CN102642963B - A comprehensive treatment method for vanadium-containing salty wastewater from stone coal extraction - Google Patents
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- 229910052720 vanadium Inorganic materials 0.000 title claims abstract description 49
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 title claims abstract description 49
- 239000003245 coal Substances 0.000 title claims abstract description 45
- 239000004575 stone Substances 0.000 title claims abstract description 42
- 239000002351 wastewater Substances 0.000 title claims abstract description 42
- 238000000605 extraction Methods 0.000 title claims abstract description 38
- 238000000034 method Methods 0.000 title claims abstract description 33
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 47
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- 238000010438 heat treatment Methods 0.000 claims description 11
- 239000012510 hollow fiber Substances 0.000 claims description 11
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical class O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 claims description 11
- 238000010612 desalination reaction Methods 0.000 claims description 10
- 230000002209 hydrophobic effect Effects 0.000 claims description 6
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- 238000001556 precipitation Methods 0.000 claims description 3
- CDBYLPFSWZWCQE-UHFFFAOYSA-L sodium carbonate Substances [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 3
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 3
- 239000000463 material Substances 0.000 claims description 2
- 238000005265 energy consumption Methods 0.000 abstract description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 abstract 2
- 238000004064 recycling Methods 0.000 abstract 2
- WAEMQWOKJMHJLA-UHFFFAOYSA-N Manganese(2+) Chemical compound [Mn+2] WAEMQWOKJMHJLA-UHFFFAOYSA-N 0.000 abstract 1
- 238000011033 desalting Methods 0.000 abstract 1
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- 229910052742 iron Inorganic materials 0.000 abstract 1
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- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
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Abstract
Description
技术领域 technical field
本发明属于含盐废水处理及综合利用领域，尤其涉及一种石煤提钒含盐废水的综合处理方法。The invention belongs to the field of saline waste water treatment and comprehensive utilization, in particular to a comprehensive treatment method for vanadium-containing waste water from stone coal extraction.
背景技术 Background technique
随着钒在钢铁、化工、航空航天等领域的广泛应用，钒的消费量不断增加。我国作为钒资源丰富的国家之一，逐渐成为世界钒市场的强有力竞争者(王永双等，我国石煤提钒及综合利用综述《钒钛》1993，4：21-31)。石煤是我国一种重要的含钒资源，具有储量大、分布广泛等特点，因此从石煤中提钒是满足今后钒需求的重要途径。在石煤提钒焙烧过程中通常需要添加一定量的工业盐作为焙烧添加剂促进钒的提取，导致提钒废水的含盐量很高(Yi-MinZhang，et al.The technology of extracting Vanadium from stone coal in China：History，currentstatus and future prospects.《Hydrometallurgy》2011，109：116～124)。这种含盐废水会腐蚀设备，如果不经处理直接外排，会导致排放区域的土壤板结，农作物受损，水体盐碱化，影响生态环境。所以，必须对此类含盐废水进行处理，同时实现废水的综合利用，降低生产成本。With the wide application of vanadium in steel, chemical industry, aerospace and other fields, the consumption of vanadium continues to increase. As one of the countries rich in vanadium resources, my country has gradually become a strong competitor in the world vanadium market (Wang Yongshuang et al., Summary of Vanadium Extraction and Comprehensive Utilization of Stone Coal in my country "Vadium and Titanium" 1993, 4: 21-31). Stone coal is an important vanadium-containing resource in my country, which has the characteristics of large reserves and wide distribution. Therefore, extracting vanadium from stone coal is an important way to meet the demand for vanadium in the future. In the roasting process of vanadium extraction from stone coal, it is usually necessary to add a certain amount of industrial salt as a roasting additive to promote the extraction of vanadium, resulting in a high salt content in vanadium extraction wastewater (Yi-MinZhang, et al. The technology of extracting Vanadium from stone coal in China: History, current status and future prospects. "Hydrometallurgy" 2011, 109: 116～124). This kind of salty wastewater will corrode equipment. If it is discharged directly without treatment, it will cause soil compaction in the discharge area, damage to crops, salinization of water body, and affect the ecological environment. Therefore, it is necessary to treat this kind of saline wastewater, and at the same time realize the comprehensive utilization of wastewater and reduce production costs.
对含盐废水进行脱盐处理，实现该类水体的无害排放是当前环保领域急需解决的问题之一。当前，对于石煤提钒含盐废水一般采用金属还原-石灰中和法处理，这种方法工艺流程简单，可以除去废水中大部分有害的重金属离子(曾凡勇，酸法石煤提钒废水处理探讨《工程设计与研究(长沙)》1996，3：62-64)，但处理后的废水仍然存在盐浓度较高的问题，需要进一步处理。Desalination treatment of saline wastewater to realize the harmless discharge of such water is one of the urgent problems in the field of environmental protection. At present, metal reduction-lime neutralization method is generally used for the treatment of vanadium extraction wastewater from stone coal. "Engineering Design and Research (Changsha)" 1996, 3: 62-64), but the treated wastewater still has the problem of high salt concentration, which needs further treatment.
当前处理含盐废水的技术有多效蒸馏和膜法处理工艺：多效蒸馏可以极大程度地浓缩含盐溶液，但由于废水的操作温度接近100℃，能量消耗很大，设备易腐蚀(于开录等，低温多效蒸馏海水淡化工程与技术进展《中国给水排水》2008，24：82-85)，同时存在设备投资巨大，处理成本很高等缺点；膜法处理工艺有反渗透和电渗析，由于处理过程中无需将废水加热到较高温度，降低了能耗，但膜法处理工艺对预处理要求较高，且膜容易污染(褚彦杰等，反渗透膜污染及其在膜面分布特征研究《水处理技术》2012，38：72-74，133)，同时由于受到膜性能的限制，浓缩程度有限，而且处理后仍有一部分二次高浓盐水排放(赵世刚等，反渗透浓水回收利用的探讨《工业用水与废水；李广等，电渗析技术的发展及应用《化学技术与开发》2008，37：28-30)，会造成环境的二次污染。The current technology for treating saline wastewater is multi-effect distillation and membrane treatment process: multi-effect distillation can greatly concentrate saline solution, but because the operating temperature of wastewater is close to 100°C, the energy consumption is large, and the equipment is easy to corrode (in Kai Lu et al., Low-temperature multi-effect distillation seawater desalination engineering and technical progress "China Water Supply and Drainage" 2008, 24: 82-85), and there are disadvantages such as huge investment in equipment and high treatment costs; membrane treatment processes include reverse osmosis and electrodialysis , because there is no need to heat the wastewater to a higher temperature during the treatment process, the energy consumption is reduced, but the membrane treatment process has higher requirements for pretreatment, and the membrane is easily polluted (Chu Yanjie et al., reverse osmosis membrane fouling and its distribution characteristics on the membrane surface Research "Water Treatment Technology" 2012, 38: 72-74, 133), at the same time, due to the limitation of membrane performance, the degree of concentration is limited, and there is still a part of secondary high-concentration brine discharge after treatment (Zhao Shigang et al., Reverse Osmosis Concentrated Water Recovery Discussion on the use of "Industrial Water and Wastewater; Li Guang et al., Development and Application of Electrodialysis Technology" Chemical Technology and Development, 2008, 37: 28-30), will cause secondary pollution to the environment.
发明内容 Contents of the invention
本发明旨在克服已有技术的缺陷，目的是提供一种能量消耗较小、处理成本较低、对环境无二次污染、能全部回收其中淡水和盐类的石煤提钒含盐废水的综合处理方法。The present invention aims to overcome the defects of the prior art, and the purpose is to provide a method for extracting vanadium-containing saline wastewater from stone coal with less energy consumption, lower treatment cost, no secondary pollution to the environment, and full recovery of fresh water and salts therein. Comprehensive processing method.
为实现上述目的，本发明采用的技术方案的具体步骤是：In order to achieve the above object, the concrete steps of the technical solution adopted in the present invention are:
第一步、预处理The first step, preprocessing
采用石灰中和-纯碱除硬-絮凝沉淀法，将石煤提钒含盐废水预处理至：Fe2+＜0.3mg/L，Mn2+＜0.1mg/L，SS＜1mg/L。Lime neutralization-soda ash removal-flocculation precipitation method is used to pretreat the saline waste water from vanadium extraction from stone coal to: Fe 2+ <0.3mg/L, Mn 2+ <0.1mg/L, SS<1mg/L.
第二步、倒极电渗析The second step, inverted electrodialysis
采用倒极电渗析对预处理后的石煤提钒含盐废水进行脱盐处理，脱盐处理过程中每2～2.5小时变换极性一次，倒极电渗析处理后的石煤提钒含盐废水盐度浓缩至100000～120000mg/L，得到淡水和浓水，其中淡水回用于石煤提钒工艺。Use inverted electrodialysis to desalinate the pretreated waste water containing vanadium from stone coal extraction. During the desalination process, the polarity is changed every 2 to 2.5 hours. concentration to 100,000-120,000 mg/L to obtain fresh water and concentrated water, of which the fresh water is reused in the vanadium extraction process from stone coal.
第三步、减压膜蒸馏The third step, vacuum membrane distillation
采用减压膜蒸馏工艺对第二步得到的浓水进行浓缩处理，浓缩处理过程中渗透侧真空度为90～95kPa，得到饱和盐水和冷凝水，冷凝水回用于石煤提钒工艺，饱和盐水进入浓水池。The concentrated water obtained in the second step is concentrated by the vacuum membrane distillation process. During the concentration process, the vacuum degree of the permeate side is 90-95kPa, and saturated brine and condensed water are obtained. The condensed water is reused in the stone coal vanadium extraction process, saturated The brine enters the brine.
第四步、结晶The fourth step, crystallization
结晶是在与浓水池相通的结晶室中进行，结晶室中预先加有固体NaCl；从浓水池进入结晶室的饱和盐水在结晶室结晶，结晶后的结晶盐通过晒盐制得工业盐，所得工业盐返回石煤提钒工艺；结晶液经过滤返回浓水池，将浓水池的上清液与电渗析产生的浓水合并，合并后的上清液与浓水经加热后返回第三步的减压膜蒸馏工艺。The crystallization is carried out in the crystallization chamber connected with the concentrated water tank, and solid NaCl is pre-added in the crystallization chamber; the saturated brine entering the crystallization chamber from the concentrated water tank is crystallized in the crystallization chamber, and the crystallized salt after crystallization is made into industrial salt by drying the salt, and the obtained Industrial salt is returned to the stone coal vanadium extraction process; the crystallization liquid is filtered and returned to the concentrated water tank, the supernatant of the concentrated water tank is combined with the concentrated water generated by electrodialysis, and the combined supernatant and concentrated water are returned to the third step after heating Vacuum membrane distillation process.
所述石煤提钒含盐废水的总盐度为10000～35000mg/L。The total salinity of the saline waste water from vanadium extraction from stone coal is 10000-35000mg/L.
所述加热的热源为工业废热，加热后的温度为55～75℃。The heat source of the heating is industrial waste heat, and the temperature after heating is 55-75°C.
所述的减压膜蒸馏中所用的膜蒸馏组件采用中空纤维式膜组件，中空纤维式膜组件的填充率为30％～60％，长径比为(3～6)∶1；中空纤维式膜组件的材质为疏水性聚偏氟乙烯或疏水性聚四氟乙烯，平均孔径为0.2μm。The membrane distillation module used in the vacuum membrane distillation adopts a hollow fiber membrane module, the filling rate of the hollow fiber membrane module is 30% ~ 60%, and the aspect ratio is (3 ~ 6): 1; The material of the membrane module is hydrophobic polyvinylidene fluoride or hydrophobic polytetrafluoroethylene, and the average pore size is 0.2 μm.
由于采用上述技术方案，本发明的加热热源为工业废热，且只需将石煤提钒含盐废水加热到55～75℃，在制备工业盐时采用晒盐工艺，故能量消耗较小；在综合处理过程中能全部回收其中的淡水和盐类，最终产物直接回用于石煤提钒工艺，实现了废水的综合利用，对环境无二次污染，处理成本低。Due to the adoption of the above-mentioned technical scheme, the heating heat source of the present invention is industrial waste heat, and it only needs to heat the saline waste water from the extraction of vanadium from stone coal to 55-75°C, and the sun-dried salt process is used in the preparation of industrial salt, so the energy consumption is relatively small; During the comprehensive treatment process, all the fresh water and salts in it can be recovered, and the final product can be directly reused in the stone coal vanadium extraction process, realizing the comprehensive utilization of wastewater, no secondary pollution to the environment, and low treatment cost.
本发明还具有工艺灵活的特点，既可用于石煤提钒含盐废水的综合处理，也可用于其他工业上含盐废水的处理、苦咸水淡化处理和海水淡化处理。The invention also has the characteristics of flexible process, and can be used not only for comprehensive treatment of saline waste water from vanadium extraction from stone coal, but also for treatment of other industrial saline waste water, brackish water desalination treatment and seawater desalination treatment.
附图说明 Description of drawings
图1为本发明的一种工艺流程框图。Fig. 1 is a kind of process flow block diagram of the present invention.
具体实施方式 Detailed ways
下面结合附图和具体实施方式对本发明作进一步描述，并非对其保护范围的限制：The present invention will be further described below in conjunction with accompanying drawing and specific embodiment, not limitation to its protection scope:
为避免重复，先将本具体实施方式所要进行综合处理的石煤提钒含盐废水的化学成分描述如下，实施例中不再赘述：总盐度为10000～35000mg/L，Ca2+为300～650mg/L，Mg2+为60～300mg/L，SS(固体悬浮物)为400～750mg/L；主要重金属离子是：Zn2+为45～75mg/L，Fe2+为30～50mg/L，Cu2+为10～30mg/L，Mn2+为0.5～4mg/L。In order to avoid repetition, the chemical composition of the vanadium-extracting salty wastewater from stone coal to be comprehensively treated in this specific embodiment is described as follows, and will not be repeated in the examples: the total salinity is 10000-35000mg/L, and Ca2 + is 300 ～650mg/L, Mg 2+ is 60～300mg/L, SS (solid suspended solids) is 400～750mg/L; main heavy metal ions are: Zn 2+ is 45～75mg/L, Fe 2+ is 30～50mg /L, Cu 2+ is 10-30mg/L, and Mn 2+ is 0.5-4mg/L.
实施例1Example 1
一种石煤提钒含盐废水的综合处理方法。其处理工艺的具体步骤如图1所示：A comprehensive treatment method for vanadium-extracting salty wastewater from stone coal. The specific steps of its processing technology are as shown in Figure 1:
第一步、预处理The first step, preprocessing
采用石灰中和-纯碱除硬-絮凝沉淀法，将石煤提钒含盐废水预处理至：Fe2+＜0.3mg/L，Mn2+＜0.1mg/L，SS＜1mg/L。Lime neutralization-soda ash removal-flocculation precipitation method is used to pretreat the saline waste water from vanadium extraction from stone coal to: Fe 2+ <0.3mg/L, Mn 2+ <0.1mg/L, SS<1mg/L.
第二步、倒极电渗析The second step, inverted electrodialysis
采用倒极电渗析对预处理后的石煤提钒含盐废水进行脱盐处理，脱盐处理过程中每2～2.5小时变换极性一次，倒极电渗析处理后的石煤提钒含盐废水盐度浓缩至100000～110000mg/L，得到淡水和浓水，其中淡水回用于石煤提钒工艺。Use inverted electrodialysis to desalinate the pretreated waste water containing vanadium from stone coal extraction. During the desalination process, the polarity is changed every 2 to 2.5 hours. concentration to 100,000-110,000 mg/L to obtain fresh water and concentrated water, of which the fresh water is reused in the vanadium extraction process from stone coal.
第三步、减压膜蒸馏The third step, vacuum membrane distillation
采用减压膜蒸馏工艺对第二步得到的浓水进行浓缩处理，浓缩处理过程中渗透侧真空度为90～95kPa，得到饱和盐水和冷凝水，冷凝水回用于石煤提钒工艺，饱和盐水进入浓水池。The concentrated water obtained in the second step is concentrated by the vacuum membrane distillation process. During the concentration process, the vacuum degree of the permeate side is 90-95kPa, and saturated brine and condensed water are obtained. The condensed water is reused in the stone coal vanadium extraction process, saturated The brine enters the brine.
第四步、结晶The fourth step, crystallization
结晶是在与浓水池相通的结晶室中进行，结晶室中预先加有固体NaCl；从浓水池进入结晶室的饱和盐水在结晶室结晶，结晶后的结晶盐通过晒盐制得工业盐，所得工业盐返回石煤提钒工艺；结晶液经过滤返回浓水池，将浓水池的上清液与电渗析产生的浓水合并，合并后的上清液与浓水经加热后返回第三步的减压膜蒸馏工艺。The crystallization is carried out in the crystallization chamber connected with the concentrated water tank, and solid NaCl is pre-added in the crystallization chamber; the saturated brine entering the crystallization chamber from the concentrated water tank is crystallized in the crystallization chamber, and the crystallized salt after crystallization is made into industrial salt by drying the salt, and the obtained Industrial salt is returned to the stone coal vanadium extraction process; the crystallization liquid is filtered and returned to the concentrated water tank, the supernatant of the concentrated water tank is combined with the concentrated water generated by electrodialysis, and the combined supernatant and concentrated water are returned to the third step after heating Vacuum membrane distillation process.
本实施例所述加热的热源为工业废热，加热后的温度为55～65℃。The heat source for heating in this embodiment is industrial waste heat, and the temperature after heating is 55-65°C.
本实施例所述的减压膜蒸馏中所用的膜蒸馏组件采用中空纤维式膜组件，中空纤维式膜组件的填充率为30％～40％，长径比为(3～4)∶1；中空纤维式膜组件的材质为疏水性聚偏氟乙烯，平均孔径为0.2μm。The membrane distillation module used in the vacuum membrane distillation described in this embodiment adopts a hollow fiber membrane module, the filling rate of the hollow fiber membrane module is 30% to 40%, and the aspect ratio is (3 to 4): 1; The hollow fiber membrane module is made of hydrophobic polyvinylidene fluoride with an average pore size of 0.2 μm.
实施例2Example 2
一种石煤提钒含盐废水的综合处理方法。其处理工艺的具体步骤如图1所示A comprehensive treatment method for vanadium-extracting salty wastewater from stone coal. The specific steps of its treatment process are shown in Figure 1
第一步、预处理The first step, preprocessing
同实施例1第一步。Same as the first step in Example 1.
第二步、倒极电渗析The second step, inverted electrodialysis
采用倒极电渗析对预处理后的石煤提钒含盐废水进行脱盐处理，脱盐处理过程中每2～2.5小时变换极性一次，倒极电渗析处理后的石煤提钒含盐废水盐度浓缩至110000～120000mg/L，得到淡水和浓水，其中淡水回用于石煤提钒工艺。Use inverted electrodialysis to desalinate the pretreated waste water containing vanadium from stone coal extraction. During the desalination process, the polarity is changed every 2 to 2.5 hours. concentration to 110,000-120,000 mg/L to obtain fresh water and concentrated water, of which the fresh water is reused in the stone coal vanadium extraction process.
第三步、减压膜蒸馏The third step, vacuum membrane distillation
同实施例1第三步。Same as the third step of Example 1.
第四步、结晶The fourth step, crystallization
除加热后的温度为65～75℃外，其余同实施例1第四步。Except that the temperature after heating is 65～75 ℃, all the other are the same as the fourth step of embodiment 1.
本实施例所述的减压膜蒸馏中所用的膜蒸馏组件采用中空纤维式膜组件，中空纤维式膜组件的填充率为40％～60％，长径比为(4～6)∶1；中空纤维式膜组件的材质为疏水性聚四氟乙烯，平均孔径为0.2μm。The membrane distillation module used in the vacuum membrane distillation described in this embodiment adopts a hollow fiber membrane module, the filling rate of the hollow fiber membrane module is 40% to 60%, and the aspect ratio is (4 to 6): 1; The hollow fiber membrane module is made of hydrophobic polytetrafluoroethylene with an average pore size of 0.2 μm.
本具体实施方式的加热热源为工业废热，且只需将石煤提钒含盐废水加热到55～75℃，在制备工业盐时采用晒盐工艺，故能量消耗较小；在处理过程中能全部回收淡水和其中的盐类，最终产物直接回用于石煤提钒工艺，实现了废水的综合利用，对环境无二次污染，处理成本低。The heating heat source in this specific embodiment is industrial waste heat, and it only needs to heat the saline waste water from the extraction of vanadium from stone coal to 55-75°C, and the sun-dried salt process is used in the preparation of industrial salt, so the energy consumption is relatively small; All fresh water and its salts are recovered, and the final product is directly reused in the stone coal vanadium extraction process, which realizes the comprehensive utilization of waste water, has no secondary pollution to the environment, and has low treatment costs.
本具体实施方式还具有工艺灵活的特点，既可用于石煤提钒含盐废水的综合处理，也可用于其他工业上含盐废水的处理、苦咸水淡化处理和海水淡化处理。This specific embodiment also has the characteristics of flexible process, which can be used not only for the comprehensive treatment of saline waste water from vanadium extraction from stone coal, but also for the treatment of other industrial saline waste water, brackish water desalination treatment and seawater desalination treatment.
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| CN103336897A (en) * | 2013-06-21 | 2013-10-02 | 武汉理工大学 | Environment evaluation method of stone coal vanadium-extracting solid waste |
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| CN108609775A (en) * | 2018-05-25 | 2018-10-02 | 北京林业大学 | A kind of method of efficient process waste incineration leachate reverse osmosis concentrated water |
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