CN114804375B - 一种生物黏泥分散抑制剂及其制备方法和应用 - Google Patents
一种生物黏泥分散抑制剂及其制备方法和应用 Download PDFInfo
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- CN114804375B CN114804375B CN202110124523.7A CN202110124523A CN114804375B CN 114804375 B CN114804375 B CN 114804375B CN 202110124523 A CN202110124523 A CN 202110124523A CN 114804375 B CN114804375 B CN 114804375B
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- dispersion inhibitor
- inhibitor according
- polyethylene glycol
- unsaturated carboxylic
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Abstract
本发明涉及一种适用于循环水冷却水的生物黏泥分散抑制剂及其制备方法和应用。所述的生物黏泥分散抑制剂由酰胺化合物、不饱和羧酸与聚乙二醇共聚物、胺基聚醚、水组成，各组分的质量比为2～30:3～30:3～40:40～90。本发明提供的生物黏泥分散抑制剂，可有效剥离、分散生物黏泥，并持续抑制生物黏泥的滋生。
Description
技术领域
本发明涉及一种生物黏泥分散抑制剂及其制备方法和应用。
背景技术
工业循环冷却水在正常运行时，一般采用氧化性杀生剂与非氧化性杀生剂交替投加控制微生物和生物黏泥。目前非氧化性杀生剂为冲击性投加方式，容易引起较大水质波动，需进行排污置换，且浓度较低时对生物黏泥剥离分散效果不佳。而工业循环冷却水中出现物料泄漏或其它异常状况时，极易导致生物黏泥大量滋生，此时常规的氧化性杀生剂、非氧化性杀生剂已不能有效杀灭生物黏泥中的细菌，也不能有效去除金属管壁上的生物黏泥，此时需投加大量的高效剥离清洗剂进行清洗，这会引起循环水浊度、COD大幅上升，水质严重恶化，需对循环冷却水进行大排大补。可见，正常运行时冲击式投加非氧化性杀生剂、异常时投加高效剥离清洗剂，都需要对循环水进行排污置换，而污水处理厂一般难以接收、处理这股排污水，并且这些排污水中含有大量杀生剂，容易对污水处理厂的微生物菌群造成破坏。
CN103535369A公开了一种生物粘泥抑制剂及其制备方法，其特征在于按重量百分比由以下组分组成：聚二亚己基三胺盐酸胍5-30％、异噻唑啉酮1-10％、有机溴1-10％、醇溶剂5-40％，余量为水。其中的有效组分均属于非氧化性杀生剂，具有较好的杀生性，但对已大量滋生的生物黏泥不具有较好的分散性。
CN104628162A公开了一种生物粘泥剥离剂及剥离循环冷却水系统中生物粘泥的方法，该生物粘泥剥离剂包括A剂和B剂，A剂为金属硼氢化物和氨基多羧酸盐，B剂为烷基酚聚氧乙烯醚，A剂和B剂各自独立保存。CN104629920A公开了一种生物粘泥剥离剂及剥离循环冷却水系统中生物粘泥的方法，该生物粘泥剥离剂包括A剂和B剂，A剂为金属硼氢化物和氨基多羧酸盐，B剂为季磷盐，A剂和B剂各自独立保存。这两件专利中的金属硼氢化物还原性极强，与水、潮湿空气、酸极易反应生成易燃烧、爆炸的氢气，不宜在工业循环冷却水中大量使用。
发明内容
本发明的目的在于提供一种能够有效剥离、分散生物黏泥并持续抑制黏泥滋生的的生物黏泥分散抑制剂及其制备方法。
本发明还提供上述生物黏泥分散抑制剂在循环水冷却水中的应用。
本发明提供的生物黏泥分散抑制剂，包括酰胺化合物、不饱和羧酸与聚乙二醇共聚物、胺基聚醚和水，各组分的质量比为2～30:3～30:3～40:40～90。
优选地，所述的生物黏泥分散剂包括酰胺化合物、不饱和羧酸与聚乙二醇共聚物、胺基聚醚、水组成，各组分的质量比为5～20:5～20:5～20:50～80。
根据本发明，所述的酰胺化合物可以为脂肪酸与氨或胺的缩合产物。
其中所述的脂肪酸选自C6-C30，优选C8-C24脂肪酸，例如肉桂酸、辛酸、癸酸、十二酸、十四酸、十六酸、十八酸、二十酸、二十二酸、二十四酸、油酸、反式油酸、椰油酸、肉豆蔻油酸、棕榈油酸、蓖麻油酸、芥酸、松香酸等。
其中所述的胺选自C1-C8，优选C1-C6的单胺或二胺，甲胺、二甲胺、乙胺、丙胺、二乙胺、乙二胺、丙二胺、丁二胺、戊二胺、己二胺等。
根据本发明，所述的酰胺化合物还可以为脂肪胺与有机酸的缩合产物。
其中所述的脂肪胺选自C6-C30，优选C8-C24脂肪胺，例如辛胺、癸胺、十二胺、十四胺、十六胺、十八胺、油胺、松香胺等。
其中所述的有机酸选自C1-C8，优选C1-C6的一元羧酸或二元羧酸，可以是饱和酸也可以是不饱和酸，优选甲酸、乙酸、丙酸、丁酸、丙烯酸、草酸、丙二酸、丁二酸、马来酸酐、柠檬酸等。
根据本发明，所述的不饱和羧酸与聚乙二醇共聚物为不饱和羧酸与烯丙氧基聚乙二醇单体的共聚物，重均分子量为2000～200000，优选6000～100000。所述共聚物可以参考专利CN110066029A的制备方法，也可以按以下方法制备：(1)将烯丙氧基聚乙二醇与磺酸或羧酸反应，得到烯丙氧基聚乙二醇磺酸盐、烯丙氧基聚乙二醇羧酸盐；(2)将不饱和羧酸，如丙烯酸、马来酸酐、衣康酸等，与烯丙氧基聚乙二醇单体，如烯丙氧基聚乙二醇、烯丙氧基聚乙二醇磺酸盐、烯丙氧基聚乙二醇羧酸盐，进行聚合反应。
其中所述不饱和羧酸选自C3-C10不饱和羧酸，优选为丙烯酸、甲基丙烯酸、马来酸、马来酸酐、衣康酸、肉桂酸等。
其中所述的烯丙氧基聚乙二醇单体选自烯丙氧基聚乙二醇、烯丙氧基聚乙二醇磺酸盐、烯丙氧基聚乙二醇羧酸盐等。
根据本发明，所述的胺基聚醚为有机胺与环氧乙烷加成的产物，通式为
其中R1、R2为H、烷基、环烷基或芳香基，但不同时为H，且R1、R2总碳数为8～40，R3为H或C1～C4的低碳烷基，聚合度n为2～40。优选R1、R2总碳数为12～30，R3为H或C1～C4的低碳烷基，聚合度n为4～20。
所述胺基聚醚可以按以下方法制备：在反应器中加入有机胺和碱，控制真空度为0～0.005MPa，升温至120～140℃，加入环氧乙烷，在140～160℃下反应，当反应器内压力降至0.01MPa以下，表明反应完成，降至室温，出料即得胺基聚醚。
其中，有机胺与环氧乙烷物质的量之比为1:2～1:40，碱占有机胺和环氧乙烷质量之和的0.1％～1.0％。
所述的碱可以是无机碱，如氢氧化钠、氢氧化钾、氢氧化锂、氢氧化镁等。
本发明生物黏泥分散抑制剂中，还可以包含表面活性剂、醇类、与水互溶的有机溶剂等。
本发明提供的生物黏泥分散抑制剂的制备方法包括，将酰胺化合物、不饱和羧酸与聚乙二醇共聚物、胺基聚醚和水，按照各组分的质量比为2～30:3～30:3～40:40～90混合均匀。
所述的生物黏泥分散抑制剂在循环冷却水中的应用，加药浓度一般为2～100mg/L，优选5～40mg/L。
本申请发明人发现，生物黏泥易吸附、沉积在金属表面，其主要成分是蛋白质、多肽和其它有机物。为了解决生物黏泥的问题，一方面是要对已产生的生物黏泥进行剥离、分散，另一方面是抑制初始产生的、微量的生物黏泥继续滋生、聚集成大量的生物黏泥。而本发明中的酰胺化合物具有长烷基链，共聚物具有水溶性、油溶性，胺基聚醚具有亲水性、亲油性，它们可以浸润、渗透至生物黏泥内部，从而将已产生的生物黏泥从金属表面剥离、分散下来，另外也能将刚刚形成的微量生物黏泥包覆、分散在水中，从而抑制其继续长大。这些分散在水中生物黏泥，可以随循环水排污水排出系统、或被循环水旁滤系统去除。
本发明的生物黏泥分散抑制剂，具有良好的表面活性和分散性，既能对已产生的大量生物黏泥进行剥离、分散，也能抑制初始产生的、微量的生物黏泥继续滋生、长大和沉积。
具体实施方式
应当理解的是，此处所描述的具体实施方式仅用于说明和解释本发明，并不用于限制本发明。
实施例及对比例中，酰胺化合物购自北京伊诺凯科技有限公司，如肉桂酸酰胺、辛酸酰胺、十二酸酰胺等。
制备例1
实施例及对比例中，胺基聚醚为自制，制备方法为：将正辛胺、氢氧化钠投加至反应瓶，抽真空至0.002MPa，升温至130℃，加入环氧乙烷，其中正辛胺和环氧乙烷物质的量之比为1:5，氢氧化钠占正辛胺和环氧乙烷质量之和的0.3％，在140℃下反应，当压力降至0.01MPa以下后，降至室温，出料，即得正辛胺聚乙二醇。
制备例2
实施例及对比例中，胺基聚醚为自制，制备方法为：将十二胺、氢氧化钠投加至反应瓶，抽真空至0.002MPa，升温至130℃，加入环氧乙烷，其中十二胺和环氧乙烷物质的量之比为1:10，氢氧化钠占十二胺和环氧乙烷质量之和的0.5％，在150℃下反应，当压力降至0.01MPa以下后，降至室温，出料，即得十二胺聚乙二醇。
制备例3
按照制备例2的方法，不同的是，十二胺改成十四胺。
制备例4
按照制备例2的方法，不同的是，十二胺改成十六胺。
制备例5
按照制备例2的方法，不同的是，十二胺改成油胺。
实施例1
生物黏泥分散抑制剂的制备：2g肉桂酸酰胺、3g丙烯酸-烯丙氧基聚乙二醇、5g正辛胺聚乙二醇与90g蒸馏水混合，配制成100g分散抑制剂A1。
实施例2
生物黏泥分散抑制剂的制备：20g辛酸酰胺、5g丙烯酸-烯丙氧基聚乙二醇磺酸盐、5g十二胺聚乙二醇与70g蒸馏水混合，配制成100g分散抑制剂A2。
实施例3
生物黏泥分散抑制剂的制备：5g十二酸酰胺、20g马来酸酐-烯丙氧基聚乙二醇羧酸盐、5g十四胺聚乙二醇与70g蒸馏水混合，配制成100g分散抑制剂A3。
实施例4
生物黏泥分散抑制剂的制备：5g十六酸酰胺、5g衣康酸-烯丙氧基聚乙二醇、20g十六胺聚乙二醇与70g蒸馏水混合，配制成100g分散抑制剂A4。
实施例5
生物黏泥分散抑制剂的制备：10g油酸酰胺、10g丙烯酸-烯丙氧基聚乙二醇、10g油胺聚乙二醇与70g蒸馏水混合，配制成100g分散抑制剂A5。
实施例6
生物黏泥分散抑制剂的制备：10g双辛酸乙二胺双酰胺、30g马来酸酐-烯丙氧基聚乙二醇磺酸盐、20g油胺聚乙二醇与40g蒸馏水混合，配制成100g分散抑制剂A6。
实施例7
生物黏泥分散抑制剂的制备：10g辛胺甲酸酰胺、10g丙烯酸-烯丙氧基聚乙二醇、10g十二胺聚乙二醇与70g蒸馏水混合，配制成100g分散抑制剂A7。
实施例8
生物黏泥分散抑制剂的制备：10g十二胺丙烯酸酰胺、10g马来酸酐-烯丙氧基聚乙二醇羧酸盐、10g十六胺聚乙二醇与70g蒸馏水混合，配制成100g分散抑制剂A8。
对比例1
将30g十四烷基二甲基苄基氯化铵(1427)与70g蒸馏水混合，得到对比例1溶液，即D1溶液。
对比例2
以100g蒸馏水作为空白对比试验溶液，即D2溶液。
对比例3
对照实施例8制备生物黏泥分散抑制剂：10g马来酸酐-烯丙氧基聚乙二醇羧酸盐、10g十六胺聚乙二醇与80g蒸馏水混合，配制成100g对比例3溶液，即D3溶液。
对比例4
对照实施例8制备生物黏泥分散抑制剂：10g十二胺丙烯酸酰胺、10g十六胺聚乙二醇与80g蒸馏水混合，配制成100g对比例4溶液，即D4溶液。
对比例5
对照实施例8制备生物黏泥分散抑制剂：10g十二胺丙烯酸酰胺、10g马来酸酐-烯丙氧基聚乙二醇羧酸盐与80g蒸馏水混合，配制成100g对比例5溶液，即D5溶液。
测试例
生物黏泥剥离性能评价试验方法：取250mL锥形瓶若干，分别加入50mL生物黏泥和50mL蒸馏水，并确保加入的生物黏泥浓度一致，摇匀后，分别加入实施例1-8中A1-A8及对比例1-5中D1-D5，且加入后药剂浓度分别为5mg/L、20mg/L、40mg/L，并立即摇匀，其中对比例2为空白对比试验。然后置于旋转仪上以150r/min转速旋转24h。先用滤纸过滤，再用0.2μm的微孔滤膜过滤，测定滤液中多糖和蛋白质的浓度。滤液中多糖和蛋白质的浓度越大，表明药剂对生物黏泥的剥离性能越好。
(1)多糖浓度的测定
采用蒽酮-硫酸法测定多糖的浓度。蒽酮试剂的制备：取2g蒽酮溶解到80％H2SO4中，以80％H2SO4定容到1L，当日配制使用。
在测定多糖前先去除蛋白质，具体方法为：取一定体积的待测溶液，加入0.2倍体积的氯仿、0.04倍体积的正丁醇和0.04倍体积的无水乙醇，振荡3min后静置，取上层液体，重复操作3次，得到待测清液。
用去除蛋白质后的待测清夜测定多糖含量，具体方法为：在干净试管中，加入1mL去除蛋白质的待测清液，将试管放入冰水浴中冷却，再加入4mL蒽酮试剂，在冰水浴中振荡摇匀，再将试管放入沸水浴中加热10min。取出后冷却，用紫外-可见分光光度计测定620nm处吸光度，根据葡萄糖标准曲线计算得出多糖浓度。
(2)蛋白质浓度的测定
采用紫外-可见分光光度法测定蛋白质的浓度。具体原理和方法为：蛋白质中酪氨酸和色氨酸残基的苯环含有共轭双键，在280nm处有强吸收峰，在一定浓度范围内，该波长处的吸光度与溶液浓度成正比，符合郎伯-比尔定律。若溶液中含有嘌呤、嘧啶等核酸类物质时，在260nm处的吸光度比280nm处更强，对280nm处测定蛋白质浓度会有较大干扰，但可以利用280nm及260nm的吸光度差值计算蛋白质含量。计算公式为
C＝1.45A280–0.74A260
式中：C，蛋白质的质量浓度，mg/L；A280，蛋白质溶液在280nm处的吸光度；A260，蛋白质溶液在260nm处的吸光度。
表1剥离性能评价试验
表1的结果显示，加入本发明的生物黏泥分散抑制剂，滤液中的多糖、蛋白质的浓度最高分别可达9.2mg/L、181mg/L，明显高于空白试验(即对比例2)，表明对生物黏泥具有较好的剥离性能。在相同有效浓度下，实施例2-8的多糖、蛋白质浓度高于对比例1最高6.2mg/L、138mg/L，表明剥离性能优于1427。
生物黏泥分散性能评价试验方法：取250mL锥形瓶若干，分别加入50mL生物黏泥和50mL蒸馏水，并确保加入的生物黏泥质量浓度一致，摇匀后，分别加入实施例1-8中A1-A8及对比例1-5中D1-D5，且加入后药剂浓度分别为5mg/L、20mg/L、40mg/L，并立即摇匀，其中对比例2为空白对比试验。在室温下静置，然后分别在加药后4h检测上清液的浊度，试验结果见表2。浊度越大表明分散性越好。
表2分散性能评价试验
表2的结果显示，加入本发明的生物黏泥分散抑制剂，上清液的浊度最高可达19.7NTU，明显高于空白试验5.0NTU(即对比例2)，表明对生物黏泥具有较好的分散性能。在相同有效浓度下，实施例2-8的浊度高于对比例1最高13.8NTU，表明分散性能优于1427。
从实施例8和对比例3、4、5的比较可以看出：十六胺聚乙二醇、马来酸酐-烯丙氧基聚乙二醇羧酸盐和十二胺丙烯酸酰胺三者混合使用后，具有协同增效作用，有助于对生物黏泥的剥离和分散。
本发明的生物黏泥分散抑制剂，对生物黏泥具有良好的剥离、分散性能，既能剥离、分散系统中已有的生物黏泥，还能分散、稳定将要滋生的生物黏泥原始微粒，抑制原始微粒的聚结和大量滋生。在实际工业循环冷却水中，可使剥离分散的生物黏泥、或将要滋生的生物黏泥原始微粒，通过排污水排出系统，或通过旁滤滤除。
Claims (17)
1.一种生物黏泥分散抑制剂，包括酰胺化合物、不饱和羧酸与聚乙二醇共聚物、胺基聚醚和水，各组分的质量比为2～30:3～30:3～40:40～90，所述的酰胺化合物为脂肪酸与氨或胺的缩合产物或脂肪胺与有机酸的缩合产物，所述的不饱和羧酸与聚乙二醇共聚物为不饱和羧酸与烯丙氧基聚乙二醇单体的共聚物，重均分子量为2000～200000，所述的胺基聚醚通式为
其中R1、R2为H、烷基、环烷基或芳香基，但不同时为H，且R1、R2总碳数为8～40，R3为H或C1～C4的低碳烷基，聚合度n为2～40。
2.按照权利要求1所述的分散抑制剂，其中，酰胺化合物、不饱和羧酸与聚乙二醇共聚物、烷基聚醚和水的质量比为5～20:5～20:5～20:50～80。
3.按照权利要求1所述的分散抑制剂，其中，所述的脂肪酸选自C6-C30脂肪酸。
4.按照权利要求1所述的分散抑制剂，其中，所述的脂肪酸选自C8-C24脂肪酸。
5.按照权利要求1所述的分散抑制剂，其中，所述的胺选自C1-C8的单胺或二胺。
6.按照权利要求1所述的分散抑制剂，其中，所述的脂肪胺选自C6-C30脂肪胺。
7.按照权利要求1所述的分散抑制剂，其中，所述的脂肪胺选自C8-C24脂肪胺。
8.按照权利要求1所述的分散抑制剂，其中，所述的有机酸选自C1-C8的一元羧酸或二元羧酸。
9.按照权利要求1所述的分散抑制剂，其中，所述的不饱和羧酸与聚乙二醇共聚物的重均分子量为6000～100000。
10.按照权利要求1所述的分散抑制剂，其中，所述不饱和羧酸选自C3-C10不饱和羧酸。
11.按照权利要求1所述的分散抑制剂，其中，所述不饱和羧酸选自丙烯酸、甲基丙烯酸、马来酸、马来酸酐、衣康酸和肉桂酸。
12.按照权利要求1所述的分散抑制剂，其中，所述的烯丙氧基聚乙二醇单体选自烯丙氧基聚乙二醇、烯丙氧基聚乙二醇磺酸盐、烯丙氧基聚乙二醇羧酸盐。
13.按照权利要求1所述的分散抑制剂，其中，R1、R2总碳数为12～30，R3为H或C1～C4的低碳烷基，聚合度n为4～20。
14.按照权利要求1所述的分散抑制剂，其中，所述胺基聚醚的制备方法包括：在反应器中加入有机胺和碱，控制真空度为0～0.005MPa，升温至120～140℃，加入环氧乙烷，在140～160℃下反应，当反应器内压力降至0.01MPa以下，降至室温，出料即得胺基聚醚。
15.按照权利要求14所述的分散抑制剂，其中，有机胺与环氧乙烷物质的量之比为1:2～1:40，碱占有机胺和环氧乙烷质量之和的0.1％～1.0％。
16.权利要求1～15之一所述生物黏泥分散抑制剂的制备方法，包括，将酰胺化合物、不饱和羧酸与聚乙二醇共聚物、胺基聚醚和水，按照各组分的质量比为2～30:3～30:3～40:40～90混合均匀。
17.权利要求1～15之一所述的生物黏泥分散抑制剂在循环冷却水中的应用，加药浓度为2～100mg/L。
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