CN112093884A - Catalytic oxidation purification method of alcohol-containing wastewater - Google Patents

Catalytic oxidation purification method of alcohol-containing wastewater Download PDF

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Publication number
CN112093884A
CN112093884A CN202010992448.1A CN202010992448A CN112093884A CN 112093884 A CN112093884 A CN 112093884A CN 202010992448 A CN202010992448 A CN 202010992448A CN 112093884 A CN112093884 A CN 112093884A
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valve
oxygen
pressure
kettle
type reactor
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陈慧
张璐
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Tianjin University of Technology
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Tianjin University of Technology
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    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/72Treatment of water, waste water, or sewage by oxidation
    • C02F1/725Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/02Treatment of water, waste water, or sewage by heating
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/72Treatment of water, waste water, or sewage by oxidation
    • C02F1/727Treatment of water, waste water, or sewage by oxidation using pure oxygen or oxygen rich gas
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C45/00Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
    • C07C45/27Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by oxidation
    • C07C45/32Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by oxidation with molecular oxygen
    • C07C45/37Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by oxidation with molecular oxygen of >C—O—functional groups to >C=O groups
    • C07C45/38Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by oxidation with molecular oxygen of >C—O—functional groups to >C=O groups being a primary hydroxyl group
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/30Organic compounds
    • C02F2101/34Organic compounds containing oxygen

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Treatment Of Water By Oxidation Or Reduction (AREA)

Abstract

The invention discloses a catalytic oxidation purification method of alcohol-containing wastewater, belonging to the technical field of chemical equipment. The catalytic oxidation purification device for the wastewater mainly containing n-hexanol comprises an oxygen inlet valve (1), an oxygen pressure stabilizing valve (2), an oxygen flow meter (3), an oxygen inlet electromagnetic valve (4), a nitrogen inlet valve (5), a nitrogen pressure stabilizing valve (6), a kettle type reactor (7), a heating layer (8), a gas distributor (9), a motor (10), a stirring paddle (11), a pressure control system (12), a pressure regulating valve (13) and a tail gas flow meter (14), and the using method based on the device comprises six steps. The invention has the advantages of simple structure, convenient operation and high automation degree, and realizes the dynamic regulation of the pressure in the whole process through the synergistic action of the pressure regulating valve (13), the pressure control system (12) and the oxygen inlet electromagnetic valve (4), thereby ensuring the pressure stability of the kettle reactor (7), and the like.

Description

Catalytic oxidation purification method of alcohol-containing wastewater
The technical field is as follows:
the invention discloses a use method of a catalytic oxidation purification device based on n-hexanol wastewater, belongs to the technical field of chemical equipment, and is applied to research on the dynamics of liquid-phase catalytic oxidation of an n-hexanol aqueous solution.
Background art:
at present, water resource pollution is one of the problems to be solved urgently in all countries in the world, pollutants in water, especially high-concentration organic pollutants and toxic harmful pollutants discharged in industrial production, are various and large in harm, some pollutants are difficult to biodegrade and have toxicity and three-cause harm, the treatment of the difficult-to-degrade organic pollutants is always a difficult problem in the field of environmental protection, the existing physicochemical treatment technology mainly has the advantages of filtration, air flotation, coagulation, adsorption and the like, although the equipment is simple, the operation is simple and convenient, the process is mature and the like, the organic pollutants are only transferred from a liquid phase to a solid phase or a gas phase, and are not completely degraded. The liquid phase oxidation purification method of waste water utilizes the air oxygen dissolved in water to oxidize organic substances, and the method has higher degradation rate than the prior physicochemical treatment technology. The hexanol is an organic solvent commonly used in industry, is widely applied to the production of fine chemicals, pharmacy and organic synthetic materials, causes environmental pollution due to small leakage and volatilization, and has stimulation on human skin and mucous membranes, so that the oxidative degradation of the hexanol in the wastewater is a very promising research direction at present.
The hexanal is an important raw material for food processing, medicine manufacturing, essence and flavor production and pesticide production, and has higher added economic value. In industrial production, n-hexanol in organic wastewater is oxidized into n-hexanal, the n-hexanal is obtained through a series of treatments such as high-temperature oxidation and extraction, and the wastewater is purified and recycled. The dynamic research plays an important role in correctly playing the potential of the catalyst and enhancing the production.
The invention content is as follows:
the invention aims to provide a hexanol wastewater catalytic oxidation purification device with simple structure, convenient use and high automation degree and a use method thereof.
The invention relates to a n-hexanol wastewater catalytic oxidation purification device, which comprises an oxygen inlet valve (1), an oxygen pressure stabilizing valve (2), an oxygen flow meter (3), an oxygen inlet electromagnetic valve (4), a nitrogen inlet valve (5), a nitrogen pressure stabilizing valve (6), a tank reactor (7), a heating layer (8), a gas distributor (9), a motor (10), a stirring paddle (11), a pressure control system (12), a pressure regulating valve (13) and a tail gas flow meter (14), and is characterized in that: the oxygen intake valve (1), the oxygen pressure stabilizing valve (2), the oxygen flow meter (3) and the oxygen intake solenoid valve (4) are sequentially connected through pipelines, the nitrogen intake valve (5) and the nitrogen pressure stabilizing valve (6) are sequentially connected through pipelines, the outlet of the oxygen intake solenoid valve (4) and the outlet of the nitrogen pressure stabilizing valve (6) are connected together through pipelines, the upper end of the kettle-type reactor (7) enters the kettle-type reactor (7) and is connected with a gas distributor (9) at the bottom of the pipeline, a heating layer (8) is attached to the outside of the kettle-type reactor (7), stirring paddles (11) are distributed at the center of the kettle-type reactor (7), the upper end of each stirring paddle (11) is connected with a motor (10), the upper end of the kettle-type reactor (7) is simultaneously connected with inlets of a pressure control system (12) and a pressure regulating valve (13) through pipelines, the outlet of the pressure regulating valve (13) is connected with the inlet of a tail gas flowmeter (14) through a pipeline, and the outlet of the tail gas flowmeter (14) is directly emptied.
The pressure control system (12) is associated with the oxygen inlet electromagnetic valve (4), the switch of the oxygen inlet electromagnetic valve (4) is controlled by the pressure control system (12), when the pressure control system (12) monitors that the actual pressure of the kettle type reactor (7) is lower than a set value, the oxygen inlet electromagnetic valve (4) is opened, and when the pressure control system (12) monitors that the actual pressure of the kettle type reactor (7) is higher than the set value, the oxygen inlet electromagnetic valve (4) is closed.
The use method of the catalytic oxidation purification device based on the n-hexanol wastewater uses the catalytic oxidation purification device based on the n-hexanol wastewater, and comprises the following steps:
(1) adding n-hexanol with the mass of m1, a catalyst with the mass of m2 and a solvent with the volume of V into a kettle-type reactor (7), wherein m 1: m2 is 1: 4-4: 1;
(2) opening a nitrogen gas inlet valve (5) and a nitrogen pressure stabilizing valve (6), ensuring the micro-positive pressure of the kettle type reactor (7), and purging the system for 5-20 minutes;
(3) adjusting the rotating speed of the motor (10) to be 100-1000 rpm, the temperature of the heating layer (8) to be 60-200 ℃, opening the oxygen inlet valve (1) and the oxygen pressure stabilizing valve (2), and controlling the flow of the oxygen flowmeter (3) to be 10-100 mL/min;
(4) the pressure of the kettle type reactor (7) is controlled to be 0.2-2 MPa through a pressure regulating valve (13), and the on-off of an oxygen inlet electromagnetic valve (4) is controlled through the feedback of a pressure controller (12);
(5) when the heating layer (8) reaches the reaction temperature and the pressure of the kettle-type reactor (7) reaches the reaction pressure, timing is started, the reaction is stopped after t time, the consumption Q1 of oxygen can be obtained according to the flow curve of the oxygen flowmeter (3), and the amount Q2 of tail gas can be obtained according to the flow curve of the tail gas flowmeter (14);
(6) and respectively carrying out gas phase analysis on the liquid phase product and the tail gas, and carrying out material balance according to the analysis result.
The use method of the device for purifying wastewater based on n-hexanol by catalytic oxidation has the following advantages:
1. the structure is simple, the layout is compact, and the operation is convenient;
2. the process of automatic overpressure pressure relief and automatic underpressure pressure supplement of the system is realized through the synergistic effect of the pressure regulating valve (13), the pressure control system (12) and the oxygen inlet electromagnetic valve (4), the whole process is dynamically regulated, when the pressure of the kettle type reactor (7) is lower than the reaction pressure, the oxygen inlet electromagnetic valve (4) is opened, oxygen is filled into the kettle type reactor (7), when the pressure of the kettle type reactor (7) is higher than the reaction pressure, the oxygen inlet electromagnetic valve (4) is closed, the pressure regulating valve (13) is opened, the amount of gas flowing out is measured through the tail gas flowmeter (14), and the pressure stability of the kettle type reactor (7) is ensured;
3. the tail gas passing through the pressure regulating valve (13) is measured by a tail gas flowmeter (14) and then is exhausted, so that the tail gas measurement is realized, and the material balance in the whole process is facilitated.
Description of the drawings:
FIG. 1 is a schematic diagram of a catalytic oxidation purification device for n-hexanol wastewater.
The specific implementation mode is as follows:
in order to make the present invention more comprehensible, preferred embodiments are described in detail below with reference to the accompanying drawings, but the present invention is not limited thereto.
As shown in figure 1, the n-hexanol wastewater catalytic oxidation purification device comprises an oxygen inlet valve (1), an oxygen pressure stabilizing valve (2), an oxygen flow meter (3), an oxygen inlet electromagnetic valve (4), a nitrogen inlet valve (5), a nitrogen pressure stabilizing valve (6), a kettle type reactor (7), a heating layer (8), a gas distributor (9), a motor (10), a stirring paddle (11), a pressure control system (12), a pressure regulating valve (13) and a tail gas flow meter (14), wherein the oxygen inlet valve (1), the oxygen pressure stabilizing valve (2), the oxygen flow meter (3) and the oxygen inlet electromagnetic valve (4) are sequentially connected through pipelines, the nitrogen inlet valve (5) and the nitrogen pressure stabilizing valve (6) are sequentially connected through pipelines, an outlet of the oxygen inlet electromagnetic valve (4) and an outlet of the nitrogen pressure stabilizing valve (6) are connected together through pipelines, and enter the kettle type reactor (7) through the upper end of the kettle type reactor (7), a gas distributor (9) is connected at the bottom of the pipeline, a heating layer (8) is attached to the outside of the kettle reactor (7), a stirring paddle (11) is distributed at the center of the kettle reactor (7), a motor (10) is connected at the upper end of the stirring paddle (11), the upper end of the kettle reactor (7) is simultaneously connected with a pressure control system (12) and an inlet of a pressure regulating valve (13) through the pipeline, an outlet of the pressure regulating valve (13) is connected with an inlet of a tail gas flowmeter (14) through the pipeline, an outlet of the tail gas flowmeter (14) is directly emptied, the pressure control system (12) is associated with an oxygen inlet electromagnetic valve (4), the on-off of the oxygen inlet electromagnetic valve (4) is controlled by the pressure control system (12), when the pressure control system (12) monitors that the actual pressure of the kettle reactor (7) is lower than a set value, the oxygen inlet electromagnetic valve (4) is opened, when the pressure control system (12) monitors that the actual pressure of the kettle type reactor (7) is higher than a set value, the oxygen gas inlet electromagnetic valve (4) is closed.
According to the structure of the n-hexanol wastewater catalytic oxidation purification device, the adopted using method of the n-hexanol wastewater catalytic oxidation purification device is as follows:
(1) adding n-hexanol with the mass of m1, a catalyst with the mass of m2 and a solvent with the volume of V into a kettle-type reactor (7), wherein m 1: m2 is 1: 4-4: 1;
(2) opening a nitrogen gas inlet valve (5) and a nitrogen pressure stabilizing valve (6), ensuring the micro-positive pressure of the kettle type reactor (7), and purging the system for 5-20 minutes;
(3) adjusting the rotating speed of the motor (10) to be 100-1000 rpm, the temperature of the heating layer (8) to be 60-200 ℃, opening the oxygen inlet valve (1) and the oxygen pressure stabilizing valve (2), and controlling the flow of the oxygen flowmeter (3) to be 10-100 mL/min;
(4) the pressure of the kettle type reactor (7) is controlled to be 0.2-2 MPa through a pressure regulating valve (13), and the on-off of an oxygen inlet electromagnetic valve (4) is controlled through the feedback of a pressure controller (12);
(5) when the heating layer (8) reaches the reaction temperature and the pressure of the kettle-type reactor (7) reaches the reaction pressure, timing is started, the reaction is stopped after t time, the consumption Q1 of oxygen can be obtained according to the flow curve of the oxygen flowmeter (3), and the amount Q2 of tail gas can be obtained according to the flow curve of the tail gas flowmeter (14);
(6) and respectively carrying out gas phase analysis on the liquid phase product and the tail gas, and carrying out material balance according to the analysis result.
Example 1
Adding 0.1g of n-hexanol, 0.2g of catalyst and 20mL of water into a kettle-type reactor (7), opening a nitrogen gas inlet valve (5) and a nitrogen pressure stabilizing valve (6), ensuring the pressure of the kettle-type reactor (7) to be 0.1MPa, purging the system for 10 minutes, adjusting the rotating speed of a motor (10) to be 300 r/min, the temperature of a heating layer (8) to be 100 ℃, opening the oxygen gas inlet valve (1) and the oxygen pressure stabilizing valve (2), controlling the flow of an oxygen flow meter (3) to be 10mL/min, controlling the pressure of the kettle-type reactor (7) to be 0.8MPa through a pressure regulating valve (13), controlling the opening and closing of an oxygen gas inlet electromagnetic valve (4) through feedback of a pressure controller (12), stopping the reaction after the heating layer (8) reaches the reaction temperature and the pressure of the kettle-type reactor (7) reaches the reaction pressure, starting timing, stopping the reaction after 6 hours, obtaining 1.52L of the oxygen according to the flow curve of the oxygen flow meter, the tail gas amount can be 0.93L according to the flow curve of the tail gas flowmeter (14), the liquid phase product is subjected to gas phase analysis, and the content of n-hexanol in the liquid phase is quantitatively calculated to be 0.02108g according to the peak area in a chromatogram, so that the catalytic conversion rate is 78.92%.

Claims (3)

1. Contain n hexyl alcohol waste water catalytic oxidation purifier, including oxygen admission valve (1), oxygen surge damping valve (2), oxygen flowmeter (3), oxygen solenoid valve (4) of admitting air, nitrogen admission valve (5), nitrogen surge damping valve (6), kettle-type reactor (7), zone of heating (8), gas distributor (9), motor (10), stirring rake (11), pressure control system (12), air-vent valve (13) and tail gas flowmeter (14), its characterized in that: the oxygen intake valve (1), the oxygen pressure stabilizing valve (2), the oxygen flow meter (3) and the oxygen intake solenoid valve (4) are sequentially connected through pipelines, the nitrogen intake valve (5) and the nitrogen pressure stabilizing valve (6) are sequentially connected through pipelines, the outlet of the oxygen intake solenoid valve (4) and the outlet of the nitrogen pressure stabilizing valve (6) are connected together through pipelines, the upper end of the kettle-type reactor (7) enters the kettle-type reactor (7) and is connected with a gas distributor (9) at the bottom of the pipeline, a heating layer (8) is attached to the outside of the kettle-type reactor (7), stirring paddles (11) are distributed at the center of the kettle-type reactor (7), the upper end of each stirring paddle (11) is connected with a motor (10), the upper end of the kettle-type reactor (7) is simultaneously connected with inlets of a pressure control system (12) and a pressure regulating valve (13) through pipelines, the outlet of the pressure regulating valve (13) is connected with the inlet of a tail gas flowmeter (14) through a pipeline, and the outlet of the tail gas flowmeter (14) is directly emptied.
2. The n-hexanol wastewater catalytic oxidation purification device of claim 1, wherein: the pressure control system (12) is associated with the oxygen inlet electromagnetic valve (4), the switch of the oxygen inlet electromagnetic valve (4) is controlled by the pressure control system (12), when the pressure control system (12) monitors that the actual pressure of the kettle type reactor (7) is lower than a set value, the oxygen inlet electromagnetic valve (4) is opened, and when the pressure control system (12) monitors that the actual pressure of the kettle type reactor (7) is higher than the set value, the oxygen inlet electromagnetic valve (4) is closed.
3. Based on the using method of the n-hexanol wastewater catalytic oxidation purification device, the n-hexanol wastewater catalytic oxidation purification device is used, and the steps are as follows:
(1) adding n-hexanol with the mass of m1, a catalyst with the mass of m2 and a solvent with the volume of V into a kettle-type reactor (7), wherein m 1: m2 is 1: 4-4: 1;
(2) opening a nitrogen gas inlet valve (5) and a nitrogen pressure stabilizing valve (6), ensuring the micro-positive pressure of the kettle type reactor (7), and purging the system for 5-20 minutes;
(3) adjusting the rotating speed of the motor (10) to be 100-1000 rpm, the temperature of the heating layer (8) to be 60-200 ℃, opening the oxygen inlet valve (1) and the oxygen pressure stabilizing valve (2), and controlling the flow of the oxygen flowmeter (3) to be 10-100 mL/min;
(4) the pressure of the kettle type reactor (7) is controlled to be 0.2-2 MPa through a pressure regulating valve (13), and the on-off of an oxygen inlet electromagnetic valve (4) is controlled through the feedback of a pressure controller (12);
(5) when the heating layer (8) reaches the reaction temperature and the pressure of the kettle-type reactor (7) reaches the reaction pressure, timing is started, the reaction is stopped after t time, the consumption Q1 of oxygen can be obtained according to the flow curve of the oxygen flowmeter (3), and the amount Q2 of tail gas can be obtained according to the flow curve of the tail gas flowmeter (14);
(6) and respectively carrying out gas phase analysis on the liquid phase product and the tail gas, and carrying out material balance according to the analysis result.
CN202010992448.1A 2020-09-21 2020-09-21 Catalytic oxidation purification method of alcohol-containing wastewater Pending CN112093884A (en)

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Application Number Priority Date Filing Date Title
CN202010992448.1A CN112093884A (en) 2020-09-21 2020-09-21 Catalytic oxidation purification method of alcohol-containing wastewater

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Application Number Priority Date Filing Date Title
CN202010992448.1A CN112093884A (en) 2020-09-21 2020-09-21 Catalytic oxidation purification method of alcohol-containing wastewater

Publications (1)

Publication Number Publication Date
CN112093884A true CN112093884A (en) 2020-12-18

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Application publication date: 20201218