CN107473291B - A kind of treatment method of high salinity wastewater - Google Patents
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Abstract
Description
技术领域technical field
本发明属于化工领域，涉及一种高盐度废水的处理方法。The invention belongs to the field of chemical industry, and relates to a treatment method of high-salinity wastewater.
背景技术Background technique
高盐度废水的处理一直是化工、环保领域的难点。在各种化工生产中，经常会产生含有大量氯化钠组分的高盐度的废水，组成成分相对复杂，除了近饱和的盐(氯化钠)以外，还会有一些有机杂质、溶解性产物、以及副产物等，使得多数常规的净化过程都无能为力。一般而言，高盐度的废水只能采用蒸馏的方式进行处理，需要消耗大量的高品位能源(过热蒸汽)，而且对设备的要求也非常高，投资、运行成本都居高不下。因此，采用低能耗、设备要求不高的方法进行高盐度废水的处理及预处理，在化工、环保方面都具有非常重要的意义。The treatment of high salinity wastewater has always been a difficulty in the fields of chemical industry and environmental protection. In various chemical production, high-salinity wastewater containing a large amount of sodium chloride components is often produced, and the composition is relatively complex. In addition to nearly saturated salt (sodium chloride), there will be some organic impurities, solubility Products, as well as by-products, make most conventional purification processes ineffective. Generally speaking, high-salinity wastewater can only be treated by distillation, which requires a lot of high-grade energy (superheated steam), and requires very high equipment, and the investment and operating costs remain high. Therefore, the treatment and pretreatment of high-salinity wastewater by methods with low energy consumption and low equipment requirements is of great significance in chemical industry and environmental protection.
由于盐水和淡水的密度不同，本发明首次提出了利用重力渗析的方法处理高盐度废水，创造性的使用了有机分离层，通过调控有机分离层的密度以及和水的亲和程度，实现了盐水中水和盐的逐步分离。其具体原理为：化工生产中产生的浓盐水，浓度大于15％时，其相对比重已经在1.10以上，而有机溶剂氯苯的密度为1.10，且和水不互溶。在静置的时候，浓盐水处于氯苯的下层，而淡水密度小于氯苯，在静置的时候处于氯苯层的上层。而苯氧乙酸(C6H5OCH2COOH)是一种亲水性的物质，可以和水形成结晶水的化合物(C6H5OCH2COOH·0.5H2O)，且可以溶解在氯苯中，而且在氯苯的存在下苯氧乙酸在水中的溶解度可以忽略不计，因此溶解了苯氧乙酸的氯苯可以作为一个分离层，不断从盐水中夺取水，而释放出来的则是不含盐的淡水，浮在氯苯层的上层，从而实现了水和盐的分离。其整个过程即可看做是在重力作用下，水渗析过有机分离层的一个过程，因此将其命名为“重力渗析法”。由于亲水的吸水剂苯氧乙酸极性较大，因此在纯氯苯中的溶解度较小，通过加入醇类等极性较大的溶剂改善氯苯对苯氧乙酸的溶解性，可以提高有机层对苯氧乙酸的溶解性，从而增加分离层的分离能力。本发明选用水溶性很小的一元醇类，如辛醇、异壬醇等常用的化工原料，根据各种醇的比重不同，将最终的有机层(包含氯苯、醇、苯氧乙酸等组分)的比重调节至1.05～1.10，获得的分离层适用于对浓盐水进行处理。Due to the different densities of salt water and fresh water, the present invention first proposes the use of gravity dialysis to treat high-salinity wastewater, creatively uses an organic separation layer, and controls the density of the organic separation layer and the degree of affinity with water. Gradual separation of water and salt. The specific principle is: when the concentration of concentrated brine produced in chemical production is greater than 15%, its relative specific gravity is already above 1.10, while the density of organic solvent chlorobenzene is 1.10, and it is immiscible with water. When standing, concentrated brine is in the lower layer of chlorobenzene, while fresh water is less dense than chlorobenzene, and is in the upper layer of chlorobenzene layer when standing. Phenoxyacetic acid (C 6 H 5 OCH 2 COOH) is a hydrophilic substance that can form crystal water with water (C 6 H 5 OCH 2 COOH·0.5H 2 O), and can be dissolved in chlorine In benzene, and in the presence of chlorobenzene, the solubility of phenoxyacetic acid in water is negligible, so the chlorobenzene in which the phenoxyacetic acid is dissolved can be used as a separation layer, continuously taking water from the brine, while the released water is not. The fresh water containing salt floats on the upper layer of the chlorobenzene layer, thereby realizing the separation of water and salt. The whole process can be regarded as a process of water dialysis through the organic separation layer under the action of gravity, so it is named "gravity dialysis method". Since the hydrophilic water-absorbing agent phenoxyacetic acid has high polarity, its solubility in pure chlorobenzene is small. By adding a solvent with high polarity such as alcohol to improve the solubility of chlorobenzene to phenoxyacetic acid, the organic The solubility of the layer to phenoxyacetic acid, thereby increasing the separation capacity of the separation layer. The present invention selects monovalent alcohols with very little water solubility, such as common chemical raw materials such as octanol and isononyl alcohol, according to the different specific gravity of various alcohols, the final organic layer (comprising chlorobenzene, alcohol, phenoxyacetic acid and other groups) The specific gravity is adjusted to 1.05-1.10, and the obtained separation layer is suitable for the treatment of concentrated brine.
发明内容SUMMARY OF THE INVENTION
本发明的目的在于提供一种高盐度废水的处理方法，使用含有吸水物质的有机分离层，在重力的作用下，使盐水中的淡水成分逐渐渗析至上层，从而实现盐-水的有效分离。The object of the present invention is to provide a method for treating high-salinity wastewater, using an organic separation layer containing water-absorbing substances, and under the action of gravity, the freshwater components in the brine are gradually dialyzed to the upper layer, thereby realizing the effective separation of salt-water .
本发明的技术方案是：The technical scheme of the present invention is:
一种高盐度废水的处理方法，以溶有吸水性物质的有机溶剂作为分离层，在重力的作用下将盐水中的水析出，实现浓水浓缩，淡水回用。A method for treating high-salinity wastewater, which uses an organic solvent in which water-absorbing substances are dissolved as a separation layer, and separates water in brine under the action of gravity, so as to realize concentrated water concentration and fresh water reuse.
所述的高盐度废水的处理方法，经过处理的盐水，含盐量范围为160g/L至饱和盐水。In the method for treating high-salinity wastewater, the salt content of the treated brine ranges from 160 g/L to saturated brine.
所述的高盐度废水的处理方法，分离层的组分为：氯苯85wt％～95wt％，吸水剂1wt％～2wt％，其余为辅助组分；其中，吸水剂为苯氧乙酸，辅助组分为一元醇。In the method for treating high salinity wastewater, the components of the separation layer are: 85wt% to 95wt% of chlorobenzene, 1wt% to 2wt% of a water absorbing agent, and the rest are auxiliary components; wherein, the water absorbing agent is phenoxyacetic acid, the auxiliary The component is a monohydric alcohol.
所述的高盐度废水的处理方法，一元醇为己醇、环己醇、正辛醇、2-乙基己醇或异壬醇。In the method for treating high salinity wastewater, the monohydric alcohol is hexanol, cyclohexanol, n-octanol, 2-ethylhexanol or isononanol.
所述的高盐度废水的处理方法，分离层的比重为1.055～1.097。In the method for treating high-salinity wastewater, the specific gravity of the separation layer is 1.055-1.097.
所述的高盐度废水的处理方法，分离层与盐水体积之比为，分离层：盐水＝(0.3～3.0)：1。In the method for treating high-salinity wastewater, the volume ratio of the separation layer to the brine is, separation layer: brine=(0.3-3.0):1.
所述的高盐度废水的处理方法，具体操作方法为：将分离层与盐水搅拌均匀，静置过夜，待淡水部分在分离层上方形成水层后，将上层淡水导出，过程可持续进行。The specific operation method of the high-salinity wastewater treatment method is as follows: stirring the separation layer and the salt water evenly, leaving it to stand overnight, and after the fresh water part forms a water layer above the separation layer, the upper layer fresh water is exported, and the process can be continued continuously.
所述的高盐度废水的处理方法，利用废热资源加速分离进程，其具体操作方法为：利用大于30℃的低品质热源，将盐水以及分离层或其混合物加热至30℃以上，再静置冷却，待淡水部分在分离层上方形成水层后，将上层淡水导出，过程可持续进行。The high-salinity wastewater treatment method utilizes waste heat resources to accelerate the separation process, and the specific operation method is as follows: using a low-quality heat source greater than 30°C, heating the brine and the separation layer or a mixture thereof to above 30°C, and then leaving it to stand. After cooling, after the fresh water part forms a water layer above the separation layer, the upper layer of fresh water is exported, and the process can continue.
所述的高盐度废水的处理方法，低品质热源是指工业中常见的废热。In the method for treating high-salinity wastewater, the low-quality heat source refers to waste heat commonly found in industry.
本发明的设计思想是：The design idea of the present invention is:
研究结果表明，本发明的方法可以有效实现浓盐水的水分离，即在重力的作用下，水“渗析”穿过有机分离层，在有机层的上方形成淡水层，不断导出淡水层，可以使分离过程连续进行，实现盐水分离。由于分离过程的中间驱动力为水在分离层中的溶解——再释放，而且水在分离层的溶解度随着温度的L高有较为明显的变化，因此温度的变化对分离过程有很明显的影响。利用工业中常见的废热(一般高于30℃即可利用，晾水塔的入水温度一般都超过这个水平)，可以明显加速处理过程。The research results show that the method of the present invention can effectively realize the water separation of concentrated brine, that is, under the action of gravity, water "dialysis" passes through the organic separation layer, and a freshwater layer is formed above the organic layer, and the freshwater layer is continuously exported, which can make The separation process is carried out continuously to realize the separation of brine. Since the intermediate driving force of the separation process is the dissolution and re-release of water in the separation layer, and the solubility of water in the separation layer changes significantly with the temperature of L, the temperature change has a significant impact on the separation process. influences. The use of common waste heat in the industry (generally higher than 30 °C can be used, and the inlet water temperature of the water drying tower generally exceeds this level) can significantly speed up the treatment process.
本发明的优点及有益效果是：The advantages and beneficial effects of the present invention are:
1、本发明能耗低、设备要求不高可以进行高盐度废水的预处理，为工业废水的进一步处理提供了基础。1. The present invention has low energy consumption and low equipment requirements, and can carry out pretreatment of high-salinity wastewater, which provides a basis for further treatment of industrial wastewater.
2、本发明可以利用废热将盐水及分离层加热，导出淡水后进行加热及冷却的循环，可以实现“废热强化的重力渗析过程”，实现加速的盐水分离操作。2. The present invention can use waste heat to heat the salt water and the separation layer, and then conduct the heating and cooling cycle after exporting the fresh water, which can realize the "waste heat-enhanced gravity dialysis process" and realize the accelerated brine separation operation.
3、本发明方法所生产的淡水适用于作为中水回用，也适用于经过环保装置进一步处理后达标排放。3. The fresh water produced by the method of the present invention is suitable for reuse as reclaimed water, and also suitable for discharge up to the standard after further treatment by an environmental protection device.
具体实施方式Detailed ways
在具体实施过程中，本发明高盐度废水的处理方法如下：In the specific implementation process, the treatment method of the high-salinity wastewater of the present invention is as follows:
按质量百分比计，将氯苯85％～95％、吸水剂(苯氧乙酸)1％～2％和其余的辅助组分(一元醇)混合制备分离层，将分离层与盐水(体积比0.3～3.0：1)搅拌均匀，静置过夜，待淡水部分在分离层上方形成水层后，将上层淡水导出，取样分析，若满足中水回用要求，可用于苯氧乙酸的生产。By mass percentage, 85%-95% of chlorobenzene, 1%-2% of water absorbing agent (phenoxyacetic acid) and the rest of the auxiliary components (monohydric alcohol) are mixed to prepare a separation layer, and the separation layer is mixed with brine (volume ratio 0.3 ~3.0:1) Stir evenly, let stand overnight, and after the fresh water part forms a water layer above the separation layer, export the upper fresh water, sample and analyze, if it meets the requirements of reclaimed water reuse, it can be used for the production of phenoxyacetic acid.
下面，通过实施例对本发明进一步详细阐述。Hereinafter, the present invention will be further described in detail through examples.
实施例一Example 1
取2吨苯氧乙酸生产过程中产生的废水注入5000L搪瓷釜中，其中含盐(氯化钠)量为300g/L，加入分离层2吨，其中分离层的组成为氯苯1900kg，正辛醇70kg，苯氧乙酸30kg，分离层比重为1.097。将混合物搅拌后静置过夜，由人孔观测分离层的上层有明显的水层生成(约50kg)。取样分析，上层水的含盐(氯化钠)量为5g/L，满足中水回用要求，可用于苯氧乙酸的生产。经过处理的盐水，含盐量范围为饱和浓度(311g/L)。Get the waste water that produces in 2 tons of phenoxyacetic acid production process and inject in 5000L enamel kettle, wherein salt (sodium chloride) amount is 300g/L, adds 2 tons of separation layer, and wherein the composition of separation layer is chlorobenzene 1900kg, n-octyl Alcohol 70kg, phenoxyacetic acid 30kg, separation layer specific gravity is 1.097. After stirring the mixture, it was left to stand overnight, and it was observed from the manhole that the upper layer of the separation layer had a clear water layer (about 50 kg). Sampling and analysis, the salt (sodium chloride) content of the upper layer water is 5g/L, which meets the requirement of reclaimed water reuse and can be used for the production of phenoxyacetic acid. The treated brine has a salt content in the range of saturated concentration (311g/L).
实施例二Embodiment 2
取2吨苯氧乙酸生产过程中产生的废水注入5000L搪瓷釜中，其中含盐(氯化钠)量为300g/L，加入分离层600kg，其中分离层的组成为氯苯540kg，环己醇48kg，苯氧乙酸12kg，分离层比重为1.085。将混合物搅拌后静置过夜，由人孔观测分离层的上层有明显的水层生成(约30kg)。取样分析，上层水的含盐(氯化钠)量为10g/L，满足中水回用要求，可用于苯氧乙酸的生产。经过处理的盐水，含盐量范围为饱和浓度(311g/L)。Get the waste water that produces in 2 tons of phenoxyacetic acid production process and inject in 5000L enamel kettle, wherein salt (sodium chloride) amount is 300g/L, adds separation layer 600kg, and wherein the composition of separation layer is chlorobenzene 540kg, cyclohexanol 48kg, 12kg of phenoxyacetic acid, and the specific gravity of the separation layer is 1.085. After stirring the mixture, it was left to stand overnight, and the upper layer of the separation layer was observed to have a clear water layer (about 30 kg) formed from the manhole. Sampling and analysis, the salt (sodium chloride) content of the upper layer water is 10g/L, which meets the requirement of reclaimed water reuse and can be used for the production of phenoxyacetic acid. The treated brine has a salt content in the range of saturated concentration (311g/L).
实施例三Embodiment 3
取1吨苯氧乙酸生产过程及洗涤过程中产生的混合废水注入5000L搪瓷釜中，其中含盐(氯化钠)量为160g/L，加入分离层3000kg，其中分离层的组成为氯苯2850kg，异辛醇120kg，苯氧乙酸30kg，分离层比重为1.070。将混合物搅拌后静置过夜，由人孔观测分离层的上层有明显的水层生成(约110kg)。取样分析，上层水的含盐(氯化钠)量为4g/L，满足中水回用要求，可用于苯氧乙酸的生产。经过处理的盐水，含盐量范围为180g/L。Get the mixed waste water that produces in 1 ton of phenoxyacetic acid production process and washing process and inject in 5000L enamel kettle, wherein salt (sodium chloride) amount is 160g/L, adds separation layer 3000kg, and wherein the composition of separation layer is chlorobenzene 2850kg , 120kg of isooctyl alcohol, 30kg of phenoxyacetic acid, and the specific gravity of the separation layer is 1.070. After the mixture was stirred, it was left to stand overnight, and it was observed from the manhole that a water layer (about 110 kg) was clearly formed in the upper layer of the separation layer. Sampling and analysis, the salt (sodium chloride) content of the upper layer water is 4g/L, which meets the requirement of reclaimed water reuse and can be used for the production of phenoxyacetic acid. The treated brine has a salt content in the range of 180g/L.
实施例四Embodiment 4
取2吨经过反复重力渗析处理过的水样(苯氧乙酸生产过程中产生的废水)，注入5000L搪瓷釜中，其中含盐(氯化钠)量为260g/L，加入分离层1000kg，其中分离层的组成为氯苯850kg，异壬醇140kg，苯氧乙酸10kg，分离层比重为1.055。将混合物搅拌后静置过夜，由人孔观测分离层的上层有明显的水层生成(约40kg)。取样分析，上层水的含盐(氯化钠)量为10g/L，满足中水回用要求，可用于苯氧乙酸的生产。经过处理的盐水，含盐量范围为270g/L。Get 2 tons of water samples (waste water produced in the production process of phenoxyacetic acid) processed through repeated gravity dialysis, inject in 5000L enamel kettle, wherein salt (sodium chloride) amount is 260g/L, add separation layer 1000kg, wherein The composition of the separation layer was 850 kg of chlorobenzene, 140 kg of isononanol, and 10 kg of phenoxyacetic acid, and the specific gravity of the separation layer was 1.055. After stirring the mixture, it was left to stand overnight, and it was observed from the manhole that a water layer (about 40 kg) was clearly formed in the upper layer of the separation layer. Sampling and analysis, the salt (sodium chloride) content of the upper layer water is 10g/L, which meets the requirement of reclaimed water reuse and can be used for the production of phenoxyacetic acid. The treated brine has a salt content in the range of 270g/L.
实施例五Embodiment 5
取2吨苯氧乙酸生产过程中产生的废水，注入5000L搪瓷釜中，其中含盐(氯化钠)量为已达到饱和，加入分离层2000kg，其中分离层的组成同实施例一。以待进入晾水塔的循环冷却水为热源，泵入搪瓷釜夹套内对釜内液体进行加热，并搅拌，待升温至30～35℃时停止加热并冷却，由人孔观测分离层的上层有明显的水层生成(约50kg)。取样分析，上层水的含盐(氯化钠)量为6g/L，满足中水回用要求，可用于苯氧乙酸的生产。经过处理的盐水，仍然为饱和状态。Get the waste water that produces in 2 tons of phenoxyacetic acid production process, inject in 5000L enamel kettle, wherein salt (sodium chloride) amount is to have reached saturation, add separation layer 2000kg, and wherein the composition of separation layer is with embodiment one. Taking the circulating cooling water to be entered into the water drying tower as the heat source, pump it into the jacket of the enamel kettle to heat the liquid in the kettle and stir it. When the temperature rises to 30-35°C, stop heating and cooling, and observe the upper layer of the separation layer through the manhole. There was significant water layer formation (about 50 kg). Sampling and analysis, the salt (sodium chloride) content of the upper layer water is 6g/L, which meets the requirement of reclaimed water reuse and can be used for the production of phenoxyacetic acid. The treated brine is still saturated.
将生成的淡水导出，重复进行此过程，结果列表如下：Export the generated fresh water and repeat this process, the result list is as follows:
对比例Comparative ratio
取2吨苯氧乙酸生产过程中产生的废水注入5000L搪瓷反应釜中，加入1.5吨氯苯，搅拌后静置过夜，第二天由人孔观测，氯苯上层无水层生成。The waste water produced in the production process of 2 tons of phenoxyacetic acid was injected into a 5000L enamel reaction kettle, and 1.5 tons of chlorobenzene was added.
实施例和对比例结果表明，本发明利用盐水、有机溶剂和淡水的密度不同，在溶剂中添加吸水性物质形成分离层，在重力的作用下逐渐分层，即下层为高盐度废水，中层为有机溶剂分离层，上层为淡水，可以进行中水回用，废热资源可以用来加速分离进程。The results of the examples and comparative examples show that the present invention utilizes the different densities of salt water, organic solvents and fresh water, and adds water-absorbing substances to the solvent to form a separation layer, which is gradually layered under the action of gravity, that is, the lower layer is high-salinity waste water, and the middle layer is high-salinity wastewater. It is an organic solvent separation layer, and the upper layer is fresh water, which can be reused for reclaimed water, and waste heat resources can be used to speed up the separation process.
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Citations (11)
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