CN106280564A - 一种表面改性超细氢氧化镁的制备方法 - Google Patents

一种表面改性超细氢氧化镁的制备方法 Download PDF

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CN106280564A
CN106280564A CN201610684079.3A CN201610684079A CN106280564A CN 106280564 A CN106280564 A CN 106280564A CN 201610684079 A CN201610684079 A CN 201610684079A CN 106280564 A CN106280564 A CN 106280564A
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magnesium hydroxide
modified superfine
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黄惠娟
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    • 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
    • C08K9/04—Ingredients treated with organic substances
    • C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
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    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
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    • C09C1/028—Compounds containing only magnesium as metal
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    • 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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    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
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    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
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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
    • 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
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    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C08K2003/2217—Oxides; Hydroxides of metals of magnesium
    • C08K2003/2224—Magnesium hydroxide
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    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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Abstract

本发明公开了一种表面改性超细氢氧化镁的制备方法,包括以下步骤:(1)选取粒径为4000‑6000目的超细氢氧化镁，在50‑100℃下高速搅拌机内以搅拌速率3000‑6000r/min对超细氢氧化镁进行搅拌预热20‑40 min；（2）然后缓慢均匀加入表面改性剂和溶剂，接着继续搅拌及表面改性时间为50‑90分钟，得到改性超细氢氧化镁。该表面改性超细氢氧化镁的制备方法制得的改性超细氢氧化镁，提高了其与高分子材料相容性好与热稳定性，可显著改善高分子复合材料的力学性能、加工流动性等。

Description

一种表面改性超细氢氧化镁的制备方法
技术领域
本发明涉及一种氢氧化镁的制备方法，尤其涉及一种表面改性超细氢氧化镁的制备方法。
背景技术
氢氧化镁是一种新型无机填充型阻燃剂，其来源广泛、价格低廉、热稳定性好、不挥发、不析出、不产生有毒气体、不腐蚀加工设备以及抑烟作用明显等诸多优点而备受关注，是公认的橡塑行业中具有阻燃、抑烟、填充三重功能的优秀阻燃剂。其阻燃原理是通过受热分解时释放出结合水，吸收大量的潜热，来降低它所填充的合成材料在火焰中的表面温度，具有抑制聚合物分解和对所产生的可燃气体进行冷却的作用；同时分解生成的氧化镁又是良好的耐火材料，也能帮助提高合成材料的抗火性能，它放出的水蒸气也可作为一种抑烟剂。
氢氧化镁的阻燃效率较低以及与基体树脂的相容性较差，要使阻燃性聚合物材料的阻燃性能达到一定要求，其添加量常常须达到阻燃性聚合物材料总质量的60%以上，这样会对阻燃性聚合物材料的加工性能和力学性能产生很大的负面影响，因此采用比表面积大、阻燃率高的超细氢氧化镁替代常规氢氧化镁粉末，但是由于超细氢氧化镁在高分子材料中分散性差，容易团聚，材料的力学性能和加工流动性均受到严重影响。因此，需要对超细氢氧化镁进行表面改性处理来提高超细氢氧化镁与高分子材料的相容性和加工流动性。
发明内容
本发明的目的是设计出表面改性超细氢氧化镁的制备方法，该表面改性超细氢氧化镁的制备方法制得的改性超细氢氧化镁，提高了其与高分子材料相容性好与热稳定性，可显著改善高分子复合材料的力学性能、加工流动性等。
这种表面改性超细氢氧化镁的制备方法，其制备步骤如下：
(1) 选取粒径为4000-6000目的超细氢氧化镁，在50-100℃下高速搅拌机内以搅拌速率3000-6000r/min对超细氢氧化镁进行搅拌预热20-40 min；
（2）然后缓慢均匀加入表面改性剂和溶剂，接着继续搅拌及表面改性时间为50-90分钟，得到改性超细氢氧化镁。
该步骤（1）中搅拌温度为85℃，搅拌速率为6000r/min，预热时间为35min。
该步骤（2）中继续搅拌及表面改性时间为60 min。
该步骤（2）中表面改性剂为磷酸酯偶联剂、硅烷偶联剂、六偏磷酸钠、硬脂酸、或二苯基甲烷二异氰酸酷中的至少一种;所述的溶剂为无水乙醇或水的至少一种。
该步骤（2）中表面改性剂的用量为超细氢氧化镁的0.5%-5%。
综上所述，本发明的表面改性超细氢氧化镁的制备方法的改性过程设备和工艺简单、生产成木低，能广泛地应用于工业生产过程中；本发明制备的改性超细氢氧化镁，提高了其与高分子材料相容性好与热稳定性，可显著改善高分子复合材料的力学性能、加工流动性；本发明制备的改性氢氧化镁应用于制备阻燃性聚合物，氢氧化镁的用量由原来占聚合物材料总质量的60%下降到占48%，得到的聚合物满足阻燃性的性能，甚至更优越。且聚合物材料的加工性能和力学性能明显改善。
具体实施方式
通过下面给出的具体实施例，可以进一步清楚了解本发明。
实施例1
首先在50℃下高速搅拌机内以搅拌速率3000转/分钟对4000目超细氢氧化镁进行搅拌预热20分钟，然后缓慢均匀加入表面改性剂磷酸酯偶联剂和溶剂无水乙醇，接着继续搅拌50 min，得到改性超细氢氧化镁。表面改性剂的用量为超细氢氧化镁的0.5%。
实施例2
在85℃下高速搅拌机内以搅拌速率5000转/分钟对5000目超细氢氧化镁进行搅拌预热35分钟，然后缓慢均匀加入表面改性剂硅烷偶联剂和六偏磷酸钠以及溶剂水，接着继续搅拌60 min，得到改性超细氢氧化镁。表面改性剂的用量为超细氢氧化镁的3%。
实施例3
在100℃下高速搅拌机内以搅拌速率6000转/分钟对5000目超细氢氧化镁进行搅拌预热40分钟，然后缓慢均匀加入表面改性剂硬脂酸和二苯基甲烷二异氰酸酷以及溶剂无水乙醇和水，接着继续搅拌90 min，得到改性超细氢氧化镁。表面改性剂的用量为超细氢氧化镁的5%。

Claims (5)

1.一种表面改性超细氢氧化镁的制备方法，其特征在于，包括以下步骤:
(1) 选取粒径为4000-6000目的超细氢氧化镁，在50-100℃下高速搅拌机内以搅拌速率3000-6000r/min对超细氢氧化镁进行搅拌预热20-40 min；
（2）然后缓慢均匀加入表面改性剂和溶剂，接着继续搅拌及表面改性时间为50-90分钟，得到改性超细氢氧化镁。
2.根据权利要求1所述的一种表面改性超细氢氧化镁的制备方法，其特征在于，所述步骤（1）中搅拌温度为85℃，搅拌速率为6000r/min，预热时间为35min。
3.根据权利要求2所述的一种表面改性超细氢氧化镁的制备方法，其特征在于，所述步骤（2）中继续搅拌及表面改性时间为60 min。
4.根据权利要求3所述的一种表面改性超细氢氧化镁的制备方法，其特征在于，所述步骤（2）中表面改性剂为磷酸酯偶联剂、硅烷偶联剂、六偏磷酸钠、硬脂酸、或二苯基甲烷二异氰酸酷中的至少一种;所述的溶剂为无水乙醇或水的至少一种。
5.根据权利要求4所述的一种表面改性超细氢氧化镁的制备方法，其特征在于，所述步骤（2）中表面改性剂的用量为超细氢氧化镁的0.5%-5%。
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109054450A (zh) * 2018-06-11 2018-12-21 洛阳中超新材料股份有限公司 表面改性氢氧化镁及其制备方法和应用
CN114395171A (zh) * 2022-01-19 2022-04-26 河南强宏镁业科技股份有限公司 一种阻燃级改性氢氧化镁及其制备方法
CN114605705A (zh) * 2022-04-21 2022-06-10 深圳市海扬粉体科技有限公司 一种表面有机改性的氢氧化镁粉体及其制备方法

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109054450A (zh) * 2018-06-11 2018-12-21 洛阳中超新材料股份有限公司 表面改性氢氧化镁及其制备方法和应用
CN109054450B (zh) * 2018-06-11 2020-05-15 洛阳中超新材料股份有限公司 表面改性氢氧化镁及其制备方法和应用
CN114395171A (zh) * 2022-01-19 2022-04-26 河南强宏镁业科技股份有限公司 一种阻燃级改性氢氧化镁及其制备方法
CN114605705A (zh) * 2022-04-21 2022-06-10 深圳市海扬粉体科技有限公司 一种表面有机改性的氢氧化镁粉体及其制备方法

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