A kind of treatment method of epichlorohydrin production waste water

Abstract

The invention belongs to the technical field of organic wastewater treatment, and in particular relates to a treatment method for epichlorohydrin production wastewater. The treatment method is to mix the catalytic oxidation aid in the epichlorohydrin production wastewater in advance, enter the oxidation reactor after preheating, and oxidize with the oxidant, so as to oxidize the organic matter in the wastewater to H 2 O.CO 2 and HCl, the reaction solution after the reaction is desalted by flash evaporation and evaporation concentration. The present invention combines soluble cobalt salt and Nd 2 o 5 The combination of / SBA-15 gives full play to the synergistic effect between the two, so that the organic matter in the wastewater can be quickly and deeply oxidized and removed; the COD content in the organic wastewater can be greatly reduced, and the water and inorganic solid salt can be effectively separated, and the water and The content of organic matter in the inorganic solid salt is low, the separated water can be reused, and the inorganic solid salt can also be used as a by-product.

Description

technical field

[0001] The invention belongs to the technical field of organic wastewater treatment, and in particular relates to a treatment method for epichlorohydrin production wastewater. Background technique

[0002] With the mass production of biodiesel, the production of its by-product crude glycerol also increases rapidly. The method of using glycerol to directly produce epichlorohydrin is more and more favored by people because of its advantages of less investment, low cost, simple production process, and clean production. However, this method will produce a large amount of high-salt organic wastewater containing glycerin in the production process of epichlorohydrin, the salt content is as high as 200g / L, and the COD content is as high as 3000mg / L or more. Due to the different saponification agents used, the types of salt in epichlorohydrin production wastewater are also different, mainly sodium chloride or calcium chloride.

[0003] Chinese patent CN101318750A di...

Examples

Embodiment 1

[0040] Add the waste water from the production of epichlorohydrin into the waste water storage tank, add the catalytic oxidation aid anhydrous cobalt chloride and stir evenly, then preheat, and after preheating, enter the porous solid catalyst Nd 2 o 5 In the oxidation reactor of / SBA-15, it reacts with the oxidant, and controls the temperature, pressure, flow rate and residence time of the reaction; after the reaction is completed, samples are taken at the outlet of the oxidation reactor for analysis, and then the treated organic wastewater enters the flash evaporation The temperature is lowered, and the solid salt is separated by centrifugation through the desalination filter. The concentrated liquid after centrifugation is returned to the filter device, and then enters the preheating device, which is applied to the process to realize the recycling of catalytic oxidation additives. The treated organic wastewater was measured for COD and calculated for its removal rate, and a...

Embodiment 2

[0045] The process parameters are:

[0046] (1) NaCl content is 15.0wt.% in the epichlorohydrin production wastewater, and COD is 5000mg / L; After adding anhydrous cobalt chloride in the epichlorohydrin production wastewater, Co 2+ The molar concentration in epichlorohydrin production wastewater is 0.3mmol / L; the preheating temperature is 150°C; the reaction temperature is 150°C, the reaction pressure is 5.0MPa, the residence time is 60min, the flow rate of wastewater is 16.7ml / min, and the oxidant for air;

[0047] (2) After testing, the removal rate of COD in the treated organic wastewater is 97.75%, and the recovery rate of NaCl is 99.1%. After the solid salt is dried, it is analyzed, and its quality index is: NaCl: 98.2wt.%; Co 2+ : 1.5 μg / g; TOC: 9.3 μg / g.

Embodiment 3

[0049] The process parameters are:

[0050] (1) CaCl in epichlorohydrin production wastewater 2 The content is 14.0wt.%, and the COD is 4500mg / L; after adding anhydrous cobalt chloride to the epichlorohydrin production wastewater, Co 2+ The molar concentration in the epichlorohydrin production wastewater is 0.2mmol / L; the preheating temperature is 250°C; the reaction temperature is 250°C, the reaction pressure is 8.0MPa, the residence time is 10min, the wastewater flow rate is 100ml / min, and the oxidant is oxygen;

[0051] (2) After testing, the removal rate of COD in the treated organic wastewater is 97.31%, and CaCl 2 The recovery rate is 99.3%, and the solid salt is analyzed after drying, and its quality index is: CaCl 2 : 98.3wt.%; Co 2+ : 1.7 μg / g; TOC: 10.0 μg / g.

technical field

[0001] The invention belongs to the technical field of organic wastewater treatment, and in particular relates to a treatment method for epichlorohydrin production wastewater. Background technique

[0002] With the mass production of biodiesel, the production of its by-product crude glycerol also increases rapidly. The method of using glycerol to directly produce epichlorohydrin is more and more favored by people because of its advantages of less investment, low cost, simple production process, and clean production. However, this method will produce a large amount of high-salt organic wastewater containing glycerin in the production process of epichlorohydrin, the salt content is as high as 200g / L, and the COD content is as high as 3000mg / L or more. Due to the different saponification agents used, the types of salt in epichlorohydrin production wastewater are also different, mainly sodium chloride or calcium chloride.

[0003] Chinese patent CN101318750A di...

Examples

Embodiment 1

[0040] Add the waste water from the production of epichlorohydrin into the waste water storage tank, add the catalytic oxidation aid anhydrous cobalt chloride and stir evenly, then preheat, and after preheating, enter the porous solid catalyst Nd 2 o 5 In the oxidation reactor of / SBA-15, it reacts with the oxidant, and controls the temperature, pressure, flow rate and residence time of the reaction; after the reaction is completed, samples are taken at the outlet of the oxidation reactor for analysis, and then the treated organic wastewater enters the flash evaporation The temperature is lowered, and the solid salt is separated by centrifugation through the desalination filter. The concentrated liquid after centrifugation is returned to the filter device, and then enters the preheating device, which is applied to the process to realize the recycling of catalytic oxidation additives. The treated organic wastewater was measured for COD and calculated for its removal rate, and a...

Embodiment 2

[0045] The process parameters are:

[0046] (1) NaCl content is 15.0wt.% in the epichlorohydrin production wastewater, and COD is 5000mg / L; After adding anhydrous cobalt chloride in the epichlorohydrin production wastewater, Co 2+ The molar concentration in epichlorohydrin production wastewater is 0.3mmol / L; the preheating temperature is 150°C; the reaction temperature is 150°C, the reaction pressure is 5.0MPa, the residence time is 60min, the flow rate of wastewater is 16.7ml / min, and the oxidant for air;

[0047] (2) After testing, the removal rate of COD in the treated organic wastewater is 97.75%, and the recovery rate of NaCl is 99.1%. After the solid salt is dried, it is analyzed, and its quality index is: NaCl: 98.2wt.%; Co 2+ : 1.5 μg / g; TOC: 9.3 μg / g.

Embodiment 3

[0049] The process parameters are:

[0050] (1) CaCl in epichlorohydrin production wastewater 2 The content is 14.0wt.%, and the COD is 4500mg / L; after adding anhydrous cobalt chloride to the epichlorohydrin production wastewater, Co 2+ The molar concentration in the epichlorohydrin production wastewater is 0.2mmol / L; the preheating temperature is 250°C; the reaction temperature is 250°C, the reaction pressure is 8.0MPa, the residence time is 10min, the wastewater flow rate is 100ml / min, and the oxidant is oxygen;

[0051] (2) After testing, the removal rate of COD in the treated organic wastewater is 97.31%, and CaCl 2 The recovery rate is 99.3%, and the solid salt is analyzed after drying, and its quality index is: CaCl 2 : 98.3wt.%; Co 2+ : 1.7 μg / g; TOC: 10.0 μg / g.

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