Original particle size activity testing device for sulfuric acid catalyst prepared by oxidizing sulfur dioxide
By designing a test device for the primary particle size activity of sulfur dioxide oxidation sulfuric acid catalyst that simulates industrial application processes, the problem of the difference between the results of measuring catalyst activity in the prior art is solved, and the accurate determination and effective evaluation of catalyst activity are achieved.
Patent Information
- Application Number
- CN202420605485.6
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2024-03-27
- Publication Date
- 2025-03-18
- Estimated Expiration
- 2034-03-27
AI Technical Summary
When determining the activity of sulfur dioxide oxidation and sulfuric acid catalyst, the detection results of using the crushed particle size catalyst are different from those of actual industrial applications, and cannot effectively reflect the activity of the sample after use.
A test device for the primary particle size activity of sulfur dioxide oxidation sulfuric acid catalyst was designed. By simulating industrial application processes, controlling the inspection conditions such as temperature, pressure, and spacespeed, and using the primary particle size catalyst for the test, the sulfur dioxide conversion rate was determined to characterize the catalyst activity.
This device can effectively reflect the activity of the catalyst in industrial applications, provide more intuitive and accurate test results, helping the catalyst user unit to timely determine whether to replace the catalyst, improve product quality and environmental protection.
Smart Images
Figure CN222636135U_ABST
Abstract
Description
Technical Field
[0001] The utility model belongs to the technical field of chemical equipment and relates to an original particle size activity test device for a catalyst for producing sulfuric acid by oxidation of sulfur dioxide. Background Art
[0002] Sulfuric acid is a major basic chemical raw material and is widely used in various industrial fields.
[0003] my country is a major producer and consumer of sulfuric acid, with nearly 1,000 production facilities and an annual output of nearly 100 million tons. The Sulfuric Acid Industry Pollutant Emission Standard (GB 26132-2010) implemented in 2011 requires that the maximum allowable emission concentration of SO2 in the tail gas of sulfuric acid plants be increased from 860 mg / m 3 Reduced to 400mg / m 3 , which puts forward more stringent requirements for the sulfuric acid production process. As the core technology of the process, the performance of the catalyst not only affects the quality of sulfuric acid products and the emission concentration of tail gas SO2, but also becomes a constraint point for the process equipment to reduce costs and increase efficiency.
[0004] The main indicators of catalyst performance include strength, abrasion, pore structure, activity, chemical composition, etc., among which the activity determination is particularly important. At present, there are two methods for determining catalyst activity, one is to use crushed particle size catalyst, and the other is to use original particle size catalyst. The reactors and determination conditions used are different.
[0005] Testing with crushed catalysts means processing or crushing the catalysts into a certain length or size before testing. Its advantages are fast and timely testing, but its disadvantages are that the test results reflect the activity after crushing, which is different from the actual activity in industrial applications. In particular, after a period of use in the industry, some active components are lost, or the surface is partially covered by pollutants and impurities. In this case, the measured activity is more different from the industrial data.
[0006] The activity test using original particle size catalysts is very similar to industrial application, and the test results more intuitively reflect the level of industrial use, especially for the detection of used samples, which provides an important basis for catalyst users to determine whether to replace the catalyst in a timely manner.
[0007] Therefore, the formulation of the "Test Method for the Original Particle Size Activity of Sulfur Dioxide Oxidation Catalysts to Produce Sulfuric Acid" will not only play a role in regulating the catalyst production market, but will also play a positive role in improving the quality of subsequent products and protecting the environment.
[0008] In order to effectively test the activity of the product in the laboratory and quickly screen out high-performance sulfur dioxide oxidation to sulfuric acid catalyst products, it is necessary to establish a set of equipment that is easy to operate, requires low investment, and has stable operation. Summary of the invention
[0009] The utility model provides an original particle size activity test device for a catalyst for producing sulfuric acid by oxidation of sulfur dioxide, so as to solve the problems of original particle size activity inspection and performance evaluation of the catalyst for producing sulfuric acid by oxidation of sulfur dioxide.
[0010] The utility model provides a sulfur dioxide oxidation sulfuric acid catalyst original particle size activity test device, which simulates the sulfur dioxide oxidation sulfuric acid catalyst industrial application process, controls the catalyst process temperature, pressure, air velocity and other test conditions, thereby obtaining the sulfur dioxide oxidation sulfuric acid catalyst original particle size activity test data. Sulfur dioxide and oxygen in the air, under the action of the sulfur dioxide oxidation sulfuric acid catalyst, generate sulfur trioxide. The sulfur dioxide volume fraction in the gas before and after the reaction is measured by absorption with an iodine standard titration solution, and the sulfur dioxide conversion rate is calculated to characterize the catalyst activity.
[0011] The main technical scheme of the utility model: a test device for the original particle size activity of a catalyst for sulfuric acid production by oxidation of sulfur dioxide, characterized in that the device comprises a sulfur dioxide conversion system and a sulfur dioxide analysis system; the sulfur dioxide conversion system comprises a gas generating device and a gas absorbing device which are sequentially connected to a raw gas source; the gas generating device comprises an air compressor, a flow regulating valve and a rotor flowmeter; the gas absorbing device comprises a mixer, a preheater and a converter which are sequentially connected, and the gas absorbing device is equipped with a controllable temperature heating, heat preservation and cooling device; the sulfur dioxide analysis system comprises an absorption bottle, a test tube, a gas cylinder and a level bottle which are sequentially connected to an outlet of the mixer and an outlet of the converter.
[0012] Generally, the raw gas source is connected to one or more parallel gas reaction devices and gas absorption devices.
[0013] The sulfur dioxide mixed gas of the raw gas source is connected to the mixer through a flow regulating valve and a rotor flow meter.
[0014] The oxygen of the raw gas source is connected to the mixer through an air compressor, a flow regulating valve and a rotor flow meter.
[0015] The reaction tube of the converter is equipped with fillers and an original particle size sample of the catalyst for producing sulfuric acid by oxidation of sulfur dioxide.
[0016] The controllable temperature heating, heat preservation and cooling device is a DCS temperature control system.
[0017] The level bottle and the reaction tube of the converter are placed in a water bath.
[0018] The absorption bottle contains absorption liquid.
[0019] The absorption bottle is communicated with the test tube, the gas cylinder and the level bottle.
[0020] The utility model provides a test device for the original particle size activity of a catalyst for producing sulfuric acid by oxidation of sulfur dioxide, which has the advantages of small size, low raw gas consumption, small catalyst loading amount and convenient loading and unloading. The unique design can effectively ensure that the temperature, pressure and air velocity of each reaction tube remain consistent, and the converter has good reproducibility, which greatly improves the work efficiency and reduces the labor cost and the waste of raw gas. BRIEF DESCRIPTION OF THE DRAWINGS
[0021] Figure 1 This is a schematic diagram of the connection structure of the original particle size activity test device for sulfur dioxide oxidation to sulfuric acid catalyst embodiment of the utility model.
[0022] In the figure, 1 is an air compressor; 2-1 to 2-2 are flow meters; 3 is a mixer; 4 is a preheater; 5 is a converter; 6-1 to 6-2 are absorption bottles; 7 is a test tube; 8 is a gas cylinder; and 9 is a level bottle. DETAILED DESCRIPTION
[0023] The technical solution of the utility model is described in detail below through specific embodiments and drawings, but the protection scope of the utility model is not limited to the embodiments. Example
[0024] A test device for the original particle size activity of sulfur dioxide oxidation catalyst for sulfuric acid production Figure 1 , mainly including sulfur dioxide conversion system and sulfur dioxide analysis system.
[0025] In the embodiment, refer to the attached Figure 1 The sulfur dioxide conversion system mainly comprises a gas generating device and a gas reaction device which are connected to a raw gas source in sequence through a metal pipe; the gas generating device comprises an air compressor (1), a flow regulating valve and a rotor flow meter (2-1 and 2-1); the gas reaction device comprises a mixer (3), a preheater (4) and a converter (5) which are connected in sequence, and the gas reaction device is equipped with a controllable temperature heating, heat preservation and cooling device; the sulfur dioxide analysis system comprises an absorption bottle (6-1 and 6-2), a test tube (7), a gas cylinder (8) and a level bottle (9), and the absorption bottles (6-1 and 6-2) have internal absorption liquid.
[0026] In the embodiment, the raw gas source is connected to a group of parallel gas reaction devices and gas absorption devices.
[0027] In the embodiment, the sulfur dioxide mixed gas of the raw gas source is connected to the mixer (3) through a flow regulating valve and a rotor flow meter (2-2); the oxygen of the raw gas source is connected to the mixer (3) through an air compressor (1), a flow regulating valve and a rotor flow meter (2-2).
[0028] In the embodiment, a filler and a sample of the original particle size of the catalyst for producing sulfuric acid by oxidation of sulfur dioxide are placed inside the reaction tube of the converter (5); the level bottle (9) and the reaction tube of the converter (5) are placed in a water bath; the absorption bottles (6-1 and 6-1) are connected to the test tube (7), the gas cylinder (8), and the level bottle (9); and the absorption bottles (6-1 and 6-2) are filled with absorption liquid.
[0029] In the embodiment, the temperature-controllable heating, heat preservation and cooling device is a DCS temperature control system (not shown in the figure).
[0030] The sulfur dioxide conversion process of the embodiment is as follows: the mixed gas containing sulfur dioxide from the first inlet of the converter of the sulfuric acid plant is adjusted by the regulating valve, and after being measured by the rotor flowmeter (2-2), it enters the mixer (3) and the air measured by the rotor meter (2-1) respectively. After the gas is fully mixed, it is preheated to a certain temperature by the preheater (4) and enters the converter (5) for a reversible exothermic reaction. At this time, most of SO2 is oxidized to SO3. The mixed gas containing SO2, SO3, etc. after the reaction flows into the system as tail gas after being kept warm. At the same time, sampling analysis is provided at the outlets of the mixer (3) and the converter (5) for analyzing the concentration of sulfur dioxide in the inlet and outlet gases of the converter. The reactor is powered on to increase the temperature, and the heating rate is about 200 ° C / h. When the temperature rises to 200 ° C, air is introduced, and the air velocity is about 2000 h -1 When the temperature rises to 350 ℃ (low temperature type) or 400 ℃ (high temperature type), stop the air flow and start the feed gas (sulfur dioxide and air) instead. The air velocity is about 2000 h -1 Continue to raise the temperature to 600 ℃ (low temperature type) or 700 ℃ (high temperature type) for heat resistance test. After 5 h of heat resistance, reduce the temperature to the activity test temperature at a rate of 200 ℃ / h. After the reactor is cooled, control and adjust the reactor temperature to 410 ℃ (low temperature type) or 485 ℃ (high temperature type), and the raw gas space velocity is 2000 h -1 After 2 h, the volume fraction of sulfur dioxide in the inlet and outlet gases was analyzed and its conversion rate was calculated.
[0031] The sulfur dioxide analysis process of the embodiment is as follows: Measure 10.00 mL of iodine standard titration solution into a test tube (7) with a volume of about 50 mL, add 2 to 3 drops of starch indicator solution, add water to 2 / 3 of the test tube, and the solution is dark blue. Connect the test tube to the rubber stopper with a capillary tube, and after confirming the seal, adjust the sealing liquid in the gas measuring tube so that the liquid level rises to the "0" scale. Open the gas analysis cock to allow the gas to pass into the test tube, and control the gas flow rate to about 300 mL‧min -1 The end point is when the color of the solution in the test tube changes from blue to colorless. Stop ventilation and read Gas tube (8)The volume of the residual gas in the test chamber is recorded, and the room temperature and atmospheric pressure at that time are recorded. The gas volume value is accurate to an integer. The test is performed every 1.5 h to 2.0 h. When the extreme difference of the sulfur dioxide conversion rate in three consecutive analyses is less than or equal to 2.0% (high temperature type) or less than or equal to 3.0% (low temperature type), the test is stopped.
[0032] Application Example 1 Select particle size: original particle size sulfur dioxide oxidation sulfuric acid catalyst sample, filling volume: 3L, raw gas: raw gas composition (volume fraction): sulfur dioxide is (7.0-9.0)%, the rest is air, pressure: normal pressure, air velocity: 2000h -1 The catalyst activity measured under the conditions of heat resistance temperature: 600℃, heat resistance time: 5h, and active temperature 410℃ is recorded as sample1.
[0033] Application Example 2 Select particle size: original particle size sulfur dioxide oxidation sulfuric acid catalyst sample, loading: 3L, raw gas: raw gas composition (volume fraction): sulfur dioxide is (7.0-9.0)%, the rest is air, pressure: normal pressure, air velocity: 2000h -1 The catalyst activity measured under the conditions of heat resistance temperature: 700℃, heat resistance time: 5h, and active temperature 485℃ is recorded as sample2.
[0034] Application Example 3 Select particle size: original particle size sulfur dioxide oxidation to sulfuric acid catalyst sample, loading: 3L, raw gas: raw gas composition (volume fraction): sulfur dioxide is (7.0-9.0)%, the rest is air, pressure: normal pressure, air velocity: 2000h -1 The catalyst activity measured under the conditions of heat resistance temperature: 600℃, heat resistance time: 2h, and active temperature 410℃ is recorded as sample3.
[0035] Application Example 4 Select particle size: original particle size sulfur dioxide oxidation sulfuric acid catalyst sample, loading: 3L, raw gas: raw gas composition (volume fraction): sulfur dioxide is (7.0-9.0)%, the rest is air, pressure: normal pressure, air velocity: 2000h -1 The catalyst activity measured under the conditions of heat resistance temperature: 600℃, heat resistance time: 5h, and active temperature 410℃ is recorded as sample4.
[0036] Application Example 5 Select particle size: original particle size sulfur dioxide oxidation to sulfuric acid catalyst sample, loading: 3L, raw gas: raw gas composition (volume fraction): sulfur dioxide is (7.0-9.0)%, the rest is air, pressure: normal pressure, air velocity: 2000h -1 , heat-resistant temperature: 700℃, heat-resistant time: 2h, and the catalyst activity measured under the conditions of active temperature 485℃ is recorded as sample5.
[0037] Application Example 6 Select particle size: original particle size sulfur dioxide oxidation sulfuric acid catalyst sample, loading: 3L, raw gas: raw gas composition (volume fraction): sulfur dioxide is (7.0-9.0)%, the rest is air, pressure: normal pressure, air velocity: 2000h -1 , heat-resistant temperature: 700℃, heat-resistant time: 5h, the catalyst activity measured under the conditions of active temperature 485℃, is recorded as sample6.
[0038] Application Example 7 Original particle size sulfur dioxide oxidation to sulfuric acid catalyst sample, filling volume: 3L, raw gas: raw gas composition (volume fraction): sulfur dioxide is (7.0-9.0)%, the rest is air, pressure: normal pressure, heat resistance temperature: 700℃, heat resistance time: 5h, active temperature 485℃, space velocity 500h -1 The catalyst activity measured under the conditions is recorded as sample7.
[0039] Application Example 8 Original particle size sulfur dioxide oxidation to sulfuric acid catalyst sample, loading: 3L, raw gas: raw gas composition (volume fraction): sulfur dioxide is (7.0-9.0)%, the rest is air, pressure: normal pressure, heat resistance temperature: 700℃, heat resistance time: 5h, active temperature 485℃, space velocity 1000h -1 The catalyst activity measured under the conditions is recorded as sample8.
[0040] Application Example 9 Sample of catalyst for sulfuric acid production by oxidation of sulfur dioxide with original particle size, loading: 3L, raw gas: raw gas composition (volume fraction): sulfur dioxide is (7.0-9.0)%, the rest is air, pressure: normal pressure, heat-resistant temperature: 600℃, heat-resistant time: 5h, active temperature 410℃, space velocity 2000h -1 The catalyst activity measured under the conditions is recorded as sample9.
[0041] Application Example 10 Original particle size sulfur dioxide oxidation to sulfuric acid catalyst sample, loading: 3L, raw gas: raw gas composition (volume fraction): sulfur dioxide is (7.0-9.0)%, the rest is air, pressure: normal pressure, heat resistance temperature: 600℃, heat resistance time: 5h, active temperature 410℃, space velocity 3000h -1 The catalyst activity measured under the conditions is recorded as sample10.
[0042] The activity data of the catalyst for producing sulfuric acid by oxidation of sulfur dioxide measured in the experiment are shown in Table 1.
[0043] Table 1 Activity of catalysts for sulfur dioxide oxidation to sulfuric acid under different conditions
[0044]
[0045] According to the original particle size activity test device of the sulfur dioxide oxidation sulfuric acid catalyst of the embodiment, the sulfur dioxide oxidation sulfuric acid catalyst products with excellent performance can be quickly screened out, and the device is easy to operate, requires little investment, and runs stably.
Claims
1. A device for testing the original particle size activity of a catalyst for sulfur dioxide oxidation to produce sulfuric acid, characterized in that The device comprises a sulfur dioxide conversion system and a sulfur dioxide analysis system; the sulfur dioxide conversion system comprises a gas generating device and a gas absorbing device which are sequentially connected to a raw gas source; the gas generating device comprises an air compressor, a flow regulating valve and a rotor flowmeter; the gas absorbing device comprises a mixer, a preheater and a converter which are sequentially connected, and the gas absorbing device is equipped with a controllable temperature heating, heat preservation and cooling device; the sulfur dioxide analysis system comprises an absorption bottle, a test tube, a gas cylinder and a level bottle which are sequentially connected to a mixer outlet and a converter outlet.
2. The original particle size activity test device for sulfur dioxide oxidation sulfuric acid catalyst according to claim 1, characterized in that The raw gas source is connected to one or more parallel gas reaction devices and gas absorption devices.
3. The original particle size activity test device for sulfur dioxide oxidation sulfuric acid catalyst according to claim 1, characterized in that The sulfur dioxide mixed gas of the raw gas source is connected to the mixer through a flow regulating valve and a rotor flow meter.
4. The original particle size activity test device for sulfur dioxide oxidation sulfuric acid catalyst according to claim 1, characterized in that The oxygen of the raw gas source is connected to the mixer through an air compressor, a flow regulating valve and a rotor flow meter.
5. The original particle size activity test device for sulfur dioxide oxidation sulfuric acid catalyst according to claim 1, characterized in that The reaction tube of the converter is equipped with fillers and an original particle size sample of the catalyst for producing sulfuric acid by oxidation of sulfur dioxide.
6. The original particle size activity test device for sulfur dioxide oxidation sulfuric acid catalyst according to claim 1, characterized in that The controllable temperature heating, heat preservation and cooling device is a DCS temperature control system.
7. The original particle size activity test device for sulfur dioxide oxidation sulfuric acid catalyst according to claim 1, characterized in that The level bottle and the reaction tube of the converter are placed in a water bath.
8. The original particle size activity test device for sulfur dioxide oxidation sulfuric acid catalyst according to claim 1, characterized in that The absorption bottle contains absorption liquid.
9. The original particle size activity test device for sulfur dioxide oxidation sulfuric acid catalyst according to claim 1, characterized in that The absorption bottle is communicated with the test tube, the gas cylinder and the level bottle.