CN1250029A - 多元共聚复合固体净水剂的生产方法 - Google Patents
多元共聚复合固体净水剂的生产方法 Download PDFInfo
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- NBIIXXVUZAFLBC-UHFFFAOYSA-N phosphoric acid Substances OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 19
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- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 description 2
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Abstract
多元共聚复合固体净水剂的生产方法,其特征是将七水硫酸亚铁在硫磷混酸中改性,以硝氯氧化剂进行氧化,经与铝酸盐复配增聚后,加入磷酸根离子,再与羧酸衍生物中酰胺的水解混合物接技共聚,最后加入晶种而制得本发明产品。本方法中氧化时间短,氧化剂用量少;磷酸根离子的介入提高了聚合物中羟基的稳定性;采用接枝共聚和加入晶种制备固体产品,较传统的脱水干燥法和药剂催化固化法节约能源,降低成本,并可制得高盐基度高稳定性产品,其净化能力强,对水质的pH值范围适应更广。
Description
本发明涉及多元共聚复合固体净水剂的生产方法,具体来讲是改性聚磷硫酸铝铁固体净水剂的生产方法。
无机絮凝剂的应用历史悠久,但无机高分子絮凝剂却是在六十年代后期才在世界上发展起来的,它比原有传统药剂絮凝效果高得多,而价格相应较低,因此有逐步成为主流药剂的趋势。我国生产聚铝与聚铁,陆续发展了多种原料和工艺制造方法,基本上是结合了我国的条件,建立起独具特色的工艺路线和生产体系,满足了我国饮用水和废水处理的发展需要。近年来,研制和应用聚合铝、铁、硅及各种复合型絮凝剂已成为热点。无机高分子絮凝剂的品种在我国已逐步形成系列:阳离子型的有聚合氯化铝(PAC)、聚合硫酸铝(PAS)、聚合磷酸铝(PAP)、聚合硫酸铁(PFS)、聚合氯化铁(PFC)、聚合磷酸铁(PFP);阴离子型的有活化硅酸(AS)、聚合硅酸(PS);无机复合型的有聚合氯化铝铁(PAFC)、聚硅酸硫酸铁(PFSS)、聚合硅酸硫酸铝(PASS)、聚合硅酸氯化铁(PFSC)、聚合氯硫酸铁(PFCS)、聚合硅酸铝(PASI)、聚合硅酸铁(PFSI)、聚合硅酸铝铁(PAFSI)、聚合磷酸铝铁(PAFP)、硅钙复合型聚合氯化铁(SCPAFC)等。美于净水剂国内已有数十种专利,如CN1156127A公开了一种多元共聚铁系净水剂的生产方法,是以硫酸亚铁和硫酸为主要原料,以硝酸锌、硝酸镁、硝酸钙为催化剂,以磷酸、盐酸为改性剂,在加温加压及充氧的条件下进行氧化、水解和聚合反应,约一小时内即可制得一种盐基度≥20%的多元共聚铁系净水剂。该净水剂成本低,净水效果优越,但生产工艺较复杂,对设备要求苛刻,且产品为液态,含水率高,不便于运输,聚合物羟基稳定性也差。
本发明的目的,在于提供一种生产高盐基度,聚合物羟基稳定性好的多元共聚复合固体净水剂的生产方法。
本发明原理如下:将七水硫酸亚铁在由硫酸、磷酸组成的混酸中于120°~140℃条件下先进行改性,然后以硝氯氧化剂于50°~75℃条件下进行氧化,经与铝酸盐复配增聚后,加入磷酸根离子对三价铁进行络合,再与羧酸衍生物中酰胺的水解混合物接枝共聚,最后加入铁盐或铝盐作晶种,从而制得本发明产品。虽然本发明产品是在聚合铝铁基础上合成的,但由于磷酸根离子介入,使两者的性能和使用PH值范围有本质的不同,仅管磷酸根参与反应的机理目前尚不很清楚,但它可直接与羟基多核络合物发生配位作用是肯定的。前述的改性剂中,硫酸和磷酸的重量比是1∶0.4~0.8;硝氯氧化剂中,硝酸和氯酸盐的重量比是2.5~3.5∶1;羧酸衍生物中酰胺可以是聚丙烯酰胺(PAM),也可以是部分水解聚丙烯酰胺(PHP)。
本方法中先对七水硫酸亚铁进行改性,使氧化工序具有时间短,温度低,氧化剂用量少和不污染环境的突出优点;磷酸根离子的介入,较大程度地提高了聚合物中羟基的稳定性;采用羧酸衍生物中酰胺的水解混合物接枝共聚和加入晶种制备固体产品,较传统的脱水干燥法或药剂催化固化法节约能源,降低成本,并可制得高盐基度、高稳定性产品,其净化能力强,对水质的PH值范围适应更广。
本发明产品与聚铁、聚铝净水剂产品稳定性和净化效果对比情况如下表:
在碱性原水中与聚铝聚铁净化效果对比数据
以下实施例可用来补充说明本发明:
实施例一:量取54ml硫磷混酸投入反应器中加热至120°~140℃,加入540g FeSO4.7H2O恒温反应40分钟。冷却物料至50℃,加入47ml硝氯氧化剂,待反应态消失后,加入66g Na3PO4于50°~75℃条件反应30分钟。然后加入14g PHP水解混合物恒温搅拌30分钟,再加入3g氯化铁恒温10分钟后,装入塑料袋中保温3~4小时。制得本发明产品531g,其盐基度26.51%,全铁含量19.60%。
实施例二:量取51ml硫磷混酸和100ml水投入反应器中加热至120°~140℃,加入34g Al(OH)3反应20分钟后,再加入500g FeSO4·7H2O。其余步骤同实施例一,Na3PO4加入量84g,氯化铝2.5g。制得本发明产品501g,其盐基度24.98%,全铁含量19.33%。
实施例三:工艺条件和步骤同实施例一,物料加入量是:硫磷混酸98kg,FeSO4·7H2O 3000kg,硝氯氧化剂230kg,Na2Al2O4216kg,PHP水解混合物56kg,氯化铝6kg。制得本发明产品3102kg,其盐基度25.36%,全铁含量18.84%。
实施例四:将3400kg FeSO4·7H2O投入反应器中加热溶解,注入107kg硫磷混酸。其余工艺条件和步骤同实施例三,物料加入量是:硝氯氧化剂260kg,Na2Al2O4245kg,PHP水解混合物62kg,氯化铁6.6kg。制得本发明产品3516kg,其盐基度25.41%,全铁含量18.76%。
Claims (4)
1、多元共聚复合固体净水剂的生产方法,其特征是:将七水硫酸亚铁在由硫酸、磷酸组成的混酸中于120°~140℃条件下先进行改性,然后以硝氯氧化剂于50°~75℃条件下进行氧化,经与铝酸盐复配增聚后,加入磷酸根离子对三价铁进行络合,再与羧酸衍生物中酰胺的水解混合物接枝共聚,最后加入铁盐或铝盐作晶种,从而制得本发明产品。
2、按照权利要求1所述的生产方法,其特征是:对七水硫酸亚铁的改性剂中,硫酸和磷酸的重量比是1∶0.4~0.8。
3、按照权利要求1所述的生产方法,其特征是:硝氯氧化剂中,硝酸和氯酸盐的重量比是2.5~3.5∶1。
4、按照权利要求1所述的生产方法,其特征是:羧酸衍生物中酰胺可以是聚丙烯酰胺(PAM),也可以是部分水解聚丙烯酰胺(PHP)。
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103203212A (zh) * | 2013-04-28 | 2013-07-17 | 湖南科技大学 | 一种聚磷硫酸铝铁絮凝剂的制备方法及应用 |
CN110282801A (zh) * | 2019-06-26 | 2019-09-27 | 绍兴绿嘉环保科技有限公司 | 一种利用废水回收生产聚铁净水剂的工艺 |
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
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CN103203212A (zh) * | 2013-04-28 | 2013-07-17 | 湖南科技大学 | 一种聚磷硫酸铝铁絮凝剂的制备方法及应用 |
CN103203212B (zh) * | 2013-04-28 | 2014-11-19 | 湖南科技大学 | 一种聚磷硫酸铝铁絮凝剂的制备方法及应用 |
CN110282801A (zh) * | 2019-06-26 | 2019-09-27 | 绍兴绿嘉环保科技有限公司 | 一种利用废水回收生产聚铁净水剂的工艺 |
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