CN115779792A - Method for treating rectifying still residues by using supercritical/subcritical water catalytic oxidation method - Google Patents
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Abstract
Description
技术领域technical field
本发明涉及环保行业固体废弃物处置领域，特别涉及一种利用超/亚临界水催化氧化法处理精馏釜残的方法。The invention relates to the field of solid waste disposal in the environmental protection industry, in particular to a method for treating rectification still residues by using a super/subcritical water catalytic oxidation method.
背景技术Background technique
聚氨酯合成革行业DMF精馏釜残是一种黑色黏稠状半固体物质，其成分为DMF、聚氨酯树脂、木粉、布毛等有机物，轻质CaCO3粉状填料等无机物及水分。根据《国家危险废物名录》(2021年版)的划分，属于危险废物。The DMF rectification still residue in the polyurethane synthetic leather industry is a black viscous semi-solid substance, which consists of DMF, polyurethane resin, wood powder, cloth wool and other organic substances, light CaCO3 powder filler and other inorganic substances and water. According to the classification of "National Hazardous Waste List" (2021 Edition), it belongs to hazardous waste.
目前，釜残的处置方式主要有填埋、焚烧和掺入煤中燃烧，成本高且易造成二次污染。釜残填埋前，需要对其进行固化稳定处理，大幅增加处理物体积及处理成本，一旦包容体发生破裂，可能会造成空气、土壤及地下水等的二次污染，因此填埋已经逐渐不被人们所接受；焚烧是国内主流的精馏釜残处理技术，其优点是可以迅速和较大程度使釜残减量化并降低其有毒有害性，但处置成本较高(约2000-3500元/吨)，排放的焚烧废气中含有多环芳烃、二噁英等持久性有机污染物；而将精馏釜残掺入到燃煤锅炉中燃烧，可以利用釜残中有机质的热量，同时又使釜残得到处置。但釜残中的无机盐在燃烧过程中析出，并积聚在锅炉壁上易对锅炉造成危害，当燃烧温度较低时同样易产生二次污染。随着近年来国家对环保越来越重视，以及国民环保理念也不断加强，合成革行业的发展已不能满足日益严格的环保政策要求。以水性聚氨酯为原料的新型PU合成革生产工艺虽然已取得重大进展，但仍无法在短期内全面取代传统生产工艺。因此，亟待创新发展更加经济、高效、环保的DMF精馏釜残处理技术。At present, the disposal methods of kettle residues mainly include landfill, incineration and combustion mixed with coal, which are costly and easy to cause secondary pollution. Before the kettle residue is landfilled, it needs to be solidified and stabilized, which greatly increases the volume of the treated material and the cost of treatment. Once the containment body ruptures, it may cause secondary pollution of air, soil, and groundwater. Therefore, landfilling has gradually become obsolete. It is accepted by people; incineration is the domestic mainstream rectification still residue treatment technology, and its advantage is that it can quickly and greatly reduce the amount of still residue and reduce its toxicity, but the disposal cost is relatively high (about 2000-3500 yuan/ tons), and the discharged incineration exhaust gas contains persistent organic pollutants such as polycyclic aromatic hydrocarbons and dioxins; while the rectification still residue is mixed into a coal-fired boiler for combustion, the heat of organic matter in the still residue can be used, and at the same time, the The remains of the kettle were disposed of. However, the inorganic salts in the kettle residue are precipitated during the combustion process and accumulate on the boiler wall, which is easy to cause damage to the boiler. When the combustion temperature is low, it is also easy to produce secondary pollution. As the country pays more and more attention to environmental protection in recent years, and the national environmental protection concept is also continuously strengthened, the development of the synthetic leather industry can no longer meet the increasingly stringent environmental protection policy requirements. Although the new PU synthetic leather production process using water-based polyurethane as raw material has made significant progress, it still cannot fully replace the traditional production process in the short term. Therefore, it is urgent to innovate and develop a more economical, efficient and environmentally friendly DMF distillation still residue treatment technology.
发明内容Contents of the invention
基于上述问题，本发明的目的在于提供一种反应快、能耗低、不易产生二次污染，且相比于焚烧等传统方法更加经济、高效的利用超/亚临界水催化氧化法处理DMF精馏釜残的方法。Based on the above problems, the object of the present invention is to provide a fast reaction, low energy consumption, difficult to produce secondary pollution, and compared with traditional methods such as incineration, more economical and efficient utilization of super/subcritical water catalytic oxidation method to process DMF refined The still residue method.
针对以上问题，提供了如下技术方案：一种利用超/亚临界水催化氧化法处理DMF精馏釜残的方法，其特征在于，按照如下步骤对精馏釜残进行无害化处理：In view of the above problems, the following technical scheme is provided: a method of utilizing super/subcritical water catalytic oxidation to process DMF rectification still residue, which is characterized in that, according to the following steps, the rectification still residue is subjected to harmless treatment:
(1)将聚氨酯合成革企业DMF精馏塔产生的精馏釜残装入高压反应釜中，并加入釜残质量5至20倍的水、釜残化学需氧量1至10倍的氧化剂以及釜残质量0.01％至10％的金属氧化物催化剂；(1) Put the rectification still residue produced by the DMF rectification tower of the polyurethane synthetic leather enterprise into the high-pressure reactor, and add water 5 to 20 times the weight of the still residue, an oxidant 1 to 10 times the chemical oxygen demand of the still residue, and 0.01% to 10% metal oxide catalyst in the residual mass of the kettle;
(2)将高压反应釜加热至300至500摄氏度，反应时间2至30分钟，使釜残与氧化剂在超/亚临界水中发生强烈的催化氧化反应，釜残中的碳氢组分被转化为二氧化碳和水，氮组分转化为氮气或氨氮，杂原子组分转化为相应的酸或无机盐；(2) The autoclave is heated to 300 to 500 degrees Celsius, and the reaction time is 2 to 30 minutes, so that the still residue and the oxidant undergo a strong catalytic oxidation reaction in super/subcritical water, and the hydrocarbon components in the still residue are converted into Carbon dioxide and water, the nitrogen component is converted into nitrogen or ammonia nitrogen, and the heteroatom component is converted into the corresponding acid or inorganic salt;
(3)反应完成后利用热交换器对余热进行回收，直至反应釜中温度接近室温，反应釜中的二氧化碳和氮气等气体由活性炭吸附处理后排放，反应釜中的废水与企业其余生产废水、员工生活污水混合后，排入污水处理系统处理，反应釜中的固体残渣主要为金属氧化物，回收后用作催化剂。(3) After the reaction is completed, the heat exchanger is used to recover the waste heat until the temperature in the reactor is close to room temperature, and the carbon dioxide and nitrogen in the reactor are discharged after being adsorbed by activated carbon. After the employees' domestic sewage is mixed, it is discharged into the sewage treatment system for treatment. The solid residue in the reactor is mainly metal oxides, which are recycled and used as catalysts.
本发明进一步设置为，以高压空气、高压氧气或双氧水作为氧化剂。The present invention is further configured to use high-pressure air, high-pressure oxygen or hydrogen peroxide as the oxidant.
本发明进一步设置为，以氧化铜、二氧化锰、氧化铈等金属氧化物作为催化剂。The present invention is further configured to use metal oxides such as copper oxide, manganese dioxide, and cerium oxide as catalysts.
本发明进一步设置为，所述催化剂采用骨架金属、金属丝网、金属颗粒、金属屑片等形式应用。The present invention is further provided that the catalyst is applied in the form of skeleton metal, wire mesh, metal particles, metal chips and the like.
本发明的进一步设置：将反应釜中的废水与企业其余生产废水、员工生活污水混合，可以将生化性较差的反应尾水通过移动床生物膜反应器、厌氧-缺氧-好氧法等生物处理工艺进行处理，降低污水处理成本。Further setting of the present invention: the wastewater in the reactor is mixed with the rest of the production wastewater of the enterprise and the domestic sewage of the employees, and the reaction tail water with poor biochemical properties can be passed through the moving bed biofilm reactor, anaerobic-anoxic-aerobic method and other biological treatment processes to reduce the cost of sewage treatment.
本发明的有益效果：采用超临界流体绿色化学技术，以超/亚临界水为反应介质，在高压反应釜中进行催化氧化反应。以超/亚临界水作为反应介质，使釜残中的有机物与氧化剂在超/亚临界水中发生强烈的催化氧化反应，在短时间内将有机物中的碳氢组分转化为二氧化碳和水，氮组分转化为氮气或氨氮，杂原子组分转化为相应的酸或无机盐。该方法具有反应快、能耗低、不易产生二次污染等优点，实现了固体废物的减量化和无害化，相比于焚烧等传统方法更加经济、高效。Beneficial effects of the present invention: the supercritical fluid green chemical technology is adopted, and the super/subcritical water is used as the reaction medium, and the catalytic oxidation reaction is carried out in a high-pressure reactor. Using super/subcritical water as the reaction medium, the organic matter in the still residue and the oxidant undergo a strong catalytic oxidation reaction in super/subcritical water, and the hydrocarbon components in the organic matter are converted into carbon dioxide, water, and nitrogen in a short time The components are converted into nitrogen or ammonia nitrogen, and the heteroatom components are converted into corresponding acids or inorganic salts. This method has the advantages of fast response, low energy consumption, and is not easy to produce secondary pollution, and realizes the reduction and harmlessness of solid waste. Compared with traditional methods such as incineration, it is more economical and efficient.
附图说明Description of drawings
图1为本发明的流程示意图。Fig. 1 is a schematic flow chart of the present invention.
具体实施方式Detailed ways
下面结合附图和实施例，对本发明的具体实施方式作进一步详细描述。以下实施例用于说明本发明，但不用来限制本发明的范围。The specific implementation manners of the present invention will be further described in detail below in conjunction with the accompanying drawings and embodiments. The following examples are used to illustrate the present invention, but are not intended to limit the scope of the present invention.
如图1所示的一种利用超/亚临界水催化氧化法处理DMF精馏釜残的方法，其特征在于，按照如下步骤对精馏釜残进行无害化处理：A kind of method that utilizes super/subcritical water catalytic oxidation method to process DMF rectification still residue as shown in Figure 1, it is characterized in that, carry out harmless treatment to rectification still residue according to the following steps:
(1)将聚氨酯合成革企业DMF精馏塔产生的精馏釜残装入高压反应釜中，并加入釜残质量5至20倍的水、釜残化学需氧量1至10倍的氧化剂以及釜残质量0.01％至10％的金属氧化物催化剂；(1) Put the rectification still residue produced by the DMF rectification tower of the polyurethane synthetic leather enterprise into the high-pressure reactor, and add water 5 to 20 times the weight of the still residue, an oxidant 1 to 10 times the chemical oxygen demand of the still residue, and 0.01% to 10% metal oxide catalyst in the residual mass of the kettle;
(2)将高压反应釜加热至300至500摄氏度，反应时间2至30分钟，使釜残与氧化剂在超/亚临界水中发生强烈的催化氧化反应，釜残中的碳氢组分被转化为二氧化碳和水，氮组分转化为氮气或氨氮，杂原子组分转化为相应的酸或无机盐；(2) The autoclave is heated to 300 to 500 degrees Celsius, and the reaction time is 2 to 30 minutes, so that the still residue and the oxidant undergo a strong catalytic oxidation reaction in super/subcritical water, and the hydrocarbon components in the still residue are converted into Carbon dioxide and water, the nitrogen component is converted into nitrogen or ammonia nitrogen, and the heteroatom component is converted into the corresponding acid or inorganic salt;
(3)反应完成后利用热交换器对余热进行回收，直至反应釜中温度接近室温，反应釜中的二氧化碳和氮气等气体由活性炭吸附处理后排放，反应釜中的废水与企业其余生产废水、员工生活污水混合后，排入污水处理系统处理，反应釜中的固体残渣主要为金属氧化物，回收后用作催化剂。(3) After the reaction is completed, the heat exchanger is used to recover the waste heat until the temperature in the reactor is close to room temperature, and the carbon dioxide and nitrogen in the reactor are discharged after being adsorbed by activated carbon. After the employees' domestic sewage is mixed, it is discharged into the sewage treatment system for treatment. The solid residue in the reactor is mainly metal oxides, which are recycled and used as catalysts.
上述步骤中，以高压空气、高压氧气或双氧水作为氧化剂。In the above steps, high-pressure air, high-pressure oxygen or hydrogen peroxide is used as the oxidizing agent.
上述步骤中，以氧化铜、二氧化锰、氧化铈等金属氧化物作为催化剂。In the above steps, metal oxides such as copper oxide, manganese dioxide, and cerium oxide are used as catalysts.
上述步骤中，所述催化剂采用骨架金属、金属丝网、金属颗粒、金属屑片等形式应用。In the above steps, the catalyst is applied in the form of skeleton metal, wire mesh, metal particles, metal chips and the like.
通过上述步骤对聚氨酯合成革企业DMF精馏塔塔底釜残进行处理。测定了釜残样品的总有机碳(TOC)含量，约为0.338g/g。釜残的工业分析结果见表1，元素分析结果见表2。Through the above steps, the bottom residue of the DMF rectification tower of the polyurethane synthetic leather enterprise is treated. The total organic carbon (TOC) content of the still residue sample was measured, and it was about 0.338g/g. See Table 1 for the industrial analysis results of the still residue, and Table 2 for the elemental analysis results.
表1DMF精馏釜残样品工业分析结果Table 1 DMF rectification kettle residual sample industrial analysis result
表2DMF精馏釜残样品元素分析结果Table 2 DMF rectification kettle residue sample elemental analysis results
通过采用上述步骤，实施例1：釜残:水质量比＝1:14，氧化剂倍数＝1.75，催化剂投加量＝0.0％，反应温度＝400摄氏度，反应时间＝10分钟。反应完成后，釜残总有机碳(TOC)、化学需氧量(COD)、总氮(TN)、氨氮(NH4 +–N)的降解率分别为98.7％、99.5％、36.5％、–50.5％，废水浓度分别为325mg/L、440mg/L、505mg/L、432mg/L。By adopting the above steps, Example 1: kettle residue: water mass ratio = 1:14, oxidant multiple = 1.75, catalyst dosage = 0.0%, reaction temperature = 400 degrees Celsius, reaction time = 10 minutes. After the reaction was completed, the degradation rates of total organic carbon (TOC), chemical oxygen demand (COD), total nitrogen (TN), ammonia nitrogen (NH 4 + -N) were 98.7%, 99.5%, 36.5%, – 50.5%, the concentration of wastewater is 325mg/L, 440mg/L, 505mg/L, 432mg/L respectively.
通过采用上述步骤，实施例2：釜残:水质量比＝1:12，氧化剂倍数＝1.50，催化剂投加量＝0.0％，反应温度＝360摄氏度，反应时间＝20分钟。反应完成后，釜残总有机碳(TOC)、化学需氧量(COD)、总氮(TN)、氨氮(NH4 +–N)的降解率分别为96.9％、98.0％、7.2％、–119.0％，废水浓度分别为883mg/L、2095mg/L、861mg/L、733mg/L。By adopting the above steps, embodiment 2: kettle residue: water mass ratio = 1:12, oxidant multiple = 1.50, catalyst dosage = 0.0%, reaction temperature = 360 degrees Celsius, reaction time = 20 minutes. After the reaction was completed, the degradation rates of total organic carbon (TOC), chemical oxygen demand (COD), total nitrogen (TN), ammonia nitrogen (NH 4 + -N) were 96.9%, 98.0%, 7.2%, – 119.0%, the concentration of wastewater is 883mg/L, 2095mg/L, 861mg/L, 733mg/L respectively.
通过采用上述步骤，实施例3：釜残:水质量比＝1:12，氧化剂倍数＝1.50，CuO催化剂投加量＝10％，反应温度＝340摄氏度，反应时间＝10分钟。反应完成后，釜残总有机碳(TOC)、化学需氧量(COD)、总氮(TN)、氨氮(NH4 +–N)的降解率分别为98.2％、98.3％、4.3％、–149.3％，浓度分别为514mg/L、1856mg/L、888mg/L、834mg/L。By adopting the above steps, Example 3: kettle residue: water mass ratio = 1:12, oxidant multiple = 1.50, CuO catalyst dosage = 10%, reaction temperature = 340 degrees Celsius, reaction time = 10 minutes. After the reaction was completed, the degradation rates of total organic carbon (TOC), chemical oxygen demand (COD), total nitrogen (TN), and ammonia nitrogen (NH 4 + -N) were 98.2%, 98.3%, 4.3%, – 149.3%, the concentration is 514mg/L, 1856mg/L, 888mg/L, 834mg/L respectively.
本实施例中，采用移动床生物膜反应器(MBBR)对反应废水与员工生活污水混合污水进行处理，在水力停留时间(HRT)＝48小时，填料投加率＝20％，化学需氧量(COD)、总氮(TN)、氨氮(NH4 +–N)、总磷(TP)的降解率分别为71.3％、92.9％、99.5％、55.6％，浓度为458mg/L、14.9mg/L、0.92mg/L、12.3mg/L，满足污水综合排放标准的三级标准(GB 8978-1996)，可以排入城镇污水处理厂进行后续处理。In this example, the moving bed biofilm reactor (MBBR) is used to treat the mixed sewage of reaction wastewater and domestic sewage of employees, at hydraulic retention time (HRT) = 48 hours, filler dosage = 20%, chemical oxygen demand (COD), total nitrogen (TN), ammonia nitrogen (NH 4 + –N), and total phosphorus (TP) degradation rates were 71.3%, 92.9%, 99.5%, and 55.6%, respectively, and the concentrations were 458mg/L, 14.9mg/L L, 0.92mg/L, 12.3mg/L, meet the third-level standard of comprehensive sewage discharge standard (GB 8978-1996), and can be discharged into urban sewage treatment plants for subsequent treatment.
以上所述仅是本发明的优选实施方式，应当指出，对于本技术领域的普通技术人员来说，在不脱离本发明技术原理的前提下，还可以做出若干改进和变型，上述假设的这些改进和变型也应视为本发明的保护范围。The above is only a preferred embodiment of the present invention, it should be pointed out that for those of ordinary skill in the art, without departing from the technical principle of the present invention, some improvements and modifications can also be made. Improvements and variations should also be regarded as the protection scope of the present invention.
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