和使用过程中低粉尘飞扬，环境友好，适应于聚烯烃、工程塑料等高端色母应用领域。
Description
技术领域
本发明涉及化工领域中一种高耐候、高分散塑料色母二氧化钛颜料的制备方法。
背景技术
色母全称叫色母粒，是一种新型高分子材料专用着色剂，亦称颜料制备物。色母主要用在塑料上。色母主要由颜料、载体和添加剂三种基本要素所组成，是把超常量的颜料均匀载附于树脂之中而制得的聚集体，可称颜料浓缩物，着色力高于颜料本身，加工时用少量色母料和未着色树脂掺混，就可达到设计颜料浓度的着色树脂或制品。具有加工方便、制品均匀、易于配色等特点。色母分为纤维用色母、薄膜用色母、电线电缆用色母、聚烯烃色母、PVC色母、注塑制品用色母等。近年来，色母正向着多功能化、高颜料含量和高技术含量方向发展，这就对钛白粉颜料性能提升提出了迫切要求。因此对塑料色母二氧化钛颜料进行表面改性处理，提升钛白粉在应用体系中的分散性能、相融性及加工性能成为了一门广泛的技术。
CN10619716 A公开了“一种超细级金红石型色母专用二氧化钛颜料及其制备方法”，采用硫酸法工艺生产，通过无机液相包膜及有机硅膜气相化包覆(汽粉处理)改性钛白粉性能，主要是通过有机硅气相化包覆解决二氧化钛分散问题，虽对钛白粉在色母应用分散性能有所提升，但因有机硅物质比重小等原因，在汽粉工序中使用有机硅处理剂会产生粉尘飞扬，会对人员安全及环境安全产生不利影响；并且，该方法有机硅膜气相化包覆二氧化钛颜料，在塑料色母高温加工过程中，耐黄变性及耐降解性也会受到一定的影响。
发明内容
本发明要解决的技术问题是提供一种高耐候性、高分散性塑料色母二氧化钛颜料的制备方法，在确保二氧化钛颜料高塑料体系相融性和分散性的前提下，二氧化钛颜料在色母粒高温塑料加工过程中，可保持良好的耐黄变性和耐降解性，二氧化钛颜料具有高耐候性、白度好、偏蓝色底相的特点，且该方法制得的二氧化钛颜料有效解决了粉尘飞扬特性，对产生、运输、应用过程中的人员安全和环境安全具有重要作用。
本发明的技术解决方案是：
一种高耐候、高分散塑料色母二氧化钛颜料的制备方法，其具体步骤为：
1.1、采用氯化法金红石型二氧化钛初品，加入一定量去离子水配制成浓度300g/L～500g/L的二氧化钛浆料，用无机碱溶液调节二氧化钛浆料pH值为4.5～5.5，加入分散剂，所述分散剂的加入量以分散剂有效成分占二氧化钛重量计为0.1％～0.5％，熟化10min～30min；
1.2、将分散的二氧化钛浆料进行研磨处理，并从水浆中除去研磨介质；
1.3、将研磨后的浆料加热升温至40℃～80℃，并在整个包覆过程维持此温度；
1.4、在30min～120min内加入0.5％～3.0％碱性铝酸盐溶液，加入量以氧化铝占二氧化钛重量计；并用无机酸或酸性铝盐溶液维持浆料pH值4.0～6.0，熟化30min～60min，形成致密铝膜第一包膜层；
1.5、继续加入无机碱溶液，调节pH值至6.5～7.5，熟化10min～30min；
1.6、在30min～120min加入聚硅氧烷液体，所述聚硅氧烷具有羟基活性基团或羧基活性基团，熟化30min～60min，形成聚合硅膜包覆层；
1.7、将上述溶液用70℃～90℃去离子水洗至滤饼电导率大于15000Ω·cm，干燥处理；
1.8、在汽粉工序加入柠檬酸酯类有机处理剂，制得塑料色母用二氧化钛颜料。
进一步的，1.1中所述分散剂为硅酸盐分散剂或磷酸盐分散剂。
进一步的，1.4中所述碱性铝盐溶液为偏铝酸钠溶液或偏铝酸钾溶液；碱性铝盐溶液浓度以Al2O3计为100g/L～200g/L。
进一步的，1.4中酸性铝盐溶液为硫酸铝溶液、三氯化铝溶液、硝酸铝溶液中一种；酸性铝盐溶液浓度以Al2O3计为60g/L～120g/L。
进一步的，1.4中所述无机酸为盐酸、硫酸、硝酸、磷酸中一种；无机酸质量浓度为10％～30％。
进一步的，1.1和1.5中的无机碱溶液为氢氧化钠溶液或氢氧化钾溶液，无机碱溶液质量浓度为10％～30％。
进一步的，所述聚硅氧烷液体加入量以聚硅氧烷固含量占二氧化钛重量0.5％～1.5％。
进一步的，1.8中柠檬酸酯类有机处理剂为柠檬酸三丁酯或乙酰柠檬酸三丁酯，柠檬酸酯类有机处理剂加入量为碳含量占二氧化钛重量0.1％～1.0％。
进一步的，所述二氧化钛初品中金红石含量99.5％以上，D50粒径为0.20μm～0.28μm。
进一步的，步骤1.2研磨处理后，二氧化钛D50粒径为280nm～287nm，粒径超过500nm的粒子＜5.5％。
与现有技术相比，本发明的有益效果是：
(1)以氯化法金红石型二氧化钛氧化初品作为制备目标产物的原料，具有粒子接近球型比例高、粒径小、粒度分布窄的特点。
(2)采用适当的包覆层组合，其中采用碱性铝盐溶液和无机酸或酸性铝盐溶液，通过控制和调整pH值，形成致密铝膜第一包膜层，有效弥补了二氧化钛的光化学活性点，提高抗变色性能；向钛白粉浆料中加入聚硅氧烷纯液或乳液，通过羟基或羧基基团与第一包覆层表面羟基等基团，形成聚合硅膜第二包覆层。有机硅膜的液相化包覆相比于气相化包覆膜层更加均匀、完整，并通过化学键合在钛白粉表面，形成的包覆层牢固，在提高产品耐候性的前提下，降低了无机氧化硅膜液相包覆结晶水含量高的特点。
(3)在汽粉工序引入具有耐高温的柠檬酸酯类有机剂，不仅起到助磨剂作用，关键在于脂类分散剂随蒸汽引入包覆在二氧化钛颗粒表面，有效改善了钛白粉与塑料树脂的相融性。
(4)该方法在传统的氧化铝包覆基础上，通过具有活性基团化学键合包覆致密有机硅膜，可最大限度减少羟基结合水含量，并将二氧化钛的亲水表面转换为疏水表面，降低吸附水含量，从根本上解决了结合水在高温塑料加工过程中的耐黄变及耐降解性能的影响；采用酯类处理剂作为外层有机包覆层，解决了钛白粉粉尘飞扬问题，并进一步加强钛白粉与树脂的相融性，提升钛白粉的体系分散性及加工性能。有效避免因体系不相融及分散不佳出现的白点、斑块等制品不合格现象。获得的产品具有高耐候、高白度，具有高塑料体系相融性和分散性，确保了塑料制品优异的加工性能和力学性能。
具体实施方式
下面结合具体实施方式对本发明做进一步描述，但本发明的应用范围应用不仅仅局限于实施例，在不脱离本发明技术思想的前提下，做出的各种替换和变更，均应在本发明的范围内。
实施例1
1.1、采用氯化法金红石型二氧化钛初品，加入一定量去离子水配制成浓度300g/L的二氧化钛浆料，所述二氧化钛初品中金红石含量99.5％，D50粒径为0.20μm；用质量浓度为30％的氢氧化钠溶液调节二氧化钛浆料pH值为4.5，加入0.1％硅酸钠溶液(硅酸钠溶液加入量以SiO2占TiO2重量计)，硅酸钠溶液以SiO2计为150g/L，熟化10min；
1.2、将分散的二氧化钛浆料进行研磨处理，D50粒径为280nm，超过500nm粒径粒子小于5.0％，从水浆中除去研磨介质；
1.3、将研磨后的浆料加热升温至40℃，并在整个包覆过程维持此温度；
1.4、在30min内加入0.5％NaAlO2溶液(加入量以氧化铝占二氧化钛重量计)，偏铝酸钠溶液浓度以Al2O3计为200g/L；并用Al2(SO4)3溶液维持浆料pH值4.0，酸性铝盐溶液浓度以Al2O3计为100g/L，熟化30min，形成致密铝膜第一包膜层；
1.5、加入质量浓度为30％的NaOH溶液，调节pH值至6.5，熟化10min；
1.6、在30min加入0.5％羟基聚硅氧烷液体(羟基聚硅氧烷液体加入量以羟基聚硅氧烷固含量占二氧化钛重量计)，熟化30min；
1.7、将上述溶液用70℃去离子水洗至滤饼电导率16000Ω·cm，干燥处理；
1.8、在汽粉工序加入柠檬酸三丁酯有机处理剂(柠檬酸三丁酯加入量为碳含量占二氧化钛重量1.0％)，制得塑料色母用二氧化钛颜料。
实施例2
1.1、采用氯化法金红石型二氧化钛初品，加入一定量去离子水配制成浓度500g/L的二氧化钛浆料，所述二氧化钛初品中金红石含量99.7％，D50粒径为0.28μm；用质量浓度为10％的氢氧化钠溶液调节二氧化钛浆料pH值为5.5，加入0.5％硅酸钠溶液(硅酸钠溶液加入量以SiO2占TiO2重量计)，硅酸钠溶液以SiO2计为150g/L，熟化30min；
1.2、将分散的二氧化钛浆料进行研磨处理，D50粒径为287nm，超过500nm粒径粒子小于5.3％，从水浆中除去研磨介质；
1.3、将研磨后的浆料加热升温至80℃，并在整个包覆过程维持此温度；
1.4、在30min内加入3.0％NaAlO2溶液(加入量以氧化铝占二氧化钛重量计)，偏铝酸钠溶液浓度以Al2O3计为100g/L；并用质量浓度15％HCI溶液维持浆料pH值6.0，熟化60min，形成致密铝膜第一包膜层；
1.5、加入质量浓度为10％的KOH溶液，调节pH值至7.5，熟化30min；
1.6、在120min加入1.5％羧基聚硅氧烷液体(羧基聚硅氧烷液体加入量以羧基聚硅氧烷固含量占二氧化钛重量计)，熟化60min；
1.7、将上述溶液用90℃去离子水洗至滤饼电导率17000Ω·cm，干燥处理；
1.8、在汽粉工序加入乙酰柠檬酸三丁酯有机处理剂(乙酰柠檬酸三丁酯加入量为碳含量占二氧化钛重量1.0％)，制得塑料色母用二氧化钛颜料。
实施例3
1.1、采用氯化法金红石型二氧化钛初品，加入一定量去离子水配制成浓度400g/L的二氧化钛浆料，所述二氧化钛初品中金红石含量99.9％，D50粒径为0.25μm；用质量浓度为20％的氢氧化钠溶液调节二氧化钛浆料pH值为5.0，加入0.3％硅酸钠溶液(硅酸钠溶液加入量以SiO2占TiO2重量计)，硅酸钠溶液以SiO2计为150g/L，熟化20min；
1.2、将分散的二氧化钛浆料进行研磨处理，D50粒径为285nm，超过500nm粒径粒子小于5.5％，从水浆中除去研磨介质；
1.3、将研磨后的浆料加热升温至60℃，并在整个包覆过程维持此温度；
1.4、在120min内加入2.0％NaAlO2溶液(加入量以氧化铝占二氧化钛重量计)，偏铝酸钠溶液浓度以Al2O3计为150g/L；并用质量浓度30％H2SO4溶液维持浆料pH值5.0，熟化40min，形成致密铝膜第一包膜层；
1.5、加入质量浓度为20％的NaOH溶液，调节pH值至7.0，熟化20min；
1.6、在30min加入1.0％端羟基聚硅氧烷液体(加入量以端羟基聚硅氧烷固含量占二氧化钛重量)，熟化40min；
1.7、将上述溶液用80℃去离子水洗至滤饼电导率15600Ω·cm，干燥处理；
1.8、在汽粉工序加入柠檬酸三丁酯有机处理剂(柠檬酸三丁酯加入量为碳含量占二氧化钛重量1.0％)，制得塑料色母用二氧化钛颜料。
对比例1重复实施例1的无机处理步骤，取消第一层无机氧化铝包膜工序。
1.1、采用氯化法金红石型二氧化钛初品，加入一定量去离子水配制成浓度300g/L的二氧化钛浆料，所述二氧化钛初品中金红石含量99.5％，D50粒径为0.20μm；用质量浓度为30％的氢氧化钠溶液调节二氧化钛浆料pH值为4.5，加入0.1％硅酸钠溶液(硅酸钠溶液加入量以SiO2占TiO2重量计)，硅酸钠溶液以SiO2计为150g/L，熟化10min；
1.2、将分散的二氧化钛浆料进行研磨处理，D50粒径为280nm，超过500nm粒径粒子小于5.0％，从水浆中除去研磨介质；
1.3、将研磨后的浆料加热升温至40℃，并在整个包覆过程维持此温度；
1.4、加入质量浓度为30％的NaOH溶液，调节pH值至6.5，熟化10min；
1.5、在30min加入0.5％羟基聚硅氧烷液体(羟基聚硅氧烷液体加入量以羟基聚硅氧烷固含量占二氧化钛重量)，熟化30min；
1.6、将上述溶液用70℃去离子水洗至滤饼电导率16000Ω·cm，干燥处理；
1.7、在汽粉工序加入柠檬酸三丁酯有机处理剂(柠檬酸三丁酯加入量为碳含量占二氧化钛重量1.0％)，制得二氧化钛颜料。
对比例2重复实施例1的无机处理步骤，取消1.6步骤第二层有机硅膜包膜工序。
1.1、采用氯化法金红石型二氧化钛初品，加入一定量去离子水配制成浓度300g/L的二氧化钛浆料，所述二氧化钛初品中金红石含量99.5％，D50粒径为0.20μm；用质量浓度为30％的氢氧化钠溶液调节二氧化钛浆料pH值为4.5，加入0.1％硅酸钠溶液(硅酸钠溶液加入量以SiO2占TiO2重量计)，硅酸钠溶液以SiO2计为150g/L，熟化10min；
1.2、将分散的二氧化钛浆料进行研磨处理，D50粒径为280nm，超过500nm粒径粒子小于5.0％，从水浆中除去研磨介质；
1.3、将研磨后的浆料加热升温至40℃，并在整个包覆过程维持此温度；
1.4、在30min内加入0.5％NaAlO2溶液(加入量以氧化铝占二氧化钛重量计)，偏铝酸钠溶液浓度以Al2O3计为200g/L；并用Al2(SO4)3溶液维持浆料pH值4.0，酸性铝盐溶液浓度以Al2O3计为100g/L，熟化30min，形成致密铝膜第一包膜层；
1.5、将上述溶液用70℃去离子水洗至滤饼电导率16000Ω·cm，干燥处理；
1.6、在汽粉工序加入柠檬酸三丁酯有机处理剂(柠檬酸三丁酯加入量为碳含量占二氧化钛重量1.0％)，制得塑料色母用二氧化钛颜料。
对比例3重复实施例1的无机处理步骤，将1.6步骤中羟基聚硅氧烷液体变为硅酸钠溶液，加入量以SiO2占TiO2重量计1.0％，浓度以SiO2计为150g/L。
1.1、采用氯化法金红石型二氧化钛初品，加入一定量去离子水配制成浓度300g/L的二氧化钛浆料，所述二氧化钛初品中金红石含量99.5％，D50粒径为0.20μm；用质量浓度为30％的氢氧化钠溶液调节二氧化钛浆料pH值为4.5，加入0.1％硅酸钠溶液(硅酸钠溶液加入量以SiO2占TiO2重量计)，硅酸钠溶液以SiO2计为150g/L，熟化10min；
1.2、将分散的二氧化钛浆料进行研磨处理，D50粒径为280nm，超过500nm粒径粒子小于5.0％，从水浆中除去研磨介质；
1.3、将研磨后的浆料加热升温至40℃，并在整个包覆过程维持此温度；
1.4、在30min内加入0.5％NaAlO2溶液(加入量以氧化铝占二氧化钛重量计)，偏铝酸钠溶液浓度以Al2O3计为200g/L；并用Al2(SO4)3溶液维持浆料pH值4.0，酸性铝盐溶液浓度以Al2O3计为100g/L，熟化30min，形成致密铝膜第一包膜层；
1.5、加入质量浓度为30％的NaOH溶液，调节pH值至6.5，熟化10min；
1.6、在30min加入0.5％羟基聚硅氧烷液体(羟基聚硅氧烷液体加入量以羟基聚硅氧烷固含量占二氧化钛重量)，熟化30min；
1.7、将上述溶液用70℃去离子水洗至滤饼电导率16000Ω·cm，干燥处理；
1.8、在汽粉工序加入柠檬酸三丁酯有机处理剂(柠檬酸三丁酯加入量为碳含量占二氧化钛重量1.0％)，制得塑料色母用二氧化钛颜料。
对比例4重复实施例1的无机处理步骤，取消1.8步骤外层有机包膜工序。
1.1、采用氯化法金红石型二氧化钛初品，加入一定量去离子水配制成浓度300g/L的二氧化钛浆料，所述二氧化钛初品中金红石含量99.5％，D50粒径为0.20μm；用质量浓度为30％的氢氧化钠溶液调节二氧化钛浆料pH值为4.5，加入0.1％硅酸钠溶液(硅酸钠溶液加入量以SiO2占TiO2重量计)，硅酸钠溶液以SiO2计为150g/L，熟化10min；
1.2、将分散的二氧化钛浆料进行研磨处理，D50粒径为280nm，超过500nm粒径粒子小于5.0％，从水浆中除去研磨介质；
1.3、将研磨后的浆料加热升温至40℃，并在整个包覆过程维持此温度；
1.4、在30min内加入0.5％NaAlO2溶液(加入量以氧化铝占二氧化钛重量计)，偏铝酸钠溶液浓度以Al2O3计为200g/L；并用Al2(SO4)3溶液维持浆料pH值4.0，酸性铝盐溶液浓度以Al2O3计为100g/L，熟化30min，形成致密铝膜第一包膜层；
1.5、加入质量浓度为30％的NaOH溶液，调节pH值至6.5，熟化10min；
1.6、在30min加入0.5％羟基聚硅氧烷液体(羟基聚硅氧烷液体加入量以羟基聚硅氧烷固含量占二氧化钛重量)，熟化30min；
1.7、将上述溶液用70℃去离子水洗至滤饼电导率16000Ω·cm，干燥，汽粉处理，制得塑料色母用二氧化钛颜料。
本发明实施例中使用的聚硅氧烷具有羧基反应活性基团或羟基反应活性基团，通过羧基/羟基反应活性基团与第一包覆层表面羟基等基团，形成包膜。
将实施例1～实施例3、对比例1～对比例4制备的二氧化钛颜料进行塑料体系应用性能测试，检测结果如表1所示。
备注：耐候性ΔE检测是制备标准塑料板在氙灯老化箱(UVA)灯照射240h的结果；黄变指数240h(△E)是制备标准塑料板在氙灯老化箱(UVA)灯照射240h的结果；拉伸强度、冲击强度是60％ABS母粒制备塑料板测试数值，粉尘飞扬情况；是长期工作在生产一线人员对粉尘飞扬情况的判断。
由表1可以看出：实施例1～实施例3制得的产品的分散性、耐候性、抗变色性及材料力学性能得到显著提升，各项指标性能优异。对比例1未进行氧化铝包覆，产品的抗黄变性能差；对比例2未进行有机硅膜包覆，产品的滤压值分散性及耐候性能差，由于分散不充分，导致制品的材料性能差；对比例3采用无机硅替代有机硅包覆，由于多结合水及吸附水存在，各种指标不理想；对比例4，未进行外层有机包覆，钛白粉粉尘飞扬严重，环境不友好。并且因与应用树脂的相融性不足，导致材料的分散及力学性能下降。
综上所述，按照本发明生产的二氧化钛颜料具有高分散性、高耐候及抗变色性和优异的材料加工性能和力学性能，适合于聚烯烃、工程塑料等高端色母应用领域。
以上仅为本发明的具体实施例而已，并不仅限制本发明，对于本领域的技术人员来说，本发明可以有各种更改和变化。凡在本发明的精神和原则之内，所作的任何修改、等同替换、改进等，均应包含在本发明的保护范围之内。
Claims (10)
1.一种高耐候、高分散塑料色母二氧化钛颜料的制备方法，其特征在于：
1.1、采用氯化法金红石型二氧化钛初品，加入一定量去离子水配制成浓度300g/L～500g/L的二氧化钛浆料，用无机碱溶液调节二氧化钛浆料pH值为4.5～5.5，加入分散剂，所述分散剂的加入量以分散剂有效成分占二氧化钛重量计为0.1％～0.5％，熟化10min～30min；
1.2、将分散的二氧化钛浆料进行研磨处理，并从水浆中除去研磨介质；
1.3、将研磨后的浆料加热升温至40℃～80℃，并在整个包覆过程维持此温度；
1.4、在30min～120min内加入0.5％～3.0％碱性铝酸盐溶液，加入量以氧化铝占二氧化钛重量计；并用无机酸或酸性铝盐溶液维持浆料pH值4.0～6.0，熟化30min～60min，形成致密铝膜第一包膜层；
1.5、继续加入无机碱溶液，调节pH值至6.5～7.5，熟化10min～30min；
1.6、在30min～120min加入聚硅氧烷液体，所述聚硅氧烷具有羟基活性基团或羧基活性基团，熟化30min～60min，形成聚合硅膜包覆层；
1.7、将上述溶液用70℃～90℃去离子水洗至滤饼电导率大于15000Ω·cm，干燥处理；
1.8、在汽粉工序加入柠檬酸酯类有机处理剂，制得塑料色母用二氧化钛颜料。
2.根据权利要求1所述的一种高耐候、高分散塑料色母二氧化钛颜料的制备方法，其特征在于：1.1中所述分散剂为硅酸盐分散剂或磷酸盐分散剂。
3.根据权利要求1所述的一种高耐候、高分散塑料色母二氧化钛颜料的制备方法，其特征在于：1.4中所述碱性铝盐溶液为偏铝酸钠溶液或偏铝酸钾溶液；碱性铝盐溶液浓度以Al2O3计为100g/L～200g/L。
4.根据权利要求1所述的一种高耐候、高分散塑料色母二氧化钛颜料的制备方法，其特征在于：1.4中酸性铝盐溶液为硫酸铝溶液、三氯化铝溶液、硝酸铝溶液中一种；酸性铝盐溶液浓度以Al2O3计为60g/L～120g/L。
5.根据权利要求1所述的一种高耐候、高分散塑料色母二氧化钛颜料的制备方法，其特征在于：1.4中所述无机酸为盐酸、硫酸、硝酸、磷酸中一种；无机酸质量浓度为10％～30％。
6.根据权利要求1所述的一种高耐候、高分散塑料色母二氧化钛颜料的的制备方法，其特征在于：1.1和1.5中的无机碱溶液为氢氧化钠溶液或氢氧化钾溶液，无机碱溶液质量浓度为10％～30％。
7.根据权利要求1所述的一种高耐候、高分散塑料色母二氧化钛颜料的制备方法，其特征在于：所述聚硅氧烷液体加入量以聚硅氧烷固含量占二氧化钛重量0.5％～1.5％。
8.根据权利要求1所述的一种高耐候、高分散塑料色母二氧化钛颜料的制备方法，其特征在于：1.8中柠檬酸酯类有机处理剂为柠檬酸三丁酯或乙酰柠檬酸三丁酯，柠檬酸酯类有机处理剂加入量为碳含量占二氧化钛重量0.1％～1.0％。
9.根据权利要求1所述的一种高耐候、高分散塑料色母二氧化钛颜料的制备方法，其特征在于：所述二氧化钛初品中金红石含量99.5％以上，D50粒径为0.20μm～0.28μm。
10.根据权利要求1所述的一种高耐候、高分散塑料色母二氧化钛颜料的制备方法，其特征在于：步骤1.2研磨处理后，二氧化钛D50粒径为280nm～287nm，粒径超过500nm的粒子＜5.5％。
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