Novel solid-liquid reaction kettle sampling device

Abstract

The utility model relates to a novel solid-liquid reaction kettle sampling device which comprises a sampling unit and a balance unit, the sampling unit is connected with a reaction kettle, the balance unit is connected with the reaction kettle and the sampling unit, a centrifugal separation unit is arranged on one side of the sampling unit, a receiving groove is formed in the lower side of the centrifugal separation unit, and a temperature control mechanism is arranged on the sampling unit; during sampling, the balance unit is opened, reactants in the reaction kettle fall to the sampling unit through the sampling opening, the balance unit is closed at the moment, the temperature control mechanism cools the reactants at the sampling unit, the reactants in the sampling unit fall to the centrifugal separation mechanism at the moment to be subjected to centrifugal separation, and separated solids are left in the centrifugal separation mechanism; the liquid is to be sampled and analyzed after being sent out through the receiving tank, the influence on the reaction conditions in the reaction kettle during sampling is small, and the device has the effect of convenient sampling operation.

Description

TECHNICAL FIELD

[0001] The present application relates to the field of chemical reaction kettles, in particular to a novel solid-liquid reaction kettle sampling device. BACKGROUND

[0002] In chemical reactions, a reaction kettle is one of the indispensable equipment. When the reaction is carried out, it is usually necessary to sample and detect the reactants in the reaction kettle.

[0003] In the related art, reference can be made to the invention patent with the publication number CN104368296A, which discloses a high-efficiency reaction kettle, comprising a shell, a feeding port is arranged on the upper end of the shell, a material taking port is arranged on the side wall of the lower end of the shell, the pipe opening of the material taking port is arranged obliquely upward, a plurality of convex flow baffles are arranged on the inner wall of the shell, the flow baffles are arranged along the axial direction of the shell, a rotating rod is arranged on the upper end of the inner wall of the shell, the rotating rod is connected with an external driving mechanism of the shell, a plurality of stirring rods are arranged on the lower end of the rotating rod, the stirring rods are composed of long and short rods and are arranged alternately, when sampling is needed, sampling and detection can be carried out from the pipe opening of the material taking port of the side wall of the shell.

[0004] When the reactants are high-temperature reactions and the intermediates are solid with good liquid absorption capacity, the sampling operation of the reactants is inconvenient, at the same time, opening the material taking port to take materials will also destroy the reaction conditions in the reaction kettle (such as the volatility of the product and the inability to contact water or air, etc.), which will cause some unnecessary side reactions. CONTENT OF THE UTILITY MODEL

[0005] In order to solve the problem that the conventional sampling operation is inconvenient and is easy to cause the increase of reaction influencing factors, the present application provides a novel solid-liquid reaction kettle sampling device.

[0006] The novel solid-liquid reaction kettle sampling device provided by the present application adopts the following technical scheme:

[0007] A novel solid-liquid reaction kettle sampling device, comprising a sampling unit for sampling from a reaction kettle and a balancing unit, the sampling unit is connected with the reaction kettle at a sampling port, the balancing unit is arranged on the reaction kettle and communicates with the inside of the reaction kettle, the balancing unit is connected with the sampling unit, the side of the sampling unit away from the reaction kettle is provided with a centrifugal separation unit for centrifugal separation of reactants, the lower side of the centrifugal separation unit is provided with a receiving groove, and a temperature control mechanism for temperature control is arranged on the sampling unit.

[0008] By adopting the technical scheme, when sampling, the balancing unit is opened, the reactant in the reaction kettle falls to the sampling unit through the sampling port, at this time the balancing unit is closed, the temperature control mechanism cools the reactant at the sampling unit, at this time the reactant at the sampling unit falls to the centrifugal separation mechanism for centrifugal separation, the separated solid remains in the centrifugal separation mechanism, and the liquid is sent out through the receiving groove and then is sampled and analyzed.

[0009] Optionally, the sampling unit comprises a sampling pipe connected with a sampling valve of the sampling port of the reaction kettle, and the temperature control mechanism comprises a heating sandwich layer arranged on the outer wall of the sampling pipe, wherein the heating sandwich layer is hollow, and a cooling water inlet and a cooling water outlet are arranged on the heating sandwich layer.

[0010] By adopting the technical scheme, the cooling water enters the heating sandwich layer through the cooling water inlet on the heating sandwich layer and is discharged through the cooling water outlet, so that the reactant in the sampling pipe is cooled, and the cooled reactant is centrifugally separated, thereby facilitating the sampling operation of the reactant.

[0011] Optionally, the centrifugal separation unit comprises a centrifuge and a centrifugal cylinder, the centrifuge is connected with the sampling pipe through a sampling pipe discharge valve, the centrifugal cylinder is rotatably arranged in the centrifuge, a filter cloth is arranged on the centrifugal cylinder, and the centrifuge is connected with the receiving groove through a discharge pipe.

[0012] By adopting the technical scheme, when the cooling is completed, the sampling pipe discharge valve is opened, the reactant is transported into the centrifugal cylinder of the centrifuge, centrifugal operation is performed, the liquid after centrifugal operation is entered into the receiving groove, and the liquid is sampled and analyzed, thereby facilitating the sampling analysis of the sample by solid-liquid separation.

[0013] Optionally, the balancing unit comprises a balancing pipe, one end of the balancing pipe is connected with the reaction kettle through a balancing pipe valve, a balancing pipe external valve is arranged on one side of the balancing pipe, one side of the balancing pipe external valve is connected with an external vacuum pump, and one end of the balancing pipe away from the reaction kettle is connected with the sampling pipe.

[0014] By adopting the technical scheme, before discharging into the sampling pipe, the vacuum pump first draws negative pressure into the balancing pipe, then the balancing pipe external valve is closed, the influence of residual gas in the pipe on sampling is reduced, then the balancing pipe valve is opened until the pressure is constant, the sampling valve of the sampling port of the reaction kettle is opened, a large amount of solid-liquid reactant is retained in the sampling pipe for sampling and cooling, the balancing pipe valve and the sampling valve are closed after sampling is completed, and the influence on the reaction condition in the reaction kettle is reduced during sampling.

[0015] Optionally, a pressure gauge is arranged on the balancing pipe.

[0016] By adopting the technical scheme, the pressure of the balance pipe and the system is monitored at any time through the pressure gauge, so as to be processed in time.

[0017] Optionally, one side of the valve connected with the balance pipe is provided with a quick connector, and the balance pipe is connected with an external gas source through the quick connector.

[0018] By adopting the technical scheme, when the cooled material in the sampling pipe falls into the centrifuge, the valve connected with the balance pipe is opened, nitrogen is introduced into the balance pipe, the sampling pipe is pressurized, and the residual reactants in the sampling pipe are all pressed into the centrifuge, so that the probability of residual reactants in the sampling pipe is reduced.

[0019] Optionally, the balance pipe is connected with an external solvent storage device through the quick connector.

[0020] By adopting the technical scheme, when the sampling is completed, the valve connected with the balance pipe is opened, solvent is introduced into the balance pipe to flush each pipeline, and the residual material in the pipeline is reduced.

[0021] Optionally, the steam drainage inlet and the steam drainage outlet are respectively arranged on opposite sides of the heating interlayer.

[0022] By adopting the technical scheme, when the sampling is completed, hot steam is introduced into the heating interlayer through the steam drainage inlet to heat the sampling pipe, nitrogen is introduced into the balance pipe at this time, the residual liquid in the sampling pipe is dried, and the residual liquid in the pipeline is reduced.

[0023] In summary, the present application has at least one of the following beneficial technical effects:

[0024] 1. When sampling, the balance unit is opened, the reactants in the reaction kettle fall into the sampling unit through the sampling port, the balance unit is closed at this time, the temperature control mechanism cools the reactants in the sampling unit, and the reactants in the sampling unit fall into the centrifugal separation mechanism for centrifugal separation, the separated solid remains in the centrifugal separation mechanism, and the liquid is sent out through the receiving groove and then sampled and analyzed. The sampling operation is convenient and has little effect on the reaction conditions in the reaction kettle.

[0025] 2. The pressure of the balance pipe and the system is monitored at any time through the pressure gauge, so as to be processed in time.

[0026] 3. When the sampling is completed, the valve connected with the balance pipe is opened, solvent is introduced into the balance pipe to flush each pipeline, and the residual material in the pipeline is reduced. Hot steam is introduced into the heating interlayer through the steam drainage inlet to heat the sampling pipe, nitrogen is introduced into the balance pipe at this time, the residual liquid in the sampling pipe is dried, and the residual liquid in the pipeline is reduced. BRIEF DESCRIPTION OF DRAWINGS

[0027] Figure 1 is a schematic diagram of the stereoscopic structure of the present application.

[0028] Figure 2 is a schematic diagram of the structure of the sampling unit of the present application.

[0029] Figure 3 is a schematic diagram of the structure of the centrifugal unit of the present application.

[0030] Those skilled in the art will understand that the elements in the drawings are shown for simplicity and clarity and are not necessarily drawn to scale. For example, the dimensions and positions of some of the elements in the drawings can be exaggerated relative to other elements to help improve the understanding of the present embodiments.

[0031] Reference signs: 1, reaction kettle; 2, reaction kettle discharge port; 3, balance pipe valve; 4, balance pipe; 5, balance pipe external valve; 6, pressure gauge; 7, sampling valve; 8, sampling pipe; 801, cooling water inlet; 802, cooling water outlet; 803, heating sandwich; 804, steam drainage air inlet; 805, steam drainage air outlet; 9, sampling pipe discharge valve; 10, centrifugal unit; 1001, connecting pipe; 1002, centrifugal cylinder; 1003, centrifugal machine; 1004, discharge pipe; 11, receiving groove; 12, quick connector. DETAILED DESCRIPTION

[0032] The present application is further described in detail below with reference to the accompanying drawings.

[0033] The present embodiments disclose a novel solid-liquid reaction reaction kettle sampling device, referring to Figure 1 , comprising a sampling unit and a balance unit, the reaction kettle 1 is provided with a reaction kettle discharge port 2 and a reaction kettle 1 sampling valve 7 at the bottom, the sampling unit is connected with the reaction kettle 1 sampling valve 7 at the sampling port of the reaction kettle 1, the balance unit is arranged on the reaction kettle 1 and communicates with the inside of the reaction kettle 1, the balance unit is connected with the sampling unit, the side away from the reaction kettle 1 of the sampling unit is provided with a centrifugal separation unit for centrifugal separation of the reactants, the lower side of the centrifugal separation unit is provided with a receiving groove 11, and the sampling unit is provided with a temperature control mechanism for temperature control. When sampling, the balance unit is opened, and then the reaction kettle 1 sampling valve 7 at the bottom of the reaction kettle 1 is opened, the reactants in the reaction kettle 1 fall to the sampling unit through the sampling port, at this time the balance unit is closed, and the temperature control mechanism cools the reactants in the sampling unit, at this time the reactants in the sampling unit fall to the centrifugal separation mechanism for centrifugal separation, the separated solids remain in the centrifugal separation mechanism, and the liquid is sent out through the receiving groove 11 and then is sampled and analyzed. The present application has little effect on the reaction conditions in the reaction kettle 1 during sampling, the sampling operation is convenient, and the present application can achieve the effect of reducing material loss during sampling without opening the kettle.

[0034] With reference to Figure 2 , the sampling unit comprises a sampling pipe 8, the upper end of which is connected with the sampling valve 7 of the sampling port of the reaction kettle 1, and the temperature control mechanism comprises a heating jacket 803 sleeved on the outer sidewall of the sampling pipe 8, the heating jacket 803 is hollow, and the heating jacket 803 is provided with a cooling water inlet 801 and a cooling water outlet 802 which are in communication with the hollow part inside the heating jacket 803. The cooling water enters the heating jacket 803 through the cooling water inlet 801 on the heating jacket 803 and is discharged through the cooling water outlet 802, so as to cool the reactants in the sampling pipe 8.

[0035] With reference to Figure 3 , the centrifugal separation unit comprises a centrifugal machine 1003 and a centrifugal cylinder 1002, the lower end of the sampling pipe 8 is connected with the centrifugal machine 1003 through a connecting pipe 1001, the connecting pipe 1001 is provided with a sampling pipe discharge valve 9, the centrifugal cylinder 1002 is rotatably installed in the centrifugal machine 1003, the centrifugal cylinder 1002 is sleeved with filter cloth, and the centrifugal machine 1003 is connected with a receiving groove 11 through a discharge pipe 1004. After cooling, the sampling pipe discharge valve 9 is opened, the reactants are transported into the centrifugal cylinder 1002 of the centrifugal machine 1003, centrifugal operation is performed, and the liquid after centrifugation enters the receiving groove 11, so that the liquid is sampled and analyzed.

[0036] With reference to Figure 1 , the balancing unit comprises a balancing pipe 4, one end of the balancing pipe 4 is connected with the reaction kettle 1 through a balancing pipe valve 3, the balancing pipe 4 is provided with a pressure gauge 6, one side of the balancing pipe 4 is provided with a balancing pipe external valve 5, one side of the balancing pipe external valve 5 is connected with an external vacuum pump, and the end of the balancing pipe 4 away from the reaction kettle 1 is connected with the sampling pipe 8. Before discharging the material into the sampling pipe 8, the vacuum pump first draws negative pressure into the balancing pipe 4 and then closes the balancing pipe external valve 5, so as to reduce the influence of residual gas in the pipe on sampling, then the balancing pipe valve 3 is opened until the pressure is constant, the sampling valve 7 of the sampling port of the reaction kettle 1 is opened, a large amount of solid-liquid reactants is retained in the sampling pipe 8 for sampling and cooling treatment, and after sampling is completed, the balancing pipe valve 3 and the sampling valve 7 are closed, so as to reduce the influence on the reaction conditions in the reaction kettle 1 during sampling.

[0037] With reference to Figure 1 , one side of the balancing pipe external valve 5 is provided with a quick connector 12, the balancing pipe 4 is connected with an external gas source through the quick connector 12, when the cooled material in the sampling pipe 8 falls into the centrifugal machine 1003, the balancing pipe external valve 5 is opened, nitrogen is introduced into the balancing pipe 4, the sampling pipe 8 is pressurized, and all the residual reactants in the sampling pipe 8 are pressed into the centrifugal machine 1003, so as to reduce the probability of residual reactants in the sampling pipe 8.

[0038] With reference to Figure 1When the sampling is completed, the balance pipe external valve 5 is opened, and solvent is introduced into the balance pipe 4 to flush the pipes, thereby reducing the residue in the pipes.

[0039] With reference to Figure 1 The steam drainage inlet 804 is used to introduce hot steam into the heating interlayer 803 to heat the sampling pipe 8, and nitrogen is introduced into the balance pipe 4 to dry the residue in the sampling pipe 8, thereby reducing the residue in the pipes.

[0040] The implementation principle of the novel solid-liquid reaction sampling device is as follows: when sampling is needed during the reaction, the balance pipe external valve 5 is opened, the vacuum pump is connected through the quick connector 12, the balance pipe 4 is pumped to vacuum, the vacuum pumping condition is observed through the pressure gauge 6, the balance pipe external valve 5 is closed, the balance pipe valve 3 is opened, when the number of the pressure gauge 6 is constant, the sampling valve 7 is opened, the solid-liquid to be sampled is filled into the sampling pipe 8, and then the sampling valve 7 and the balance pipe valve 3 are closed.

[0041] The cooling water inlet 801 and the cooling water outlet 802 are opened to cool the reactants in the sampling pipe 8, the centrifuge 1003 is started until the rotation speed is stable, the sampling pipe discharge valve 9 is opened to discharge the reactants into the centrifuge 1003, nitrogen is introduced into the balance pipe 4 external valve to press the residue in the sampling pipe 8 into the centrifuge 1003, and then the residue is centrifuged, and the sampling liquid falls into the receiving groove 11 through the discharge pipe 1004 to sample and analyze the liquid in the receiving groove 11.

[0042] When the sampling is completed, the quick connector 12 is connected to the external solvent storage device, the pipes are flushed with ethanol, water and the reaction container in sequence, when all the liquid is discharged, the quick connector 12 is connected to nitrogen, the steam drainage inlet 804 is used to heat the sampling pipe 8 to dry the residue in the sampling pipe 8, and then the nitrogen is removed and the balance pipe 4 external valve is closed, and the above sampling process can be repeated.

[0043] The above are the preferred embodiments of the present application, and are not intended to limit the protection scope of the present application, so that: any equivalent changes made according to the structure, shape, principle of the present application should be covered within the protection scope of the present application.

Claims

1. A novel sampling device for a solid-liquid reaction vessel, comprising a sampling unit for sampling from the reaction vessel (1) and a balancing unit, wherein the sampling unit is connected to the reaction vessel (1) at the sampling port, characterized in that: The balancing unit is located on the reactor (1) and communicates with the interior of the reactor (1). The balancing unit is connected to the sampling unit. The sampling unit is provided with a centrifugal separation unit for centrifugating the reactants on the side away from the reactor (1). A receiving tank (11) is provided on the lower side of the centrifugal separation unit. A temperature control mechanism for temperature control is provided on the sampling unit.

2. The novel solid-liquid reaction vessel sampling device according to claim 1, characterized in that: The sampling unit includes a sampling tube (8), which is connected to the sampling valve (7) at the sampling port of the reactor (1). The temperature control mechanism includes a heating jacket (803) sleeved on the outer circumferential wall of the sampling tube (8). The heating jacket (803) is hollow and has a cooling water inlet (801) and a cooling water outlet (802).

3. The novel solid-liquid reaction vessel sampling device according to claim 2, characterized in that: The centrifugal separation unit includes a centrifuge (1003) and a centrifuge cylinder (1002). The centrifuge (1003) is connected to the sampling tube (8) through a sampling tube discharge valve (9). The centrifuge cylinder (1002) is rotatably installed inside the centrifuge (1003). A filter cloth is sleeved on the centrifuge cylinder (1002). The centrifuge (1003) is connected to the receiving tank (11) through a discharge pipe (1004).

4. A novel solid-liquid reaction vessel sampling device according to claim 2, characterized in that: The balancing unit includes a balancing pipe (4), one end of which is connected to the reactor (1) via a balancing pipe valve (3). An external balancing pipe valve (5) is provided on one side of the balancing pipe (4), and one side of the external balancing pipe valve (5) is connected to an external vacuum pump. The end of the balancing pipe (4) away from the reactor (1) is connected to the sampling pipe (8).

5. A novel solid-liquid reaction vessel sampling device according to claim 4, characterized in that: A pressure gauge (6) is installed on the balance tube (4).

6. A novel solid-liquid reaction vessel sampling device according to claim 4, characterized in that: A quick connector (12) is provided on one side of the external valve (5) of the balance pipe, and the balance pipe (4) is connected to an external air source through the quick connector (12).

7. A novel solid-liquid reaction vessel sampling device according to claim 6, characterized in that: The balance tube (4) is connected to an external solvent storage device via the quick connector (12).

8. A novel sampling device for a solid-liquid reaction vessel according to claim 2, characterized in that: The heating interlayer (803) is provided with a steam drain inlet (804) and a steam drain outlet (805) on opposite sides.

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