CN106700523A - 一种纳米水滑石复合材料的制备方法 - Google Patents
一种纳米水滑石复合材料的制备方法 Download PDFInfo
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- GDVKFRBCXAPAQJ-UHFFFAOYSA-A dialuminum;hexamagnesium;carbonate;hexadecahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Al+3].[Al+3].[O-]C([O-])=O GDVKFRBCXAPAQJ-UHFFFAOYSA-A 0.000 title claims abstract description 31
- 229910001701 hydrotalcite Inorganic materials 0.000 title claims abstract description 31
- 229960001545 hydrotalcite Drugs 0.000 title claims abstract description 31
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- 125000000467 secondary amino group Chemical class [H]N([*:1])[*:2] 0.000 claims abstract 2
- 239000013067 intermediate product Substances 0.000 claims description 28
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- 229910019142 PO4 Inorganic materials 0.000 claims description 12
- 239000010452 phosphate Substances 0.000 claims description 11
- 239000000047 product Substances 0.000 claims description 11
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 claims description 10
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- 150000004645 aluminates Chemical class 0.000 description 1
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 1
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- QAOWNCQODCNURD-UHFFFAOYSA-M hydrogensulfate Chemical compound OS([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-M 0.000 description 1
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- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 description 1
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- 229910001862 magnesium hydroxide Inorganic materials 0.000 description 1
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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
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/78—Compounds containing aluminium and two or more other elements, with the exception of oxygen and hydrogen
- C01F7/784—Layered double hydroxide, e.g. comprising nitrate, sulfate or carbonate ions as intercalating anions
- C01F7/785—Hydrotalcite
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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
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
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Abstract
本发明提供了一种纳米水滑石复合材料的制备方法：通过对纳米水滑石进行分散及改性，再通过α‑羧基环己基磺酸，双十二烷基仲胺进行插层改性，制得纳米水滑石阻燃剂。
Description
技术领域
本发明涉及一种阻燃剂的制备方法，尤其是一种纳米水滑石复合材料的制备方法。
背景技术
金属化合物,特别是过渡金属化合物对聚合物的抑烟效果很好,但由于价格昂贵,并在加工过程中多数金属化合物会破坏聚合物的热稳定性,难以在实际生产中 应用。填料型阻燃剂,如氢氧化铝、氢氧化镁等,通过在受热过程中分解产生大量水蒸气,使得气相中的氧气浓度和可燃性挥发物的浓度明显下降,同时产生的水能吸收大量的热量而起到阻燃和抑烟作用。然而,由于大量地添加和填料粒径大,严重影响了聚合物的力学性能。纳米材料的开发为解决这一问题提供了有效的途径。纳米层状双金属氢氧化物(简称水滑石,LDHs)对UPVC阻燃抑烟及机械性能的影响可避免上述缺点。
CN102120856B公开了一种聚氯乙烯/有机水滑石纳米复合材料，其组成以重量百分比计为：聚氯乙烯35～85％、有机水滑石1～10％、阻燃剂1～10％、其他助剂13～45％。其中，所述有机水滑石以重量百分比计，其主要组成为：水滑石类化合物60～95％，环氧化合物5～40％。还公开了上述聚氯乙烯/有机水滑石纳米复合材料的制备方法。本发明制备的聚氯乙烯/有机水滑石纳米复合材料，水滑石在聚氯乙烯基体中呈纳米级分散，该复合材料成本低，加工性能及力学性能良好，阻燃抑烟性能得到显著提高：LOI≥40，烟密度等级≤75；耐热性也得到大幅度提高。
CN104479173A公开了一种埃洛石纳米管水滑石复合物及其制备方法，该复合物是由埃洛石纳米管和水滑石两种无机纳米材料组成，其中所述的水滑石原位生长于埃洛石纳米管的表面，呈片状结构。其制备方法具体包括以下几个步骤：1)将可溶性镁盐和可溶性铝盐溶于去离子水中，室温下搅拌混合均匀；2)向步骤1)所制得的混合盐溶液中加入埃洛石纳米管，然后超声分散形成均匀溶液；3)在强力搅拌状态下，向步骤2)所制得的溶液中缓慢加入由氢氧化钠和碳酸钠组成的溶液，添加结束后，将其置于烘箱中静止晶化一定时间；4)将沉淀物过滤，水洗，干燥，研磨后得到复合物。该复合物可以用作热塑性和热固性类高分子材料的阻燃剂，PVC基高分子材料的热稳定剂和聚氨酯类弹性纤维的耐氯添加剂。
CN104194117A公开了一种高性能纳米复合材料，由以下重量份数的原料制成：低密度聚乙烯30-40份；水滑石5-15份；聚酰胺树脂10-15份；纳米粉体10-20份；消泡剂0.3-0.4份；成膜助剂1-2份；防冻剂0.2-0.5份；阻燃剂5-8份；发泡剂1-3份；竹炭纤维2-10份；耐磨剂0.5-2份。本发明性能好，稳定性高，添加的纳米粉体和耐磨剂相互结合，提高了高性能纳米复合材料的耐磨性能，同时竹炭纤维又增加了高性能纳米复合材料的韧性，适用范围广。
无机复合阻燃剂的制备一般采用公知的干法改性的方法，用高速搅拌机进行混合，同时添加通用的有机改性剂进行表面改性，通用的有机改性剂如：钛酸酯、铝酸酯、硅烷或脂肪酸等，所制得的水滑石纳米材料阻燃效果较差。
发明内容
本发明目的在于解决现有技术中存在的上述技术问题，提供一种纳米水滑石复合材料的制备方法。为了解决上述技术问题，本发明采用如下技术方案：一种纳米水滑石复合材料的制备方法，其特征在于制备步骤包括：
（1）按重量份，分别称取100份七水硫酸镁MgSO4·7H2O和40-80份18水合硫酸铝Al2(SO4)3·18H2O溶解于500-1000份去离子水，得到中间产物1；
（2）按重量份，将30-60份NaOH与5-15份Na2CO3溶解于500-1000份去离子水中得到中间产物2；
（3）按重量份，取100份中间产物1放入反应釜中，温度30-80℃，加入50-100份中间产物2，0.5-2份月桂酸单乙醇酰胺磷酸酯,0.1-1份四甲基胍硫酸氢盐，温度至50～80℃，反应2-5h，自然冷却到室温，加入过滤、洗涤，烘干，既得中间产物3；
（4）按重量份，取100份中间产物3，0.1-1份α-羧基环己基磺酸，0.1-1份双十二烷基仲胺，500-1000份去离子水,80-120℃反应10-40小时，过滤，洗涤，干燥，得到插层改性的水滑石阻燃剂。
所述磷酸酯类活化剂所述磷酸酯类表面活性剂包括月桂酸单乙醇酰胺磷酸酯，三苯乙基苯酚聚氧乙烯醚磷酸酯，壬基酚聚氧乙烯醚磷酸酯的1种或多种。
所述月桂酸单乙醇酰胺磷酸酯，α-羧基环己基磺酸，双十二烷基仲胺均为市售产品。
所述四甲基胍硫酸氢盐为市售产品，如中科院兰州化学物理研究所生产的产品。
本发明由于采用了上述技术方案，具有以下有益效果：
通过加入月桂酸单乙醇酰胺磷酸酯，四甲基胍硫酸氢盐离子液对纳米水滑石进行分散，结晶及改性，通过α-羧基环己基磺酸，0.1-1份双十二烷基仲胺进行插层改性，制得纳米水滑石阻燃剂，使得阻燃剂颗粒与尼龙6的相容性好，总热释放量降低率可提高40%以上。
具体实施方式
以下实例仅仅是进一步说明本发明，并不是限制本发明保护的范围。
实施例1：
（1）按重量份，分别称取100份七水硫酸镁MgSO4·7H2O和65份18水合硫酸铝Al2(SO4)3·18H2O溶解于800份去离子水，得到中间产物1；
（2）按重量份，将55份NaOH与7份Na2CO3溶解于800份去离子水中得到中间产物2；
（3）按重量份，取100份中间产物1放入反应釜中，温度56℃，加入70份中间产物2，0.5份月桂酸单乙醇酰胺磷酸酯,0.3份四甲基胍硫酸氢盐，温度至67℃，反应4h，自然冷却到室温，加入过滤、洗涤，烘干，既得中间产物3；
（4）按重量份，取100份中间产物3，0.6份α-羧基环己基磺酸，0.8份双十二烷基仲胺，700份去离子水,100℃反应20小时，过滤，洗涤，干燥，得到插层改性的水滑石阻燃剂。产品编号M-1。
实施例2：
（1）按重量份，分别称取100份七水硫酸镁MgSO4·7H2O和40份18水合硫酸铝Al2(SO4)3·18H2O溶解于500份去离子水，得到中间产物1；
（2）按重量份，将30份NaOH与5份Na2CO3溶解于500份去离子水中得到中间产物2；
（3）按重量份，取100份中间产物1放入反应釜中，温度30℃，加入50份中间产物2，0.5份三苯乙基苯酚聚氧乙烯醚磷酸酯,0.1份四甲基胍硫酸氢盐，温度至50℃，反应2h，自然冷却到室温，加入过滤、洗涤，烘干，既得中间产物3；
（4）按重量份，取100份中间产物3，0.1份α-羧基环己基磺酸，0.1份双十二烷基仲胺，500份去离子水,80℃反应40小时，过滤，洗涤，干燥，得到插层改性的水滑石阻燃剂。产品编号M-2。
实施例3：
（1）按重量份，分别称取100份七水硫酸镁MgSO4·7H2O和80份18水合硫酸铝Al2(SO4)3·18H2O溶解于1000份去离子水，得到中间产物1；
（2）按重量份，将60份NaOH与15份Na2CO3溶解于1000份去离子水中得到中间产物2；
（3）按重量份，取100份中间产物1放入反应釜中，温度80℃，加入100份中间产物2，2份壬基酚聚氧乙烯醚磷酸酯,1份四甲基胍硫酸氢盐，温度至80℃，反应5h，自然冷却到室温，加入过滤、洗涤，烘干，既得中间产物3；
（4）按重量份，取100份中间产物3，1份α-羧基环己基磺酸，1份双十二烷基仲胺，1000份去离子水,120℃反应10小时，过滤，洗涤，干燥，得到插层改性的水滑石阻燃剂。产品编号M-3。
比较例1：月桂酸单乙醇酰胺磷酸酯不加入，其它同实施例1。所得产品编号为M-4。
比较例2：四甲基胍硫酸氢盐不加入，其它同实施例1。所得产品编号为M-5。
比较例3：α-羧基环己基磺酸不加入，其它同实施例1。所得产品编号为M-6。
比较例4：
双十二烷基仲胺不加入，其它同实施例1。所得产品编号为M-7。
实施例4：
将加入实施例1-3以及对比例1-3的阻燃剂15wt%加入到业内公知的标准尼龙6混合料中，到按GB/T 20284-2006检测总热释放量降低率。
表1不同工艺做出的试验样品阻燃性能的比较
| 编号 | 总热释放量降低率% |
| M-1 | 40.6 |
| M-2 | 40.1 |
| M-3 | 42.1 |
| M-4 | 32.9 |
| M-5 | 33.7 |
| M-6 | 34.6 |
| M-7 | 38.5 |
| 未加入阻燃剂混合料 | 14.4 |
Claims (3)
1.一种纳米水滑石复合材料的制备方法，其特征在于制备步骤包括：
（1）按重量份，分别称取100份七水硫酸镁MgSO4·7H2O和40-80份18水合硫酸铝Al2(SO4)3·18H2O溶解于500-1000份去离子水，得到中间产物1；
（2）按重量份，将30-60份NaOH与5-15份Na2CO3溶解于500-1000份去离子水中得到中间产物2；
（3）按重量份，取100份中间产物1放入反应釜中，温度30-80℃，加入50-100份中间产物2，0.5-2份磷酸酯类表面活性剂，0.1-1份四甲基胍硫酸氢盐，温度至50～80℃，反应2-5h，自然冷却到室温，加入过滤、洗涤，烘干，既得中间产物3；
（4）按重量份，取100份中间产物3，0.1-1份α-羧基环己基磺酸，0.1-1份双十二烷基仲胺，80-120℃反应10-40小时，过滤，洗涤，干燥，得到插层改性的水滑石阻燃剂。
2.权利要求1所述的一种纳米水滑石复合材料的制备方法，其特征在于: 所述磷酸酯类表面活性剂包括月桂酸单乙醇酰胺磷酸酯，三苯乙基苯酚聚氧乙烯醚磷酸酯，壬基酚聚氧乙烯醚磷酸酯。
3.一种根据权利要求1所述纳米水滑石复合材料的制备方法得到的纳米水滑石复合材料。
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