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Resource utilization method for high-salt wastewater from epichlorohydrin preparation through glycerol method

A technology for epichlorohydrin and high-salt wastewater, applied in chemical instruments and methods, separation/purification of alkali metal chlorides and carboxylic acid compounds, etc. , to achieve the effect of simple process flow, low recyclable resources and low secondary pollution

Inactive Publication Date: 2016-06-08
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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Problems solved by technology

Ningbo Huanyang Chemical Co., Ltd. adopts multi-effect evaporation and crystallization purification process in CN101798154B to recover anhydrous calcium chloride, but this method cannot degrade organic matter, the resource utilization rate is low, and the impurity content of calcium chloride produced is relatively high
In CN103342434A, Ningbo Huanyang Chemical Co., Ltd. adopts the Fenton oxidation technology and wet oxidation technology in the advanced oxidation method to pretreat the saponified wastewater, which improves the quality of calcium chloride, but this technology has the following disadvantages: from the perspective of cost Considering that Fenton oxidation technology is not suitable for saponification wastewater treatment with COD greater than 6000mg / L, when the wastewater COD is high, the mineralization rate of Fenton oxidation technology is low; in this patent, iron-carbon filler is used as the catalyst in wet oxidation , when the reaction temperature is greater than 180°C, the carbon in the filler will gradually oxidize to carbon dioxide, and under the harsh reaction conditions of wet oxidation, metallic iron will also dissolve quickly, so this filler is not suitable for high-temperature wet oxidation system; in this patent The maximum reaction pressure is 1.6MPa. When the reaction temperature is high, it is impossible to ensure that the wastewater is in a liquid state in the reaction tower; the oxidant used in this patent is pure oxygen, and the inner wall of the reactor is made of titanium. In the high-temperature pure oxygen system, titanium has a certain The probability of spontaneous combustion occurs, so the system has a high risk factor
[0007] As can be seen from the prior art described above, there are many defects in it, which seriously affects the application of these technologies in saponification wastewater treatment

Method used

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  • Resource utilization method for high-salt wastewater from epichlorohydrin preparation through glycerol method
  • Resource utilization method for high-salt wastewater from epichlorohydrin preparation through glycerol method
  • Resource utilization method for high-salt wastewater from epichlorohydrin preparation through glycerol method

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Embodiment 1

[0035] Take 1L of glycerol method epichlorohydrin high-salt wastewater, add 48g of 37wt% concentrated hydrochloric acid to the adjustment tank to adjust to pH = 3, dilute the wastewater by 4 times with deionized water, add CuCl 2 As a catalyst, its dosage is 0.5wt.% of the high-salt wastewater. Then it is mixed with air through the pipeline and then enters the heat exchanger to be heated to 220°C, and finally enters the catalytic wet oxidation reaction tower for reaction. The catalytic wet oxidation reaction temperature is 255°C, the reaction pressure is 5.5MPa, and the waste water space velocity is 2h -1 , the gas flow rate is 80mL / min. The effluent is cooled to 60°C in the heat exchanger. The reaction results are shown in Table 1.

Embodiment 2

[0037] Take 1L of glycerol method epichlorohydrin high-salt wastewater, add 48g of 38wt% concentrated hydrochloric acid to the adjustment tank to adjust to pH=2, dilute the wastewater by 4 times with deionized water, add NiCl 2 and ZnCl 2 (Molar ratio 1:1) as a catalyst, its dosage is 0.4wt.% of high-salt wastewater. Then it is mixed with air through the pipeline and then enters the heat exchanger to be heated to 240°C, and finally enters the catalytic wet oxidation reaction tower for reaction. The catalytic wet oxidation reaction temperature is 265°C, the reaction pressure is 6.0MPa, and the waste water space velocity is 2h -1 , the gas flow rate is 80mL / min. The effluent is cooled to 50°C in a heat exchanger. The reaction results are shown in Table 1.

Embodiment 3

[0039] Take 1L of glycerol method epichlorohydrin high-salt wastewater, add 48g of 37wt% concentrated hydrochloric acid to the adjustment tank to adjust to pH=3, dilute the wastewater by 3 times with deionized water, add FeCl 3 As a catalyst, its dosage is 0.3wt.% of the high-salt wastewater. Then it is mixed with air through the pipeline and then enters the heat exchanger to be heated to 240°C, and finally enters the catalytic wet oxidation reaction tower for reaction. The catalytic wet oxidation reaction temperature is 270°C, the reaction pressure is 6.5MPa, and the waste water space velocity is 1~2h -1 , The gas flow rate is 40-80mL / min. The effluent is cooled to 40°C in a heat exchanger. The reaction results are shown in Table 1.

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Abstract

The present invention relates to a resource utilization technology for high-salt wastewater from epichlorohydrin preparation through a glycerol method, and belongs to the high-salt difficultly-degraded organic wastewater treatment. The technology comprises three operation units such as catalytic wet oxidation, acetic acid recovery and catalyst recovery. According to the present invention, the high-salt wastewater resource utilization technology has advantages of simple process, high treatment efficiency, small occupation area, resource recycling, low secondary pollution and the like; the sodium acetate recovered through the technology can be adopted as the raw material of the environmentally friendly snow melting agent, the TOC of the generated purified NaCl solution is less than 10 mg / L, and the generated purified NaCl solution can be adopted as the ion membrane caustic soda production raw material; and with the use of the technology, the economical and cyclically-developable green epichlorohydrin production process can be formed for enterprises.

Description

technical field [0001] The invention relates to a resource utilization method for preparing epichlorohydrin high-salt wastewater by glycerin method. The method can recover sodium acetate and high-purity NaCl from the glycerin method epichlorohydrin production wastewater, and realize resource utilization of pollutants. High-salt refractory organic wastewater treatment field. Background technique [0002] Since the 1980s, human demand for epoxy resin has grown rapidly, which has promoted the rapid development of epichlorohydrin production. Epichlorohydrin (Epichlorohydrin, ECH) is an important organic chemical raw material, which is widely used in chemical industry, light industry, medicine, electronic appliances and other industries. 85% of epichlorohydrin in my country is used to produce epoxy resin. Epichlorohydrin is mostly produced by propylene high-temperature chlorination method and propylene acetate method. The main raw materials of these two methods all depend on the...

Claims

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Application Information

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IPC IPC(8): C02F9/04C07C51/42C07C53/10C01D3/06C02F103/36
Inventor 卫皇曌孙承林王森于杨荣欣李敬美
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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