CN1706877A - 多元共聚改性petg聚酯制备工艺 - Google Patents

多元共聚改性petg聚酯制备工艺 Download PDF

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CN1706877A
CN1706877A CN 200510040004 CN200510040004A CN1706877A CN 1706877 A CN1706877 A CN 1706877A CN 200510040004 CN200510040004 CN 200510040004 CN 200510040004 A CN200510040004 A CN 200510040004A CN 1706877 A CN1706877 A CN 1706877A
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esterification
pta
ipa
polycondensation
petg polyester
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CN1317316C (zh
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姚榕楠
唐盛平
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Tang Shengping
Yao Rongnan
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Abstract

本发明涉及一种化工产品的制备工艺，特别是一种多元共聚改性PETG聚酯的制备工艺。采用如下工艺步骤：a.配料：采用单体为对苯二甲酸(PTA)、简苯二甲酸(IPA)、新戌二醇(NPG)、乙二醇(MEG)及金属催化剂，其各组份按一定摩尔比配料；b.酯化反应：酯化反应温度控制在：210～260℃，反应压力为：0.01～0.25MPa，反应时间：180～260min，c.缩聚反应：缩聚反应温度控制在：275～285℃，真空度：0.098～0.1MPa，反应时间：180～200min。本发明利用四元单体混合经酯化和缩聚反应而得到非结晶倾向的高聚合物，制备工艺简单，操作方便，它改变了原PET聚酯的特性，使产品具有高透明、高收缩率、热封粘接性强、适用性强的优点。

Description

多元共聚改性PETG聚酯制备工艺
所属技术领域
本发明涉及一种化工产品的制备工艺，特别是一种多元共聚改性PETG聚酯的制备工艺。
背景技术
目前生产PETG聚酯的制备工艺，一般采用两种原料：对苯二甲酸和乙二醇，将对苯二甲酸和乙二醇合成制得PETG聚酯，这类聚酯为具有结晶性的PETG聚酯，只是应用于纺丝和聚酯薄膜上，应用范围不广。
发明内容
本发明以对苯二甲酸、简苯二甲酸、新戌二醇、乙二醇为主要原料，按一定配比，在催化剂作用下依次投入半连续化装置进行酯化反应和缩聚反应，从而制备得到多元共聚改性PETG聚酯。
实现本发明的具体技术方案为：一种多元共聚改性PETG聚酯制备工艺，采用如下工艺步骤：
a.配料：采用单体为对苯二甲酸(PTA)、简苯二甲酸(IPA)、新戌二醇(NPG)、乙二醇(MEG)及金属催化剂，其摩尔比：
PTA∶IPA＝1∶0.08～0.35，
(PTA+IPA)∶MEG∶NPG＝1∶1.25～1.75∶0.08～40，
b.酯化反应：苯二甲酸(PTA)、简苯二甲酸(IPA)、新戌二醇(NPG)、乙二醇(MEG)在金属催化剂催化下进行酯化反应，酯化反应温度控制在210～260℃，反应压力为0.01～0.25MPa，反应时间180～260min，
c.缩聚反应：在酯化反应结束后进行缩聚反应，缩聚反应温度控制在275～285℃，真空度0.098～0.1MPa，反应时间180～200min。
d.缩聚反应完成后得到PETG聚酯，再进行切粒、成品检验、包装。
具体地讲：上述金属催化剂采用Sb2O3。
本发明利用四元单体混合经酯化和缩聚反应而得到非结晶倾向的高聚合物，制备工艺简单，操作方便，它改变了原PETG聚酯的特性，使产品具有高透明、高收缩率、热封粘接性强、适用性强的优点。
具体实施方式
准备三只500ml的烧瓶，在烧瓶中装有电流搅拌器，玻璃温度计(测温范围为0～360℃)、分馏柱以及吸滤瓶、台式真空泵。
根据所加配方的摩尔比不同，可以制得适合各种应用领域的PETG聚酯，以下采用两种不同摩尔配比的配方制备PETG聚酯。
实施例一：
对苯二甲酸：92g
对苯二甲酸乙二醇酯：74g
简位酸：13.2g
新戌二醇：150g
乙二醇：80g
催化剂(Sb2O3)：0.056g
稳定剂：0.03g
抗氧剂：0.08g
实施例二：
对苯二甲酸：72g，
对苯二甲酸乙二醇酯：43g
简位酸：158g
新戌二醇：8.3g
乙二醇：119g
催化剂(Sb2O3)：0.056g
稳定剂：0.03g，
抗氧剂：0.08g
将上述配方的原料投入500ml烧瓶中，密封存放，缓慢升温进行酯化反应，温度控制在210～260℃，观察反应瓶内液体呈透明，酯化水分出约18～20ml，此时作为酯化反应结束，然后进行预缩聚和高真空缩聚，预缩聚开始缓慢减压抽空，从0.02～0.1MPa，减压时间需45～60min，然后开始高真空缩聚，温度控制在285℃，缩聚时间控制在180～250min，完成制备。之后进行切粒、检验、包装。
按上述实施例一摩尔配比最后所得PETG聚酯的特性粘度为η＝0.75，熔点为170～175℃；按实施例二摩尔配比最后所得PETG聚酯的特性粘度为η＝0.78，熔点为185～200℃。

Claims (2)

1.一种多元共聚改性PETG聚酯制备工艺，其特征是采用如下工艺步骤：
a.配料：采用单体为对苯二甲酸(PTA)、简苯二甲酸(IPA)、新戌二醇(NPG)、乙二醇(MEG)及金属催化剂，其摩尔比：
PTA∶IPA＝1∶0.08～0.80，
(PTA+IPA)∶MEG∶NPG＝1∶1.25～1.75∶0.08～40；
b.酯化反应：苯二甲酸(PTA)、简苯二甲酸(IPA)、新戌二醇(NPG)、乙二醇(MEG)在金属催化剂催化下进行酯化反应，酯化反应温度控制在：210～260℃，反应压力为：0.01～0.25MPa，反应时间：180～260min；
c.缩聚反应：在酯化反应结束后进行缩聚反应，缩聚反应温度控制在：275～285℃，真空度：0.098～0.1MPa，反应时间：180～200min；
d.缩聚反应完成后得到PETG聚酯，再进行切粒、成品检验、包装。
2.根据权利要求1所述的多元共聚改性PETG聚酯制备工艺，其特征是：所述金属催化剂为Sb2O3。
CNB2005100400043A 2005-05-14 2005-05-14 多元共聚改性petg聚酯制备工艺 Expired - Fee Related CN1317316C (zh)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102718951A (zh) * 2012-05-17 2012-10-10 杨小明 双酸一醇共聚改性pet-a及其单向热收缩膜制备工艺
CN102964575A (zh) * 2012-12-07 2013-03-13 富维薄膜（山东）有限公司 改性聚酯及其制备方法
CN106188509A (zh) * 2016-08-11 2016-12-07 哈尔滨工业大学 一种高透光性聚酯薄膜前驱体的制备方法

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP4121295B2 (ja) * 2002-03-22 2008-07-23 ロンシール工業株式会社 樹脂組成物および該樹脂組成物を用いたシート・フィルム

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102718951A (zh) * 2012-05-17 2012-10-10 杨小明 双酸一醇共聚改性pet-a及其单向热收缩膜制备工艺
CN102718951B (zh) * 2012-05-17 2013-11-27 杨小明 双酸一醇共聚改性pet-a及其单向热收缩膜制备工艺
CN102964575A (zh) * 2012-12-07 2013-03-13 富维薄膜（山东）有限公司 改性聚酯及其制备方法
CN106188509A (zh) * 2016-08-11 2016-12-07 哈尔滨工业大学 一种高透光性聚酯薄膜前驱体的制备方法

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