CN220584142U - Sulfur capacity measuring device of normal temperature zinc oxide desulfurizing agent - Google Patents

Sulfur capacity measuring device of normal temperature zinc oxide desulfurizing agent Download PDF

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CN220584142U
CN220584142U CN202322043555.1U CN202322043555U CN220584142U CN 220584142 U CN220584142 U CN 220584142U CN 202322043555 U CN202322043555 U CN 202322043555U CN 220584142 U CN220584142 U CN 220584142U
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gas
sulfur
absorption
measuring device
desulfurizing agent
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钟立宏
史志刚
李敏
杨爱军
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China Petroleum and Chemical Corp
Sinopec Nanjing Chemical Industry Corp
Research Institute of Sinopec Nanjing Chemical Industry Co Ltd
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China Petroleum and Chemical Corp
Sinopec Nanjing Chemical Industry Corp
Research Institute of Sinopec Nanjing Chemical Industry Co Ltd
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Abstract

The utility model belongs to the technical field of chemical equipment, and relates to a sulfur capacity measuring device of a normal-temperature zinc oxide desulfurizing agent, which is characterized by comprising a sulfur absorbing system and a sulfur analyzing system; the sulfur absorption system comprises a gas reaction device and a gas absorption device which are sequentially connected with a raw material gas source; the gas reaction device comprises a water saturation bottle and a reaction tube which are connected in sequence, and is provided with a temperature-controllable heating and heat-preserving device; the gas absorbing device comprises an absorbing bottle; the sulfur analysis system comprises a quartz tube and an absorption tube which are sequentially connected with an oxygen source, wherein a Gao Wending carbon furnace is arranged outside a magnetic boat arranged in the quartz tube. The utility model has the advantages of small volume, low consumption of raw gas, small filling amount of desulfurizing agent, convenient loading and unloading and the like, the unique design can effectively ensure that the temperature, the pressure and the airspeed of each reaction tube are kept consistent, a plurality of reaction tubes can be arranged for simultaneously detecting a plurality of samples at one time, the parallelism and the reproducibility of the device are ensured, the working efficiency is greatly improved, and the labor cost and the waste of raw gas are reduced.

Description

Sulfur capacity measuring device of normal temperature zinc oxide desulfurizing agent
Technical Field
The utility model belongs to the technical field of chemical equipment, and relates to a sulfur capacity measuring device of a normal-temperature zinc oxide desulfurizing agent.
Background
The industrial gases such as natural gas, refinery gas and synthetic gas contain different kinds of sulfides, generally H 2 In recent years, the content of sulfides in industrial gases has been greatly increased with the increase in the use ratio of inferior crude oil and inferior coal. The presence of these sulfides can have a very adverse effect on the catalysts of the subsequent stages, on the downstream product processing, on the environmental protection and on the corrosion protection of the equipment, and must therefore be removed.
The prior process for removing sulfide has two types of dry method and wet method, and the normal temperature dry desulfurization is paid attention to because of the advantages of simple process, convenient operation, low cost and the like. The normal temperature dry desulfurization is widely applied due to the characteristics of large low temperature sulfur capacity, wide operating temperature range, high desulfurization precision and the like by adopting a normal temperature zinc oxide desulfurizing agent.
The desulfurizing agent has huge market demand and numerous production enterprises. Due to the lack of a unified laboratory desulfurizing agent performance test device, quality disputes existing in production enterprises and users cannot be effectively treated, and uneven product quality in the market is caused.
In order to standardize the market, a unified testing device is established, the effects of standardizing the production and market of the zinc oxide desulfurizing agent and improving the product quality are necessarily achieved, and meanwhile, the following improvement of the product quality and the environmental protection are also positively promoted.
The performance of zinc oxide desulphurants is generally expressed in terms of sulfur capacity; it is related to the self-performance and the reaction condition, and the performance quality is directly related to the stable operation and the product yield of the whole production device. In order to effectively detect the sulfur capacity of the product in a laboratory and rapidly screen out the desulfurizer product with excellent performance, a set of device which is simple and convenient to operate, low in investment and stable in operation needs to be established.
Disclosure of Invention
The utility model provides a sulfur capacity measuring device of a normal-temperature zinc oxide desulfurizing agent, which aims to solve the problems of sulfur capacity inspection and performance evaluation of the normal-temperature zinc oxide desulfurizing agent.
According to the sulfur capacity measuring device for the normal-temperature zinc oxide desulfurizing agent, provided by the utility model, the sulfur capacity test data of the desulfurizing agent are obtained by simulating the industrial application flow of the zinc oxide desulfurizing agent and controlling the test conditions such as the temperature, the pressure, the airspeed and the like of the desulfurizing process. Zinc oxide and hydrogen sulfide or partial organic sulfide react to generate zinc sulfide, so that sulfide in the raw material gas is removed. The sulfur capacity of the desulfurizing agent was calculated by measurement using a combustion neutralization method.
The main technical scheme of the utility model is as follows: the sulfur capacity measuring device of the normal temperature zinc oxide desulfurizer is characterized by comprising a sulfur absorbing system and a sulfur analyzing system; the sulfur absorption system comprises a gas reaction device and a gas absorption device which are sequentially connected with a raw material gas source; the gas reaction device comprises a water saturation bottle and a reaction tube which are connected in sequence, and is provided with a temperature-controllable heating and heat-preserving device; the gas absorbing device comprises an absorbing bottle; the sulfur analysis system comprises a quartz tube and an absorption tube which are sequentially connected with an oxygen source, wherein a Gao Wending carbon furnace is arranged outside a magnetic boat arranged in the quartz tube.
Typically, the source gas source is connected to one or more sets of parallel gas reaction units and gas absorption units.
The raw material gas source is connected with the gas reaction device through a raw material gas valve, a flow regulating valve and a rotameter.
And quartz sand and a desulfurizing agent sample are arranged in the reaction tube.
The temperature-controllable heating and heat-preserving device is a water bath box.
The water saturation bottle and the reaction tube are arranged in a water bath box.
The absorption liquid is arranged in the absorption bottle.
And the oxygen source is connected with the quartz tube through the pressure reducing valve and the rotameter.
The quartz tube is connected with two or more absorption tubes in series.
The sulfur capacity measuring device provided by the utility model has the advantages of small volume, low consumption of raw gas, small filling amount of desulfurizing agent, convenience in loading and unloading and the like, the unique design can effectively ensure that the temperature, the pressure and the airspeed of each reaction tube are kept consistent, a plurality of reaction tubes can be arranged for simultaneously detecting a plurality of samples at one time, the parallelism and the reproducibility of the device are ensured, the working efficiency is greatly improved, and the labor cost and the waste of raw gas are reduced.
Drawings
FIG. 1 is a schematic diagram of a sulfur absorption system of a sulfur capacity measuring device for a normal temperature zinc oxide desulfurizing agent according to an embodiment of the utility model.
Fig. 2 is a schematic diagram of a sulfur analysis system of a sulfur capacity measuring device for a normal temperature zinc oxide desulfurizing agent according to an embodiment of the utility model.
In the figure, 1-a raw material gas valve; 2-1-2-3-rotameter; 3-1 to 3-2-water saturated bottle; 4-1 to 4-2 water bath boxes; 5-1 to 5-2-reaction tubes; 6-1 to 6-2-absorption bottle; 7, an oxygen steel cylinder; 8-a pressure reducing valve; 9-a quartz tube; 10-a high-temperature carbon-fixing furnace; 11-1 to 11-2-absorption tube.
Description of the embodiments
The technical scheme of the present utility model will be described in detail by means of specific embodiments and drawings, but the scope of the present utility model is not limited to the embodiments.
Examples
The sulfur capacity measuring device for normal temperature zinc oxide desulfurizing agent is shown in fig. 1 and 2, and mainly comprises a sulfur absorption system and a sulfur analysis system.
In the embodiment, referring to fig. 1, the sulfur absorption system mainly comprises a gas reaction device and a gas absorption device which are sequentially connected with a raw material gas source through a metal pipe and a flexible hose; the gas reaction device comprises a water saturation bottle and a reaction tube which are connected in sequence, and the gas absorption device comprises an absorption bottle, wherein absorption liquid is arranged in the absorption bottle.
In the embodiment, a raw material air source is respectively connected with two parallel water saturation bottles (3-1-3-2), two reaction tubes (5-1-5-2) and two absorption bottles (6-1-6-2) in sequence through a raw material air valve 1, two flow regulating valves and two rotameters (2-1-2).
In the embodiment, the water saturation bottle (3-1) and the reaction tube (5-1) are arranged in the water bath box (4-1), and the water saturation bottle (3-2) and the reaction tube (5-2) are arranged in the water bath box (4-2).
In the examples, the reaction tube was internally filled with quartz sand and desulfurizing agent samples.
In the embodiment, referring to fig. 2, the sulfur analysis system mainly comprises a quartz tube 9 and an absorption tube which are sequentially connected with an oxygen steel bottle 7 through a pressure reducing valve 8 and a rotameter (2-3), wherein a Gao Wending carbon furnace 10 is arranged outside a magnetic boat in the quartz tube 9, and the quartz tube 9 is connected with two absorption tubes (11-1-11-2) in series.
The sulfur absorption process of the examples is as follows: the sulfur-containing hydrogen sulfide (sulfur mass concentration was (4X 10) from the raw material gas valve (1) -3 ~6×10 -3 )㎏/m 3 ) The mixed gas is metered by a rotameter (2-1, 2-2) (a certain airspeed is controlled), and then enters a water saturation bottle (3-1, 3-2) and a reaction tube (5-1, 5-2) respectively for sulfur absorption reaction, and the gas after sulfur absorption is discharged after passing through an absorption bottle (6-1, 6-2), and the temperatures of the water saturation bottle and the reaction tube are controlled by a water bath box (4-1, 4-2). The water bath was warmed to 40 ℃. Opening a feed gas valve, introducing feed gas, and adjusting and controlling the airspeed to 1000h -1 The system pressure is normal pressure. After several hours, the sulfur mass concentration in the tail gas was started to be measured at 1 hour intervals. If the mass concentration of sulfur in the tail gas is increased, the measurement is changed to 30min or 15min for one time. If the mass concentration of sulfur in the tail gas exceeds 0.4 mug/m for two times 3 When the flow is stopped, the flow is stopped immediatelyAnd (5) material gas. Discharging the sulfur-absorbed sample, removing quartz sand, grinding all the quartz sand into uniform powder, drying at 120 ℃ for 1h, and measuring the sulfur capacity of the desulfurizing agent by a combustion neutralization method.
The sulfur analysis procedure of the examples is as follows: weighing (0.1-0.2 g of sulfur-absorbing and processed sample to 0.0001g, and uniformly placing in a magnetic boat. Heating a Gao Wending carbon furnace to (1050-1100) DEG C, regulating the oxygen flow to 100mL/min, pouring 15mL of hydrogen peroxide solution into each of the two absorption tubes and connecting the two absorption tubes in series at the outlet of the quartz tube, rapidly pushing the magnetic boat into the middle of the quartz tube, plugging the rubber plug immediately, (15-20) min later, taking down the two absorption tubes, pouring the absorption liquid into a 250mL conical flask, and washing the inner wall of the absorption tube. Adding (2-3) bromocresol green-methyl red indicator liquid, and using sodium hydroxide standard titration solution to drop until the red color is changed into light green as an end point.
Application example 1 selecting granularity: 0.425-0.85 mm desulfurizing agent sample, loading: 2.0mL, feed gas: the mass concentration of sulfur in the raw material gas is (4-6) g/m 3 The balance being nitrogen, pressure: atmospheric pressure, airspeed: 1000h -1 Ratio of steam to gas: saturated water vapor at 40 ℃. The sulfur capacity of the desulfurizing agent is measured at the temperature of 20 ℃ and is recorded as sample1.
Application example 2 selecting granularity: 0.425-0.85 mm desulfurizing agent sample, loading: 2.0mL, feed gas: (the mass concentration of sulfur in the raw material gas is (4-6) g/m 3 Nitrogen for the rest), pressure: atmospheric pressure, airspeed: 1000h -1 Ratio of steam to gas: saturated water vapor at 40 ℃. The sulfur capacity of the desulfurizing agent is measured at the temperature of 40 ℃ and is recorded as sample2.
Application example 3 selecting granularity: 0.425-0.85 mm desulfurizing agent sample, loading: 2.0mL, feed gas: (the mass concentration of sulfur in the raw material gas is (4-6) g/m 3 Nitrogen for the rest), pressure: atmospheric pressure, airspeed: 1000h -1 Ratio of steam to gas: saturated water vapor at 40 ℃. The sulfur capacity of the desulfurizing agent is measured at the temperature of 70 ℃ and is recorded as sample3.
Application example 4 selecting granularity: 0.425-0.85 mm desulfurizing agent sample, loading: 2.0mL, feed gas: (the mass concentration of sulfur in the raw material gas is (4-6) g/m 3 Nitrogen for the rest), pressure: atmospheric pressure, steam-gas ratio: saturated water vapor at 40 ℃, temperature: 40 ℃ and the airspeed is changed to 500h -1 The sulfur capacity of the desulfurizing agent is measured under the condition and is recorded as sample4.
Application example 5 selecting granularity: 0.425-0.85 mm desulfurizing agent sample, loading: 2.0mL, feed gas: (the mass concentration of sulfur in the raw material gas is (4-6) g/m 3 Nitrogen for the rest), pressure: atmospheric pressure, steam-gas ratio: saturated water vapor at 40 ℃, temperature: 40 ℃ and the airspeed is changed to 1000h -1 The sulfur capacity of the desulfurizing agent is measured under the condition and is recorded as sample5.
Application example 6 selecting granularity: 0.425-0.85 mm desulfurizing agent sample, loading: 2.0mL, feed gas: (the mass concentration of sulfur in the raw material gas is (4-6) g/m 3 Nitrogen for the rest), pressure: atmospheric pressure, steam-gas ratio: saturated water vapor at 40 ℃, temperature: 40 ℃. Changing airspeed to 2000h -1 The sulfur capacity of the desulfurizing agent is measured under the condition and is recorded as sample6.
Application example 7 selecting granularity: 0.425-0.85 mm desulfurizing agent sample, loading: 2.0mL, feed gas: (the mass concentration of sulfur in the raw material gas is (4-6) g/m 3 Nitrogen for the rest), pressure: atmospheric pressure, airspeed: 1000h -1 Temperature: 40 ℃. The sulfur capacity of the desulfurizing agent is measured under the condition of no water vapor and is recorded as sample7.
Application example 8 selecting granularity: 0.425-0.85 mm desulfurizing agent sample, loading: 2.0mL, feed gas: (the mass concentration of sulfur in the raw material gas is (4-6) g/m 3 Nitrogen for the rest), pressure: atmospheric pressure, airspeed: 1000h -1 Temperature: 40 ℃. The sulfur capacity of the desulfurizing agent is measured under the condition that the steam-gas ratio is 40 ℃ saturated steam, and is recorded as sample8.
The sulfur capacity of the desulfurizing agent is shown in table 1.
TABLE 1 Sulfur capacities of Zinc oxide desulfurizing Agents at Normal temperature under different conditions
Numbering device Reaction temperature, DEG C Reaction space velocity, h -1 Ratio of steam to gas Conversion, percent
Sample1 20 1000 Saturated water vapor at 40 DEG C 8.26
Sample2 40 1000 Saturated water vapor at 40 DEG C 9.97
Sample3 70 1000 Saturated water vapor at 40 DEG C 10.71
Sample4 40 500 Saturated water vapor at 40 DEG C 11.06
Sample5 40 1000 Saturated water vapor at 40 DEG C 10.11
Sample6 40 2000 Saturated water vapor at 40 DEG C 8.32
Sample7 40 1000 - 8.41
Sample8 40 1000 Saturated water vapor at 40 DEG C 10.14
According to the sulfur capacity measuring device of the normal-temperature zinc oxide desulfurizing agent, desulfurizing agent products with excellent performances can be rapidly screened out, and the device is simple and convenient to operate, low in investment and stable in operation.

Claims (8)

1. The sulfur capacity measuring device of the normal-temperature zinc oxide desulfurizing agent is characterized by comprising a sulfur absorbing system and a sulfur analyzing system; the sulfur absorption system comprises a gas reaction device and a gas absorption device which are sequentially connected with a raw material gas source; the gas reaction device comprises a water saturation bottle and a reaction tube which are connected in sequence, and is provided with a temperature-controllable heating and heat-preserving device; the gas absorbing device comprises an absorbing bottle; the sulfur analysis system comprises a quartz tube and an absorption tube which are sequentially connected with an oxygen source, wherein a Gao Wending carbon furnace is arranged outside a magnetic boat arranged in the quartz tube.
2. The sulfur capacity measuring device as claimed in claim 1, wherein the source gas source is connected to one or more of a group of gas reaction means and a group of gas absorption means in parallel.
3. The sulfur capacity measuring device as claimed in claim 1 or 2, wherein the raw gas source is connected to the gas reaction device through a raw gas valve, a flow rate regulating valve, a rotameter.
4. The sulfur capacity measuring device as defined in claim 1, wherein said reaction tube is internally provided with quartz sand and a desulfurizing agent sample.
5. The sulfur capacity measuring device as claimed in claim 1, wherein the temperature controllable heating and heat preserving device is a water bath.
6. The sulfur capacity measuring device as claimed in claim 1 or 5, wherein said water saturated bottle and said reaction tube are placed in a water bath.
7. The sulfur capacity measuring device as defined in claim 1, wherein said absorption bottle contains an absorption liquid.
8. The sulfur capacity measuring device as defined in claim 1, wherein the oxygen source is connected to the quartz tube through a pressure reducing valve and a rotameter.
CN202322043555.1U 2023-08-01 2023-08-01 Sulfur capacity measuring device of normal temperature zinc oxide desulfurizing agent Active CN220584142U (en)

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CN202322043555.1U CN220584142U (en) 2023-08-01 2023-08-01 Sulfur capacity measuring device of normal temperature zinc oxide desulfurizing agent

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