CN114437338B - 一种聚醚醚酮的合成方法 - Google Patents
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- C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
- C08G65/34—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from hydroxy compounds or their metallic derivatives
- C08G65/38—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from hydroxy compounds or their metallic derivatives derived from phenols
- C08G65/40—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from hydroxy compounds or their metallic derivatives derived from phenols from phenols (I) and other compounds (II), e.g. OH-Ar-OH + X-Ar-X, where X is halogen atom, i.e. leaving group
- C08G65/4012—Other compound (II) containing a ketone group, e.g. X-Ar-C(=O)-Ar-X for polyetherketones
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- C08G65/38—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from hydroxy compounds or their metallic derivatives derived from phenols
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Abstract
本发明提供一种聚醚醚酮的合成方法，在制备聚醚醚酮时，在聚醚醚酮合成中利用醇钠类反应物进行反应，提高了生产效率。乙醇钠碱性强，可以与对苯二酚迅速成盐，提高了2.5小时反应速度，降低对苯二酚高温氧化风险，得到聚合物颜色更白，并且反应结束后无对苯二酚单体残余，能够精确控制单体配比，更好的控制聚合物分子量和分子量分布。乙醇钠与对苯二酚反应产物是酚钠盐和乙醇，乙醇的沸点较低，容易从反应体系分离出去，聚合反应之后无残留二苯砜；乙醇钠代替碳酸盐作为催化剂可以提高生产效率，分离后的乙醇蒸气冷凝回收,作为后处理溶剂使用，脱除二苯砜，降低生产成本。
Description
技术领域
本发明公开一种聚醚醚酮的合成方法，提供新的生产方法，是对传统的聚醚醚酮的生产方法的改进，属于高分子材料技术领域。
背景技术
聚醚醚酮具有高机械性能、耐热性、耐化学腐蚀等优异性能，是一类高性能特种工程塑料，在航空航天、汽车工业、电子和核能等高技术领域有着广泛的用途。其最早商业化品种由英国ICI公司1981年最先推向市场的聚醚醚酮树脂。
目前，聚醚醚酮主要由4，4′-二氟二苯甲酮与对苯二酚，以二苯砜为溶剂，在碳酸钠的催化下合成。工业生产的聚醚醚酮需要回收溶剂二本砜以降低成本。传统碳酸钠的碱性不足，生成对苯二酚钠盐速度较慢，合成时间较长，而且反应结束后仍有单体对苯二酚残留，在后续的精制过程中氧化生成红色的醌类物质溶于丙酮和乙醇，降低了回收二本砜的纯度。影响下一次生产聚醚醚酮，造成其成品颜色过深的问题。
传统的制备方法是以二苯砜为溶剂，4，4′-二氟二苯甲酮和对苯二酚为聚合单体，Na2CO3/K2CO3为催化剂制备聚醚醚酮。碳酸盐碱性较低，与对苯二酚反应较慢。专利CN102627747B中以NaOH/KOH为催化剂量代替Na2CO3/K2CO3。氢氧化物的碱性强，但是仍比乙醇钠的碱性弱，副产物水难以排出，且不能直接回收利用。
发明内容
本发明提供一种聚醚醚酮的合成方法，在制备聚醚醚酮时，在聚醚醚酮合成中利用醇钠类反应物进行反应，提高了生产效率。解决了现有聚醚醚酮的合成技术状况存在的不足和问题。
本发明的技术解决方案如下：将乙醇钠与对苯二酚以2：1的物质量比投入熔融二苯砜中，先反应生成对苯二酚的钠盐，然后再投入4，4′-二氟二苯甲酮聚合反应合成聚醚醚酮。
本发明所述的一种聚醚醚酮合成的方法，具体步骤如下：
在连续通入氮气的状态下将2mol二苯砜、0.5mol对苯二酚与1mol乙醇钠加热至140℃持续一小时，生成气体分离排出；加入0.5mol的4，4′-二氟二苯甲酮，升温至310℃持续1.5小时；取出冷却后粉碎，用丙酮洗5次，去离子水洗5次，160℃烘10小时，即得。
本发明涉及的醇钠选自：乙醇钠或甲醇钠。
本发明反应过程结构式如下：
本发明用乙醇钠代替碳酸钠，乙醇钠碱性强，可以与对苯二酚迅速成盐，大大提高了反应速度，并且反应结束后无对苯二酚单体残余。醇钠代替碳酸钠，副产物醇可以回收利用，无多余的废气排出，更加节能环保。
本发明的积极效果在于：
本发明用乙醇钠代替碳酸钠，乙醇钠碱性强，可以与对苯二酚迅速成盐，提高了2.5小时反应速度，降低对苯二酚高温氧化风险，得到聚合物颜色更白，并且反应结束后无对苯二酚单体残余，能够精确控制单体配比，更好的控制聚合物分子量和分子量分布。乙醇钠与对苯二酚反应产物是酚钠盐和乙醇，乙醇的沸点较低，容易从反应体系分离出去，聚合反应之后无残留二苯砜；乙醇钠代替碳酸盐作为催化剂可以提高生产效率，分离后的乙醇蒸气冷凝回收,作为后处理溶剂使用，脱除二苯砜，降低生产成本。
本发明成盐效果稳定高效，在分子链增长过程中无气泡生成，聚合反应后无对苯二酚单体残余，操作简单，提高聚醚醚酮产品质量。
附图说明
图1为实施例1红外透射光谱；
图2为实施例2红外透射光谱。
具体实施方式
通过以下实施例进一步举例描述本发明，并不以任何方式限制本发明，在不背离本发明的技术解决方案的前提下，对本发明所作的本领域普通技术人员容易实现的任何改动或改变都将落入本发明的权利要求范围之内。
实施例1
在连接分水器、冷凝器以及搅拌器的1000ml密封四口烧瓶中连续通入氮气，投入436g（2mol）二苯砜，55.1g（0.5mol）对苯二酚与68g（1mol）乙醇钠，加热至180℃持续一小时，生成气体通过冷凝管和分离器分离。然后加入109.1g（0.5mol）4，4′-二氟二苯甲酮，1小时内升温至310℃持续1小时后加入3g4，4′-二氟二苯甲酮继续搅拌0.5小时，将烧瓶中的混合物倒出至光滑的不锈钢板上冷却，冷却后的物料粉碎，用丙酮洗5次，去离子水洗5次，装入不锈钢托盘放入烘箱中160℃烘10小时，得到聚醚醚酮产品，其红外透射光谱见附图1。结构式如下：
实施例2
在连接分水器、冷凝器以及搅拌器的1000ml密封四口烧瓶中连续通入氮气，投入436g（2mol）二苯砜，55.1g（0.5mol）对苯二酚与54g（1mol）甲醇钠，加热至180℃持续一小时，生成气体通过冷凝管和分离器分离。然后加入109.1g（0.5mol）4，4′-二氟二苯甲酮，1小时内升温至310℃持续1小时后加入3g4，4′-二氟二苯甲酮继续搅拌0.5小时，将烧瓶中的混合物倒出至光滑的不锈钢板上冷却，冷却后的物料粉碎，用丙酮洗5次，去离子水洗5次，装入不锈钢托盘放入烘箱中160℃烘10小时，得到聚醚醚酮产品，其红外透射光谱见附图2；结构式如下：
实施例3
对比案例：在连接分水器、冷凝器以及搅拌器的1000ml密封四口烧瓶中连续通入氮气，投入109.1g（0.5mol）4，4′-二氟二苯甲酮，58.3g（1.1mol）碳酸钠，436g（2mol）二苯砜，55.1g（0.5mol）对苯二酚。加热至180℃持续一小时，生成气体直接排出。2小时内升温至310℃持续2小时后加入3g4，4′-二氟二苯甲酮继续搅拌1小时，将烧瓶中的混合物倒出至光滑的不锈钢板上冷却，冷却后的物料粉碎，用丙酮洗5次，去离子水洗5次，装入不锈钢托盘放入烘箱中160℃烘10小时，得到聚醚醚酮产品。
实施例1和实施例2丙酮洗时无颜色出现，而实施例3丙酮洗时丙酮变为暗红色，说明有小分子对苯二酚发生了氧化。证明碳酸钠聚合反应不完全，而醇钠参与反应的没有该现象，说明醇钠在反应过程中的效率更高。
Claims (1)
1.一种聚醚醚酮的合成方法，其特征在于：
在连续通入氮气的状态下将2mol二苯砜、0.5mol对苯二酚与1mol乙醇钠加热至140℃持续一小时，生成气体分离排出；加入0.5mol的4，4′-二氟二苯甲酮，升温至310℃持续1.5小时；取出冷却后粉碎，用丙酮洗5次，去离子水洗5次，160℃烘10小时，即得。
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| JP5534815B2 (ja) * | 2007-10-31 | 2014-07-02 | 株式会社カネカ | ポリエーテルエーテルケトン、及び、ポリマー材料の精製方法 |
| JP5762327B2 (ja) * | 2011-05-30 | 2015-08-12 | 上野製薬株式会社 | ２，５−ジヒドロキシテレフタル酸の製造方法 |
| CN102408329B (zh) * | 2011-10-17 | 2014-04-23 | 上海安诺芳胺化学品有限公司 | 2，4-二羟基苯甲酸的制备方法 |
| CN102627747B (zh) * | 2012-04-10 | 2014-01-15 | 赵延辉 | 一种聚醚醚酮的合成方法 |
| CN104497239A (zh) * | 2014-12-17 | 2015-04-08 | 江门市优巨新材料有限公司 | 一种低色度、高热稳定性封端的聚醚醚酮树脂的工业化合成方法 |
| CN107573500A (zh) * | 2017-08-16 | 2018-01-12 | 宜宾天原集团股份有限公司 | 一种高纯聚醚醚酮树脂的制备方法 |
| CN107474201A (zh) * | 2017-08-16 | 2017-12-15 | 宜宾天原集团股份有限公司 | 一种高热稳定性封端聚醚醚酮树脂的制备方法 |
| CN107722275A (zh) * | 2017-09-20 | 2018-02-23 | 长春工业大学 | 新型侧链磺化聚芳醚酮砜质子交换膜及其制备方法 |
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