CN108084372B - 一种盐酸林可霉素用聚合物材料的制备方法 - Google Patents

一种盐酸林可霉素用聚合物材料的制备方法 Download PDF

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CN108084372B
CN108084372B CN201711196931.3A CN201711196931A CN108084372B CN 108084372 B CN108084372 B CN 108084372B CN 201711196931 A CN201711196931 A CN 201711196931A CN 108084372 B CN108084372 B CN 108084372B
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王艺霖
王新
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Abstract

本发明涉及一种盐酸林可霉素用聚合物材料的制备方法。按重量份计,在反应釜中加入环糊精,四甲基丙基环戊二烯,双酚A环氧乙烯基酯,3,4‑环氧环己烯甲基‑3,4‑环氧环己烯酸酯,2‑(三甲基硅基)‑7‑氯呋喃并[3,2‑B]吡啶,2‑甲基呋喃‑3‑(2‑甲基‑4,5‑二氢呋喃‑3‑)硫醚,异辛基苯酚聚氧乙烯醚磺酸二乙醇胺盐,过氧化新癸酸异丙苯酯,水,聚乙烯醇,升温,反应产物经水洗,干燥,即得到盐酸林可霉素用聚合物材料。

Description

一种盐酸林可霉素用聚合物材料的制备方法
技术领域
本发明涉及一种盐酸林可霉素用助剂,尤其是一种盐酸林可霉素用聚合物材料的制备方法。
背景技术
盐酸林可霉素为窄谱抗生素,作用与红霉素相似,对革兰阳性球菌有较好作用,特别对厌气菌、金葡菌及肺炎球菌有高效。其作用机制和红霉素相似,属抑菌剂。主要抑制细菌细胞蛋白质的合成,临床主要用于敏感菌引起的各种感染,如肺炎、脑膜炎、心内膜炎、蜂窝织炎、扁桃体炎、丹毒,疖及泌尿系统感染等。由于本品可进入骨组织中,和骨有特殊亲和力,故特别适用于厌气菌引起的感染及金葡菌性骨髓炎。
CN105237593A 公开了一种盐酸林可霉素的提取方法,其工艺步骤为将林可霉素发酵液经酸化预处理、双水相萃取、丁醇提取、盐酸反萃取、活性炭脱色、丙酮结晶和干燥得到固体产物盐酸林可霉素。
CN104356179A 公开了一种盐酸林可霉素提纯工艺,其包括如下步骤:S1、吸附步骤:依次经溶解、脱色、过滤、稀释、调节pH、上柱得到饱和树脂柱;S2、水洗步骤:依次经压干、水洗、再压干得到第二次干燥的饱和树脂柱;S3、解析步骤:经饱和正丁醇解析得到解析液;S4、浓缩结晶步骤:依次经盐酸结晶、丙酮重结晶、干燥后得到成品。
现有的盐酸林可霉素所采用的提纯工艺,大多使用树脂或活性炭作为吸附剂进行吸附。有着吸附速度慢,吸附效果不强的缺点,仍需要使用其他提纯手段再次提纯,研发一种吸附速度快,容量大的新型盐酸林可霉素提纯用吸附剂,可以简化提纯环节的工艺,节省时间和能耗。
发明内容
本发明的目的是:提供一种盐酸林可霉素用聚合物材料的制备方法,其特征在于制备步骤包括:
按重量份计,在反应釜中加入环糊精,四甲基丙基环戊二烯,双酚A环氧乙烯基酯,3,4-环氧环己烯甲基-3,4-环氧环己烯酸酯,2-(三甲基硅基)-7-氯呋喃并[3,2-B]吡啶,2-甲基呋喃-3-(2-甲基-4,5-二氢呋喃-3-)硫醚,异辛基苯酚聚氧乙烯醚磺酸二乙醇胺盐,过氧化新癸酸异丙苯酯,水,聚乙烯醇,升温至75-85℃,反应15-25h,产物经水洗,干燥,即得到盐酸林可霉素用聚合物材料。
所述的四甲基丙基环戊二烯,其质量用量为环糊精的1-5%。
所述的双酚A环氧乙烯基酯,其质量用量为环糊精的1-5%。
所述的3,4-环氧环己烯甲基-3,4-环氧环己烯酸酯,其质量用量为环糊精的1-5%。
所述的2-(三甲基硅基)-7-氯呋喃并[3,2-B]吡啶,其质量用量为环糊精的0.1-1%。
所述的2-甲基呋喃-3-(2-甲基-4,5-二氢呋喃-3-)硫醚,其质量用量为环糊精的0.1-0.5%。
所述的异辛基苯酚聚氧乙烯醚磺酸二乙醇胺盐,其质量用量为环糊精的0.01-0.1%。
所述的过氧化新癸酸异丙苯酯,其质量用量为环糊精的1-5%。
所述的水,其质量用量为环糊精的300-900%。
所述的聚乙烯醇,其质量用量为环糊精的1-5%。
所述的环糊精,四甲基丙基环戊二烯,双酚A环氧乙烯基酯,3,4-环氧环己烯甲基-3,4-环氧环己烯酸酯,2-(三甲基硅基)-7-氯呋喃并[3,2-B]吡啶,2-甲基呋喃-3-(2-甲基-4,5-二氢呋喃-3-)硫醚,异辛基苯酚聚氧乙烯醚磺酸二乙醇胺盐,过氧化新癸酸异丙苯酯,水,聚乙烯醇均为市售产品。
本发明的产品具有以下有益效果:
(1)吸附剂产品具有良好的力学性能和耐热耐化性,不易破碎,不易变性,吸附效果稳定。
(2)吸附剂产品的比表面积大,吸附速度快,且吸附容量大,对于盐酸林可霉素中含有的有色杂质和有机杂质具有一定的针对性。
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
在反应釜中,加入环糊精100Kg,四甲基丙基环戊二烯2.5Kg,双酚A环氧乙烯基酯3Kg,3,4-环氧环己烯甲基-3,4-环氧环己烯酸酯2.5Kg,2-(三甲基硅基)-7-氯呋喃并[3,2-B]吡啶0.5Kg,2-甲基呋喃-3-(2-甲基-4,5-二氢呋喃-3-)硫醚0.3Kg,异辛基苯酚聚氧乙烯醚磺酸二乙醇胺盐0.05Kg,过氧化新癸酸异丙苯酯1.5Kg,水400Kg,聚乙烯醇3Kg,升温至80℃,反应20h,产物经水洗,干燥,即得到盐酸林可霉素用聚合物材料。
实施例2
在反应釜中,加入环糊精100Kg,四甲基丙基环戊二烯1Kg,双酚A环氧乙烯基酯1Kg,3,4-环氧环己烯甲基-3,4-环氧环己烯酸酯1Kg,2-(三甲基硅基)-7-氯呋喃并[3,2-B]吡啶0.1Kg,2-甲基呋喃-3-(2-甲基-4,5-二氢呋喃-3-)硫醚0.1Kg,异辛基苯酚聚氧乙烯醚磺酸二乙醇胺盐0.01Kg,过氧化新癸酸异丙苯酯1Kg,水300Kg,聚乙烯醇1Kg,升温至75℃,反应15h,产物经水洗,干燥,即得到盐酸林可霉素用聚合物材料。
实施例3
在反应釜中,加入环糊精100Kg,四甲基丙基环戊二烯5Kg,双酚A环氧乙烯基酯5Kg,3,4-环氧环己烯甲基-3,4-环氧环己烯酸酯5Kg,2-(三甲基硅基)-7-氯呋喃并[3,2-B]吡啶1Kg,2-甲基呋喃-3-(2-甲基-4,5-二氢呋喃-3-)硫醚0.5Kg,异辛基苯酚聚氧乙烯醚磺酸二乙醇胺盐0.1Kg,过氧化新癸酸异丙苯酯5Kg,水900Kg,聚乙烯醇5Kg,升温至85℃,反应25h,产物经水洗,干燥,即得到盐酸林可霉素用聚合物材料。
对比例1
不加入四甲基丙基环戊二烯,其他条件同实施例1。
对比例2
不加入双酚A环氧乙烯基酯,其他条件同实施例1。
对比例3
不加入3,4-环氧环己烯甲基-3,4-环氧环己烯酸酯,其他条件同实施例1。
对比例4
不加入2-(三甲基硅基)-7-氯呋喃并[3,2-B]吡啶,其他条件同实施例1。
对比例5
不加入2-甲基呋喃-3-(2-甲基-4,5-二氢呋喃-3-)硫醚,其他条件同实施例1。
对比例6
不加入异辛基苯酚聚氧乙烯醚磺酸二乙醇胺盐,其他条件同实施例1。
实施例4
将纯度约为95%的盐酸林可霉素粗品通入装有500g实施例1-3和对比例1-6制出的吸附剂产品的1000mL交换柱中,温度60℃,流速0.5BV/h,条件下吸附提纯,用气相色谱检测流出液的质量百分含量,见表1。
表1:不同工艺生产出的盐酸林可霉素吸附剂吸附提纯后的盐酸林可霉素纯度。

Claims (1)

1.一种盐酸林可霉素用聚合物材料的制备方法,其特征在于包括如下步骤:
按重量份计,在反应釜中加入 环糊精,四甲基丙基环戊二烯,双酚A环氧乙烯基酯,3,4-环氧环己烯甲基-3,4-环氧环己烯酸酯,2-(三甲基硅基)-7-氯呋喃并[3,2-B]吡啶,2-甲基呋喃-3-(2-甲基-4,5-二氢呋喃-3-)硫醚,异辛基苯酚聚氧乙烯醚磺酸二乙醇胺盐,过氧化新癸酸异丙苯酯,水,聚乙烯醇,升温至75-85℃,反应15-25h,产物经水洗,干燥,即得到盐酸林可霉素用聚合物材料;
所述的四甲基丙基环戊二烯,其质量用量为 环糊精的1-5%;所述的双酚A环氧乙烯基酯,其质量用量为 环糊精的1-5%;所述的3,4-环氧环己烯甲基-3,4-环氧环己烯酸酯,其质量用量为 环糊精的1-5%;所述的2-(三甲基硅基)-7-氯呋喃并[3,2-B]吡啶,其质量用量为环糊精的0.1-1%;所述的2-甲基呋喃-3-(2-甲基-4,5-二氢呋喃-3-)硫醚,其质量用量为环糊精的0.1-0.5%;所述的异辛基苯酚聚氧乙烯醚磺酸二乙醇胺盐,其质量用量为 环糊精的0.01-0.1%;所述的过氧化新癸酸异丙苯酯,其质量用量为 环糊精的1-5%;所述的水,其质量用量为 环糊精的300-900%;所述的聚乙烯醇,其质量用量为 环糊精的1-5%。
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