CN114539815A - 一种高遮盖高分散性改性微硅粉及其制备方法 - Google Patents
一种高遮盖高分散性改性微硅粉及其制备方法 Download PDFInfo
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- CN114539815A CN114539815A CN202210192476.4A CN202210192476A CN114539815A CN 114539815 A CN114539815 A CN 114539815A CN 202210192476 A CN202210192476 A CN 202210192476A CN 114539815 A CN114539815 A CN 114539815A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims description 71
- 239000011863 silicon-based powder Substances 0.000 title claims description 69
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical class O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 37
- 238000000576 coating method Methods 0.000 claims abstract description 36
- 239000011248 coating agent Substances 0.000 claims abstract description 34
- 239000002245 particle Substances 0.000 claims abstract description 34
- 229910021487 silica fume Inorganic materials 0.000 claims abstract description 31
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 27
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 27
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 17
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 17
- 239000010936 titanium Substances 0.000 claims abstract description 17
- 239000002994 raw material Substances 0.000 claims abstract description 12
- 239000002002 slurry Substances 0.000 claims description 42
- 239000000463 material Substances 0.000 claims description 25
- 238000003756 stirring Methods 0.000 claims description 17
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 claims description 17
- 239000004576 sand Substances 0.000 claims description 16
- 239000000243 solution Substances 0.000 claims description 15
- 239000007864 aqueous solution Substances 0.000 claims description 14
- QXJQHYBHAIHNGG-UHFFFAOYSA-N trimethylolethane Chemical compound OCC(C)(CO)CO QXJQHYBHAIHNGG-UHFFFAOYSA-N 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 13
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- 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 10
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 9
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- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical compound [Na]OP1(=O)OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])O1 GCLGEJMYGQKIIW-UHFFFAOYSA-H 0.000 claims description 7
- 235000019982 sodium hexametaphosphate Nutrition 0.000 claims description 7
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 claims description 7
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
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- 238000009501 film coating Methods 0.000 claims description 6
- ZJCCRDAZUWHFQH-UHFFFAOYSA-N Trimethylolpropane Chemical compound CCC(CO)(CO)CO ZJCCRDAZUWHFQH-UHFFFAOYSA-N 0.000 claims description 4
- 238000010902 jet-milling Methods 0.000 claims description 4
- 238000003801 milling Methods 0.000 claims description 4
- HXKKHQJGJAFBHI-UHFFFAOYSA-N 1-aminopropan-2-ol Chemical compound CC(O)CN HXKKHQJGJAFBHI-UHFFFAOYSA-N 0.000 claims description 3
- 239000004115 Sodium Silicate Substances 0.000 claims description 3
- 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 3
- 150000007942 carboxylates Chemical class 0.000 claims description 3
- 229940102253 isopropanolamine Drugs 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 3
- 229910052911 sodium silicate Inorganic materials 0.000 claims description 3
- 239000007785 strong electrolyte Substances 0.000 claims description 3
- 239000011164 primary particle Substances 0.000 claims description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 abstract description 36
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- -1 lithopone Chemical compound 0.000 abstract description 4
- 239000000049 pigment Substances 0.000 abstract description 4
- 239000002537 cosmetic Substances 0.000 abstract description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 abstract 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 abstract 1
- GHPGOEFPKIHBNM-UHFFFAOYSA-N antimony(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Sb+3].[Sb+3] GHPGOEFPKIHBNM-UHFFFAOYSA-N 0.000 abstract 1
- 235000014692 zinc oxide Nutrition 0.000 abstract 1
- 239000011787 zinc oxide Substances 0.000 abstract 1
- 229910052726 zirconium Inorganic materials 0.000 abstract 1
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 15
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 13
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- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 239000000428 dust Substances 0.000 description 3
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- 229910052710 silicon Inorganic materials 0.000 description 3
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- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 2
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- 229910000519 Ferrosilicon Inorganic materials 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 238000003723 Smelting Methods 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
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- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 2
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- 238000005303 weighing Methods 0.000 description 2
- 229910001021 Ferroalloy Inorganic materials 0.000 description 1
- KKCBUQHMOMHUOY-UHFFFAOYSA-N Na2O Inorganic materials [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
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- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
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- C09C1/30—Silicic acid
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- C08K3/36—Silica
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Abstract
本发明公开了一种高遮盖高分散性改性微硅粉及其制备方法。所述的高遮盖高分散性改性微硅粉的遮盖力为70%以上,分散性能为35微米以下,是以微硅粉颗粒为原料,经前处理、钛包膜、铝包膜和后处理步骤制备得到。制备方法包括前处理、锆包膜、铝包膜和后处理步骤。本发明所述的高遮盖高分散性改性微硅粉适用于普通涂料、汽车底漆、化妆品领域的钛白粉的遮盖率为70%以上,分散性能为35微米以下,改性后的微硅粉根据适用领域的要求不同全部或部分替代钛白粉、锌白、立德粉、锑白、铅白等颜料。
Description
技术领域
本发明属于冶金技术领域,具体涉及一种高遮盖高分散性改性微硅粉及其制备方法。
背景技术
微硅粉是铁合金在冶炼硅铁和工业硅(金属硅)时,矿热电炉内产生出大量挥发性很强的SiO2和Si气体,气体排空后与空气迅速氧化冷凝沉淀,经收尘器收集得到的工业粉尘。该工业粉尘主要含SiO2,夹带着K2O、Na2O、Ca、F2O3、Al2O3等杂质。微硅粉目前可以广泛地应用于混凝土、冶金球团助剂、耐火材料、水泥材料等领域,但应用的产品附加值不高,微硅粉基本属于固体废弃物被迫消耗。云南某地生产工业硅及硅铁时产生大量的微硅粉,年累计产生微硅粉2万多吨,由于微硅粉价格低廉,厂址地理位置偏僻,微硅粉没有市场,几乎成为废弃物,即占地又污染环境。
微硅粉粒径通常在0.2-5μm之间,适用于涂料、塑料、造纸、橡胶等颜填料领域,但直接将工业生产的微硅粉用于涂料、塑料、造纸、橡胶等领域会出现低遮盖力和分散性差的问题。因此研究微硅粉的改性高值化利用具有重要意义。
钛白粉是一种重要的无机化工颜料,主要成分为二氧化钛。在涂料、油墨、造纸、塑料橡胶、化纤、陶瓷等工业中有重要用途,但钛白粉价格较为昂贵,如在生产涂料使用时往往仅做为颜料部分添加。若能将微硅粉表面改性后全部或部分替代钛白粉使用,不仅能够大幅降低产品成本,也能改变微硅粉目前固体废弃物的处境。
发明内容
针对现有微硅粉处理技术和生产技术中的不足,本发明提供了一种包膜微硅粉的制备方法,具体为高遮盖高分散包膜改性微硅粉的制备方法,能有效提高微硅粉在涂料、塑料、橡胶等领域的树脂体系下的高遮盖性能。
本发明的第一目的在于提供一种高遮盖高分散性改性微硅粉;第二目的在于提供所述的高遮盖高分散性改性微硅粉的制备方法。
本发明的第一目的是这样实现的,所述的高遮盖高分散性改性微硅粉的遮盖力为70%以上,分散性能为35微米以下,是以微硅粉颗粒为原料,经前处理、钛包膜、铝包膜和后处理步骤制备得到。
本发明的第二目的是这样实现的,包括前处理、钛包膜、铝包膜和后处理步骤,具备包括:
A、前处理:
1)微硅粉浆料制备:将原料微硅粉颗粒加入到脱盐水中制备成浆料,调节浆料pH值为6.5~9,加入分散剂搅拌均匀得到浆料a;
2)砂磨分散:将浆料a置于砂磨机中使微硅粉颗粒的团聚体完全分散,呈现原级粒子状态得到物料b;
B、钛包膜:将物料b升温至25~60℃后加入四氯化钛水溶液,持续搅拌,用碱溶液在10~180min内缓慢调节pH值至5.0~12.5后,熟化15~60min即完成钛膜包覆得到物料c;
C、铝包膜:将物料c中顺流加入含铝化合物,加入时间控制在10~120min内,再持续搅拌10~30min后,用酸或碱溶液在30-120min内缓慢调节pH值至6.5~9.0后,熟化15~60min即完成铝膜包覆得到物料d;
D、后处理:
1)将物料d经压滤、洗涤去除可溶性盐得到滤饼e,将滤饼e将干燥粉碎得到粉末f;
2)将粉末f进行气流粉碎,同时加入三羟甲基丙烷得到目标物高遮盖高分散性改性微硅粉。
具体操作方法如下:
a.微硅粉浆料制备:将微硅粉颗粒加入脱盐水中制备成浆料,调节浆pH值至6.5-9和加入分散剂。所述脱盐水是将所含易于除去的强电解质除去或减少到一定程度的水,剩余含盐量应在1~5 毫克/升之间。
b.砂磨分散:将步骤a所得到的浆料放到砂磨机中,控制转速和砂磨时间,使微硅粉颗粒的团聚体完全分散,呈现原级粒子状态。
c.钛包膜:将物料b升温至25~60℃后加入四氯化钛水溶液,持续搅拌,用碱溶液在10~180min内缓慢调节pH值至5.0~12.5后,熟化15~60min即完成钛膜包覆得到物料c;钛膜包覆完毕,在微硅粉颗粒表面上包覆不定型的水合二氧化钛。包裹钛膜后的微硅粉具备了遮盖性能,具体性能体现在实施例中。
d. 铝包膜:将物料c中顺流加入含铝化合物,加入时间控制在10~120min内,再持续搅拌10~30min后,用酸或碱溶液在30-120min内缓慢调节pH值至6.5~9.0后,熟化15~60min即完成铝膜包覆得到物料d,铝膜包覆完毕;这是在微硅粉颗粒表面上包覆复合型水合铝膜。包裹铝膜后的微硅粉具备了分散性能,具体性能体现在实施例中。
e.压滤、洗涤、干燥:将步骤d所得的浆料压滤、洗涤,去除浆料中的可溶性盐,使滤饼的电阻率≥80Ω·m,将滤饼在85℃~350℃下干燥,粉碎成粉末。
f.有机包膜及粉碎:将步骤e所得到的微硅粉粉末进行汽流粉碎,同时加入三羟甲基乙烷(TME),得到最终产品。进一步提高包膜微硅粉的润湿分散性能。
上述步骤a中的微硅粉基料浆料浓度为250 g/L~500g/L。
上述步骤a中的分散剂为六偏磷酸钠、硅酸钠、羧酸盐、异丙醇胺的一种或几种组合加入,分散剂添加量为微硅粉含量的1‰~9‰。
上述步骤b中砂磨机的转速制在300 ~2000r/min,砂磨时间为3min~20min。
上述步骤b中砂磨分散后微硅粉颗粒的粒度分布D(50)控制0.30μm~0.60μm。
上述步骤c中四氯化钛水溶液的浓度为80g/L~140g/L(以TiO2计),加入量为微硅粉质量的10%~25%(以TiO2计)。
上述步骤c中加入含四氯化钛水溶液和碱的搅拌速度为250r/min~400 r/min。
上述步骤d中含铝化合物为硫酸铝和偏铝酸钠等,其浓度为50g/L~280g/L(以Al2O3计),加入量为微硅粉质量的0.5%~5%(以Al2O3计)。
上述步骤d中加入含铝化合物和酸或碱的搅拌速度为250r/min~400 r/min。
上述步骤e中压滤设备为隔膜压滤机和转鼓过滤机等,滤饼固含量≥65%。
上述步骤e中干燥设备为箱式干燥箱和闪蒸干燥器,干燥后水分含量≤0.2%。
上述步骤f中汽流粉碎的载体为过热蒸汽、压缩空气、压缩氮气等。
上述步骤f中三羟甲基乙烷(TME)加入量为微硅粉质量的1~5‰,加入方式为汽流粉碎机的入口或出口。
本发明中用于调节浆料pH的主要为酸或碱,包括浓硫酸(浓度质量分数为98%)、50%硫酸、20%硫酸、盐酸(质量分数为36.5%)、柠檬酸(质量分数为50%、20%、10%)、氢氧化钠(质量分数为20%、10%)、碳酸钠(质量分数为20%、10%)等。
本发明的有益效果:
(1)本发明制备的微硅粉表面包覆活性水合二氧化钛、复合型水合氧化铝膜和有机膜。活性水合二氧化钛大大提高微硅粉的遮盖力,同时少量的混合型水合氧化铝膜和有机膜有助于提高微硅粉在树脂中的分散性能。
(2)根据适用领域不同,钛白粉的价格在2~4万元/吨。微硅粉粒径形貌与钛白粉类似,化学性质稳定,但微硅粉成本低廉,仅200-300元/吨。经本工艺表面改性后的微硅粉产业化后的成本在2000~3000元/吨,替代钛白粉后能够大幅降低后续产品成本。
(3)本发明制备的高遮盖高分散性改性微硅粉的遮盖力能够达到92.36%,同时分散性能够达到25微米。适用于普通涂料、汽车漆面、化妆品领域的钛白粉的遮盖率为90%以上,分散性能为30微米以下,改性后的微硅粉根据适用领域的要求不同全部或部分替代钛白,可以达到相同的效果。
(4)工艺流程简单,容易实现产业化。
附图说明
图1为本发明高遮盖高分散性改性微硅粉制备方法工艺流程示意图;
图2为本发明实施例1制备得到的高遮盖高分散性改性微硅粉的TEM(透射电镜)图谱示意图。
具体实施方式
下面结合实施例和附图对本发明作进一步的说明,但不以任何方式对本发明加以限制,基于本发明教导所作的任何变换或替换,均属于本发明的保护范围。
本发明所述的高遮盖高分散性改性微硅粉的遮盖力为70%以上,分散性能为35微米以下,是以微硅粉颗粒为原料,经前处理、钛包膜、铝包膜和后处理步骤制备得到。
本发明所述的高遮盖高分散性改性微硅粉的制备方法,包括前处理、钛包膜、铝包膜和后处理步骤,具备包括:
A、前处理:
1)微硅粉浆料制备:将原料微硅粉颗粒加入到脱盐水中制备成浆料,调节浆料pH值为6.5~9,加入分散剂搅拌均匀得到浆料a;
2)砂磨分散:将浆料a置于砂磨机中使微硅粉颗粒的团聚体完全分散,呈现原级粒子状态得到物料b;
B、钛包膜:将物料b升温至25~60℃后加入四氯化钛水溶液,持续搅拌,用碱溶液在10~180min内缓慢调节pH值至5.0~12.5后,熟化15~60min即完成钛膜包覆得到物料c;
C、铝包膜:将物料c中顺流加入含铝化合物,加入时间控制在10~120min内,再持续搅拌10~30min后,用酸或碱溶液在30-120min内缓慢调节pH值至6.5~9.0后,熟化15~60min即完成铝膜包覆得到物料d;
D、后处理:
1)将物料d经压滤、洗涤去除可溶性盐得到滤饼e,将滤饼e将干燥粉碎得到粉末f;
2)将粉末f进行气流粉碎,同时加入三羟甲基丙烷得到目标物高遮盖高分散性改性微硅粉。
A步骤1)中所述的脱盐水是将所含易于除去的强电解质除去或减少到一定程度的水,剩余含盐量在1~5mg/L。
A步骤1)中所述的分散剂为六偏磷酸钠、硅酸钠、羧酸盐和异丙醇胺中的一种或几种,添加量为原料微硅粉颗粒质量的1~9‰。
A步骤1)中浆料a 的浓度为250~500g/L。
A步骤2)中所述的砂磨机的转速控制在300~2000r/min,砂磨时间为3~20min。
B步骤中所述的四氯化钛水溶液的浓度为80~140g/L,加入量为原料微硅粉颗粒质量的10~25%。
C步骤中所述的含铝化合物为硫酸铝或偏铝酸钠,含铝化合物的浓度以Al2O3计为50~280g/L,加入量为原料微硅粉颗粒质量的0.5~5%。
D步骤2)中气流粉碎的载体为过热蒸汽、压缩空气或压缩氮气。
D步骤2)中三羟甲基丙烷的加入量为原料微硅粉颗粒质量的1~5‰,加入方式为气流粉碎机的入口或出口。
下面以具体实施案例对本发明做进一步说明:
实施例1
配制浓度为350g/L的微硅粉浆料1L,加入2‰的六偏磷酸钠(以P2O5计),采用砂磨机分散10min,转数控制在1200r/min,置于粉体改性反应釜中加热并搅拌至30℃,30min缓慢添加浓度为100g/L的四氯化钛水溶液,四氯化钛水溶液的总量以TiO2计为微硅粉的10%,60min缓慢加入氢氧化钠调节pH值到6.0,添加完成后熟化30min。30min缓慢添加偏铝酸钠溶液,添加浓度为150g/L的偏铝酸钠溶液,偏铝酸的总量以Al2O3计为微硅粉的2.5%,添加完成后熟化30min。用硫酸调节pH为6.8,熟化30min。然后压滤洗涤,在105℃干燥后采用气流粉碎,并在粉碎过程中加入TME,TME的添加量为微硅粉的2‰,粉碎完成即得成品。
实施例2
配制浓度为350g/L的微硅粉浆料1L,加入2‰的六偏磷酸钠(以P2O5计),采用砂磨机分散15min,转数控制在800r/min,置于粉体改性反应釜中加热并搅拌至40℃,45min缓慢添加浓度为100g/L的四氯化钛水溶液,四氯化钛水溶液的总量以TiO2计为微硅粉的15%,60min缓慢加入氢氧化钠调节pH值到6.0,添加完成后熟化30min。30min缓慢添加偏铝酸钠溶液,添加浓度为150g/L的偏铝酸钠溶液,偏铝酸的总量以Al2O3计为微硅粉的4.0%,添加完成后熟化30min。用硫酸调节pH为6.5,熟化30min。然后压滤洗涤,在105℃干燥后采用气流粉碎,并在粉碎过程中加入TME,TME的添加量为微硅粉的3‰,粉碎完成即得成品。
实施例3
配制浓度为350g/L的微硅粉浆料1L,加入2‰的六偏磷酸钠(以P2O5计),采用砂磨机分散8min,转数控制在1500r/min,置于粉体改性反应釜中加热并搅拌至50℃,50min缓慢添加浓度为100g/L的四氯化钛水溶液,四氯化钛水溶液的总量以TiO2计为微硅粉的16%,60min缓慢加入氢氧化钠调节pH值到6.0,添加完成后熟化30min。30min缓慢添加偏铝酸钠溶液,添加浓度为150g/L的偏铝酸钠溶液,偏铝酸的总量以Al2O3计为微硅粉的2.5%,添加完成后熟化30min。用硫酸调节pH为7.0,熟化30min。然后压滤洗涤,在105℃干燥后采用气流粉碎,并在粉碎过程中加入TME,TME的添加量为微硅粉的3‰,粉碎完成即得成品。
实施例4
配制浓度为350g/L的微硅粉浆料1L,加入2‰的六偏磷酸钠(以P2O5计),采用砂磨机分散6min,转数控制在1800r/min,置于粉体改性反应釜中加热并搅拌至60℃,30min缓慢添加浓度为100g/L的四氯化钛水溶液,四氯化钛水溶液的总量以TiO2计为微硅粉的20%,60min缓慢加入氢氧化钠调节pH值到6.0,添加完成后熟化30min。30min缓慢添加偏铝酸钠溶液,添加浓度为150g/L的偏铝酸钠溶液,偏铝酸的总量以Al2O3计为微硅粉的4.0%,添加完成后熟化30min。用硫酸调节pH为6.0,熟化30min。然后压滤洗涤,在105℃干燥后采用气流粉碎,并在粉碎过程中加入TME,TME的添加量为微硅粉的4‰,粉碎完成即得成品。
将实施例1~4成品和未包覆样品配置成遮盖力检测浆料。采用同一种漆料把试样以一定的配方和方法制成漆浆,在遮盖力测试纸上用湿膜制备器制得厚度相同的涂膜,自然晾干,采用分光光度计对黑底和白底上的样品进行测定,通过PCQC 色彩品质控制系统软件直接表征试样的遮盖力。具体测试方法如下:
(1)漆浆制备:在玻璃瓶中称入100g玻璃研磨微珠,称取50g丙烯酸(或醇酸)清漆置于瓶中,加入12g试样,将装有物料的玻璃瓶置于振荡混匀机中,振荡研磨90min。
(2)涂膜制备:采用自动涂膜器将钛白粉漆浆用100μm的湿膜制备器在遮盖力测试纸上涂刷形成涂膜,涂膜置于室温下晾干。
(3)遮盖力测定:采用CM-2600d分光光度计对涂膜后的白底和黑底进行测定,通过PCQC 色彩品质控制系统软件直接表征试样的遮盖力。
将实施例1~4成品和未包覆样品配置成分散性检测浆料,称取3.0000g样品置于平磨仪的下层玻璃板中间,用两只注射器分别抽取2.8000g标准浆料。先加2.8000g标准浆料,用调刀将其调匀,在上层玻璃板上抹净调刀,施加1KN的力,研磨两遍,每遍25转,每磨一遍用调刀将浆状物收于玻璃板中间,研磨完毕,再加2.8000g标准浆料,用调刀将其和浆状物混匀,收于蜡光纸中备用。将足够量的样品滴入刮板细度计沟槽的深端,并使样品略有溢出(滴入数滴样品,以能充满沟槽略有多余为宜)。注意取样要有代表性,勿使样品夹带气泡,因气泡在细度计上显现出来与颗粒一样,会影响细度的观察。用两手的大姆指和食指捏住刮刀,将刮刀的刀口提到细度计沟槽最深一端,与细度计表面相接触,将刮刀垂直于细度计的表面,在1—2秒内使刮刀以均匀的速度由沟槽深部向浅部刮过,要施加足够的压力于刮刀上,以使沟槽中充满样品,多余的浆料被刮掉。
刮样后在3秒内,按如下方法从侧面观察细度计,观察时视线与沟槽平面成20—30°角,同时要在易于看出沟槽中样品状况的光线下进行观察。要注意刮完后立即观察,因时间过长有返粗现象,影响结果的准确性。观察样品首先出现密集颗粒点处,确定横跨沟槽3毫米宽的条带内若出现5个以上颗粒的位置为分散细度数值读取点。
样品按照上述测试其遮盖力时,数值越大遮盖力越高。测试其分散性时,数值越大分散性越差。测试结果如表1所示。
表1实施例样品遮盖率和分线性能对比
Claims (10)
1.一种高遮盖高分散性改性微硅粉,其特征在于,所述的高遮盖高分散性改性微硅粉的遮盖力为70%以上,分散性能为35微米以下,是以微硅粉颗粒为原料,经前处理、钛包膜、铝包膜和后处理步骤制备得到。
2.一种权利要求1所述的高遮盖高分散性改性微硅粉的制备方法,其特征在于,包括前处理、钛包膜、铝包膜和后处理步骤,具备包括:
A、前处理:
1)微硅粉浆料制备:将原料微硅粉颗粒加入到脱盐水中制备成浆料,调节浆料pH值为6.5~9,加入分散剂搅拌均匀得到浆料a;
2)砂磨分散:将浆料a置于砂磨机中使微硅粉颗粒的团聚体完全分散,呈现原级粒子状态得到物料b;
B、钛包膜:将物料b升温至25~60℃后加入四氯化钛水溶液,持续搅拌,用碱溶液在10~180min内缓慢调节pH值至5.0~12.5后,熟化15~60min即完成钛膜包覆得到物料c;
C、铝包膜:将物料c中顺流加入含铝化合物,加入时间控制在10~120min内,再持续搅拌10~30min后,用酸或碱溶液在30-120min内缓慢调节pH值至6.5~9.0后,熟化15~60min即完成铝膜包覆得到物料d;
D、后处理:
1)将物料d经压滤、洗涤去除可溶性盐得到滤饼e,将滤饼e干燥粉碎得到粉末f;
2)将粉末f进行气流粉碎,同时加入三羟甲基乙烷(TME)得到目标物高遮盖高分散性改性微硅粉。
3.根据权利要求2所述的制备方法,其特征在于,A步骤1)中所述的脱盐水是将所含易于除去的强电解质除去或减少到一定程度的水,剩余含盐量在1~5mg/L。
4.根据权利要求2所述的制备方法,其特征在于,A步骤1)中所述的分散剂为六偏磷酸钠、硅酸钠、羧酸盐和异丙醇胺中的一种或几种,添加量为原料微硅粉颗粒质量的1~9‰。
5.根据权利要求2所述的制备方法,其特征在于,A步骤1)中浆料a 的浓度为250~500g/L。
6.根据权利要求2所述的制备方法,其特征在于,A步骤2)中所述的砂磨机的转速控制在300~2000r/min,砂磨时间为3~20min。
7.根据权利要求2所述的制备方法,其特征在于,B步骤中所述的四氯化钛水溶液的浓度为80~140g/L,加入量为原料微硅粉颗粒质量的10~25%。
8.根据权利要求2所述的制备方法,其特征在于,C步骤中所述的含铝化合物为硫酸铝或偏铝酸钠,含铝化合物的浓度以Al2O3计为50~280g/L,加入量为原料微硅粉颗粒质量的0.5~5%。
9.根据权利要求2所述的制备方法,其特征在于,D步骤2)中气流粉碎的载体为过热蒸汽、压缩空气或压缩氮气。
10.根据权利要求2所述的制备方法,其特征在于,D步骤2)中三羟甲基丙烷的加入量为原料微硅粉颗粒质量的1~5‰,加入方式为气流粉碎机的入口或出口。
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