CN1911998A - 聚乙烯醇与糖的共聚物及其制备的方法 - Google Patents

聚乙烯醇与糖的共聚物及其制备的方法 Download PDF

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CN1911998A
CN1911998A CN 200610105080 CN200610105080A CN1911998A CN 1911998 A CN1911998 A CN 1911998A CN 200610105080 CN200610105080 CN 200610105080 CN 200610105080 A CN200610105080 A CN 200610105080A CN 1911998 A CN1911998 A CN 1911998A
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polyvinyl alcohol
multipolymer
pva
sugar
copolymer
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CN100554330C (zh
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刘昭铁
孙平
陈静
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Shaanxi Normal University
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Abstract

本发明涉及的是聚乙烯醇与糖的共聚物及其制备方法。该共聚物以聚乙烯醇链为基础，将糖接枝到聚乙烯醇链上，糖可以为单糖、低聚糖、环糊精、淀粉等。其制备工艺包括以下步骤：(1)将聚乙烯醇和糖溶于热水，待全部溶解后降温至50～70℃；(2)在50～70℃加入浓度约30％NaOH水溶液，搅拌12h；(2)在50～70℃加入交联剂，搅拌反应12h，加入适量丙酮终止反应，得黄色溶胶，用稀盐酸中和。对所得溶胶进行分离和提纯，干燥即得聚乙烯醇与糖的共聚物。该发明具有制备工艺简单易行，对设备无特殊要求，成本低廉等特点。

Description

聚乙烯醇与糖的共聚物及其制备的方法
技术领域
本发明涉及聚乙烯醇与糖的共聚物及其制备方法，属于高分子制备及其应用领域。
背景技术
聚乙烯醇(Poly(vinyl alcohol)，简称PVA)是由聚醋酸乙烯酯经碱催化醇解而得到的一种优良的药用辅料。它具有良好的水溶性和成膜性，并且其膜的机械性能优良。安全性实验证明PVA毒性很低且无刺激性，日本和美国等都已批准用于医药和食品工业。
PVA具有合成方便、安全低毒、产品质量易于控制、价格便宜、使用方便等特点。因此，PVA是具有再次开发潜力的优良药用辅料。目前，在医药制剂中PVA主要用于制作微型胶囊的囊材、膜剂和涂膜剂的成膜材料等，应用效果良好。PVA无毒且具有优良的粘接性能，在药物制剂的生产和研究中，也常被用来做片剂的粘合剂。PVA用作片剂的骨架材料，能缓释、控释药物。PVA溶于水且具有很低的表面张力，在制备载药微球或微囊中，既可作微球或微囊的致孔剂，也可作分散介质。由于PVA具有无毒性及良好的生物相容性和力学性能，现已被广泛用于生物医用材料。作为药物载体，PVA也显示出其优越的控制释放性能。同时，糖类物质无毒、无副作用、生物相容性好且能在体内降解成可被机体吸收的小分子营养物质。淀粉、环糊精(CD)等糖类物质是被广泛应用的生物医用材料。若用简单的方法将糖类引入到PVA聚合物中，可使PVA的性能得到改变和提高，特别是将环糊精引入到聚乙烯醇聚合物后，不仅使聚乙烯醇兼有环糊精的包结功能，提高药物的缓释效果而且成本较低。因此，多糖修饰的PVA产品具有重要的应用价值。
发明内容
本发明介绍了聚乙烯醇与糖的共聚物及其制备方法。该方法是以聚乙烯醇和糖为原料，在碱性条件下“一锅”交联反应即可得到聚乙烯醇与糖的共聚物，其具有制备工艺简单易行，对设备无特殊要求，成本低廉，多糖固载量高等特点。
本发明的合成方法如下：
将PVA、糖和水加入到三颈烧瓶中，在80～90℃水浴加热下搅拌溶解，然后降温至50～70℃，并慢慢滴加浓度为30％NaOH水溶液，继续搅拌12h。
按交联剂与糖单元物质的量比，一次性将交联剂加入上述混合液中，在50～70℃下搅拌反应12h后，加入适量丙酮终止反应，得黄色溶胶，用稀盐酸中和。对所得溶胶进行分离和提纯，干燥，即得PVA与糖的共聚物。
具体实施方式    本发明的实现过程由以下实施例详细说明：
实施例一：聚乙烯醇β-环糊精共聚物1
将3.00g PVA、10.00g β-CD和40mL水加入到150mL三颈烧瓶中，90℃水浴加热下搅拌溶解，然后降温至60℃，并慢慢滴加入浓度为30％NaOH水溶液30mL，继续搅拌12h。
按环氧氯丙烷(Epi)与β-CD物质的量比为1∶1，一次性将Epi加入上述混合液中，在60℃下搅拌反应12h后，加入适量丙酮终止反应，得淡黄色溶胶，用稀盐酸中和。用乙醇沉析法对所得溶胶进行分离和提纯，然后将溶剂抽干，真空干燥，即得聚乙烯醇β-环糊精共聚物1。
1H NMR(300MHz，D2O)：δ4.9(s，7H，β-CD 1-H)，3.3～3.9(m，74H，β-CD、连接体和PVA2-H)，1.5(t，54H，PVA 1-H).
实施例二：聚乙烯醇β-环糊精共聚物2
将Epi与β-CD物质的量比为1∶2，按实施例一合成，得β-环糊精聚乙烯醇共聚物2。
1H NMR(300MHz，D2O)：δ4.9(s，7H，β-CD 1-H)，3.3～3.9(m，81H，β-CD、连接体和PVA2-H)，1.5(t，48H，PVA 1-H).
实施例三：聚乙烯醇β-环糊精共聚物3
将Epi与β-CD物质的量比为1∶4，按实施例一合成，得β-环糊精聚乙烯醇共聚物3。
1H NMR(300MHz，D2O)：δ4.9(s，7H，β-CD 1-H)，3.3～3.9(m，69H，β-CD、连接体和PVA2-H)，1.5(t，27H，PVA 1-H).
实施例四：聚乙烯醇β-环糊精共聚物4
将Epi与β-CD物质的量比为1∶7，按实施例一合成，得凝胶状β-环糊精聚乙烯醇共聚物4。
实施例五：聚乙烯醇β-环糊精共聚物5
将Epi与β-CD物质的量比为1∶10，按实施例一合成，得凝胶状β-环糊精聚乙烯醇共聚物5。
实施例六：聚乙烯醇β-环糊精淀粉共聚物
将3.00g PVA、5.00g β-CD、5.00g淀粉和40mL水加入到150mL三颈烧瓶中，90℃水浴加热下搅拌溶解，然后降温至60℃，并慢慢滴加入浓度为30％NaOH水溶液30mL，继续搅拌12h。
按Epi与β-CD物质的量比为1∶8，一次性将Epi加入上述混合液中，在60℃下搅拌反应12h后，加入适量丙酮终止反应，得淡黄色凝胶，用稀盐酸中和。用乙醇沉析法对所得溶胶进行分离和提纯，然后将溶剂抽干，真空干燥，即得聚乙烯醇β-环糊精淀粉共聚物凝胶。

Claims (5)

1、聚乙烯醇与糖的共聚物及其制备的方法，其特征在于聚乙烯醇与糖类物质共聚。
2、根据权利要求1所述的聚乙烯醇与糖类的共聚物，糖可以是单糖、低聚糖、环糊精、淀粉等糖类物质，交联剂为环氧氯丙烷或可在碱性条件下能与羟基反应的交联剂。
3、权利要求1所述的聚乙烯醇与糖的共聚物，其特征在于制备工艺包括以下步骤：
(1)将聚乙烯醇和糖共同溶于热水，待全部溶解后降温至50～70℃；
(2)在50～70℃加入浓度约为30％NaOH水溶液，反应体系中NaOH浓度为10～25％，搅拌12h；
(3)在50～70℃加入交联剂，搅拌反应12h，加入适量丙酮终止反应，用稀盐酸中和。对所得溶胶进行分离和提纯，然后将溶剂抽干，干燥，即得聚乙烯醇与糖的共聚物。
4、根据权利要求3所述的共聚物的合成，改变聚乙烯醇与多糖的比例可得到水溶性共聚物或可被水溶胀的共聚物凝胶。
5、根据权利要求3所述的共聚物的合成，改变环氧氯丙烷与多糖的比例可得到水溶性共聚物或可被水溶胀的共聚物凝胶。
CNB2006101050802A 2006-08-31 2006-08-31 聚乙烯醇β-环糊精共聚物的制备方法 Expired - Fee Related CN100554330C (zh)

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Publication number Priority date Publication date Assignee Title
CN101284896B (zh) * 2007-12-28 2010-06-02 北京航空航天大学 壳寡糖-聚l-色氨酸接枝共聚物的均相合成方法

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JP3072425B1 (ja) * 1999-07-26 2000-07-31 村田機械株式会社 ロ―ル紙の空芯受渡し装置
CN1114654C (zh) * 2001-03-27 2003-07-16 武汉大学 香芋生物全降解薄膜及其制法
CN1181123C (zh) * 2002-04-28 2004-12-22 武汉金宝生物环保科技有限公司 淀粉生物全降解薄膜及其制备方法

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* Cited by examiner, † Cited by third party
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CN101284896B (zh) * 2007-12-28 2010-06-02 北京航空航天大学 壳寡糖-聚l-色氨酸接枝共聚物的均相合成方法

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