CN114933390A - 一种盐酸多西环素生产中产生的含苯胺类废水的处理方法 - Google Patents
一种盐酸多西环素生产中产生的含苯胺类废水的处理方法 Download PDFInfo
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Abstract
本发明公开了一种盐酸多西环素生产中产生的含苯胺类废水的处理方法,属于废水处理技术领域。该方法包括:将回收乙酰苯胺母液先调pH值后蒸馏浓缩;蒸馏产生蒸馏液不降温,高温下经过活性炭多级串联吸附处理;经吸附后的废水直接进行高温芬顿处理,调节废水pH,加入铁屑搅拌一段时间后加入双氧水处理;将上述处理过的废水加入PAC和阴离子PAM混合溶液絮凝静置处理后,分析苯胺含量和COD值。该方法采用高温活性炭吸附法、高温芬顿法以及PAC+阴离子PAM混合絮凝法联用处理苯胺废水,成本较为低廉且高效,处理后废水的苯胺值可以降到1ppm以下,且废水的COD值也下降明显,减少环境污染,实现工业废水再利用,满足环保要求。
Description
技术领域
本发明属于废水处理技术领域,具体涉及一种苯胺类废水的处理方法。
背景技术
盐酸多西环素是由土霉素经过氯代、脱水、氢化、成盐等步骤制得,其中氯代反应是指土霉素在甲醇溶液中与氯代乙酰苯胺反应得到11α-氯-6,12-半缩酮土霉素的过程,其母液为含有乙酰苯胺的甲醇溶液,将甲醇回收,所得蒸馏残渣主要为乙酰苯胺、四环素的降解产物及少量甲醇,因此将蒸馏残渣与清水一定比例混合加热过滤,滤液降温再过滤即可得回收乙酰苯胺,所得滤液中含有乙酰苯胺和少量甲醇,将该滤液进行蒸馏浓缩处理时,就会产生含有苯胺、少量乙酰苯胺和甲醇的废水。而苯胺类废水具有很强的生物毒性且不易生物降解,对环境和水体的污染相当严重。随着工业的发展,会有越来越多的苯胺类废水排入环境中,因此,苯胺类废水的治理越来越引起有关部门的重视。为减轻苯胺类废水对环境的污染,保护环境,实现对废水的有效治理已成为世界范围内环境保护领域急需解决的难题。
现有苯胺类废水处理技术主要有:1)物理法:包括吸附法、萃取法、液膜分离法等;2)化学法:包括芬顿氧化法、光催化氧化法、超临界水氧化法、二氧化氯氧化法、超声波降解法、电化学降解法等;3)生物法:包括好氧生化降解法、厌氧生化降解法、优势菌处理法等。对于这几种苯胺类废水的传统处理方法而言,化学法和生物法不能够回收利用苯胺,物理法虽然能够回收苯胺,但单一的物理法对苯胺去处理效率很难达到国家标准。而目前我国大部分企业对含苯胺类废水通常采用单一的氧化法处理,难以取得理想的效果,因此,迫切需要改进含苯胺类废水的处理方法,将毒性高、难生物讲解的污染物尽可能的降解或转化为易降解的物质,经简单的处理以达到较好的效果。
发明内容
针对现有技术中存在的问题,本发明要解决的技术问题在于提供一种苯胺类废水的处理方法,该处理方法可以减少环境污染,实现工业废水再利用,为企业带来利润,满足环保要求。
为了解决上述问题,本发明所采用的技术方案如下:
一种盐酸多西环素生产中产生的含苯胺类废水的处理方法,包括以下步骤:
1)将回收乙酰苯胺母液调pH值后蒸馏;
2)将蒸馏液不降温,高温下经过活性炭多级串联吸附处理;
3)经吸附后的废水直接进行高温芬顿处理,调节废水pH为3-4,加入铁屑搅拌一段时间后加入双氧水处理;
4)将上述处理过的废水加入PAC和阴离子PAM混合溶液絮凝静置处理。
所述苯胺类废水的处理方法,步骤1)中,将母液调至pH值为5~6。
所述苯胺类废水的处理方法,步骤2)中,吸附法采用活性炭多级串联吸附,废水的温度为80-90℃。
所述苯胺类废水的处理方法,高温芬顿的温度为70-80℃。
所述苯胺类废水的处理方法,铁屑的加入质量为废水中苯胺质量的3-5倍,H2O2与Fe2+的摩尔比为8-12。
所述苯胺类废水的处理方法,废水加完双氧水处理后,用液碱调节废水pH为6.5-7.5。
所述苯胺类废水的处理方法,配制PAC溶液浓度为5%~10%,阴离子PAM溶液浓度为0.2%~0.5%。废水与PAC溶液、阴离子PAM溶液的质量比为:1∶0.001~0.002∶0.001~0.002。
有益效果:与现有的技术相比,本发明的优点包括:
本发明主要是采用采用活性炭吸附法、高温芬顿法以及絮凝法联用来处理苯胺废水,本发明中使用的吸附方法为高温下废水进行活性炭多级串联吸附,虽然高温下吸附会使吸附效率下降,但是本发明采用活性炭多级串联的方式来吸附,可以保证对废水完全吸附的同时,还能保证活性炭会吸附饱和。工业生产过程中回收乙酰苯胺的废水经蒸馏后不需降温直接进活性炭吸附柱,吸附后的废水温度较高有利于下一步的芬顿反应,且使用多级活性炭吸附以及高温芬顿法效率更高,比起传统的处理方法,其工艺较为简单,也更加节能。并且采用PAC+PAM混合絮凝的方式处理芬顿处理后的废水,降低色度的同时,大大降低了絮凝的时间。采取上述步骤可以将毒性高、难生物降解的污染物尽可能的降解或转化为易降解的物质,处理效果较好,且苯胺的去除率达到99%以上,COD的去除率达到99%以上。
具体实施方式
为使本发明的上述目的、特征和优点能够更加明显易懂,下面结合具体实施例对本发明的具体实施方式做详细的说明。
实施例1
一种盐酸多西环素生产中产生的含苯胺类废水的处理方法,步骤如下:
1)取车间回收乙酰苯胺母液1000mL(乙酰苯胺:0.51%,苯胺:1525ppm,COD:28000ppm),使用氢氧化钠溶液调pH值为:5.2,蒸馏得蒸馏液(苯胺:1123ppm,COD:12350ppm)800mL,将蒸馏液加入烧杯中,连接搅拌器,开动搅拌,常温下加入活性炭进行吸附;
2)经吸附后的废水温度控制在25℃,用HCl调节pH=4,加入4.5g铁屑,搅拌10min后,加入90mL 30%H2O2溶液,搅拌20min;
3)将上述废水用液碱调节pH=7.5,先加入1.5g 10%的PAC溶液,再加入1.5g0.5%的PAM溶液,搅拌0.5h;
4)将上述废水静置30min后过滤,取样检测,测得苯胺含量为107ppm,COD值为1825ppm,苯胺去除率为92.9%,COD去除率为93.5%。
实施例2
一种盐酸多西环素生产中产生的含苯胺类废水的处理方法,步骤如下:
1)取车间回收乙酰苯胺母液1000mL(乙酰苯胺:0.51%,苯胺:1525ppm,COD:28000ppm),使用氢氧化钠溶液调pH值为:5.5,蒸馏得蒸馏液(苯胺:1125ppm,COD:12360ppm)800mL,将蒸馏液加入烧杯中,连接搅拌器,开动搅拌,80℃下加入活性炭保温进行吸附;
2)经吸附后的废水温度控制在75℃,用HCl调节pH=3.5,加入4.5g铁屑,搅拌10min后,加入90mL 30%H2O2溶液,搅拌20min;
3)将上述废水用液碱调节pH=7.5,先加入1.5g 10%的PAC溶液,再加入1.5g0.5%的PAM溶液,搅拌0.5h;
4)将上述废水静置30min后过滤,取样检测,测得苯胺含量为4.2ppm,COD值为285ppm,苯胺去除率为99.72%,COD去除率为98.98%。
实施例3
一种盐酸多西环素生产中产生的含苯胺类废水的处理方法,步骤如下:
1)将车间回收乙酰苯胺母液1000L(乙酰苯胺:0.55%,苯胺:1625ppm,COD:32500ppm)使用氢氧化钠溶液调pH值为:6,蒸馏所得蒸馏液不降温,直接通入多级活性炭串联吸附柱;
2)经吸附后的废水温度控制在80℃,用HCl调节pH=3,加入4Kg铁屑,搅拌10min后加入80L 30%H2O2溶液,搅拌30min;
3)将上述废水用液碱调节pH=7.5,1Kg 9%的PAC溶液,再加入1Kg0.5%的PAM溶液,搅拌0.5h;
4)将上述废水静置30min后,取样检测,测得苯胺含量为0.8ppm,COD值为185ppm,苯胺去除率为99.95%,COD去除率为99.43%。
Claims (8)
1.一种盐酸多西环素生产中产生的含苯胺类废水的处理方法,其特征在于,步骤包括:
1)将回收乙酰苯胺母液调pH值后蒸馏;
2)将蒸馏液不降温,高温下经过活性炭多级串联吸附处理;
3)经吸附后的废水直接进行高温芬顿处理,调节废水pH为3-4,加入铁屑搅拌一段时间后加入双氧水处理;
4)将上述处理过的废水加入PAC和阴离子PAM混合溶液絮凝静置处理。
2.根据权利要求1所述的含苯胺类废水的处理方法,其特征在于:步骤1)中,将母液调至pH值为5~6。
3.根据权利要求1所述的含苯胺类废水的处理方法,其特征在于:步骤2)中,吸附法采用活性炭多级串联吸附,废水的温度为80-90℃。
4.根据权利要求1所述的含苯胺类废水的处理方法,其特征在于:步骤3)中,高温芬顿处理温度为70-80℃。
5.根据权利要求1所述的含苯胺类废水的处理方法,其特征在于:步骤3)中,铁屑的加入量为废水中苯胺量的3-5倍,H2O2与Fe2+的摩尔比为8-12。
6.根据权利要求1所述的含苯胺类废水的处理方法,其特征在于:步骤3)中,废水加完双氧水处理后,用液碱调节废水pH为6.5-7.5。
7.根据权利要求1所述的含苯胺类废水的处理方法,其特征在于:步骤4)中,配制PAC溶液浓度为5%~10%,阴离子PAM溶液浓度为0.2%~0.5%。
8.根据权利要求8所述的含苯胺类废水的处理方法,其特征在于:步骤4)中,所述废水与PAC溶液、阴离子PAM溶液的质量比为:1∶0.001~0.002∶0.001~0.002。
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CN110921898A (zh) * | 2019-12-04 | 2020-03-27 | 山东潍坊润丰化工股份有限公司 | 一种含氟苯胺类化合物的废水处理方法 |
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CN110282798A (zh) * | 2019-06-14 | 2019-09-27 | 广东省石油与精细化工研究院 | 一种合成取代苯并咪唑的有机废水的处理方法 |
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