CN106566308A - 一种水性涂料用交联聚乙烯亚胺改性碳酸钙粉体及其制备方法 - Google Patents

一种水性涂料用交联聚乙烯亚胺改性碳酸钙粉体及其制备方法 Download PDF

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CN106566308A
CN106566308A CN201610914960.8A CN201610914960A CN106566308A CN 106566308 A CN106566308 A CN 106566308A CN 201610914960 A CN201610914960 A CN 201610914960A CN 106566308 A CN106566308 A CN 106566308A
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calcium carbonate
modified calcium
carbonate powder
powder body
polyethyleneimine
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陈永忠
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QINGYANG YONGCHENG CALCIUM INDUSTRY Co Ltd
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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
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/24—Acids; Salts thereof
    • C08K3/26—Carbonates; Bicarbonates
    • 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
    • C08K9/04—Ingredients treated with organic substances
    • 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
    • C08K9/10—Encapsulated ingredients
    • 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
    • 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
    • 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
    • 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
    • C09C3/10—Treatment with macromolecular organic compounds
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • C09D7/60—Additives non-macromolecular
    • C09D7/61—Additives non-macromolecular inorganic
    • C09D7/62—Additives non-macromolecular inorganic modified by treatment with other compounds
    • 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
    • C08K3/24—Acids; Salts thereof
    • C08K3/26—Carbonates; Bicarbonates
    • C08K2003/265—Calcium, strontium or barium carbonate

Abstract

本发明公开了一种水性涂料用交联聚乙烯亚胺改性碳酸钙粉体，该改性碳酸钙粉体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，随后在其表面原位生成交联聚乙烯亚胺薄膜，最终制得的改性碳酸钙粉体具有稳定的两亲性，在水性涂料体系中既能与树脂分子亲和，又能与溶剂良好分散共存，不易沉降，达到优良的填充改性效果。

Description

一种水性涂料用交联聚乙烯亚胺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，尤其涉及一种水性涂料用交联聚乙烯亚胺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，提供一种水性涂料用交联聚乙烯亚胺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：
一种水性涂料用交联聚乙烯亚胺改性碳酸钙粉体，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、聚环氧氯丙烷0.4-0.8、N，N-二甲基甲酰胺60-80。
所述的一种水性涂料用交联聚乙烯亚胺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）将聚乙烯亚胺、聚环氧氯丙烷一起投入中N，N-二甲基甲酰胺，搅拌至其完全溶解后投入预改性碳酸钙粉体，超声搅拌混合40-50min，随后将体系加热至95-105℃，反应3-3.5h，反应结束后抽滤，抽滤物水洗2-3次后在80℃烘箱内干燥处理，干燥后的产物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，随后在其表面原位生成交联聚乙烯亚胺薄膜，最终制得的改性碳酸钙粉体具有稳定的两亲性，在水性涂料体系中既能与树脂分子亲和，又能与溶剂良好分散共存，不易沉降，达到优良的填充改性效果。
具体实施方式
一种水性涂料用交联聚乙烯亚胺改性碳酸钙粉体，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、聚环氧氯丙烷0.4、N，N-二甲基甲酰胺60。
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）将聚乙烯亚胺、聚环氧氯丙烷一起投入中N，N-二甲基甲酰胺，搅拌至其完全溶解后投入预改性碳酸钙粉体，超声搅拌混合40min，随后将体系加热至95℃，反应3h，反应结束后抽滤，抽滤物水洗2次后在80℃烘箱内干燥处理，干燥后的产物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D50：0.45μm；粘度：28.2mPa.s活化度：90.3%；吸油值：0.20ml/g；沉降体积：1.02ml/g。

Claims (2)

1.一种水性涂料用交联聚乙烯亚胺改性碳酸钙粉体，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、聚环氧氯丙烷0.4-0.8、N，N-二甲基甲酰胺60-80。
2.如权利要求1所述的一种水性涂料用交联聚乙烯亚胺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）将聚乙烯亚胺、聚环氧氯丙烷一起投入中N，N-二甲基甲酰胺，搅拌至其完全溶解后投入预改性碳酸钙粉体，超声搅拌混合40-50min，随后将体系加热至95-105℃，反应3-3.5h，反应结束后抽滤，抽滤物水洗2-3次后在80℃烘箱内干燥处理，干燥后的产物经研磨分散即得所述的改性碳酸钙粉体。
CN201610914960.8A 2016-10-20 2016-10-20 一种水性涂料用交联聚乙烯亚胺改性碳酸钙粉体及其制备方法 Pending CN106566308A (zh)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111608014A (zh) * 2020-04-13 2020-09-01 仙鹤股份有限公司 一种高性能低定量字典纸及其制备方法
CN111663371A (zh) * 2020-05-12 2020-09-15 仙鹤股份有限公司 一种柔版印刷烟用接装原纸的制备方法

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111608014A (zh) * 2020-04-13 2020-09-01 仙鹤股份有限公司 一种高性能低定量字典纸及其制备方法
CN111608014B (zh) * 2020-04-13 2022-07-15 仙鹤股份有限公司 一种高性能低定量字典纸及其制备方法
CN111663371A (zh) * 2020-05-12 2020-09-15 仙鹤股份有限公司 一种柔版印刷烟用接装原纸的制备方法

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