CN113457212A - 一种同时提高间甲基苯酚纯度和改善其色度的捕集剂制备与使用方法 - Google Patents
一种同时提高间甲基苯酚纯度和改善其色度的捕集剂制备与使用方法 Download PDFInfo
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Abstract
本发明公开了一种同时提高间甲基苯酚纯度和改善其色度的捕集剂制备与使用方法,属于分离、提纯技术领域。主要包括捕集剂应用、分离以及再生等步骤,搭配所述旋转搅拌器,将金属离子与适宜的载体混合,使用所述多孔、高比表面积捕集剂,将溶液中其他酚类杂质,定向捕集后团聚,同时,将溶液中影响色度的一些多聚物杂质,一同捕捉,实现双功能化,其应用方法,在分离、提纯技术领域中,具有高效、快捷、低成本等优势。同时,也适用于其他酚类溶液,比如,对甲基苯酚、邻甲基苯酚、苯酚等纯度的提升、色度的改善,具有较好的适用性,实用性。
Description
技术领域
本发明属于分离、提纯技术领域,具体涉及一种同时提高间甲基苯酚纯度和改善其色度的捕集剂制备与使用方法。
背景技术
甲酚作为重要的精细化工原料,在塑料、食品、染料、农药、医药等领域都具有重要用途。其获取方式,主要从煤焦油提取为主,其产品成分复杂,常含有对甲酚、间甲酚和邻甲酚等异构体,因其沸点较近,分离、提纯能耗较高,利用率一般较低。作为一种替代方式,以苯酚、甲苯作为原料,烷基化工业合成法逐渐得到推广。然而,不管何种方式生产的甲酚,总是含有少量的二甲酚杂质,更糟糕的是,其与甲酚沸点十分接近,相对挥发度接近于1,传统精馏,需要过多的塔板数,投资高、能耗大,也不易分离。
市场现流通的甲酚,色度均50Hazen左右,极易与空气中的氧结合,形成带颜色的醌类物质,限制了其在下游产品中应用,与此同时,随着国内环境利好,香料、维生素等行业得到快速发展,加大了对高纯度、低色度甲酚需求量,因此提出一种同时提高间甲基苯酚纯度和改善其色度的捕集剂制备与使用方法,便显得迫切需求,意义重大。
专利CN108147948A、CNll0683939A相继提出,低温环境下,间/对甲酚与二甲酚异构体在溶剂中,分配能力存在不同,选择适宜温度,使用常规较低沸点得复配溶剂,能够提高纯化间/对甲酚纯度、降低色度。
然而,该方法不但需要搭建低温环境,能耗高,成本大,而且均涉及到石油醚、乙二醇二甲醚、甲基环己烷、戊烷等有异味、易挥发、易燃性、有毒害化学试剂的使用,因此,该方法将会因成本、能耗、环保等原因,限制其大力推广。
发明内容
针对现有的技术不足等问题,本发明公开了一种同时提高间甲基苯酚纯度和改善其色度的捕集剂制备与使用方法,具体的,提供一种用于酚类溶液提纯与色度改善的捕集剂制备方法,即,将金属离子与适宜的载体混合,载体赋予所述捕集剂多孔、高比表面积性能,在定向络合苯酚、甲氧基酚、二甲酚、醌等其他酚类杂质同时,将溶液中影响色度的一些多聚物,比如胡敏素、多聚物、不溶物等,一同捕集,搭配独特旋转搅拌器模式,实现高效、快捷、低成本分离提纯效果。
同时,该方法也可以广泛应用于吸附分离技术领域中的其他酚类溶液,比如对甲基苯酚、邻甲基苯酚、苯酚等,纯度的提升、色度的改善,具有较好的适用性,实用性。
一种同时提高酚类物质纯度和改善其色度的捕集剂制备与使用方法,包括以下步骤:
(1)捕集剂应用:将捕集剂放入装有待处理溶液的反应器中,调整温度和转速,搅拌一段时间后,逐滴加入碱溶液,调整环境PH值,一定时间后,所述溶液由淡黄色或深黄色逐渐变淡,直至为无色;其中,所述捕集剂包括载体和负载于载体上的金属离子,所述金属离子包括但不限于Mg2+、Zn2+、Ca2+、Al3+、Fe3+、Ba2+、Pb2+、Cu2+、Cr6+、Mn2+中的一种或多种,所述载体包括但不限于分子筛、Al2O3、SiO2、TiO2、ZrO2、Fe3O4、活性炭中的一种或几种;
(2)捕集剂分离与再生:步骤(1)结束后,将所述捕集剂与处理后的溶液进行分离,分离后的捕集剂依次经过酸溶液、有机溶剂清洗后,烘干,焙烧,得到再生后的捕集剂。
进一步,所述捕集剂使用时将其装填至旋转搅拌器的格栅中,然后放入装有待处理溶液的反应器中,步骤(1)结束后,移除所述旋转搅拌器,将捕集剂与处理后的溶液进行分离。
进一步,所述金属离子优选Mg2+、Ba2+、Zn2+中的一种或几种;所述载体颗粒大小为12-40目,优选Al2O3、活性炭;所述分子筛包括但不限于3A、4A、5A中的一种或几种。
进一步,所述步骤(1)中,适宜温度和转速下,搅拌5-10min后,逐滴加入碱溶液;所述捕集剂与待处理溶液的质量比为0.005-0.025,所述温度为25-85℃,所述转速为100-700rpm;更进一步,优选所述温度为40℃,转速为400rpm。
进一步,所述步骤(1)中,所述碱溶液包括但不限于碳酸氢钠、碳酸钠、氢氧化钠、氨水中的一种或几种;所述碱溶液浓度为0.5-2.5mol/L,所述PH值范围为7.2-9,所述时间为15-90min。更进一步,所述碱溶液,优选1.2mol/L碳酸氢钠,所述PH值优选为7.6,所述时间优选为45min。
进一步,所述步骤(2)中,所述酸溶液包括但不限于卤化酸、硝酸、硫酸中的一种或几种;所述酸溶液浓度为0.5-1.5mol/L,所述有机溶剂包括但不限于甲醇、乙醇、丙酮、乙酸乙酯、二氯甲烷中的一种或几种;更进一步,所述酸溶液优选1.1mol/L稀硫酸,所述有机溶剂优选乙醇、乙酸乙酯。
进一步,所述步骤(2)中,所述烘干条件为45-105℃烘干6-8h,焙烧条件为250-450℃焙烧3-6h,焙烧气氛为空气,空气流速为5-25ml/min。
进一步,步骤(2)中,收集分离捕集剂后的溶液,添加干燥剂后,使用惰性气体驱赶液面上方空气,密封遮阳存储;所述干燥剂为无水氯化钙、无水硫酸钠中的一种或几种;所述干燥剂添加质量占为0.5-2%,所述惰性气体为氮气、氩气、氦气中的一种或几种。
进一步,所述捕集剂的制备方法为:室温环境下,将所述载体与所述金属的盐溶液混合,回收多余盐溶液,烘干,焙烧,得到所述捕集剂。
进一步,所述金属的盐溶液为卤化盐、硝酸盐、硫酸盐中的一种或几种;所述金属离子盐溶液优选Mg2+、Ba2+、Zn2+的氯化盐、硫酸盐溶液;所述金属的盐溶液与所述载体混合方式为包括但不限于浸渍、蒸发、离子交换、机械混合中一种或几种;所述载体与所述盐溶液质量配比为1.5-2.5;所述烘干条件为105-120℃烘干6-24h,焙烧条件为350-550℃焙烧3-8h。
更进一步,所述捕集剂制备中,以及所述捕集剂再生中,所述活性炭载体,烘干、焙烧,需要惰性气体氛围下进行;所述其他载体,所述捕集剂再生中,期间需要供给5-25ml/min空气。
进一步,所述酚类物质为间甲基苯酚、对甲基苯酚、邻甲基苯酚、苯酚中的一种或几种。更进一步,所述酚类物质为间甲基苯酚。
有益效果
1)本发明提供一种用于酚类溶液提纯与色度改善的捕集剂制备方法,操作简单,成本低廉,适用性强,具有双功能化作用;
2)本发明提出一种吸附分离方法,即旋转搅拌器装置,实现高效、快捷、低成本分离提纯效果;
3)本发明提供一种同时提高间甲基苯酚纯度和改善其色度的捕集剂制备与使用方法,通过载体上金属离子络合溶液中杂质酚类,将其成团聚集,同时多孔、高比表面积载体,将溶液中的胡敏素、多聚物、不溶物,一同捕集,实现一套工序,双倍效益;
4)同时,上述方法,也适用于其他酚类溶液,比如,对甲基苯酚、邻甲基苯酚、苯酚等纯度的提升、色度的改善,具有较好的适用性,实用性。
附图说明
图1是本发明的一种同时提高间甲基苯酚纯度和改善其色度的方法中所述旋转搅拌器装置示意图。
图2是本发明的一种同时提高间甲基苯酚纯度和改善其色度的方法工作原理演示图。
图3是本发明的一种同时提高间甲基苯酚纯度和改善其色度的方法处理前(A)与处理后(B)对比图。
具体实施方式
下面结合附图以较佳实施例进行进一步描述,以使本发明的优点和特征能更易于被本领域技术人员理解,从而对本发明的保护范围做出更为清楚明确的界定。
实施例1
如图1所示,所述旋转搅拌器,参数如下:
采用316L材质;直径40-50mm;高度30mm;容积30-50ml;筛网60-80目;转数100-700rpm;格栅数目2-4;反应器250-500ml;温度范围25-250℃;
捕集剂制备:
采用自制活性炭(SBET=900-1300m2/g,Vtotal=1.0-1.2cm3/g,Size:0.8-1.2mm;)作为载体,与氯化锌混合(AC∶ZnCl2=1.5∶1);在105-110℃烘干8-12h,将上述烘干后,管式电炉中350-550℃,焙烧1.5-3h,自然降为室温,期间采用0.1-0.5L/min N2氛围环境,随后,使用温和的软化水洗涤,去除表面残留盐痕,焦油、细粉等,过滤后,60-80℃下烘干8-24h;得到捕集剂,备用。
实施例2
如图2所示,捕集剂工作原理:
将实施例1中制备的捕集剂装填至所述旋转搅拌器中,采用四格栅式,添加量40.5g,通过联轴器与电机连接,穿过封板密封圈,放入250ml装好待处理溶液反应器底部1/3处,盖好封盖。
通过旋转搅拌器旋转,捕集剂中的金属离子与溶液中的苯酚、甲氧基酚、二甲酚、醌,等杂质酚类发生络合反应,将其捕捉聚集起来,期间可以通过调节体系PH值,实现定向吸附分离效果,与此同时,所采用的多孔、高比表面积载体,将溶液中的胡敏素、多聚物、不溶物,一同捕集,实现双功能化,一套工序,双倍效益。
实施例3
采用GC分析法,依据文献余少文,王彩媚,陈英.气相色谱法检测间甲酚中有关物质.药物分析杂志.2020,40(7):1284-1291;
修改如下:
气相色谱:7820A;毛细管柱:安捷伦CP-Chirasil-Dex CB(25m×0.25mm×0.25μm);检测器:FID;进样口:250℃;检测器:250℃;进样量:0.2μL,分流比80∶1;柱温:初始60℃,以10℃/min升温至140℃,再以5℃/min升温至220℃,保持1min;载气:氮气;样品浓度:5-10mg/ml;溶剂:正戊醇。
实施例4
如图3所示,处理条件如下:162ml淡黄色溶液A,成分如下表所示;转速为120rpm,反应温度45℃;搅拌10min后,加入1mol/L Na2CO3溶液,调节PH值为7.6;提高搅拌转速至400rpm;处理时间45min;获得低色度溶液B;采用实施例1装置,基于实施例2原理,实施例3分析方法,数据结果如下:
,表1
以上所述仅为本发明的实施例,并非因此限制本发明的专利范围,凡是利用本发明说明书及附图内容所作的等效结构或等效流程变换,或直接或间接运用在其他相关的技术领域,均同理包括在本发明的专利保护范围内。
Claims (10)
1.一种提高酚类物质纯度和改善其色度的方法,其特征在于,所述方法包括以下步骤:
(1)捕集剂应用:将捕集剂放入装有待处理溶液的反应器中,调整温度和转速,搅拌一段时间后,逐滴加入碱溶液,调整环境PH值,一定时间后,所述溶液由淡黄色或深黄色逐渐变淡,直至为无色;其中,所述捕集剂包括载体和负载于载体上的金属离子,所述金属离子为Mg2+、Zn2+、Ca2+、Al3+、Fe3+、Ba2+、Pb2+、Cu2+、Cr6+、Mn2+中的一种或多种,所述载体为分子筛、Al2O3、SiO2、TiO2、ZrO2、Fe3O4、活性炭中的一种或多种;
(2)捕集剂分离与再生:步骤(1)结束后,将所述捕集剂与处理后的溶液进行分离,分离后的捕集剂依次经过酸溶液、有机溶剂清洗后,烘干,焙烧,得到再生后的捕集剂。
2.根据权利要求l所述的一种提高酚类物质纯度和改善其色度的方法,其特征在于,所述捕集剂使用时装填至旋转搅拌器的格栅中,然后放入装有待处理溶液的反应器中,步骤(1)结束后,移除所述旋转搅拌器,将捕集剂与处理后的溶液进行分离。
3.根据权利要求1所述的一种提高酚类物质纯度和改善其色度的方法,其特征在于,所述步骤(1)中,适宜温度和转速下,搅拌5-10min后,逐滴加入碱溶液;所述捕集剂与待处理溶液的质量比为0.005-0.025,所述温度为25-85℃,所述转速为100-700rpm;所述分子筛包括3A、4A、5A中的一种或多种;所述金属离子为Mg2+、Ba2+、Zn2+中的一种或几种。
4.根据权利要求1所述的一种提高酚类物质纯度和改善其色度的方法,其特征在于,所述步骤(1)中,所述碱溶液为碳酸氢钠、碳酸钠、氢氧化钠、氨水中的一种或多种;所述碱溶液浓度为0.5-2.5mol/L,所述PH值范围为7.2-9,所述时间为15-90min。
5.根据权利要求1所述的一种提高酚类物质纯度和改善其色度的方法,其特征在于,所述步骤(2)中,所述酸溶液为卤化酸、硝酸、硫酸中的一种或几种;所述酸溶液浓度为0.5-1.5mol/L,所述有机溶剂为甲醇、乙醇、丙酮、乙酸乙酯、二氯甲烷中的一种或几种;所述烘干条件为45-105℃烘干6-8h,焙烧条件为250-450℃焙烧3-6h,焙烧气氛为空气,空气流速为5-25ml/min。
6.根据权利要求1所述的一种提高酚类物质纯度和改善其色度的方法,其特征在于,步骤(2)中,收集分离捕集剂后的溶液,添加干燥剂后,使用惰性气体驱赶液面上方空气,密封遮阳存储;所述干燥剂为无水氯化钙、无水硫酸钠中的一种或几种;所述干燥剂添加质量占为0.5-2%,所述惰性气体为氮气、氩气、氦气中的一种或几种。
7.根据权利要求1所述的一种提高酚类物质纯度和改善其色度的方法,其特征在于,所述捕集剂的制备方法为:室温环境下,将所述载体与所述金属的盐溶液混合,回收多余盐溶液,烘干,焙烧,得到所述捕集剂。
8.根据权利要求7所述的一种提高酚类物质纯度和改善其色度的方法,其特征在于,所述金属的盐溶液为卤化盐、硝酸盐、硫酸盐中的一种或几种;所述金属的盐溶液与所述载体混合方式为:浸渍、蒸发、离子交换、机械混合中一种或几种;所述载体与所述盐溶液质量配比为1.5-2.5;所述烘干条件为105-120℃烘干6-24h,焙烧条件为350-550℃焙烧3-8h。
9.根据权利要求1所述的一种提高酚类物质纯度和改善其色度的方法,其特征在于,所述酚类物质为间甲基苯酚、对甲基苯酚、邻甲基苯酚、苯酚中的一种或几种。
10.根据权利要求9所述的一种提高酚类物质纯度和改善其色度的方法,其特征在于,所述酚类物质为间甲基苯酚。
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