Automatic evaluation and analysis device for triethylene diamine catalyst
By designing an automatic evaluation and analysis device for triethylenediamine catalysts, and using technical means such as preheating pipes and ceramic spheres, online gas chromatographs and catalyst reaction separation devices, the problems of insufficient raw material preheating and high ammonia content are solved. , achieving efficient catalyst evaluation and improvement of automation.
Patent Information
- Application Number
- CN202323567214.0
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2023-12-26
- Publication Date
- 2025-02-11
- Estimated Expiration
- 2033-12-26
AI Technical Summary
The existing triethylenediamine catalyst performance evaluation methods have problems such as insufficient preheating of raw materials, high ammonia content in the reaction liquid, increasing catalyst loading and on-site environmental pollution.
A triethylene diamine catalyst automatic evaluation and analysis device was designed, and a preheater combining preheating tubes with ceramic spheres was used to ensure that the raw materials were fully preheated; an online gas chromatograph was used instead of manual sampling and analysis, and the constant flow pump and The raw material mixer automatically mixes the raw materials, and the catalyst reaction separation device automatically carries out catalytic reaction and exhaust gas treatment; the heating layer is outsourced in the reaction liquid storage tank to reduce the solubility of ammonia.
The complete preheating of raw materials is achieved, the catalyst loading volume and ammonia content in the reaction liquid are reduced, the degree of automation is improved, the risks and costs of manual operation are reduced, and the sanitation status of the on-site environment is improved.
Smart Images
Figure CN222461394U_ABST
Abstract
Description
Technical Field
[0001] The utility model belongs to the technical field of compound testing equipment, and specifically relates to an automatic evaluation and analysis device for a triethylenediamine catalyst. Background Art
[0002] Triethylenediamine (TEDA) is an organic synthesis intermediate, which is widely used in the production of various products such as polyurethane foam, elastomers, plastics and coatings. The preparation process of triethylenediamine is often inseparable from catalysts and catalyst performance evaluation devices.
[0003] At present, the method for evaluating the performance of triethylenediamine catalyst is to prepare ethylenediamine and deionized water into a 40% to 50% organic aqueous solution, which is then preheated and gasified or directly introduced into a catalyst bed at a certain temperature for reaction. The reaction gas is collected by condensation or gas-liquid separation tank, and sampling, detection and analysis are performed at intervals. The purpose of preparing the reaction system into an aqueous solution is that water as a diluent can promote the desorption and diffusion of reactants and products, improve the stability of the catalyst and delay the deactivation of carbon deposition. However, the specific heat capacity of water is large. If the raw materials are not preheated or the preheating temperature is low, when the liquid raw materials contact the high-temperature catalyst, they will absorb a large amount of heat to reduce the catalyst bed temperature, reduce the raw material conversion rate and product yield, and therefore it is necessary to increase the catalyst bed height, resulting in an increase in the catalyst loading. At the same time, the preparation of triethylenediamine produces ammonia as a by-product, and a large amount of ammonia will be dissolved in the collected reaction liquid. Since ammonia has a strong pungent odor, the on-site environmental odor is large during manual sampling and analysis, which affects the physical and mental health of personnel. Therefore, a triethylenediamine catalyst evaluation and analysis device with a high degree of automation and capable of being separated from manual operation is required. Utility Model Content
[0004] The technical problem to be solved by the utility model is to provide a triethylenediamine catalyst evaluation and analysis device with a high degree of automation which can fully preheat raw materials and reduce the ammonia content of reaction liquid.
[0005] In order to solve the above technical problems, the utility model provides a triethylenediamine catalyst automatic evaluation and analysis device, comprising an ethylenediamine storage tank and a deionized water storage tank, wherein the ethylenediamine storage tank and the deionized water storage tank are respectively connected to a raw material mixer through a first constant flow pump (), and then the raw material mixer is connected to at least one catalyst reaction separation device through a preheater, and the catalyst reaction separation device is combined into one through a multi-input and one-output selection valve, and then connected to an online gas chromatograph through a two-position three-way electromagnetic valve and a rotor flowmeter;
[0006] The catalyst reaction separation device comprises a fixed bed reactor, a condenser, a gas-liquid separator, a reaction liquid storage tank and a second constant flow pump which are connected in sequence.
[0007] As an improvement of the automatic evaluation and analysis device for triethylenediamine catalyst of the utility model:
[0008] The preheater comprises a preheating tube, the outer surface of the preheating tube is covered with a first electric heating device, and the inner surface is filled with ceramic balls; the inlet of the preheating tube is connected to the outlet end of the raw material mixer, and the outlet is connected to at least one fixed bed reactor through a multi-way joint.
[0009] As a further improvement of the automatic evaluation and analysis device for triethylenediamine catalyst of the utility model:
[0010] The fixed bed reactor comprises a reactor tube, the reactor tube is covered with a second electric heating device on the outside and filled with a catalyst to be tested; the inlet end of the reactor tube is connected to a multi-way connector;
[0011] A temperature digital display device is arranged outside the reactor tubes, and a temperature probe of the temperature digital display device extends into the reactor tubes.
[0012] As a further improvement of the automatic evaluation and analysis device for triethylenediamine catalyst of the utility model:
[0013] The condenser is a double-layer shell, and the space between the double-layer shells is a flow path for the condensation circulating liquid; the lower part of the outer shell of the condenser is provided with a condensate inlet, and the upper part is provided with a condensate outlet;
[0014] The outlet end of the reactor tube is connected to the inlet end of the condenser.
[0015] As a further improvement of the automatic evaluation and analysis device for triethylenediamine catalyst of the utility model:
[0016] The gas-liquid separator includes a feed conduit, one end of which is connected to the outlet end of the condenser, and the other end extends to the lower part of the inner cavity of the gas-liquid separator; a separator outlet is provided at the bottom of the gas-liquid separator, and a tail gas outlet is provided at the top, and the tail gas outlet is connected to the tail gas treatment device after passing through a first pressure gauge and a first one-way valve in sequence.
[0017] As a further improvement of the automatic evaluation and analysis device for triethylenediamine catalyst of the utility model:
[0018] The reaction liquid storage tank is wrapped with a heating layer on the outside, and is provided with an ammonia outlet and a reaction liquid inlet on the top, and a reaction liquid outlet on the bottom. The ammonia outlet is connected to the tail gas treatment device after passing through the second pressure gauge and the second one-way valve in sequence; the reaction liquid inlet is connected to the separator discharge port at the bottom of the gas-liquid separator through a stop valve; the reaction liquid inlet is connected to the multi-inlet and one-outlet selection valve after passing through the second constant flow pump.
[0019] The beneficial effects of the utility model are mainly reflected in:
[0020] 1. The utility model adopts the method of filling ceramic balls inside the preheating tube to play a turbulent role, increase the heating area of the raw material, ensure the full gasification of the raw material, and reduce the loading amount of the catalyst;
[0021] 2. The utility model adopts an online gas chromatograph to replace manual sampling and manual analysis and detection, adopts a constant flow pump and a raw material mixer to automatically mix two kinds of raw materials, and adopts a catalyst reaction separation device to automatically perform a catalytic reaction and absorb tail gas. The automation level is high, which solves the problem that the odor of the on-site environment affects the physical and mental health of personnel. At the same time, the analysis results are timely and accurate, saving labor costs;
[0022] 3. The utility model wraps a heating belt on the outside of the reaction liquid storage tank to heat the reaction liquid, reduce the solubility of ammonia, and improve the accuracy of online analysis and detection of liquid samples. BRIEF DESCRIPTION OF THE DRAWINGS
[0023] The specific implementation of the utility model is further described in detail below with reference to the accompanying drawings.
[0024] Figure 1 It is a schematic diagram of an automatic evaluation and analysis device for triethylenediamine catalyst of the utility model;
[0025] Figure 2 for Figure 1 A schematic diagram of the structure of the preheater 5;
[0026] Figure 3 for Figure 1 A schematic structural diagram of a fixed bed reactor 7;
[0027] Figure 4 for Figure 1 A schematic diagram of the structure of the condenser 8;
[0028] Figure 5 for Figure 1 A schematic diagram of the structure of the gas-liquid separator 9;
[0029] Figure 6 for Figure 1 A schematic structural diagram of the reaction liquid storage tank 10. DETAILED DESCRIPTION
[0030] The present invention is further described below in conjunction with specific embodiments, but the protection scope of the present invention is not limited thereto:
[0031] Example 1: A triethylenediamine catalyst automatic evaluation and analysis device, such as Figure 1-6As shown, it includes an ethylenediamine storage tank 1, a deionized water storage tank 2, a first constant flow pump 3-1, a raw material mixer 4, a preheater 5, a catalyst reaction separation device, a rotor flowmeter 13, an online gas chromatograph 14 and an exhaust gas treatment device 16.
[0032] The ethylenediamine storage tank 1 is used to store ethylenediamine liquid, and the deionized water storage tank 2 is used to store deionized water. The ethylenediamine storage tank 1 and the deionized water storage tank 2 are respectively connected to the inlet end of the raw material mixer 4 through a first constant flow pump 3-1. By setting the flow rate and flow velocity of the first constant flow pump 3-1 on the two pipelines, different amounts of raw materials are pumped into the mixer 4 for uniform mixing, so as to realize automatic configuration of a certain concentration of organic aqueous solution, saving the time and energy spent on manual configuration of the solution, and improving the working efficiency.
[0033] The outlet end of the raw material mixer 4 is connected to the preheater 5, which includes a preheating tube 5-1, a first electric heating device 5-2 and ceramic balls 5-3. The preheating tube 5-1 is a metal pipe, and the first electric heating device 5-2 is sheathed on the outside to provide a heat source to preheat the organic aqueous solution flowing through the preheating tube 5-1. A certain number of ceramic balls 5-3 are filled inside the preheating tube 5-1, which can play a certain role in disturbing the raw material, increase the heating area of the raw material, make the raw material more fully heated, and shorten the temperature difference between the raw material and the catalyst.
[0034] The inlet of the preheating tube 5-1 is connected to the outlet of the raw material mixer 4, and then the outlet of the preheating tube 5-1 is connected to two or more catalyst reaction separation devices through a multi-way joint 6, each of which includes a fixed bed reactor 7, a condenser 8, a gas-liquid separator 9, a reaction liquid storage tank 10 and a second constant flow pump 3-2 connected in sequence. The multi-way joint 6 can select a three-way joint, a four-way joint or a five-way joint according to the number of fixed bed reactors 7 actually connected.
[0035] The fixed bed reactor 7 includes a reactor tube 7-1, a second electric heating device 7-2, a catalyst to be tested 7-3 and a temperature digital display device 7-4. The reactor tube 7-1 is covered with a second electric heating device 7-2 to heat the catalyst to the required temperature for activity and provide the heat energy required for the reaction, and the catalyst to be tested 7-3 is filled inside. The inlet of the reactor tube 7-1 is connected to the outlet of the multi-way connector 6, and the raw material enters the reactor tube 7-1 along the pipeline to contact the catalyst to be tested 7-3 and undergo a catalytic reaction. The reactor tube 7-1 is provided with a temperature digital display device 7-4 outside, and the temperature probe of the temperature digital display device 7-4 extends into the reactor tube 7-1 to monitor the temperature inside the reactor tube 7-1 and the reaction temperature.
[0036] The outlet end of the reactor tube 7-1 is sequentially connected to a condenser 8, a gas-liquid separator 9 and a reaction liquid storage tank 10. The condenser 8, the gas-liquid separator 9 and the reaction liquid storage tank 10 are all closed containers.
[0037] The condensers 8 are all double-layer shells, and the space between the double-layer shells is a condensation circulating liquid flow path. The lower part of the outer shell of the condenser 8 is provided with a condensate inlet 8-1, and the upper part is provided with a condensate outlet 8-2. The outlet end of the reactor tube 7-1 is connected to the inlet end of the condenser 8 through a pipeline, so as to pass the reaction liquid generated by the reaction with the catalyst 7-3 to be tested in the fixed bed reactor 7 into the inner cavity of the condenser 8. The condensation circulating liquid enters from the condensate inlet 8-1 and exits from the condensate outlet 8-2, so as to condense the reaction liquid and improve the condensation efficiency.
[0038] The gas-liquid separator 9 includes a feed conduit 9-5, one end of which is connected to the outlet end of the condenser 8 through a pipeline, and the other end extends to the lower part of the inner cavity of the gas-liquid separator 9. A separator outlet is provided at the bottom of the gas-liquid separator 9. A tail gas outlet 9-4 is provided at the top of the gas-liquid separator 9. The tail gas outlet 9-4 is connected to the tail gas treatment device 16 through a pipeline after passing through the first pressure gauge 9-2 and the first one-way valve 9-3 in sequence, so as to discharge the waste gas. The first pressure gauge 9-2 is used to detect whether the pressure in the gas-liquid separator 9 is abnormal, and the first one-way valve 9-3 is used to prevent the tail gas absorption liquid from being sucked back into the gas-liquid separator 9. A certain amount of acid absorption liquid is installed inside the tail gas treatment device 16, and the air inlet pipe is inserted below the liquid level, and the air outlet pipe is above the liquid level.
[0039] The reaction liquid storage tank 10 is wrapped with a heating layer 10-1 on the outside, which is used to heat the reaction liquid at a constant temperature, reduce the solubility of ammonia in the reaction liquid, and improve the accuracy of the test results. The heating layer 10-1 can be electrically heated. An ammonia outlet 10-2 and a reaction liquid inlet 10-4 are provided at the top of the reaction liquid storage tank 10, and a reaction liquid outlet 10-3 is provided at the bottom. The ammonia outlet 10-2 is connected to the tail gas treatment device 16 through a pipeline after passing through the second pressure gauge 10-5 and the second one-way valve 10-6 in sequence, so as to discharge ammonia. The reaction liquid inlet 10-4 is connected to the discharge port at the bottom of the gas-liquid separator 9 through a stop valve 9-1, and the stop valve 9-1 is used to control the outflow of the reaction liquid.
[0040] The reaction liquid outlet 10-3 of the reaction liquid storage tank 10 is connected to the inlet end of the multi-input and one-output selection valve 11 through the second constant flow pump 3-2, so as to select the reaction liquid in different reaction liquid storage tanks 10 for detection when multiple reaction liquid storage tanks 10 are connected in parallel (that is, when multiple catalyst reaction separation devices are connected in parallel).
[0041] The outlet of the multi-input and one-output selector valve 11 is divided into two paths after passing through the two-position three-way solenoid valve 12, one path is connected to the online gas chromatograph 14 after passing through the rotor flowmeter 13, and the other path is the cleaning liquid discharge pipeline 15. The second constant flow pump 3-2 is used to transport the reaction liquid in the reaction liquid storage tank 10 to the online gas chromatograph 14 along the conduit. The two-position three-way solenoid valve 12 can control the flow of the liquid. By controlling the switch state of the valve, the fluid can stop, pass and reverse flow in the pipeline. The rotor flowmeter 13 can accurately control the amount of samples required for detection, and then transport them to the online gas chromatograph 14 for detection. After the detection is completed or when the sample source is changed, the liquid in the pipeline between the two-position three-way solenoid valve 12 and the rotor flowmeter 13 can be refluxed to the cleaning liquid discharge pipeline 15 by controlling the two-position three-way solenoid valve 12, avoiding the situation where the sample detected last time stays in the pipeline and causes inaccurate detection results.
[0042] The specific method of using the utility model is as follows:
[0043] 1. Loading catalyst:
[0044] Different types of catalysts to be tested 7-3 are loaded in appropriate amounts into different reactor tubes 7-1.
[0045] 2. Heating:
[0046] Turn on the power of the first electric heating device 5-2 and the second electric heating device 7-2, prepare for preheating the raw materials and heat the catalyst 7-3 to the temperature required for activity.
[0047] 3. Feed raw materials to react:
[0048] The two first constant flow pumps 3-1 are turned on to deliver ethylenediamine and deionized water to the raw material mixer 4 at a certain flow rate and velocity for uniform mixing, and then flow into the preheater 5 for preheating. The preheated raw gas enters each reactor tube 7-1 to contact with different types of catalysts to be tested 7-3 and react to produce different gases. The reacted gases are converted into liquid reaction liquid after passing through the condenser 8 and the gas-liquid separator 9, and enter each reaction liquid storage tank 10, and ammonia is removed under the action of the external constant temperature heating layer 10-1.
[0049] 4. Analysis and testing:
[0050] The reaction liquid in different reaction liquid storage tanks 10 is selected by a multi-input and one-output selection valve 11.
[0051] The reaction liquid is discharged from the cleaning liquid discharge pipeline 15 under the control of the two-position three-way solenoid valve 12 and the rotor flowmeter 13 along the pipeline under the action of the second constant flow pump 3-2. Finally, the optimal process parameters and catalyst types are determined based on the test results.
[0052] Finally, it should be noted that the above examples are only some specific embodiments of the present invention. Obviously, the present invention is not limited to the above examples, and there are many variations. All variations that can be directly derived or associated with the content disclosed by a person skilled in the art should be considered as the protection scope of the present invention.
Claims
1. A triethylenediamine catalyst automatic evaluation and analysis device, characterized in that: The invention comprises an ethylenediamine storage tank (1) and a deionized water storage tank (2), wherein the ethylenediamine storage tank (1) and the deionized water storage tank (2) are respectively connected to a raw material mixer (4) through a first constant flow pump (3-1), and then the raw material mixer (4) is connected to at least one catalyst reaction separation device through a preheater (5), and the catalyst reaction separation device is combined into one through a multi-input and one-output selection valve (11), and then connected to an online gas chromatograph (14) through a two-position three-way electromagnetic valve (12) and a rotor flowmeter (13); The catalyst reaction separation device comprises a fixed bed reactor (7), a condenser (8), a gas-liquid separator (9), a reaction liquid storage tank (10) and a second constant flow pump (3-2) which are connected in sequence.
2. The automatic evaluation and analysis device for triethylenediamine catalyst according to claim 1, characterized in that: The preheater (5) comprises a preheating tube (5-1), the outer portion of the preheating tube (5-1) is covered with a first electric heating device (5-2), and the inner portion is filled with ceramic balls (5-3); the inlet of the preheating tube (5-1) is connected to the outlet end of the raw material mixer (4), and the outlet is connected to at least one fixed bed reactor (7) through a multi-way connector (6).
3. The automatic evaluation and analysis device for triethylenediamine catalyst according to claim 2, characterized in that: The fixed bed reactor (7) comprises a reactor tube (7-1), the reactor tube (7-1) is covered with a second electric heating device (7-2) on the outside and filled with a catalyst to be tested (7-3) inside; the inlet end of the reactor tube (7-1) is connected to a multi-way connector (6); A temperature digital display device (7-4) is provided outside the reactor tube array (7-1), and a temperature probe of the temperature digital display device (7-4) extends into the reactor tube array (7-1).
4. The automatic evaluation and analysis device for triethylenediamine catalyst according to claim 3, characterized in that: The condenser (8) is a double-layer shell, and the space between the double-layer shells is a flow path for the condensed circulating liquid; the lower part of the outer shell of the condenser (8) is provided with a condensate inlet (8-1), and the upper part is provided with a condensate outlet (8-2); The outlet end of the reactor tube (7-1) is connected to the inlet end of the condenser (8).
5. The automatic evaluation and analysis device for triethylenediamine catalyst according to claim 4, characterized in that: The gas-liquid separator (9) comprises a feed conduit (9-5), one end of which is connected to the outlet end of the condenser (8), and the other end of which extends to the lower part of the inner cavity of the gas-liquid separator (9); a separator outlet is provided at the bottom of the gas-liquid separator (9), and a tail gas outlet (9-4) is provided at the top; the tail gas outlet (9-4) passes through a first pressure gauge (9-2) and a first one-way valve (9-3) in sequence and is connected to a tail gas treatment device (16).
6. The automatic evaluation and analysis device for triethylenediamine catalyst according to claim 5, characterized in that: The reaction liquid storage tank (10) is wrapped with a heating layer (10-1) on the outside, and is provided with an ammonia outlet (10-2) and a reaction liquid inlet (10-4) on the top, and a reaction liquid outlet (10-3) on the bottom. The ammonia outlet (10-2) is connected to the tail gas treatment device (16) after passing through a second pressure gauge (10-5) and a second one-way valve (10-6) in sequence; the reaction liquid inlet (10-4) is connected to the separator discharge port at the bottom of the gas-liquid separator (9) through a stop valve (9-1); the reaction liquid inlet (10-4) is connected to the multi-input and one-output selection valve (11) after passing through a second constant flow pump (3-2).