Experimental reaction system for nitrogen protection sampling

Abstract

The utility model provides an experimental reaction system for nitrogen protection sampling, which is characterized in that a three-way valve is opened to be communicated with the outside, nitrogen is introduced into the system through a gas inlet needle tube to replace air, then the three-way valve is disconnected from the outside, and the three-way valve is opened to enable a first connecting pipe to be communicated with a nitrogen balloon; the sampling needle tube extends to the position below the liquid level in the sample bottle, nitrogen continues to be introduced, the pressure of the nitrogen above the liquid level in the sample bottle is increased so that a sample can be pressed into the sampling needle tube, then the sample is guided into the constant-pressure dropping funnel through the first hose, sampling is achieved, and the sample can be added into a reaction container through the constant-pressure dropping funnel when needing to be added into the reaction container. Oxygen and moisture are isolated in the process, normal sampling is ensured, the capacity can be determined by the sampling time length, convenience and rapidness are achieved, and the problem that large-capacity sampling is inconvenient to carry out in the prior art is solved.

Description

Technical Field

[0001] The utility model relates to the technical field of chemical experimental equipment, in particular to an experimental reaction system for nitrogen protection sampling. Background Art

[0002] Some highly active chemical reagents (such as boron tribromide solution, Grignard reagent, butyl lithium, etc., or anhydrous and oxygen-free solvents) generally need to be sampled under the protection of inert gas (such as nitrogen) to avoid mixing oxygen and water during the sampling process, otherwise it may cause unnecessary oxygen and water to participate in the subsequent chemical reaction process, resulting in chemical reaction failure. In the range of 10μl to 10ml, laboratories often use syringes to absorb and drip under nitrogen protection to achieve the requirements of anhydrous and oxygen-free. However, 10ml to 100ml cannot be absorbed at one time using a syringe because of the large quantity. In the case of repeated absorption and dripping, trace amounts of oxygen and water may enter the reaction system, resulting in reaction failure, and repeated operations bring inconvenience to the experimental process, reduce experimental efficiency, and reduce the success rate of the experiment. In addition, a glove box will also be used. First, the chemical reagents with sampling are placed in the glove box, and then the air is replaced by nitrogen or other inert gases to fill the glove box with inert gas. Finally, the sampling operation is performed, and the next step is performed after nitrogen protection. However, the device is large in size, inconvenient to operate, inefficient, and easily causes the remaining sample to become inactivated after the sample bottle is opened. Utility Model Content

[0003] In view of the deficiencies in the prior art, the utility model provides an experimental reaction system for nitrogen protection sampling, which solves the problem in the prior art that it is inconvenient to perform sampling of a larger volume.

[0004] According to an embodiment of the utility model, an experimental reaction system for nitrogen protection sampling includes a reaction container, a constant pressure dropping funnel and a sample bottle, the constant pressure dropping funnel is vertically arranged, the reaction container includes a first connecting pipe and a second connecting pipe, the first connecting pipe is connected to a nitrogen balloon, a three-way valve is arranged on the first connecting pipe, the three-way valve has three interfaces and two of them are respectively connected to the first connecting pipe and the nitrogen balloon, and the other is connected to the outside; the second connecting pipe is connected to the lower end of the constant pressure dropping funnel, a first hose is connected between the upper end of the constant pressure dropping funnel and the sample bottle, the first hose is connected to a sampling needle tube that is telescopically extended into the sample bottle, and the sample bottle is also provided with an air inlet needle tube connected thereto, and the air inlet needle tube is connected to a nitrogen source to supply nitrogen.

[0005] In the above embodiment, before sampling, the three-way valve is opened to connect with the outside world, nitrogen is introduced into the system through the air inlet needle tube to replace the air, and then the three-way valve is disconnected from the outside world, and the three-way valve is opened to connect the first connecting pipe and the nitrogen balloon, and the sampling needle tube is extended below the liquid surface in the sample bottle, and nitrogen is continued to be introduced. The nitrogen pressure above the liquid surface in the sample bottle increases, and the sample can be pressed into the sampling needle tube, and then introduced into the constant pressure dropping funnel through the first hose to achieve sampling. When the sample needs to be added to the reaction container, it can be added through the constant pressure dropping funnel. Oxygen and moisture are isolated during the process to ensure that the sampling is carried out normally, and the capacity can be determined by the length of the sampling time, which is convenient and quick, and solves the problem of inconvenience in sampling larger volumes in the prior art.

[0006] Furthermore, a third connecting pipe is provided on the reaction container, a thermometer is installed on the third connecting pipe, and a temperature sensing end of the thermometer is located in the reaction container.

[0007] Furthermore, the sample bottle is also provided with a first rubber stopper, and both the air inlet needle tube and the sampling needle tube extend into the sample bottle through the first rubber stopper.

[0008] Furthermore, the sampling needle tube includes a straight tube section and a needle connected to one end of the straight tube section, and the other end of the straight tube section is connected to the first hose.

[0009] Furthermore, a second rubber stopper is provided at the upper end of the constant pressure dropping funnel, a guide needle tube is penetrated through the second rubber stopper, and an end of the first hose away from the sampling needle tube is also connected to the guide needle tube.

[0010] Furthermore, the lower end of the constant pressure dropping funnel is connected to a guide tube connected thereto, a sleeve is also provided outside the guide tube, the upper end of the sleeve is fixedly connected to the guide tube, the lower end of the guide tube is located inside the sleeve, the lower end of the sleeve is connected to the ground joint of the second connecting pipe, a balance tube is also connected between the upper end of the constant pressure dropping funnel and the sleeve, and a valve is also installed on the guide tube.

[0011] Furthermore, the air inlet needle tube is connected to the nitrogen source via a second hose.

[0012] Furthermore, a flow valve is also arranged on the second hose.

[0013] Compared with the prior art, the utility model has the following beneficial effects:

[0014] During the sampling process, the sample reagent does not come into contact with the outside world, and is isolated from oxygen and moisture. The capacity can be determined by the length of the sampling time, and is suitable for sampling in the range of 10-100ml. It is convenient and fast, and solves the problem in the prior art that it is inconvenient to sample larger volumes. BRIEF DESCRIPTION OF THE DRAWINGS

[0015] Figure 1The overall structure of the embodiment of the utility model is shown in FIG. Figure 1 ;

[0016] Figure 2 The overall structure of the embodiment of the utility model is shown in FIG. Figure 2 ;

[0017] Figure 3 for Figure 2 A schematic diagram of the enlarged local structure at center A;

[0018] Figure 4 A schematic diagram of the sampling needle structure of an embodiment of the utility model;

[0019] In the above drawings:

[0020] Reaction container 1, constant pressure dropping funnel 2, sample bottle 3, first connecting pipe 4, second connecting pipe 5, nitrogen balloon 6, three-way valve 7, first hose 8, sampling needle tube 9, air inlet needle tube 10, third connecting pipe 11, thermometer 12, first rubber stopper 13, second rubber stopper 14, guide needle tube 15, second hose 16, flow valve 17, straight pipe section 18, needle 19, guide tube 20, sleeve 21, balance tube 22, valve 23. DETAILED DESCRIPTION

[0021] The technical solution of the present utility model is further described below in conjunction with the accompanying drawings and embodiments.

[0022] In the description of the present invention, it should be understood that the terms "center", "longitudinal", "lateral", "length", "width", "thickness", "up", "down", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inside", "outside", "clockwise", "counterclockwise", "axial", "radial", "circumferential" and the like indicate orientations or positional relationships based on the orientations or positional relationships shown in the accompanying drawings, and are only for the convenience of describing the present invention and simplifying the description, and do not indicate or imply that the referred device or element must have a specific orientation, be constructed and operated in a specific orientation, and therefore should not be understood as a limitation on the present invention.

[0023] In an exemplary embodiment, Figure 1 , 2As shown, this embodiment provides an experimental reaction system for nitrogen protection sampling, which includes a reaction container 1, a constant pressure dropping funnel 2 and a sample bottle 3. The constant pressure dropping funnel 2 is a vertically arranged straight tube structure. The reaction container 1 includes a first connecting pipe 4 and a second connecting pipe 5. The first connecting pipe 4 is connected to a nitrogen balloon 6. A three-way valve 7 is arranged on the first connecting pipe 4. The three-way valve 7 has three interfaces, two of which are respectively connected to the first connecting pipe 4 and the nitrogen balloon 6, and the other is connected to the outside world; the second connecting pipe 5 is connected to the constant pressure dropping funnel 2 The lower end of the constant pressure dropping funnel 2 is connected, a first hose 8 is connected between the upper end of the constant pressure dropping funnel 2 and the sample bottle 3, the first hose 8 is connected to a sampling needle tube 9 that is telescopically extended into the sample bottle 3, the sample bottle 3 is also provided with an air inlet needle tube 10 that is connected thereto, the air inlet needle tube 10 is connected to a nitrogen source for supplying nitrogen, and a third connecting pipe 11 can also be connected to the reaction container 1, a thermometer 12 is installed on the third connecting pipe 11, and the temperature sensing end of the thermometer 12 is located in the reaction container 1, which can display the temperature of the reactants in the reaction container 1.

[0024] In the above embodiment, before sampling, the three-way valve 7 is opened to communicate with the outside world, and nitrogen is introduced into the system through the air inlet needle tube 10 to replace the air, and then the three-way valve 7 is disconnected from the outside world, and the three-way valve 7 is opened to connect the first connecting pipe 4 and the nitrogen balloon 6, and the sampling needle tube 9 is extended below the liquid level in the sample bottle 3, and nitrogen is continuously introduced. The nitrogen pressure above the liquid level in the sample bottle 3 increases, and the sample can be pressed into the sampling needle tube 9, and then introduced into the constant pressure dropping funnel 2 through the first hose 8 to achieve sampling. When it is necessary to add a sample to the reaction container 1, the addition can be achieved through the constant pressure dropping funnel 2. In the process, oxygen and moisture are isolated to ensure that the sampling is carried out normally, and the capacity can be determined by the length of the sampling time, which is convenient and fast, and solves the problem of inconvenience in sampling a larger capacity in the prior art;

[0025] Specifically, when replacing the air, the sampling needle tube 9 is located above the liquid level in the sample bottle 3. At this time, the nitrogen introduced will enter the sampling needle tube 9 through the first hose 8 and enter the constant pressure dropping funnel 2. The constant pressure dropping funnel 2 is connected to the reaction container 1 below, so that the nitrogen can also enter the reaction container 1, and then be discharged outward through the three-way valve 7. In this way, the air can be replaced. Generally, the replacement can be carried out for 10-30 seconds, and then the sampling operation can be started. Specifically, before sampling, other reactants can be added to the reaction container 1, and then nitrogen replacement can be carried out. This also ensures that the reaction system is also carried out under nitrogen protection.

[0026] In a further exemplary embodiment, Figure 1-4As shown, the sample bottle 3 is also plugged with a first rubber stopper 13, and the air inlet needle tube 10 and the sampling needle tube 9 both pass through the first rubber stopper 13 and extend into the sample bottle 3. The sampling needle tube 9 and the air inlet needle tube 10 can be removed from the first rubber stopper 13. After removal, the hole on the first rubber stopper 13 can be restored to deform and close, thereby isolating the inside and the outside. A new first rubber stopper 13 can be replaced after multiple uses. Similarly, the upper end of the constant pressure dropping funnel 2 can also be plugged with a similar second rubber stopper 14, and a guide needle tube 15 is penetrated by the second rubber stopper 14. The end of the first hose 8 facing away from the sampling needle tube 9 is also connected to the guide needle tube 15, and the guide needle tube 15 can also It can be taken and put in the same way as the sampling needle tube 9 and the air intake needle tube 10; further, the air intake needle tube 10 is connected to the nitrogen source through a second hose 16, and a flow valve 17 is also provided on the second hose 16, so that the flow rate of nitrogen can be conveniently adjusted (the nitrogen flow rate can generally be adjusted to 200ml / min). In more detail, the specific structures of the air intake needle tube 10, the sampling needle tube 9 and the guide needle tube 15 can be similar, and generally corrosion-resistant metal materials can be used. The first hose 8 and the second hose 16 can also be corrosion-resistant rubber tubes, which can be deformed and smoothly elastically sleeved with the sampling needle tube 9, the guide needle tube 15 and the air intake needle tube 10;

[0027] More specifically, the sampling needle tube 9 includes a straight tube section 18 and a needle 19 connected to one end of the straight tube section 18, and the other end of the straight tube section 18 is connected to the first hose 8. The straight tube section 18 has a certain length to accommodate the needle 19 to smoothly extend below the liquid surface and to be lifted above the liquid surface, and the two can also be disassembled, such as by a threaded connection.

[0028] In a further exemplary embodiment, Figure 1-3As shown, the lower end of the constant pressure dropping funnel 2 is connected with a guide tube 20 in communication therewith, and a sleeve 21 is also sleeved outside the guide tube 20, the upper end of the sleeve 21 is fixedly connected to the guide tube 20, the lower end of the guide tube 20 is located in the sleeve 21, and the lower end of the sleeve 21 is ground-connected to the second connecting pipe 5, a balance pipe 22 is also connected between the upper end of the constant pressure dropping funnel 2 and the sleeve 21, and a valve 23 is also installed on the guide tube 20, the outer wall of the sleeve 21 and the inner wall of the second connecting pipe 5 are respectively ground-connected structures, and the two can have the required sealing after being connected (in the actual operation process, vaseline can also be applied between the two to ensure the sealed connection), and at the same time, it can also be smoothly Disassembly; the guide tube 20 and the valve 23 thereon can smoothly allow the sample sampled into the constant pressure dropping funnel 2 to flow into the reaction vessel 1 below. Specifically, when nitrogen replacement is performed, the valve 23 can be opened or closed. When closed, the nitrogen entering can enter the sleeve 21 through the set balance pipe 22, and then enter the reaction vessel 1 below; during the sampling process, the valve 23 is closed. At this time, the sample is temporarily stored in the constant pressure dropping funnel 2. When it needs to be added to the reaction vessel 1, the valve 23 can be opened again. At this time, the balance pipe 22 makes the constant pressure dropping funnel 2 and the reaction vessel 1 in an isobaric state to ensure smooth dripping of the sample.

[0029] Finally, it should be noted that the above embodiments are only used to illustrate the technical solution of the utility model rather than to limit it. Although the utility model has been described in detail with reference to the preferred embodiments, ordinary technicians in the field should understand that the technical solution of the utility model can be modified or replaced by equivalents without departing from the purpose and scope of the technical solution of the utility model, which should be included in the scope of the claims of the utility model.

Claims

1. An experimental reaction system for nitrogen protection sampling, characterized in that: It includes a reaction container, a constant pressure dropping funnel and a sample bottle, the constant pressure dropping funnel is vertically arranged, the reaction container includes a first connecting pipe and a second connecting pipe, the first connecting pipe is connected to a nitrogen balloon, a three-way valve is arranged on the first connecting pipe, the three-way valve has three interfaces, two of which are respectively connected to the first connecting pipe and the nitrogen balloon, and the other is connected to the outside; the second connecting pipe is connected to the lower end of the constant pressure dropping funnel, a first hose is connected between the upper end of the constant pressure dropping funnel and the sample bottle, the first hose is connected to a sampling needle tube that telescopically extends into the sample bottle, the sample bottle is also provided with an air inlet needle tube connected thereto, and the air inlet needle tube is connected to a nitrogen source to supply nitrogen.

2. The nitrogen protection sampling experimental reaction system according to claim 1, characterized in that: The reaction container is also provided with a third connecting pipe, on which a thermometer is installed, and a temperature sensing end of the thermometer is located in the reaction container.

3. The nitrogen protection sampling experimental reaction system according to claim 1, characterized in that: The sample bottle is also provided with a first rubber stopper, and the air inlet needle tube and the sampling needle tube both pass through the first rubber stopper and extend into the sample bottle.

4. The nitrogen protection sampling experimental reaction system according to claim 3, characterized in that: The sampling needle tube comprises a straight tube section and a needle connected to one end of the straight tube section, and the other end of the straight tube section is connected to the first hose.

5. The nitrogen protection sampling experimental reaction system according to claim 1, characterized in that: The upper end of the constant pressure dropping funnel is also plugged with a second rubber stopper, a guide needle tube is penetrated through the second rubber stopper, and the end of the first hose away from the sampling needle tube is also connected to the guide needle tube.

6. The nitrogen protection sampling experimental reaction system according to claim 1, characterized in that: The lower end of the constant pressure dropping funnel is connected to a guide tube connected thereto, a sleeve is also sleeved on the outside of the guide tube, the upper end of the sleeve is fixedly connected to the guide tube, the lower end of the guide tube is located in the sleeve, the lower end of the sleeve is connected to the ground joint of the second connecting pipe, a balance pipe is also connected between the upper end of the constant pressure dropping funnel and the sleeve, and a valve is also installed on the guide tube.

7. The nitrogen protection sampling experimental reaction system according to any one of claims 1 to 6, characterized in that: The air inlet needle tube is connected to the nitrogen source via a second hose.

8. The nitrogen protection sampling experimental reaction system according to claim 7, characterized in that: The second hose is also provided with a flow valve.

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