CN106752097A - 一种具有良好生物相容性的改性碳酸钙粉体及其制备方法 - Google Patents

一种具有良好生物相容性的改性碳酸钙粉体及其制备方法 Download PDF

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CN106752097A
CN106752097A CN201610914957.6A CN201610914957A CN106752097A CN 106752097 A CN106752097 A CN 106752097A CN 201610914957 A CN201610914957 A CN 201610914957A CN 106752097 A CN106752097 A CN 106752097A
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calcium carbonate
carbonate powder
modified calcium
good biocompatibility
powder
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陈永忠
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QINGYANG YONGCHENG CALCIUM INDUSTRY Co Ltd
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QINGYANG YONGCHENG CALCIUM INDUSTRY Co Ltd
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/19Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/02Compounds of alkaline earth metals or magnesium
    • C09C1/021Calcium carbonates
    • C09C1/022Treatment with inorganic compounds
    • C09C1/024Coating
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C3/00Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/06Treatment with inorganic compounds
    • C09C3/063Coating
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C3/00Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/08Treatment with low-molecular-weight non-polymer organic compounds
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C3/00Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/10Treatment with macromolecular organic compounds
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/19Oil-absorption capacity, e.g. DBP values
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/22Rheological behaviour as dispersion, e.g. viscosity, sedimentation stability
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/90Other properties not specified above

Abstract

本发明公开了一种具有良好生物相容性的改性碳酸钙粉体,本发明将碳酸钙先经过钛酸酯偶联剂/乙醇溶液湿法球磨预处理,改善其分散性,提高表面反应活性,随后将其投入纳米羟基磷灰石/聚乙烯亚胺复合溶液中,在其表面交联生成具有良好生物相容性的膜层,有效的改善了碳酸钙粉体的生物相容性,使用感更佳,且改性后的碳酸钙粉体悬浮性好,具有两亲性,在水性及有机介质中均能良好分散,作为化妆品填料的使用价值更高。

Description

一种具有良好生物相容性的改性碳酸钙粉体及其制备方法
技术领域
本发明涉及无机粉体表面改性技术领域,尤其涉及一种具有良好生物相容性的改性碳酸钙粉体及其制备方法。
背景技术
碳酸钙是一种十分常见的无机粉末填料,其价格低廉、无毒无味、白度高、硬度好等优点,在橡胶制品、造纸、油墨、塑料、涂料等等领域均有广泛的应用,然而,碳酸钙本质上一种无机矿物质,与有机物质亲和相容性较差,直接填充将会导致产品性能严重劣化,使用范围严重受限,因此,在实际应用中需要对碳酸钙粉体进行改性处理。
目前主要的改性方法有机械细化法、表面改性剂如偶联剂、脂肪酸及其盐、表面活性剂等改性两大类,两种方法各有其优势,改性后的碳酸钙性能也得到一定的改善。《硬脂酸-钛酸酯偶联剂改性重质碳酸钙粉体研究》一文以硬脂酸、钛酸酯偶联剂作为复合改性剂,无水乙醇作为分散剂,采用湿法球磨对粉体进行改性处理,取得了较为理想的改性效果,但是这种方法制备得到的产品为疏水性产品,在水性油墨、水性涂料领域应用受到限制,且附加功能不足,仅限于补强增韧用,需要做进一步的改性处理,以扩宽其使用范围。
发明内容
本发明目的就是为了弥补已有技术的缺陷,提供一种具有良好生物相容性的改性碳酸钙粉体及其制备方法。
本发明是通过以下技术方案实现的:
一种具有良好生物相容性的改性碳酸钙粉体,该改性碳酸钙粉体由以下重量份的原料制成:碳酸钙50、聚乙烯亚胺1-2、钛酸酯偶联剂2-3、无水乙醇60-80、纳米羟基磷灰石4-5、十二烷基磺酸钠0.1-0.2、去离子水70-80。
所述的一种具有良好生物相容性的改性碳酸钙粉体的制备方法包括以下步骤:
(1)先将钛酸酯偶联剂、碳酸钙一起投入无水乙醇中,球磨40-50min后热风干燥,完全除去溶剂,研磨分散后得预改性碳酸钙粉体备用;
(2)将十二烷基磺酸钠投入去离子水中,搅拌至其完全溶解后加入纳米羟基磷灰石,超声搅拌混合2-3h,制成纳米羟基磷灰石溶胶,随后加入步骤(1)制备的预改性碳酸钙粉体,继续搅拌分散2-3h后加入聚乙烯亚胺,体系加热至60-80℃,搅拌反应4-5h,反应结束后产物经干燥处理,所得物料经研磨分散即得所述的改性碳酸钙粉体。
本发明的优点是:本发明将碳酸钙先经过钛酸酯偶联剂/乙醇溶液湿法球磨预处理,改善其分散性,提高表面反应活性,随后将其投入纳米羟基磷灰石/聚乙烯亚胺复合溶液中,在其表面交联生成具有良好生物相容性的膜层,有效的改善了碳酸钙粉体的生物相容性,使用感更佳,且改性后的碳酸钙粉体悬浮性好,具有两亲性,在水性及有机介质中均能良好分散,作为化妆品填料的使用价值更高。
具体实施方式
一种具有良好生物相容性的改性碳酸钙粉体,该改性碳酸钙粉体由以下重量份的原料制成:碳酸钙50、聚乙烯亚胺1、钛酸酯偶联剂2、无水乙醇60、纳米羟基磷灰石4、十二烷基磺酸钠0.1、去离子水70。
该实施例粉体的制备方法包括以下步骤:
(1)先将钛酸酯偶联剂、碳酸钙一起投入无水乙醇中,球磨40min后热风干燥,完全除去溶剂,研磨分散后得预改性碳酸钙粉体备用;
(2)将十二烷基磺酸钠投入去离子水中,搅拌至其完全溶解后加入纳米羟基磷灰石,超声搅拌混合2h,制成纳米羟基磷灰石溶胶,随后加入步骤(1)制备的预改性碳酸钙粉体,继续搅拌分散2h后加入聚乙烯亚胺,体系加热至60℃,搅拌反应4h,反应结束后产物经干燥处理,所得物料经研磨分散即得所述的改性碳酸钙粉体。
制得的碳酸钙粉体性能测试结果为:
粒度D50:0.95μm;粘度:32.5mPa.s活化度:94.2%;吸油值:0.28ml/g;沉降体积:1.26ml/g。

Claims (2)

1.一种具有良好生物相容性的改性碳酸钙粉体,其特征在于,该改性碳酸钙粉体由以下重量份的原料制成:碳酸钙50、聚乙烯亚胺1-2、钛酸酯偶联剂2-3、无水乙醇60-80、纳米羟基磷灰石4-5、十二烷基磺酸钠0.1-0.2、去离子水70-80。
2.如权利要求1所述的一种具有良好生物相容性的改性碳酸钙粉体的制备方法,其特征在于,其制备方法包括以下步骤:
(1)先将钛酸酯偶联剂、碳酸钙一起投入无水乙醇中,球磨40-50min后热风干燥,完全除去溶剂,研磨分散后得预改性碳酸钙粉体备用;
(2)将十二烷基磺酸钠投入去离子水中,搅拌至其完全溶解后加入纳米羟基磷灰石,超声搅拌混合2-3h,制成纳米羟基磷灰石溶胶,随后加入步骤(1)制备的预改性碳酸钙粉体,继续搅拌分散2-3h后加入聚乙烯亚胺,体系加热至60-80℃,搅拌反应4-5h,反应结束后产物经干燥处理,所得物料经研磨分散即得所述的改性碳酸钙粉体。
CN201610914957.6A 2016-10-20 2016-10-20 一种具有良好生物相容性的改性碳酸钙粉体及其制备方法 Pending CN106752097A (zh)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108102430A (zh) * 2017-12-08 2018-06-01 安徽新涛新材料科技股份有限公司 一种超细活性重质碳酸钙的制备方法

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108102430A (zh) * 2017-12-08 2018-06-01 安徽新涛新材料科技股份有限公司 一种超细活性重质碳酸钙的制备方法

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