WO2022061557A1 - 磺基水杨酸银络合物复合循环水处理剂及其应用法 - Google Patents

磺基水杨酸银络合物复合循环水处理剂及其应用法 Download PDF

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WO2022061557A1
WO2022061557A1 PCT/CN2020/116946 CN2020116946W WO2022061557A1 WO 2022061557 A1 WO2022061557 A1 WO 2022061557A1 CN 2020116946 W CN2020116946 W CN 2020116946W WO 2022061557 A1 WO2022061557 A1 WO 2022061557A1
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treatment agent
water treatment
silver
circulating water
sulfosalicylic acid
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PCT/CN2020/116946
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English (en)
French (fr)
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许心青
刘辉
赵晓辉
陈绩峰
方定国
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南京天香菊生物技术有限公司
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Priority to PCT/CN2020/116946 priority Critical patent/WO2022061557A1/zh
Publication of WO2022061557A1 publication Critical patent/WO2022061557A1/zh

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    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/50—Treatment of water, waste water, or sewage by addition or application of a germicide or by oligodynamic treatment
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F5/00—Softening water; Preventing scale; Adding scale preventatives or scale removers to water, e.g. adding sequestering agents
    • C02F5/08—Treatment of water with complexing chemicals or other solubilising agents for softening, scale prevention or scale removal, e.g. adding sequestering agents
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F5/00—Softening water; Preventing scale; Adding scale preventatives or scale removers to water, e.g. adding sequestering agents
    • C02F5/08—Treatment of water with complexing chemicals or other solubilising agents for softening, scale prevention or scale removal, e.g. adding sequestering agents
    • C02F5/10—Treatment of water with complexing chemicals or other solubilising agents for softening, scale prevention or scale removal, e.g. adding sequestering agents using organic substances

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  • the invention relates to a reaction method of a water treatment agent, in particular to a composite circulating water treatment agent of a silver sulfosalicylate complex and an application thereof.
  • Industrial cooling circulating water systems generally have problems of scale, dirt, corrosion, bacteria and algae, pipe network corrosion and control of concentration multiples.
  • chemical agents such as corrosion and scale inhibitors and fungicides are added, which is the so-called circulating water treatment agent.
  • the current industrial circulating water treatment agents mostly use phosphorus-based descaling agents containing organic phosphonic acid, but the organic phosphonic acid has a high phosphorus content, which will lead to eutrophication of the water area, promote the growth of algae, and appear phosphorus scale, red tide and other phenomena;
  • Bactericides are mostly used isoxazoline, chlorine preparations, quaternary ammonium salts and other fungicides, but they are extremely irritating, corrosive and toxic, damage human health and pollute the environment. Therefore, it is of great practical significance to find an environmentally friendly and energy-saving water treatment agent.
  • the sulfonic acid group is a strong water-soluble strong acid group, which has the effect of anti-scaling, while sulfosalicylic acid is a good metal complexing agent, and it is environmentally friendly; silver has the effect of sterilizing and killing algae , and harmless to human body and environment. Therefore, it is speculated that the complex of sulfosalicylic acid and silver element to form a silver sulfosalicylic acid complex can be used for industrial circulating water treatment, and plays the role of anti-scaling, sterilization and algae killing.
  • the object of the present invention is to provide a kind of silver sulfosalicylate complex composite circulating water treatment agent and its application and its preparation method, to solve the problems raised in the above-mentioned background technology.
  • a kind of sulfosalicylic acid silver complex composite circulating water treatment agent includes the following components and contents: 30-50 parts of inorganic zinc salt corrosion inhibitor zinc sulfate , 20-35 parts of organic nitrogen azole corrosion inhibitor benzotriazole, 50-80 parts of glacial acetic acid and dimethylformamide mixture
  • the application of the described silver sulfosalicylate complex composite circulating water treatment agent comprises the following processing steps:
  • the mother liquor was filtered to obtain colorless and transparent crystals; from the obtained crystals, select crystals with a complete appearance, defect-free and ideal shape development as seed crystals, put them into a weighing bottle and place them in a desiccator for later use;
  • Reaction of water treatment agent 29.97g of sulfosalicylic acid and 20.03g of silver nitrate in 1) are added to the reaction solution composed of 50g of water, the temperature is controlled at 0°C to 10°C, and the stirring reaction is about 1.5 hours, which is the When the composite circulating water treatment agent is invented, the mass fraction of the silver sulfosalicylate complex in the water treatment agent is respectively 50%.
  • the ratio of the sulfosalicylic acid to the content of silver is that 1 mol of silver sulfosalicylic acid is greater than or equal to 1 mol.
  • the silver compound is monovalent.
  • sulfosalicylic acid silver complex complex circulating water treatment agent comprises the following components and contents: inorganic zinc salt corrosion inhibitor zinc sulfate 30-50 parts, organic azole corrosion inhibitor benzotriazepine 20-35 parts of azole, 50-80 parts of mixed solution of glacial acetic acid and dimethylformamide
  • a silver sulfosalicylate complex composite circulating water treatment agent and its application add the water treatment agent containing the silver sulfosalicylate complex into industrial water; the Adding the water treatment agent to the industrial water requires that the concentration of the silver sulfosalicylate complex in the industrial water be 5-50 ppm.
  • concentration outside this range is also possible, but the concentration is too low and the effect is poor, and the concentration It is too high and wastes reagents. According to the specific industrial water quality of different applications, the concentration range of 5-50ppm is selected.
  • the silver sulfosalicylate complex is in the aqueous solution. It has the functions of no discoloration and precipitation, anti-scaling and descaling, sterilization and algae killing, no need to use other scale inhibitors, sterilization and algaecide, environmental protection and energy saving. The best choice for reducing emissions.
  • Reaction of water treatment agent 29.97g of sulfosalicylic acid and 20.03g of silver nitrate in 1) are added to the reaction solution composed of 50g of water, the temperature is controlled at 0°C to 10°C, and the stirring reaction is about 1.5 hours, which is the When the composite circulating water treatment agent is invented, the mass fraction of the silver sulfosalicylate complex in the water treatment agent is respectively 50%.

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Agricultural Chemicals And Associated Chemicals (AREA)

Abstract

本发明公开了一种磺基水杨酸银络合物复合循环水处理剂及其应用，一种磺基水杨酸银络合物复合循环水处理剂，它包括以下成分和含量：无机锌盐类缓蚀剂硫酸锌30—50份、有机氮唑类缓蚀剂苯并三氮唑20—35份、冰乙酸和二甲基甲酰胺混合液50—80份。本发明的有益效果是：该发明一种磺基水杨酸银络合物复合循环水处理剂及其应用在水溶液中具有不发生变色及沉淀、防垢除垢、杀菌灭藻等功效，无需再使用其他阻垢剂和杀菌、杀藻剂，环保节能。

Description

磺基水杨酸银络合物复合循环水处理剂及其应用法 技术领域
本发明涉及水处理剂的反应方法，具体为一种磺基水杨酸银络合物复合循环水处理剂及其应用。
背景技术
工业冷却循环水系统普遍存在水垢、污垢、腐蚀、菌藻、管网腐蚀和浓缩倍数的控制问题，一般采用添加缓蚀阻垢剂和杀菌剂等化学药剂，就是所谓的循环水处理药剂。目前的工业循环水处理剂较多采用含有机膦酸的磷系除垢剂，但有机膦酸含磷较高，会导致水域富营养化，促进藻类生长，出现磷垢、赤潮等现象；另外，杀菌剂较多采用异塞唑啉类、氯制剂、季铵盐等杀菌剂，但它们具有极强的刺激性、腐蚀性和毒性，损害人体健康和污染环境。因此寻找一种环保且节能的水处理剂具有重要的现实意义。
现已知磺酸基团是一个强水溶性的强酸性基团，具有防垢阻垢作用，而磺基水杨酸是很好的金属络合剂，而且环保；银元素具有杀菌杀藻功效，且对人体和环境无害。因此推测将磺基水杨酸与银元素络合形成磺基水杨酸银络合物可用于工业循环水处理，起防垢阻垢、杀菌杀藻的作用。
发明内容
本发明的目的在于提供一种磺基水杨酸银络合物复合循环水处理剂及其应用及其制作方法，以解决上述背景技术中提出的问题。
本发明的目的是通过下述技术方案予以实现：一种磺基水杨酸银络合物复合循环水处理剂，它包括以下成分和含量：无机锌盐类缓蚀剂硫酸锌30—50份、有机氮唑类缓蚀剂苯并三氮唑20—35份、冰乙酸和二甲基甲酰胺混合液50—80份
所述的磺基水杨酸银络合物复合循环水处理剂的应用，包括如下工艺步骤：
1)籽晶的培养：使用分析纯的磺基水杨酸和碳酸氢铵为原料，摩尔比为1:1，称取磺基水杨酸25.42g(0.1mol)和碳酸氢铵37.91g(0.1mol)混合溶解在100mL高纯水中，加热升温到50℃，搅拌1h左右，无晶体析出，将热溶液用0.15μm孔径的滤膜过滤以除去杂质颗粒，然后将滤液冷却至室温进行蒸发，经过72h的蒸发，过滤母液可获得无色透明的晶体；从所获得的晶体中选取外观完整无缺陷形状发育理想的晶体作为籽晶，放入称量瓶置于干燥器中备用；
2)溶液的饱和点的测定：将溶液在高于饱和点10℃的水浴中过热48h后，用0.15μm孔径的滤膜预过滤，滤除溶液中的杂质颗粒。将滤液转移到生长瓶后，先在高于饱和点10℃的水浴中过热48h以上，然后将事先准备好的籽晶安装在晶架上，放入烘箱预热后移入生长瓶；在高温条件下，先对其进行微溶，待籽晶表面可能夹带的微晶全部溶解后降温至饱和点开始生长。生长过程中晶体没有出现明显的缺陷，溶液也没有自发结晶；经过72h的生长时间生长出45×20×18mm3的大尺寸透明晶体；
3)水处理剂的反应：将1)中29.97g磺基水杨酸，20.03g硝酸银加入50g水组成的反应液中，控制温度0℃～10℃，搅拌反应约1.5小时，即为本发明复合循环水处理剂，则磺基水杨酸银络合物在水处理剂中的质量分数分别为50％。
所述磺基水杨酸相对于银的含量的比例为银1mol磺基水杨酸大于等于1mol。
所述银化合物为一价。
所述的一种磺基水杨酸银络合物复合循环水处理剂包括以下成分和含量：无机锌盐类缓蚀剂硫酸锌30—50份、有机氮唑类缓蚀剂苯并三氮唑20—35份、冰乙酸和二甲基甲酰胺混合液50—80份
本发明的有益效果是：该发明一种磺基水杨酸银络合物复合循环水处理 剂及其应用将含磺基水杨酸银络合物的水处理剂加入工业用水中；所述水处理剂加入工业用水中要求磺基水杨酸银络合物在所述工业用水中的浓度为5-50ppm，当然该范围以外的浓度也是可以的，但浓度太低作用效果较差，浓度太高又浪费试剂，根据具体的不同应用的工业用水水质在5-50ppm浓度范围选择，比如对于水质很差的选择较高浓度则效果较好；并且磺基水杨酸银络合物在水溶液中具有不发生变色及沉淀、防垢除垢、杀菌灭藻等功效，无需再使用其他阻垢剂和杀菌、杀藻剂，环保节能，是磷基水处理剂的换代产品，是企业实施节能减排的最佳选择。
具体实施方式
下面结合具体实施方式进一步的说明，但是下文中的具体实施方式不应当做被理解为对本体发明的限制。本领域普通技术人员能够在本发明基础上显而易见地作出的各种改变和变化，应该均在发明的范围之内。
一种磺基水杨酸银络合物复合循环水处理剂的应用，包括如下工艺步骤：
实施例1：
1)籽晶的培养：使用分析纯的磺基水杨酸和碳酸氢铵为原料，摩尔比为1:1，称取磺基水杨酸25.42g(0.1mol)和碳酸氢铵37.91g(0.1mol)混合溶解在100mL高纯水中，加热升温到50℃，搅拌1h左右，无晶体析出，将热溶液用0.15μm孔径的滤膜过滤以除去杂质颗粒，然后将滤液冷却至室温进行蒸发，经过72h的蒸发，过滤母液可获得无色透明的晶体。从所获得的晶体中选取外观完整无缺陷形状发育理想的晶体作为籽晶，放入称量瓶置于干燥器中备用；
2)溶液的饱和点的测定：将溶液在高于饱和点10℃的水浴中过热48h后，用0.15μm孔径的滤膜预过滤，滤除溶液中的杂质颗粒。将滤液转移到生长瓶后，先在高于饱和点10℃的水浴中过热48h以上，然后将事先准备好的籽晶安装在晶架上，放入烘箱预热后移入生长瓶。在高温条件下，先对 其进行微溶，待籽晶表面可能夹带的微晶全部溶解后降温至饱和点开始生长；生长过程中晶体没有出现明显的缺陷，溶液也没有自发结晶；经过72h的生长时间生长出45×20×18mm3的大尺寸透明晶体；
3)水处理剂的反应：将1)中13.74g磺基水杨酸，6.26g氧化银加入80g水组成的反应液中，控制温度0℃～10℃，搅拌反应约1小时，即为本发明复合循环水处理剂，则磺基水杨酸银络合物在水处理剂中的质量分数分别为20％；
实施例2：
1)籽晶的培养：使用分析纯的磺基水杨酸和碳酸氢铵为原料，摩尔比为1:1，称取磺基水杨酸25.42g(0.1mol)和碳酸氢铵37.91g(0.1mol)混合溶解在100mL高纯水中，加热升温到50℃，搅拌1h左右，无晶体析出，将热溶液用0.15μm孔径的滤膜过滤以除去杂质颗粒，然后将滤液冷却至室温进行蒸发，经过72h的蒸发，过滤母液可获得无色透明的晶体。从所获得的晶体中选取外观完整无缺陷形状发育理想的晶体作为籽晶，放入称量瓶置于干燥器中备用；
2)溶液的饱和点的测定：将溶液在高于饱和点10℃的水浴中过热48h后，用0.15μm孔径的滤膜预过滤，滤除溶液中的杂质颗粒。将滤液转移到生长瓶后，先在高于饱和点10℃的水浴中过热48h以上，然后将事先准备好的籽晶安装在晶架上，放入烘箱预热后移入生长瓶。在高温条件下，先对其进行微溶，待籽晶表面可能夹带的微晶全部溶解后降温至饱和点开始生长。生长过程中晶体没有出现明显的缺陷，溶液也没有自发结晶。经过72h的生长时间生长出45×20×18mm3的大尺寸透明晶体；
3)水处理剂的反应：将1)中29.97g磺基水杨酸，20.03g硝酸银加入50g水组成的反应液中，控制温度0℃～10℃，搅拌反应约1.5小时，即为本发明复合循环水处理剂，则磺基水杨酸银络合物在水处理剂中的质量分数分别 为50％。
实施例3：
1)籽晶的培养：使用分析纯的磺基水杨酸和碳酸氢铵为原料，摩尔比为1:1，称取磺基水杨酸25.42g(0.1mol)和碳酸氢铵37.91g(0.1mol)混合溶解在100mL高纯水中，加热升温到50℃，搅拌1h左右，无晶体析出，将热溶液用0.15μm孔径的滤膜过滤以除去杂质颗粒，然后将滤液冷却至室温进行蒸发，经过72h的蒸发，过滤母液可获得无色透明的晶体。从所获得的晶体中选取外观完整无缺陷形状发育理想的晶体作为籽晶，放入称量瓶置于干燥器中备用；
2)溶液的饱和点的测定：将溶液在高于饱和点10℃的水浴中过热48h后，用0.15μm孔径的滤膜预过滤，滤除溶液中的杂质颗粒。将滤液转移到生长瓶后，先在高于饱和点10℃的水浴中过热48h以上，然后将事先准备好的籽晶安装在晶架上，放入烘箱预热后移入生长瓶。在高温条件下，先对其进行微溶，待籽晶表面可能夹带的微晶全部溶解后降温至饱和点开始生长。生长过程中晶体没有出现明显的缺陷，溶液也没有自发结晶。经过72h的生长时间生长出45×20×18mm3的大尺寸透明晶体；
3)水处理剂的反应：将1)中11.27g磺基水杨酸，8.73g乳酸银，3g硫酸锌，1g苯并三氮唑，2g二甲基甲酰胺和74g水置于搅拌容器中控制温度0℃～10℃，搅拌反应约1小时，即为本发明复合循环水处理剂，则磺基水杨酸银络合物、无机锌盐类缓蚀剂、有机氮唑类缓蚀剂和助溶剂在水处理剂中的质量分数分别为20％、3％、1％和2％。
以上描述仅为本申请的较佳实施例以及对所运用技术原理的说明。本领域技术人员应当理解，本申请中所涉及的发明范围，并不限于上述技术特征的特定组合而成的技术方案，同时也应涵盖在不脱离所述发明构思的情况下，由上述技术特征或其等同特征进行任意组合而形成的其它技术方案。例如上 述特征与本申请中公开的(但不限于)具有类似功能的技术特征进行互相替换而形成的技术方案。

Claims (4)

  1. 一种磺基水杨酸银络合物复合循环水处理剂，其特征在于：它包括以下成分和含量：无机锌盐类缓蚀剂硫酸锌30—50份、有机氮唑类缓蚀剂苯并三氮唑20—35份、冰乙酸和二甲基甲酰胺混合液50—80份。
  2. 根据权利要求1一种磺基水杨酸银络合物复合循环水处理剂的应用法，其特征在于：包括如下工艺步骤：
    1)籽晶的培养：使用分析纯的磺基水杨酸和碳酸氢铵为原料，摩尔比为1:1，称取磺基水杨酸25.42g(0.1mol)和碳酸氢铵37.91g(0.1mol)混合溶解在100mL高纯水中，加热升温到50℃，搅拌1h左右，无晶体析出，将热溶液用0.15μm孔径的滤膜过滤以除去杂质颗粒，然后将滤液冷却至室温进行蒸发，经过72h的蒸发，过滤母液可获得无色透明的晶体；从所获得的晶体中选取外观完整无缺陷形状发育理想的晶体作为籽晶，放入称量瓶置于干燥器中备用；
    2)溶液的饱和点的测定：将溶液在高于饱和点10℃的水浴中过热48h后，用0.15μm孔径的滤膜预过滤，滤除溶液中的杂质颗粒。将滤液转移到生长瓶后，先在高于饱和点10℃的水浴中过热48h以上，然后将事先准备好的籽晶安装在晶架上，放入烘箱预热后移入生长瓶；在高温条件下，先对其进行微溶，待籽晶表面可能夹带的微晶全部溶解后降温至饱和点开始生长。生长过程中晶体没有出现明显的缺陷，溶液也没有自发结晶；经过72h的生长时间生长出45×20×18mm3的大尺寸透明晶体；
    3)水处理剂的反应：将1)中29.97g磺基水杨酸，20.03g硝酸银加入50g水组成的反应液中，控制温度0℃～10℃，搅拌反应约1.5小时，即为本发明复合循环水处理剂，则磺基水杨酸银络合物在水处理剂中的质量分数分别为50％。
  3. 根据权利要求2所述的一种磺基水杨酸银络合物复合循环水处理剂的应用，其特征在于：所述磺基水杨酸相对于银的含量的比例为银1mol磺基水 杨酸大于等于1mol。
  4. 根据权利要求2一种磺基水杨酸银络合物复合循环水处理剂的应用，其特征在于：所述银化合物为一价。
PCT/CN2020/116946 2020-09-23 2020-09-23 磺基水杨酸银络合物复合循环水处理剂及其应用法 WO2022061557A1 (zh)

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CN102718328A (zh) * 2012-05-31 2012-10-10 重庆安碧捷生物科技有限公司 环保型磺基水杨酸银络合物复合循环水处理剂及其应用
CN103696018A (zh) * 2013-12-18 2014-04-02 中国科学院福建物质结构研究所 一种新型荧光晶体材料磺基水杨酸铵及其制备与用途
CN104611737A (zh) * 2013-11-05 2015-05-13 无锡市雪江环境工程设备有限公司 一种咪唑-磺基水杨酸镀银电镀液及电镀方法
KR20200054873A (ko) * 2018-11-12 2020-05-20 동우 화인켐 주식회사 은 박막 식각액 조성물 및 이를 이용한 식각 방법 및 금속 패턴의 형성 방법

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Publication number Priority date Publication date Assignee Title
CN102718328A (zh) * 2012-05-31 2012-10-10 重庆安碧捷生物科技有限公司 环保型磺基水杨酸银络合物复合循环水处理剂及其应用
CN104611737A (zh) * 2013-11-05 2015-05-13 无锡市雪江环境工程设备有限公司 一种咪唑-磺基水杨酸镀银电镀液及电镀方法
CN103696018A (zh) * 2013-12-18 2014-04-02 中国科学院福建物质结构研究所 一种新型荧光晶体材料磺基水杨酸铵及其制备与用途
KR20200054873A (ko) * 2018-11-12 2020-05-20 동우 화인켐 주식회사 은 박막 식각액 조성물 및 이를 이용한 식각 방법 및 금속 패턴의 형성 방법

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