CN114539817A - 一种改性钛白粉的制备方法 - Google Patents
一种改性钛白粉的制备方法 Download PDFInfo
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- CN114539817A CN114539817A CN202210239191.1A CN202210239191A CN114539817A CN 114539817 A CN114539817 A CN 114539817A CN 202210239191 A CN202210239191 A CN 202210239191A CN 114539817 A CN114539817 A CN 114539817A
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- titanium dioxide
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- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical class [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 97
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 48
- 238000012986 modification Methods 0.000 claims abstract description 26
- 230000004048 modification Effects 0.000 claims abstract description 26
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 12
- 235000021355 Stearic acid Nutrition 0.000 claims abstract description 11
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims abstract description 11
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000008117 stearic acid Substances 0.000 claims abstract description 11
- 239000003607 modifier Substances 0.000 claims abstract description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 19
- 239000002002 slurry Substances 0.000 claims description 17
- 238000005406 washing Methods 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- 239000001038 titanium pigment Substances 0.000 claims description 10
- 239000002537 cosmetic Substances 0.000 claims description 9
- 235000019441 ethanol Nutrition 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 7
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 5
- 238000000227 grinding Methods 0.000 claims description 5
- 238000000967 suction filtration Methods 0.000 claims description 5
- 150000003608 titanium Chemical class 0.000 claims description 5
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 4
- CDQSJQSWAWPGKG-UHFFFAOYSA-N butane-1,1-diol Chemical compound CCCC(O)O CDQSJQSWAWPGKG-UHFFFAOYSA-N 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 238000012545 processing Methods 0.000 claims description 2
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 2
- 235000010215 titanium dioxide Nutrition 0.000 description 42
- 230000000475 sunscreen effect Effects 0.000 description 9
- 239000000516 sunscreening agent Substances 0.000 description 8
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 6
- 239000010453 quartz Substances 0.000 description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 6
- 230000035484 reaction time Effects 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- GVJHHUAWPYXKBD-UHFFFAOYSA-N (±)-α-Tocopherol Chemical compound OC1=C(C)C(C)=C2OC(CCCC(C)CCCC(C)CCCC(C)C)(C)CCC2=C1C GVJHHUAWPYXKBD-UHFFFAOYSA-N 0.000 description 4
- 239000006071 cream Substances 0.000 description 4
- 239000000203 mixture Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000009210 therapy by ultrasound Methods 0.000 description 3
- 230000002087 whitening effect Effects 0.000 description 3
- 229930003427 Vitamin E Natural products 0.000 description 2
- 239000010495 camellia oil Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 2
- WIGCFUFOHFEKBI-UHFFFAOYSA-N gamma-tocopherol Natural products CC(C)CCCC(C)CCCC(C)CCCC1CCC2C(C)C(O)C(C)C(C)C2O1 WIGCFUFOHFEKBI-UHFFFAOYSA-N 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- 235000019198 oils Nutrition 0.000 description 2
- 239000004006 olive oil Substances 0.000 description 2
- 235000008390 olive oil Nutrition 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 229940046009 vitamin E Drugs 0.000 description 2
- 235000019165 vitamin E Nutrition 0.000 description 2
- 239000011709 vitamin E Substances 0.000 description 2
- FMRHJJZUHUTGKE-UHFFFAOYSA-N Ethylhexyl salicylate Chemical compound CCCCC(CC)COC(=O)C1=CC=CC=C1O FMRHJJZUHUTGKE-UHFFFAOYSA-N 0.000 description 1
- 230000006750 UV protection Effects 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- KTUQUZJOVNIKNZ-UHFFFAOYSA-N butan-1-ol;hydrate Chemical compound O.CCCCO KTUQUZJOVNIKNZ-UHFFFAOYSA-N 0.000 description 1
- 239000013064 chemical raw material Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- CNXJITYCNQNTBD-UHFFFAOYSA-L dipotassium;hexadecyl phosphate Chemical compound [K+].[K+].CCCCCCCCCCCCCCCCOP([O-])([O-])=O CNXJITYCNQNTBD-UHFFFAOYSA-L 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004945 emulsification Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000001815 facial effect Effects 0.000 description 1
- -1 facial mask Substances 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 238000003760 magnetic stirring Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
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- WCJLCOAEJIHPCW-UHFFFAOYSA-N octyl 2-hydroxybenzoate Chemical compound CCCCCCCCOC(=O)C1=CC=CC=C1O WCJLCOAEJIHPCW-UHFFFAOYSA-N 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
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- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- RMGVATURDVPNOZ-UHFFFAOYSA-M potassium;hexadecyl hydrogen phosphate Chemical compound [K+].CCCCCCCCCCCCCCCCOP(O)([O-])=O RMGVATURDVPNOZ-UHFFFAOYSA-M 0.000 description 1
- 230000004224 protection Effects 0.000 description 1
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Abstract
本发明涉及钛白粉改性技术领域，具体涉及一种改性钛白粉的制备方法，包括一次改性和二次改性，所述一次改性和二次改性采用的改性剂分别为硬脂酸和硅烷偶联剂，所述改性钛白粉的制备方法通过对钛白粉进行改性，以使其改善护肤品质量和使用体验。
Description
技术领域
本发明涉及钛白粉改性技术领域，尤其涉及一种改性钛白粉的制备方法。
背景技术
钛白粉，是一种重要的无机化工颜料，主要成分为二氧化钛。钛白粉学名为二氧化钛，二氧化钛是一款使用范围非常广泛的无机化工原料。钛白粉广泛应用于涂料、塑料、造纸、印刷油墨、化纤、橡胶、化妆品等领域，当然不同领域有专属的钛白粉级别。
我们日常化妆品使用的是化妆品级二氧化钛，它具有化学性质稳定，白度高、遮盖力强、耐候性较强、且无毒害的特点。涂抹后对会产生增白的脸部视觉效果，所以钛白粉常用于美白霜、粉底、粉饼、珍珠膏、面膜、防晒护肤以及化妆品中。
钛白粉为彩妆类化妆品中最基础且消费量较大的原料之一。未经改性的纳米级钛白粉颗粒具有亲水性强、吸油量大、易团聚和光催化活性强等缺点，因此在化妆品的应用中受到一定的限制。改性后的钛白粉加入到化妆品中能够极大提高化妆品的抗紫外能力以及白度等。
发明内容
为解决上述技术问题，本发明的目的在于提供一种改性钛白粉的制备方法，所述改性钛白粉的制备方法通过对钛白粉进行改性，以使其改善护肤品质量和使用体验。
为达到上述技术效果，本发明采用了以下技术方案：
第一方面，本发明提供一种改性钛白粉的制备方法，包括以下步骤：
S1：取钛白粉制备为钛白粉浆液；
S2：调节钛白粉浆液的pH至8-10，并升温至60℃，加入硬脂酸，在搅拌状态下进行一次改性，在该反应中，所加入的一次改性剂硬脂酸为钛白粉质量的1-5％，优选为2％，反应时长为4-7h。
S3：将钛白粉浆液升温至70-85℃，调节pH值至3-4，在搅拌状态下按照钛白粉质量的1％-2％加入硅烷偶联剂进行二次改性，反应时长为5-8h。
S4：二次改性后趁热进行抽滤并进行多次洗涤，洗涤过程采用75％的乙醇溶液，以去除未反应的硅烷偶联剂，经烘干、研磨后获得改性钛白粉。
进一步地，所述S1具体为：将钛白粉加入至醇水溶液或无水乙醇中进行搅拌分散。
进一步地，所述醇水溶液中的醇为丙醇、正丁醇、丙二醇、丁二醇中的一种或多种。
进一步地，所述S1具体为还至少包括超声处理步骤。
第二方面，本发明还提供一种改性钛白粉，所述改性钛白粉采用权利要求 1-4任意一项所述的制备方法进行制备。
第三方面，本发明还提供上述改性钛白粉在制备化妆品和护肤品中的应用。
与现有技术相比，本发明的有益效果为：
本发明所提供的一种改性钛白粉的制备方法反应步骤简单易用控制，且改性成本较低，且改性后的钛白粉更加适宜添加于护肤品中，可有效地改善护肤品的使用性能。
具体实施方式
下面将对本发明技术方案的实施例进行详细的描述。以下实施例仅用于更加清楚地说明本发明的技术方案，因此只作为示例，而不能以此来限制本发明的保护范围。
需要说明的是，下述实施方案中所述实验方法，如无特殊说明，均为常规方法，所述试剂和材料，如无特殊说明，均可从商业途径获得。
实施例1
本实施例提供一种改性钛白粉，其具体制备方法如下：
S1：取一定量的钛白粉加入至75％的正丁醇水溶液中进行超声，超声条件为50-70kHZ，强度为200-250W/L，时间为20-30min，以制备钛白粉浆液；
S2：调节上述钛白粉浆液的pH至8-9，并升温至60℃，加入钛白粉质量1％的加入硬脂酸，在搅拌状态下进行一次改性，反应时长为4-5h。
S3：将步骤S2制备得到的钛白粉浆液升温至70℃，调节pH值至3，在搅拌状态下取钛白粉质量的1％加入硅烷偶联剂进行二次改性，反应时长为5-6h。
S4：二次改性后趁热进行抽滤并进行多次洗涤，洗涤过程采用75％的乙醇溶液洗涤2-4次，以去除未反应的硅烷偶联剂和硬脂酸，经烘干、研磨后获得改性钛白粉。
实施例2
本实施例提供一种改性钛白粉，其具体制备方法如下：
S1：取一定量的钛白粉加入至75％的乙醇水溶液中进行超声，超声条件为 50-65kHZ，强度为200-300W/L，时间为30-50min，以制备钛白粉浆液；
S2：调节上述钛白粉浆液的pH至9-10，并升温至60℃，加入钛白粉质量 2％的加入硬脂酸，在搅拌状态下进行一次改性，反应时长为4-5h。
S3：将步骤S2制备得到的钛白粉浆液升温至80℃，调节pH值至3-4，在搅拌状态下取钛白粉质量的2％加入硅烷偶联剂进行二次改性，反应时长为8h。
S4：二次改性后趁热进行抽滤并进行多次洗涤，洗涤过程采用75％的乙醇溶液洗涤2-4次，以去除未反应的硅烷偶联剂和硬脂酸，经烘干、研磨后获得改性钛白粉。
实施例3
本实施例提供一种改性钛白粉，其具体制备方法如下：
S1：取一定量的钛白粉加入至75％的乙醇水溶液中进行超声，超声条件为 50-65kHZ，强度为200-250W/L，时间为45-50min，以制备钛白粉浆液；
S2：调节上述钛白粉浆液的pH至9-10，并升温至60℃，加入钛白粉质量 5％的加入硬脂酸，在搅拌状态下进行一次改性，反应时长为7h。
S3：将步骤S2制备得到的钛白粉浆液升温至85℃，调节pH值至3-4，在搅拌状态下取钛白粉质量的1.6％加入硅烷偶联剂进行二次改性，反应时长为7 h。
S4：二次改性后趁热进行抽滤并进行多次洗涤，洗涤过程采用75％的乙醇溶液洗涤2-4次，以去除未反应的硅烷偶联剂和硬脂酸，经烘干、研磨后获得改性钛白粉。
实施例4
(1)制备
采用实施例1-实施例3制备得到的改性钛白粉、以及市售钛白粉(购买自上海盈承新材料有限公司)分别制备防晒产品，该防晒产品的组分如表1：
表1防晒产品中各原料组成
| 橄榄油 | 60份 |
| 山茶油 | 40份 |
| 甘油 | 5份 |
| 钛白粉 | 15份 |
| 水杨酸辛酯 | 3份 |
| 鲸蜡醇磷酸酯钾 | 3份 |
| 维生素E | 2份 |
| 丁二醇 | 2份 |
制备方法如下：
先取配方量的橄榄油、山茶油以及甘油于70℃下进行搅拌混合，采用磁力搅拌以获得均一的油相，然后取鲸蜡醇磷酸酯钾、维生素E以及丁二醇加入至上述体系中并进行持续地搅拌，最后将钛白粉、水杨酸辛酯加入至乳化体系中，混合均匀，自然冷却，制得防晒产品。
采用如表1所示的原料并按照上述方法将其制备成为防晒产品，将制得的产品分别标记为产品1-产品4,，并对防晒产品进行评价，评价结果如表2所示：
(2)外观检测
对产品1-产品4进行外观和使用肤感评价，评价结果如表2所示：
表2防晒产品检测实施例
(3)防晒效果检测
测试方法如下：取等量的产品1-产品4均匀涂于透紫外石英片上(2 mg/cm2)，静待15min；将涂满防晒霜的石英片置于紫外线强度测试仪探头上，测此时石英片下的紫外线指数并记录，使用紫外灯置于该透紫外石英片的上方对该透紫外石英片进行照射。记录每组测试数据，每组石英片均取三个不同的测试点进行测试，测试结果如表3所示：
表3产品1-产品4的防晒效果检测
以上实施例仅用以说明本发明的技术方案而非限制，尽管参照较佳实施例对本发明进行了详细说明，本领域的普通技术人员应当理解，可以对本发明的技术方案进行修改或者等同替换，而不脱离本发明技术方案的宗旨和范围，其均应涵盖在本发明的权利要求范围当中。本发明未详细描述的技术、形状、构造部分均为公知技术。
Claims (7)
1.一种改性钛白粉的制备方法，其特征在于：包括一次改性和二次改性，所述一次改性和二次改性采用的改性剂分别为硬脂酸和硅烷偶联剂。
2.如权利要求1所述的一种改性钛白粉的制备方法，其特征在于，包括以下步骤：
S1：取钛白粉制备为钛白粉浆液；
S2：调节钛白粉浆液的pH至8-10，并升温至60℃，加入硬脂酸进行一次改性；
S3：将钛白粉浆液升温至70-85℃，调节pH值至3-4，加入硅烷偶联剂进行二次改性；
S4：二次改性后趁热进行抽滤并进行多次洗涤，以去除未反应的硅烷偶联剂，经烘干、研磨后获得改性钛白粉。
3.如权利要求1所述的一种改性钛白粉的制备方法，其特征在于：所述S1具体为：将钛白粉加入至醇水溶液或无水乙醇中进行搅拌分散。
4.如权利要求3所述的一种改性钛白粉的制备方法，其特征在于：所述醇水溶液中的醇为丙醇、正丁醇、丙二醇、丁二醇中的一种或多种。
5.如权利要求1所述的一种改性钛白粉的制备方法，其特征在于：所述S1具体为还至少包括超声处理步骤。
6.一种改性钛白粉，其特征在于：所述改性钛白粉采用权利要求1-4任意一项所述的制备方法进行制备。
7.如权利要求6所述的一种改性钛白粉在制备化妆品和护肤品中的应用。
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