CN112093884A - Catalytic oxidation purification method of alcohol-containing wastewater - Google Patents
Catalytic oxidation purification method of alcohol-containing wastewater Download PDFInfo
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- 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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- 239000002351 wastewater Substances 0.000 title claims abstract description 22
- 230000003647 oxidation Effects 0.000 title claims abstract description 21
- 238000007254 oxidation reaction Methods 0.000 title claims abstract description 21
- 230000003197 catalytic effect Effects 0.000 title claims abstract description 20
- 238000000034 method Methods 0.000 title claims abstract description 17
- 238000000746 purification Methods 0.000 title claims abstract description 17
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 title abstract description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 70
- 239000001301 oxygen Substances 0.000 claims abstract description 70
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 70
- ZSIAUFGUXNUGDI-UHFFFAOYSA-N hexan-1-ol Chemical compound CCCCCCO ZSIAUFGUXNUGDI-UHFFFAOYSA-N 0.000 claims abstract description 48
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 46
- 239000007789 gas Substances 0.000 claims abstract description 38
- 230000000087 stabilizing effect Effects 0.000 claims abstract description 23
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 21
- 230000001105 regulatory effect Effects 0.000 claims abstract description 18
- 238000010438 heat treatment Methods 0.000 claims abstract description 15
- 238000003756 stirring Methods 0.000 claims abstract description 10
- 238000006243 chemical reaction Methods 0.000 claims description 16
- 238000001595 flow curve Methods 0.000 claims description 8
- 239000007791 liquid phase Substances 0.000 claims description 8
- 238000004458 analytical method Methods 0.000 claims description 7
- 230000001276 controlling effect Effects 0.000 claims description 6
- 239000003054 catalyst Substances 0.000 claims description 5
- 239000012071 phase Substances 0.000 claims description 5
- 229910001873 dinitrogen Inorganic materials 0.000 claims description 4
- 239000000463 material Substances 0.000 claims description 4
- 238000010926 purge Methods 0.000 claims description 4
- 239000002904 solvent Substances 0.000 claims description 3
- 238000013016 damping Methods 0.000 claims 2
- 239000000126 substance Substances 0.000 abstract description 3
- 230000002195 synergetic effect Effects 0.000 abstract description 2
- JARKCYVAAOWBJS-UHFFFAOYSA-N hexanal Chemical compound CCCCCC=O JARKCYVAAOWBJS-UHFFFAOYSA-N 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 5
- 238000011282 treatment Methods 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 3
- 229910001882 dioxygen Inorganic materials 0.000 description 3
- 239000003344 environmental pollutant Substances 0.000 description 3
- 239000002957 persistent organic pollutant Substances 0.000 description 3
- 231100000719 pollutant Toxicity 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000015271 coagulation Effects 0.000 description 1
- 238000005345 coagulation Methods 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 239000000796 flavoring agent Substances 0.000 description 1
- 235000019634 flavors Nutrition 0.000 description 1
- 238000005188 flotation Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 210000004400 mucous membrane Anatomy 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 238000010525 oxidative degradation reaction Methods 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 230000000638 stimulation Effects 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/02—Treatment of water, waste water, or sewage by heating
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/727—Treatment of water, waste water, or sewage by oxidation using pure oxygen or oxygen rich gas
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
- C07C45/27—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by oxidation
- C07C45/32—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by oxidation with molecular oxygen
- C07C45/37—Preparation 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
- C07C45/38—Preparation 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
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/34—Organic 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
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.
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Application publication date: 20201218 |