Vaporization mixing preheating device for carbon monoxide sulfur-tolerant shift catalyst activity test

Abstract

The utility model belongs to the technical field of chemical equipment, and relates to a vaporization mixing preheating device for an activity test of a carbon monoxide sulfur-tolerant shift catalyst, which is characterized by comprising a barrel and a shell, and an electric heating jacket, an embedded temperature control thermocouple sleeve and a heat insulation layer are arranged between the barrel and the shell; a temperature measuring thermocouple sleeve is inserted into the top of the cylinder body; the upper side part of the cylinder is connected with the air outlet, the bottom is connected with the air inlet, and the lower side part is connected with the water inlet. The device is connected with the reactor through a pipeline, so that the investment cost is low, the occupied area is small, and the operation is convenient; a special steel material is adopted, so that heat transfer is better, and temperature balance in the barrel body is more facilitated; the special structure of the cylinder is beneficial to vaporization, mixing and preheating of water.

Description

Technical Field

[0001] The invention belongs to the technical field of chemical equipment, and specifically relates to a vaporization mixing preheating device used for an activity test of a carbon monoxide sulfur-resistant conversion catalyst. Background Art

[0002] The sulfur-tolerant carbon monoxide shift catalyst is widely used in the petrochemical industry. Compared with the traditional iron-chromium and copper-zinc shift catalysts, it has the advantages of large operating flexibility, high activity, low poisoning, and unlimited sulfur resistance. Therefore, it can meet the needs of the development of raw materials to heavy raw materials and can be used as a shift catalyst for sulfur-containing carbon monoxide industrial gas generated by gasification of residual oil or coal. The application of this catalyst not only greatly simplifies the process flow, but also has significant energy-saving effects.

[0003] Due to differences in formulation and production process, some products will become inactivated and pulverized during industrial use, which poses a huge risk to the safety and stable production of manufacturers. Therefore, the activity evaluation of sulfur-tolerant shift catalysts before industrial application is particularly important.

[0004] Carbon monoxide in the raw gas reacts with a certain proportion of water vapor under the action of the carbon monoxide sulfur-resistant shift catalyst to produce carbon dioxide and hydrogen. The carbon monoxide volume fraction in the gas before and after the reaction is analyzed by a gas chromatograph (or other carbon monoxide analyzer), and its carbon monoxide conversion rate is calculated to characterize the catalyst activity. The water content in the raw gas is generally brought in by water vaporization. By controlling the vaporization mixing preheating device, the water content in the raw gas can be controlled so that the gas entering the reactor is evenly mixed and reaches a certain preheating temperature. Summary of the invention

[0005] The utility model provides a vaporization mixing preheating device to solve the problem of stable water content in raw gas, so that the gas entering the reactor is evenly mixed and reaches a certain preheating temperature, thereby ensuring the accuracy of the test result.

[0006] Purpose of the invention: Whether the stable water content in the raw gas of the carbon monoxide sulfur-resistant shift catalyst active reaction is evenly mixed and reaches a certain preheating temperature is the key to whether the activity test result is accurate. The present invention uses a special vaporization mixing preheating device to allow the raw gas to fully contact and mix with water at a certain temperature and reach a certain preheating temperature to obtain a corresponding, uniform gas source containing water vapor at a certain temperature.

[0007] Technical solution: A vaporization mixing preheating device for the activity test of a carbon monoxide sulfur-resistant shift catalyst, characterized in that it comprises a cylinder and an outer shell, an electric heating sleeve, an embedded temperature-controlling thermocouple sleeve and an insulation layer are arranged between the cylinder and the outer shell; a temperature-measuring thermocouple sleeve is inserted at the top of the cylinder; the upper side of the cylinder is connected to the air outlet, the bottom is connected to the air inlet, and the lower side is connected to the water inlet.

[0008] Generally, the temperature-controlling thermocouple sleeve and the temperature-measuring thermocouple sleeve are inserted with detachable thermocouples.

[0009] The electric heating jacket and the thermocouple are connected to a temperature control system.

[0010] The cylinder body is internally provided with alloy wood shavings filler.

[0011] The bottom of the cylinder is connected to a sewage outlet, so that the accumulated water in the cylinder can be drained at any time, so that the quality of water vapor is effectively guaranteed.

[0012] The electric heating sleeve includes an electric furnace wire with bowl-shaped magnetic beads, the electric furnace wire is wrapped with aluminum silicate felt, tied and fixed by iron wire, and filled with pearlite powder for heat preservation. It is used for heating the vaporization mixing preheating device and temperature control is performed by thermocouple.

[0013] The water inlet is provided with a water atomizing nozzle, which is beneficial to water vaporization and full mixing with the raw gas.

[0014] The thermal insulation layer of the utility model is generally composed of aluminum silicate felt, pearlite powder, etc. to maintain the temperature of the vaporization mixing preheating device.

[0015] The cylinder of the utility model is made of corrosion-resistant high-strength special alloy steel, the shell is made of high-strength low-alloy steel, and the bolt cap is made of stainless steel.

[0016] The utility model also includes connecting pipelines well known in the art.

[0017] The working process of the utility model is as follows: first, start the electric heater to heat the cylinder to a preset temperature; open the air inlet pipe to introduce raw gas; open the water inlet pipe to atomize the quantitative water entering, and the vaporized water vapor fully contacts with the raw gas, and the gas carrying water vapor and having a certain temperature enters the reactor through the gas outlet pipe with insulation.

[0018] Beneficial effects: 1. The device is connected to the reactor by pipeline, with low investment cost, small footprint and easy operation. 2. The use of special steel material has better heat transfer and is more conducive to temperature balance in the cylinder. 3. The special structure of the cylinder is conducive to the vaporization, mixing and preheating of water. BRIEF DESCRIPTION OF THE DRAWINGS

[0019] Figure 1 It is a schematic structural diagram of a vaporization mixing preheating device used for the activity test of a carbon monoxide sulfur-resistant shift catalyst according to an embodiment of the utility model.

[0020] In the figure: 1—air outlet; 2—shell; 3—insulation layer; 4—temperature-controlling thermocouple sleeve; 5—electric heating sleeve; 6—drain outlet; 7—air inlet; 8—water inlet; 9—atomizing nozzle; 10—cylinder; 11—filler; 12—temperature-measuring thermocouple sleeve. DETAILED DESCRIPTION

[0021] The utility model is further described below in conjunction with the implementation modes and the accompanying drawings. Example

[0022] This embodiment is a vaporization mixing preheating device for the activity test of carbon monoxide sulfur-resistant shift catalyst. Figure 1 , mainly including a cylinder 10, an air inlet 7, a sewage outlet 6, an electric heating jacket 5, an insulation layer 3, a temperature control system (not shown in the figure), an air outlet 1, a temperature-controlling thermocouple sleeve 4, a temperature-measuring thermocouple sleeve 12, a filler 11, a water inlet 8 and a shell 2.

[0023] In the embodiment, an electric heating sleeve 5, an embedded temperature-controlling thermocouple sleeve 4 and an insulation layer 3 are arranged between the cylinder 10 and the shell 2; a temperature-measuring thermocouple sleeve 12 is inserted at the top of the cylinder 10; the upper side of the cylinder 10 is connected to the air outlet 1, the bottom is connected to the air inlet 7, and the lower side is connected to the water inlet 8. The water inlet 8 is provided with a water atomizing nozzle 9, which is conducive to water vaporization and fully mixed with the raw gas. The cylinder 10 is built with alloy shavings filler 11. The bottom of the cylinder 10 is connected to the drain port 6, and the accumulated water in the cylinder is drained at any time, so that the quality of the water vapor is effectively guaranteed.

[0024] In the embodiment, the temperature-controlling thermocouple sleeve 4 and the temperature-measuring thermocouple sleeve 12 are inserted with detachable thermocouples, and the electric heating sleeve 5 and the thermocouples are connected to a temperature control system.

[0025] In the embodiment, the electric heating jacket 5 includes an electric furnace wire with bowl-shaped magnetic beads, the electric furnace wire is wrapped with aluminum silicate felt, tied and fixed by iron wire, and filled with pearlite powder for heat preservation. It is used for heating the vaporization mixing preheating device, and the temperature is controlled by a thermocouple.

[0026] In the embodiment, the insulation layer is generally composed of aluminum silicate felt, perlite powder, etc. to maintain the temperature of the vaporization mixing preheating device.

[0027] The cylinder body is made of corrosion-resistant high-strength special alloy steel, the shell is made of high-strength low-alloy steel, and the bolt cap is made of stainless steel.

[0028] This embodiment also includes connecting pipes well known in the art.

[0029] Specific operation process of the preheating device in the embodiment: Under normal circumstances, the raw gas enters the vaporization mixing preheating device through the air inlet pipe, a certain amount of water is atomized through the water inlet nozzle, the vaporized water vapor fully contacts the raw gas, and the gas with water vapor and a certain temperature enters the reactor through the gas outlet pipe with insulation. The gas coming out of the reactor is cooled by the condenser, and after being measured by the rotor flowmeter, one way goes to the analysis system, and the other way goes through the water seal bottle and then emptied.

[0030] The raw gas (by volume fraction) is composed of carbon monoxide (28% to 32%), carbon dioxide (6% to 10%), hydrogen (35% to 55%), total sulfur (as H2S) greater than 0.007%, oxygen less than 0.5%, and the rest is inert gas.

[0031] Connect the reactor filled with catalyst to the test system. After the leak test meets the requirements, insert the thermocouple into the thermocouple sleeve so that its hot end is located in the middle of the catalyst bed.

[0032] Feed gas into the reactor at a space velocity of 750 h -1 When the reactor temperature rises to 180°C, the total sulfur (in terms of H2S) is added to the feed gas at a concentration of 50 g / Nm 3 ~70g / Nm 3 The vulcanizing agent is added until the reactor temperature drops from 350°C to 250°C, and the sulfur addition is stopped, and the vulcanization is completed.

[0033] After the vulcanization is completed, the carburetor is heated to about 280℃, the insulation tube is heated to about 180℃, the raw gas valve is switched, and the system pressure is controlled and adjusted to (0.8±0.02)MPa and the raw gas space velocity is (2500±50)h. -1 , the volume ratio of water vapor to raw gas is 0.5±0.02 (the determination of the volume ratio of water vapor to raw gas is shown in Appendix D), the activity measurement temperature is (200±1)℃, and after stabilization and maintenance for 3 hours, the volume fraction of carbon monoxide in the reactor inlet and outlet gas is measured every 1.5h~2.0h, and the carbon monoxide conversion rate is calculated. When the extreme difference of the carbon monoxide conversion rate for three consecutive times is not greater than 1.0%, the test can be terminated.

[0034] After the test, close the main valve of raw gas, drain and reduce the pressure of the system, and discharge the condensed water in the condenser. When the system drops to normal pressure, turn off the horizontal flow pump, stop water injection, and finally cut off the power supply of the system.

[0035] The test results are as follows: the activity of the catalyst in furnace 1# is 90.6%, the activity of the catalyst in furnace 2# is 91.5%, and the absolute difference between the parallel measurement results is no more than 3%.

Claims

1. A vaporization mixing preheating device for carbon monoxide sulfur-tolerant shift catalyst activity test, characterized in that: It includes a cylinder and an outer shell, an electric heating sleeve, an embedded temperature-controlling thermocouple sleeve and an insulation layer are arranged between the cylinder and the outer shell; a temperature-measuring thermocouple sleeve is inserted at the top of the cylinder; the upper side of the cylinder is connected to the air outlet, the bottom is connected to the air inlet, and the lower side is connected to the water inlet.

2. A vaporization mixing preheating device for carbon monoxide sulfur-resistant shift catalyst activity test according to claim 1, characterized in that The temperature-controlling thermocouple sleeve and the temperature-measuring thermocouple sleeve are inserted with detachable thermocouples.

3. A vaporization mixing preheating device for carbon monoxide sulfur-resistant shift catalyst activity test according to claim 1 or 2, characterized in that The electric heating jacket and the thermocouple are connected to the temperature control system.

4. A vaporization mixing preheating device for carbon monoxide sulfur-resistant shift catalyst activity test according to claim 1, characterized in that The cylinder is filled with alloy wood chips.

5. The vaporization mixing preheating device for the activity test of carbon monoxide sulfur-resistant shift catalyst according to claim 1, characterized in that The bottom of the cylinder is connected to a sewage outlet.

6. A vaporization mixing preheating device for carbon monoxide sulfur-resistant shift catalyst activity test according to claim 3, characterized in that The electric heating sleeve comprises an electric furnace wire with bowl-shaped magnetic beads in series, the electric furnace wire is wrapped with aluminum silicate felt, tied and fixed by iron wire, and filled with pearlite powder for heat preservation.

7. The vaporization mixing preheating device for the activity test of carbon monoxide sulfur-resistant shift catalyst according to claim 1 is characterized in that The water inlet is provided with a water atomizing nozzle.

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