Digestion reflux absorption device

Abstract

The present invention relates to a digestion reflux absorption apparatus, which comprises: a gas supply module for outputting nitrogen; the reaction module comprises a first test tube, a chlorine-containing solution and a first quartz sieve plate, the chlorine-containing solution and the first quartz sieve plate are arranged in the first test tube, the first test tube is connected with the gas supply module to receive nitrogen, the chlorine-containing solution reacts to generate chlorine, and the chlorine is mixed with the nitrogen to form chlorine-containing mixed gas; the absorption module comprises a second test tube, an absorption solution and a second quartz sieve plate, the absorption solution and the second quartz sieve plate are arranged in the second test tube, the second test tube is connected with the first test tube, and the absorption solution absorbs chlorine in the chlorine-containing mixed gas. Through the first quartz sieve plate and the second quartz sieve plate in the first test tube and the second test tube, bubbling is uniform, the chlorine gas absorption rate is improved, through the first anti-suck-back module and the second anti-suck-back module, the solution suck-back condition is prevented, the experiment safety is guaranteed, and the data accuracy is improved.

Description

Technical Field

[0001] The invention relates to the technical field of environmental monitoring, in particular to a digestion reflux absorption device. Background Art

[0002] Chemical Oxygen Demand (COD) is a method of measuring the content of reducing substances in water by oxidation-reduction. It is an important indicator for characterizing the degree of organic pollution and purification in water.

[0003] Chloride ions are commonly found in water bodies, especially in seawater and high-salt wastewater such as wastewater discharged from chlor-alkali plants, oil fields and other industrial enterprises. As an important indicator of water quality discharge standards, the limit of chemical oxygen demand is constantly decreasing. The presence of chloride ions in water will seriously affect the accuracy of COD determination results in water quality. At present, the chemical oxygen demand digestion reflux absorption device for high-salt water has problems such as insufficient chlorine absorption and the inability of chlorine in the reaction container to be completely absorbed by the absorption liquid. Summary of the invention

[0004] The purpose of the present invention is to overcome the defects of the prior art and provide a digestion reflux absorption device to solve the problem that the existing digestion reflux absorption device has insufficient chlorine absorption and the chlorine in the reaction container cannot be completely absorbed by the absorption liquid.

[0005] The technical solution for achieving the above-mentioned purpose is: a digestion reflux absorption device, comprising: a gas supply module, the gas supply module outputs nitrogen; a reaction module, the reaction module comprises a first test tube, and a chlorine-containing solution and a first quartz sieve plate placed in the first test tube, the first test tube is connected to the gas supply module by a conduit for receiving the nitrogen, the chlorine-containing solution reacts to produce chlorine, the nitrogen and the chlorine are mixed to form a mixed gas containing chlorine, and the mixed gas containing chlorine is output from the upper port of the first test tube; an absorption module, the absorption module comprises a second test tube, and an absorption solution and a second quartz sieve plate placed in the second test tube, the second test tube is connected to the first test tube by the conduit, and the second test tube receives the chlorine-containing mixed gas output by the first test tube, and the absorption solution in the second test tube absorbs the chlorine in the chlorine-containing mixed gas.

[0006] A further improvement of the digestion reflux absorption device of the present invention is that the gas supply module is provided with a pressure reducing valve and / or a flow regulating valve to control the output of nitrogen.

[0007] A further improvement of the digestion reflux absorption device of the present invention is that the reaction module also includes a heating base arranged at the bottom of the first test tube.

[0008] A further improvement of the digestion reflux absorption device of the present invention is that it also includes: a first anti-backflow module, which is arranged between the gas supply module and the reaction module, and the first anti-backflow module includes a first conical flask, a first input conduit and a first output conduit, and the first input conduit is connected to the gas supply module for introducing the nitrogen in the gas supply module into the first conical flask, and the first output conduit is connected to the reaction module for introducing the nitrogen in the first conical flask into the first test tube of the reaction module.

[0009] A further improvement of the digestion reflux absorption device of the present invention is that it also includes: a cooling module, which is arranged between the reaction module and the absorption module. The cooling module includes a water tank and a condenser. The lower end of the condenser is connected to the upper end of the first test tube for receiving the chlorine-containing mixed gas produced by the reaction in the first test tube, and the upper end of the condenser is connected to the second test tube for cooling the chlorine-containing mixed gas produced by the reaction in the first test tube and introducing it into the second test tube.

[0010] A further improvement of the digestion reflux absorption device of the present invention is that it also includes: a second anti-backflow module, which is arranged between the cooling module and the absorption module, and the second anti-backflow module includes a second conical flask, a second input conduit and a second output conduit, and the second input conduit is connected to the cooling module, and is used to introduce the chlorine-containing mixed gas discharged from the cooling module after cooling into the second conical flask, and the second output conduit is connected to the second test tube of the absorption module, and is used to introduce the chlorine-containing mixed gas in the second conical flask into the second test tube.

[0011] A further improvement of the digestion reflux absorption device of the present invention is that the lower opening of the outer tube of the condenser is provided as a water inlet, and the upper opening is provided as a water outlet.

[0012] A further improvement of the digestion reflux absorption device of the present invention is that the first quartz sieve plate is arranged at 1 / 10 to 3 / 10 of the distance from the bottom of the first test tube, and the first quartz sieve plate controls the uniform bubbling of the chlorine-containing solution.

[0013] A further improvement of the digestion reflux absorption device of the present invention is that the second quartz sieve plate is arranged at 1 / 10 to 3 / 10 of the distance from the bottom of the second test tube, and the second quartz sieve plate controls the uniform bubbling of the absorption solution.

[0014] A further improvement of the digestion reflux absorption device of the present invention is that the first test tube of the reaction module also includes a silver sulfate-sulfuric acid solution.

[0015] In a digestion reflux absorption device of the present invention, the first quartz sieve plate and the second quartz sieve plate in the first test tube and the second test tube can make bubbling uniform and improve the absorption rate of chlorine gas. The first anti-backflow module and the second anti-backflow module are provided to prevent the occurrence of solution backflow, thereby ensuring the safety of the experiment and improving the accuracy of data. BRIEF DESCRIPTION OF THE DRAWINGS

[0016] Figure 1 It is a structural schematic diagram of a digestion reflux absorption device of the present invention.

[0017] Figure 2 The present invention is a flow chart of a method for measuring the chemical oxygen demand in high-salt water quality using a digestion reflux absorption device.

[0018] In the figure: 10, gas supply module; 20, reaction module; 21, first test tube; 22, chlorine-containing solution; 23, first sieve plate; 24, heating base; 30, absorption module; 31, second test tube; 32, absorption solution; 33, second sieve plate; 40, first anti-backflow module; 41, first input conduit; 42, first output conduit; 43, first conical flask; 50, second anti-backflow module; 51, second input conduit; 52, second output conduit; 53, second conical flask; 60, cooling module; 61, condenser. DETAILED DESCRIPTION

[0019] The present invention will be further described below in conjunction with the accompanying drawings and specific embodiments.

[0020] See also Figure 1 , showing a schematic diagram of the structure of a digestion reflux absorption device of the present invention. The present invention provides a digestion reflux absorption device, comprising: a gas supply module 10, the gas supply module 10 outputs nitrogen.

[0021] The gas supply module 10 includes a nitrogen bottle or a nitrogen generator, which can provide a stable nitrogen output.

[0022] The reaction module 20 includes a first test tube 21, a chlorine-containing solution 22 and a first quartz sieve plate 23 placed in the first test tube 21. The first test tube 21 is connected to the gas supply module 10 through a conduit for receiving nitrogen. The chlorine-containing solution 22 reacts to produce chlorine. The nitrogen and chlorine are mixed to form a mixed gas containing chlorine. The mixed gas containing chlorine is output from the upper port of the first test tube 21.

[0023] Among them, the first test tube 21 is connected to the gas supply module 10 through a conduit. The side bottom opening of the first test tube 21 is used to input nitrogen. Nitrogen is an inert gas and does not affect or participate in the reaction process of the chlorine-containing solution 22. The chlorine-containing mixed gas includes nitrogen, chlorine, and water vapor evaporated by the solution when heated.

[0024] The absorption module 30 includes a second test tube 31, an absorption solution 32 placed in the second test tube 31, and a second quartz sieve plate 33. The second test tube 31 is connected to the first test tube 21 through a conduit, and the second test tube 31 receives the chlorine-containing mixed gas generated by the first test tube 21. The absorption solution 32 in the second test tube 31 absorbs the chlorine-containing mixed gas.

[0025] The absorption solution 32 is an alkaline solution, and the concentration of the alkaline solution can be set to adjust the chlorine absorption rate and enhance the absorption capacity.

[0026] The present invention provides a digestion reflux absorption device, in which a gas supply module 10 is provided with a pressure reducing valve and / or a flow regulating valve to control the output of nitrogen.

[0027] The flow rate of nitrogen is adjusted by a pressure reducing valve and is controlled between 1 ml / min and 10 ml / min to ensure uniformity of bubbling.

[0028] The present invention provides a digestion reflux absorption device, wherein the reaction module 20 further comprises a heating base 24 disposed at the bottom of the first test tube 21 .

[0029] The heating base 24 can use a heating furnace to heat the first test tube 21. The heating base 24 is in direct contact with the first test tube 21, and temperature control needs to be done well to ensure uniform heating and safety of the experiment.

[0030] See also Figure 1 , showing a schematic diagram of the structure of a digestion reflux absorption device of the present invention. The present invention provides a digestion reflux absorption device, further comprising: a first anti-backflow module 40, the first anti-backflow module 40 is arranged between the gas supply module and the reaction module, the first anti-backflow module 40 comprises a first conical flask, a first input conduit and a first output conduit, and the first input conduit is connected to the gas supply module for introducing the nitrogen in the gas supply module into the first conical flask, and the first output conduit is connected to the reaction module for introducing the nitrogen in the first conical flask into the first test tube of the reaction module.

[0031] Among them, the first anti-backflow module 40 is used to prevent the solution from being backflowed when nitrogen is input. The first input conduit 41 is directly connected to the nitrogen bottle or the nitrogen generator, and the first output conduit 42 needs to be arranged in a "J" shape, which can effectively prevent the chlorine-containing solution 22 in the first test tube 21 from being backflowed into the gas supply module 10.

[0032] In this embodiment, the first input conduit extends into the first conical flask for a length shorter than the first output conduit extends into the first conical flask. In other embodiments, the lengths of the input conduit and the output conduit extending into the conical flask can be adjusted according to the gas density, which is not limited here.

[0033] See also Figure 1 , showing a schematic diagram of the structure of a digestion reflux absorption device of the present invention. The present invention provides a digestion reflux absorption device, further comprising: a cooling module 60, the cooling module 60 is arranged between the reaction module 20 and the absorption module 30, the cooling module 60 comprises a water tank, a condenser 61, the lower end of the condenser 61 is connected to the upper end of the first test tube 21, for receiving the chlorine-containing mixed gas discharged from the first test tube 21, the upper end of the condenser 61 is connected to the second test tube 31, for cooling the chlorine-containing mixed gas discharged from the first test tube 21 and introducing it into the second test tube 31.

[0034] The cooling module 60 condenses the water vapor evaporated from the first test tube 21 , and it is necessary to ensure that the input water temperature is within a suitable range (generally 15-25° C.).

[0035] In this embodiment, the condenser 61 is arranged vertically, and the condenser 61 enters from the bottom and exits from the top. The condenser 61 is a spherical condenser 61. The cooling area of ​​the spherical condenser 61 is large. With the same cooling area, the length of the condenser 61 can be shortened, thereby improving the distillation effect. Since the inner core tube is spherical, it is easy for distillate to accumulate in the spherical part, so it is not suitable for an inclined distillation device, and is mostly used in a vertical distillation device.

[0036] See also Figure 1 , showing a schematic diagram of the structure of a digestion reflux absorption device of the present invention. The present invention provides a digestion reflux absorption device, further comprising: a second anti-backflow module 50, the second anti-backflow module 50 is arranged between the reaction module and the absorption module, the second anti-backflow module 50 comprises a second conical flask 51, a second input conduit 52 and a second output conduit 53, and the second input conduit 52 is connected to the cooling module, and is used to introduce the chlorine-containing mixed gas discharged after cooling by the cooling module into the second conical flask, and the second output conduit is connected to the second test tube of the absorption module, and is used to introduce the chlorine-containing mixed gas in the second conical flask into the second test tube.

[0037] In this embodiment, the upper port of the cooling module 60 is the output port of the cooled chlorine-containing mixed gas, the second input conduit 51 is directly connected to the output port to receive the chlorine-containing mixed gas, and the second output conduit 52 also needs to be arranged in a "J" shape, which can effectively prevent the absorption solution 32 in the second test tube 31 from flowing out.

[0038] In this embodiment, the spherical condenser 61 needs to be cleaned before use, and the expanded part of the upper end of the spherical condenser 61 is connected to the second input conduit 51 of the second anti-backflow module 50 using a rubber plug with a hole punched in it.

[0039] In this embodiment, the extension length of the second input conduit in the second conical flask is less than the extension length of the second output conduit in the second conical flask. In other embodiments, the extension lengths of the second input conduit and the second output conduit in the second conical flask can be adjusted according to the gas density, which is not limited here.

[0040] See also Figure 1 , showing a schematic diagram of the structure of a digestion reflux absorption device of the present invention. The present invention provides a digestion reflux absorption device, wherein the lower opening of the outer tube of the condenser 61 is set as the water inlet, and the upper opening is the water outlet.

[0041] The chlorine-containing mixed gas generated by the reaction of the chlorine-containing solution 22 in the first test tube 21 is transmitted from bottom to top along the inner core tube. The high-temperature chlorine-containing mixed gas encounters the cooling effect of the external cooling water in the inner core tube. The water vapor contained in the chlorine-containing mixed gas directly condenses into water droplets on the tube wall of the inner core tube and flows back to the first test tube 21.

[0042] See also Figure 1 , showing a schematic diagram of the structure of a digestion reflux absorption device of the present invention. The present invention provides a digestion reflux absorption device, wherein a first quartz sieve plate 23 is disposed at 1 / 10 to 3 / 10 of the distance from the bottom of a first test tube 21, and the first quartz sieve plate 23 controls the bubbling of a chlorine-containing solution 22 to be uniform.

[0043] The first sieve plate 23 is horizontally arranged in the first test tube 21 , the liquid level of the chlorine-containing solution 22 is higher than the first quartz sieve plate 23 , and the uniformity of nitrogen bubbling is adjusted by the first quartz sieve plate 23 .

[0044] The present invention provides a digestion reflux absorption device, wherein the second quartz sieve plate 33 is arranged at 1 / 10 to 3 / 10 of the distance from the bottom of the second test tube 31 , and the second quartz sieve plate 33 controls the bubbling of the absorption solution 32 to be uniform.

[0045] Among them, the second quartz sieve plate 33 is horizontally arranged in the second test tube 31, and the second quartz sieve plate 33 is located at 1 / 10 to 3 / 10 of the bottom of the second test tube. The liquid level of the absorption solution 32 is higher than the second quartz sieve plate 33. The second quartz sieve plate 33 is used to adjust the uniformity of bubbling when the mixed gas containing chlorine is input into the absorption solution 32, so that the chlorine is fully in contact with the absorption solution 32, thereby improving the absorption rate of chlorine.

[0046] See also Figure 1 , showing a schematic diagram of the structure of a digestion reflux absorption device of the present invention. The present invention provides a digestion reflux absorption device, wherein the first test tube 21 of the reaction module 20 also includes a silver sulfate-sulfuric acid solution.

[0047] Among them, silver sulfate-sulfuric acid solution is used as the reactant of the experiment, and the silver sulfate-sulfuric acid solution needs to be injected from the upper port of the condenser 61 of the cooling module 60 to prevent direct injection from causing local boiling and splashing, and also avoid affecting the experimental data, thereby ensuring the safety of the experiment and the validity of the data.

[0048] See also Figure 2 , showing a flow chart of a method for measuring chemical oxygen demand in high-salinity water quality using a digestion reflux absorption device. The present invention provides a method for measuring chemical oxygen demand in high-salinity water quality using a digestion reflux absorption device, characterized in that it comprises the following steps:

[0049] Execute step S210: assemble the digestion reflux absorption device in sequence and check the air tightness of the entire device.

[0050] The airtightness of the inspection device is indispensable in order to ensure the safety of the experiment and the validity of the entire experimental data. Next, step S220 is executed.

[0051] Execute step S220: add the chlorine-containing solution 22 and the absorption solution 32 into the first test tube 21 and the second test tube 31 of the reaction module 20 and the absorption module 30 respectively.

[0052] The liquid levels in the first test tube 21 and the second test tube 31 are higher than the locations where the first quartz sieve plate 23 and the second quartz sieve plate 33 are set. Then, step S230 is performed.

[0053] Execute step S230: add the silver sulfate-sulfuric acid solution into the first test tube 21 .

[0054] The silver sulfate-sulfuric acid solution needs to be slowly injected from the upper port of the condenser 61, and after the silver sulfate-sulfuric acid solution is added, the first test tube 21 needs to be shaken to mix it evenly, and then step S240 is executed.

[0055] Execute step S240: turn on the water tank switch of the cooling module 60 to allow cooling water to flow into the condenser pipe 61, and control the flow rate of the cooling water.

[0056] Here, first turn on the cooling water, let the cooling water enter from the lower port of the outer tube of the condenser 61 and exit from the upper port, check whether the water flow is normal, adjust the water temperature to a suitable range, and then execute step S250.

[0057] Execute step S250: input nitrogen through the gas supply module 10.

[0058] The flow rate of nitrogen is controlled between 1 ml / min and 10 ml / min, so that bubbles generated after nitrogen enters the chlorine-containing solution 22 are evenly dispersed by the first sieve plate 23, and then step S260 is executed.

[0059] Execute step S260: start the heating base 24 under the first test tube 21.

[0060] Among them, the heating base 24 is tightly fitted to the bottom of the first test tube 21, the temperature range of the heating base 24 is adjusted, and the first test tube 21 is heated to allow the chlorine-containing solution 22 to fully react. The generated chlorine is transported along the inner core tube together with the nitrogen and evaporated water vapor. The water vapor is cooled by cooling water, condensed on the inner core tube wall of the condenser 61, and flows back to the first test tube 21. The chlorine-containing mixed gas continues to be transported to the first anti-backflow module 40 and the absorption module 30. Then, step S270 is executed.

[0061] Execute step S270: After refluxing for 2 hours, stop heating, adjust the flow rate of nitrogen to 20-50 mL / min, and continue to introduce nitrogen for 20-30 minutes.

[0062] After the heating stops, nitrogen is continuously introduced to allow the chlorine-containing solution 22 to react fully. For the accuracy of the experimental data, step S280 is then performed.

[0063] Execute step S280: after the solution in the first test tube 21 is cooled, disassemble the digestion reflux absorption device.

[0064] The first test tube 21 and the second test tube 31 are removed respectively, and distilled water is added from the upper end of the disassembled condenser tube 61 to rinse the inner wall of the condenser tube 61. Then, step S290 is performed.

[0065] Execute step S290: measure the chloride ion content of the solution in the second test tube 31.

[0066] The solution in the second test tube 31 can be transferred to a titration bottle, and then an indicator is added to the titration bottle, and the titration device titrates the reactant into the titration bottle, and the titration is stopped when the color change of the solution in the titration bottle is identified. The amount of reactant consumed by chloride ions in the water sample is calculated from the volume of the reactant used, that is, the chloride ion content.

[0067] The present invention is described in detail above in conjunction with the embodiments of the drawings. A person skilled in the art can make various changes to the present invention according to the above description. Therefore, certain details in the embodiments should not be construed as limiting the present invention, and the scope of protection of the present invention shall be the scope defined by the attached claims.

Claims

1. A digestion reflux absorption device, characterized in that: include: A gas supply module, wherein the gas supply module outputs nitrogen; A reaction module, the reaction module comprising a first test tube, and a chlorine-containing solution and a first quartz sieve plate placed in the first test tube, the first test tube is connected to the gas supply module through a conduit, and is used to receive the nitrogen gas, the chlorine-containing solution reacts to produce chlorine gas, the nitrogen gas and the chlorine gas are mixed to form a mixed gas containing chlorine gas, and the mixed gas containing chlorine gas is output from the upper port of the first test tube; The absorption module includes a second test tube, an absorption solution placed in the second test tube, and a second quartz sieve plate. The second test tube is connected to the first test tube through the conduit, and the second test tube receives the chlorine-containing mixed gas output by the first test tube. The absorption solution in the second test tube absorbs chlorine in the chlorine-containing mixed gas.

2. A digestion reflux absorption device according to claim 1, characterized in that: The gas supply module is provided with a pressure reducing valve and / or a flow regulating valve to control the output of nitrogen.

3. A digestion reflux absorption device according to claim 1, characterized in that: The reaction module also includes a heating base arranged at the bottom of the first test tube.

4. A digestion reflux absorption device according to claim 1, characterized in that: Also includes: A first anti-backflow module, wherein the first anti-backflow module is disposed between the gas supply module and the reaction module, and comprises a first conical flask, a first input conduit and a first output conduit, wherein the first input conduit is connected to the gas supply module and is used to introduce the nitrogen in the gas supply module into the first conical flask, and the first output conduit is connected to the reaction module and is used to introduce the nitrogen in the first conical flask into the first test tube of the reaction module.

5. A digestion reflux absorption device according to claim 1, characterized in that: Also includes: A cooling module is arranged between the reaction module and the absorption module, and includes a water tank and a condenser. The lower end of the condenser is connected to the upper end of the first test tube for receiving the chlorine-containing mixed gas produced by the reaction in the first test tube, and the upper end of the condenser is connected to the second test tube for cooling the chlorine-containing mixed gas produced by the reaction in the first test tube and introducing it into the second test tube.

6. A digestion reflux absorption device according to claim 5, characterized in that: Also includes: A second anti-backflow module, the second anti-backflow module is arranged between the cooling module and the absorption module, the second anti-backflow module includes a second conical flask, a second input conduit and a second output conduit, and the second input conduit is connected to the cooling module, and is used to introduce the chlorine-containing mixed gas discharged from the cooling module after cooling into the second conical flask, and the second output conduit is connected to the second test tube of the absorption module, and is used to introduce the chlorine-containing mixed gas in the second conical flask into the second test tube.

7. A digestion reflux absorption device according to claim 5, characterized in that: The lower opening of the outer tube of the condenser is used as a water inlet, and the upper opening is used as a water outlet.

8. A digestion reflux absorption device according to claim 1, characterized in that: The first quartz sieve plate is arranged at 1 / 10 to 3 / 10 of the distance from the bottom of the first test tube, and the first quartz sieve plate controls the uniform bubbling of the chlorine-containing solution.

9. A digestion reflux absorption device according to claim 1, characterized in that: The second quartz sieve plate is arranged at 1 / 10 to 3 / 10 of the distance from the bottom of the second test tube, and the second quartz sieve plate controls the bubbling of the absorption solution to be uniform.

10. A digestion reflux absorption device according to claim 1, characterized in that: The first test tube of the reaction module also includes a silver sulfate-sulfuric acid solution.

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