CN106566286A - 一种表面修饰硝酸镧杂化硅胶的改性碳酸钙粉体及其制备方法 - Google Patents

一种表面修饰硝酸镧杂化硅胶的改性碳酸钙粉体及其制备方法 Download PDF

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CN106566286A
CN106566286A CN201610914965.0A CN201610914965A CN106566286A CN 106566286 A CN106566286 A CN 106566286A CN 201610914965 A CN201610914965 A CN 201610914965A CN 106566286 A CN106566286 A CN 106566286A
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calcium carbonate
modified
carbonate powder
lanthanum
silica gel
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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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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT 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
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/02—Compounds of alkaline earth metals or magnesium
    • C09C1/021—Calcium carbonates
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT 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
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/02—Compounds of alkaline earth metals or magnesium
    • C09C1/021—Calcium carbonates
    • C09C1/022—Treatment with inorganic compounds
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT 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
    • C09C3/00—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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    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT 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
    • C09C3/00—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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    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT 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
    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/06—Treatment with inorganic compounds
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT 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
    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/08—Treatment with low-molecular-weight non-polymer organic compounds
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    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/12—Treatment with organosilicon compounds

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Abstract

本发明公开了一种表面修饰硝酸镧杂化硅胶的改性碳酸钙粉体，该改性碳酸钙粉体将稀土镧盐与γ‑环氧丙氧丙基三甲氧基硅烷、正硅酸乙酯混合水解杂化，形成含镧盐的杂化硅溶胶，再将其与碳酸钙、钛酸酯偶联剂/乙醇溶液湿法球磨处理，最终在其表面牢固修饰稀土镧盐杂化硅胶的改性碳酸钙粉体，改性后的碳酸钙具有良好的表面分散性和活化度，疏水性好，性能稳定持久，并赋予碳酸钙长效的抗腐蚀能力，改善其填充效果。

Description

一种表面修饰硝酸镧杂化硅胶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，尤其涉及一种表面修饰硝酸镧杂化硅胶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，提供一种表面修饰硝酸镧杂化硅胶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：
一种表面修饰硝酸镧杂化硅胶的改性碳酸钙粉体，该改性碳酸钙粉体由以下重量份的原料制成：碳酸钙50、钛酸酯偶联剂2-3、γ-环氧丙氧丙基三甲氧基硅烷1-2、正硅酸乙酯0.4-0.5、无水乙醇60-80、硝酸镧0.1-0.2、去离子水5-8、氨水适量。
所述的一种表面修饰硝酸镧杂化硅胶的改性碳酸钙粉体的制备方法包括以下步骤：
（1）先将去离子水与4-5重量份的无水乙醇混合，随后加入γ-环氧丙氧丙基三甲氧基硅烷、正硅酸乙酯、硝酸镧，搅拌混合均匀后滴加氨水，调节体系pH值为8-8.5，体系在50-60℃温度下水解8-10h后备用；
（2）将钛酸酯偶联剂、碳酸钙一起投入无水乙醇中，搅拌混合均匀后加入步骤（1）制备的物料，球磨分散40-50min后水洗2-3次，所得物料热风干燥，完全干燥后研磨分散，即得所述的改性碳酸钙粉体。
本发明的优点是：本发明将稀土镧盐与γ-环氧丙氧丙基三甲氧基硅烷、正硅酸乙酯混合水解杂化，形成含镧盐的杂化硅溶胶，再将其与碳酸钙、钛酸酯偶联剂/乙醇溶液湿法球磨处理，最终在其表面牢固修饰稀土镧盐杂化硅胶的改性碳酸钙粉体，改性后的碳酸钙具有良好的表面分散性和活化度，疏水性好，性能稳定持久，并赋予碳酸钙长效的抗腐蚀能力，改善其填充效果。
具体实施方式
一种表面修饰硝酸镧杂化硅胶的改性碳酸钙粉体，该改性碳酸钙粉体由以下重量份的原料制成：碳酸钙50、钛酸酯偶联剂2、γ-环氧丙氧丙基三甲氧基硅烷1、正硅酸乙酯0.4、无水乙醇60、硝酸镧0.1、去离子水5、氨水适量。
该实施例粉体的制备方法包括以下步骤：
（1）先将去离子水与4重量份的无水乙醇混合，随后加入γ环氧丙氧丙基三甲氧基硅烷、正硅酸乙酯、硝酸镧，搅拌混合均匀后滴加氨水，调节体系pH值为8，体系在50℃温度下水解8h后备用；
（2）将钛酸酯偶联剂、碳酸钙一起投入无水乙醇中，搅拌混合均匀后加入步骤（1）制备的物料，球磨分散40min后水洗2次，所得物料热风干燥，完全干燥后研磨分散，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D50：0.62μm；粘度：24.5mPa.s活化度：94.5%；吸油值：0.12ml/g；沉降体积：1.85ml/g。

Claims (2)

1.一种表面修饰硝酸镧杂化硅胶的改性碳酸钙粉体，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、钛酸酯偶联剂2-3、γ-环氧丙氧丙基三甲氧基硅烷1-2、正硅酸乙酯0.4-0.5、无水乙醇60-80、硝酸镧0.1-0.2、去离子水5-8、氨水适量。
2.如权利要求1所述的一种表面修饰硝酸镧杂化硅胶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）先将去离子水与4-5重量份的无水乙醇混合，随后加入γ-环氧丙氧丙基三甲氧基硅烷、正硅酸乙酯、硝酸镧，搅拌混合均匀后滴加氨水，调节体系pH值为8-8.5，体系在50-60℃温度下水解8-10h后备用；
（2）将钛酸酯偶联剂、碳酸钙一起投入无水乙醇中，搅拌混合均匀后加入步骤（1）制备的物料，球磨分散40-50min后水洗2-3次，所得物料热风干燥，完全干燥后研磨分散，即得所述的改性碳酸钙粉体。
CN201610914965.0A 2016-10-20 2016-10-20 一种表面修饰硝酸镧杂化硅胶的改性碳酸钙粉体及其制备方法 Pending CN106566286A (zh)

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