Sampling device for high-pressure hydrogenation kettle
Technical Field
The utility model relates to a sampling device of reation kettle, in particular to a sampling device for high-pressure hydrogenation cauldron.
Background
Catalytic hydrogenation is a common unit reaction in chemical and pharmaceutical production processes, and how to safely and conveniently take out reaction liquid from a hydrogenation kettle for analysis without influencing the reaction is solved in the field.
At present, the conventional method for sampling a high-pressure hydrogenation kettle is to cool, decompress and replace with nitrogen, then take out reaction liquid from the hydrogenation kettle for analysis, namely, sample after terminating the reaction, if the analysis result is not ideal, raise the temperature again and boost the pressure to continue the reaction, on one hand, the time of a production bench is prolonged, the energy consumption and the material consumption are increased, and on the other hand, the reaction is extremely unfavorable. The second method is to install two bleeder valves at the bottom discharge gate of hydrogenation cauldron additional and take a sample, because pressure, temperature all are higher in the hydrogenation cauldron, and the uncontrollable ejection of compact speed is very big to the harm of sampling personnel, and hydrogenation cauldron bottom is higher from ground, need build the platform and just can operate, and is extremely inconvenient. The third method is that a sampling bypass is arranged at an air inlet pipe under the hydrogenation kettle liquid, an air inlet valve is closed during sampling, a sampling bypass valve is opened, reaction liquid is pressed out by utilizing the pressure in the hydrogenation kettle, at the moment, hydrogen with higher pressure in the air inlet pipe is discharged firstly, if the hydrogen is directly discharged on site, accidents such as fire, explosion and the like are easily caused carelessly, the method is extremely dangerous, and the problems that the pressure and the temperature in the hydrogenation kettle are higher, the discharging speed cannot be controlled, and the harm to sampling personnel is large exist.
Therefore, designing and manufacturing a safe and convenient sampling device is an urgent need in the high-pressure hydrogenation production process.
SUMMERY OF THE UTILITY MODEL
An object of the utility model is to the shortcoming that above-mentioned sample process exists, provide a high-pressure hydrogenation cauldron sampling device, make the sample safe, convenient, do not exert an influence to the reaction simultaneously, guarantee that production goes on smoothly.
The utility model discloses a realize like this: a sampling device for high-pressure hydrogenation cauldron which characterized in that: the sampling device comprises a nitrogen inlet pipeline, a hydrogen inlet pipeline and a sampling pipeline, wherein the nitrogen inlet pipeline is provided with a nitrogen valve bank, and the hydrogen inlet pipe is provided with a hydrogen valve bank; the nitrogen gas inlet pipeline and the hydrogen gas inlet pipeline are communicated with the submerged gas inlet pipe through a hydrogen valve group through a gas inlet valve; the hydrogen inlet pipeline is communicated with the sampling pipeline after passing through the hydrogen valve group; the sample pipeline is equipped with sample feed valve, sample bleeder valve, has set gradually atmospheric valve, sight glass and spark arrester through the sample pipeline between sample feed valve and the sample bleeder valve.
Generally, the nitrogen valve set consists of two valves and a check valve.
The hydrogen valve group consists of two valves and a check valve.
The sampling volume is determined by the volume of the sampling line.
And a heat exchange sleeve is arranged on the outer side of the sampling pipeline.
The valves and pipelines are all made of stainless steel.
The pressure grades of the various valves and pipelines are consistent with the design pressure of the high-pressure hydrogenation kettle.
Compared with the prior art, the utility model provides a high-pressure hydrogenation cauldron sampling device has solved the high-pressure hydrogenation cauldron and has carried out the problem of convenient, safe sample at any time in normal reaction process to avoid the influence to the reaction, guarantee that production goes on smoothly.
Drawings
Fig. 1 is a schematic view of a connection structure of a sampling device for a high-pressure hydrogenation kettle according to an embodiment of the present invention.
In the figure, a 1-nitrogen valve bank, a 2-hydrogen valve bank, a 3-air inlet valve, a 4-sampling feed valve, a 5-sampling discharge valve, a 6-emptying valve, a 7-sight glass and an 8-flame arrester are arranged; AB-submerged air inlet pipe, BCDE and DF-sampling pipeline.
Detailed Description
The present invention will be described in detail with reference to the accompanying drawings and examples. It is to be understood that the description of the embodiments herein is for purposes of illustration and explanation only and is not intended to limit the invention.
Examples
As shown in fig. 1, a sampling device for a high-pressure hydrogenation kettle mainly comprises a nitrogen valve set 1 (comprising two valves and check valves), a hydrogen valve set 2 (comprising two valves and check valves), an air inlet valve 3, an underwater air inlet pipe AB, sampling tube furnaces BCDE and DF, a sampling feed valve 4, a sampling discharge valve 5, an emptying valve 6, a sight glass 7 and a flame arrester 8. Connection relationship of sampling device: the nitrogen inlet pipeline is provided with a nitrogen valve group 1, and the hydrogen inlet pipe is provided with a hydrogen valve group 2; the nitrogen gas inlet pipeline and the hydrogen gas inlet pipeline are communicated with a submerged gas inlet pipe through a hydrogen valve group 2 through a gas inlet valve 3; the hydrogen inlet pipeline is communicated with the sampling pipeline after passing through the hydrogen valve group 2; the sample pipeline is equipped with sample feed valve 4, sample bleeder valve 5, has set gradually atmospheric valve 6, sight glass 7 and spark arrester 8 through the sample pipeline between sample feed valve 4 and the sample bleeder valve 5.
The sampling volume of the sampling device of the embodiment is determined by the volumes of the sampling pipelines BCDE and DF; the outer side of the sampling pipeline is provided with a heat exchange sleeve which can be used for sampling high-temperature materials and easily solidified materials. The valve and the pipeline are made of stainless steel, the process connection adopts the connection of a concave-convex welding flange, and the pressure grade of the valve, the pipeline and the flange is consistent with the design pressure of the hydrogenation kettle. As hydrogenation catalysts are involved in hydrogenation reactions, the hydrogenation catalysts are Raney nickel, pd/C and Pt/C which are solid, and all valves are stainless steel ball valves in order to prevent the valves from being blocked or damaged. Because the device relates to hydrogen, the sampling tube emptying system is provided with a flame arrester, and the safe emission of tail gas is ensured.
The sampling device of the embodiment is operated according to the following method when sampling:
(1) Before the reaction, the sampling pipe is replaced by nitrogen: and (3) closing the hydrogen valve group 2, the emptying valve 6 and the sampling discharge valve 5 of the hydrogenation kettle, opening the nitrogen valve group 1 and the sampling feed valve 4 for nitrogen replacement, and repeating for 3 to 4 times. After the nitrogen replacement is finished, closing the nitrogen valve group 1, the sampling feed valve 4 and the blow-down valve 6 for standby;
(2) During sampling, the nitrogen valve group 1, the hydrogen valve group 2 and the sampling discharge valve 5 are ensured to be in a closed state, the hydrogenation kettle air inlet valve 3, the sampling feed valve 4 and the blow-down valve 6 are slowly opened for exhausting, tail gas is blown down through the flame arrester 8, the sight glass 7 is closely observed, the hydrogenation kettle air inlet valve 3 is immediately closed until liquid materials appear in the sight glass 7, and the sampling discharge valve 5 is slowly opened for sampling;
(3) When the discharge of the sampling discharge valve 5 is slowed down, the nitrogen valve group 1 is slowly opened to purge the sampling pipeline, and the blown liquid is collected in the sampling bottle, so that the sampling is finished.
The sampling device of the high-pressure hydrogenation kettle of the embodiment solves the problem of how to safely and conveniently sample in the hydrogenation reaction process, and ensures the smooth production.
Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.