Method and device for preparing insoluble sulfur by using Claus liquid sulfur

Abstract

The invention provides a method and a device for preparing insoluble sulfur by using Claus liquid sulfur, and belongs to the technical field of fine chemicals. The invention provides a method for preparing insoluble sulfur by using Claus liquid sulfur, which comprises the following steps: quenching the Claus liquid sulfur to obtain the insoluble sulfur. According to the method, the insoluble sulfur is prepared from the Claus liquid sulfur, the quality of the prepared insoluble sulfur is equivalent to that of the insoluble sulfur prepared by an existing melting method, low-cost preparation of the insoluble sulfur is realized, energy sources are saved, new choices with higher benefits are provided for related factories and enterprises for recycling sulfur by utilizing the Claus method, and the method is suitable for industrial production. And the original production line is not influenced.

Description

Technical Field

[0001] The invention relates to the technical field of fine chemicals, and in particular to a method and a device for preparing insoluble sulfur by using Claus liquid sulfur. Background Art

[0002] Insoluble sulfur (IS) refers to sulfur that is insoluble in carbon disulfide (CS2). Its scientific name is sulfur homopolymer, also known as polysulfur. Its relative molecular mass is 3200-40000. It is generally used as an advanced accelerator and vulcanizer for rubber, and has a very large market development space.

[0003] The preparation methods of insoluble sulfur disclosed in the prior art require the addition of stabilizers or the heating to 240-280° C., or even the gasification of liquid sulfur to obtain sulfur gas, such as CN1424247A, CN1323026C, and CN111547684A, etc., all of which have the problem of high cost.

[0004] The Claus process is a relatively mature multi-unit processing technology. At present, many oil refineries and gas refineries use the Claus process to treat acid gases and recover sulfur. Compared with other sulfur recovery methods, this method has the advantages of low cost, simple process, and small footprint, so the Claus process is widely used in chemical production. After optimizing and improving the Claus process, its sulfur recovery rate can reach more than 99.4%, greatly reducing the sulfide emissions into the atmosphere and meeting current environmental protection requirements. In the Claus sulfur recovery unit, many condensers are usually set between the Claus reactors to cool the Claus liquid sulfur (high-temperature liquid sulfur), which causes a waste of resources. Summary of the invention

[0005] In view of this, the purpose of the present invention is to provide a method and device for preparing insoluble sulfur using Claus liquid sulfur. The present invention uses Claus sulfur to recover liquid sulfur to prepare insoluble sulfur, which is more convenient and has lower cost. Compared with Claus sulfur recovery, it creates greater economic value, not only adjusts the industrial structure and effectively solves the problem of overcapacity, but also improves economic benefits and promotes economic development. It is of great significance to achieve sustainable economic development and build environmentally friendly and resource-saving enterprises.

[0006] In order to achieve the above-mentioned object of the invention, the present invention provides the following technical solutions:

[0007] The invention provides a method for preparing insoluble sulfur by using Claus liquid sulfur, which comprises the following steps: rapidly cooling the Claus liquid sulfur to obtain insoluble sulfur.

[0008] Preferably, the temperature of the Claus liquid sulfur is 200-350°C.

[0009] Preferably, the rapid cooling temperature is 0-60°C, and the rapid cooling temperature drop rate is 5-50°C / min.

[0010] Preferably, the temperature of the quenched medium is not higher than 90°C.

[0011] Preferably, the quenching medium is water.

[0012] Preferably, a stabilizer is also added during the rapid cooling, and the stabilizer is diphenylethylene or decabromodiphenylethane.

[0013] Preferably, the mass ratio of the Claus liquid sulfur to the stabilizer is 100:0.6.

[0014] Preferably, after the rapid cooling, the obtained solid is further subjected to extraction separation, the extractant for the extraction separation comprises CS2, and the mass ratio of the solid to the extractant is 1:1 to 1:25.

[0015] The present invention also provides a device for preparing insoluble sulfur using Claus liquid sulfur, comprising:

[0016] A combustion furnace, a Claus furnace, a process gas cooler and a Claus reactor connected in sequence;

[0017] The outlet of the Claus reactor is communicated with a process gas cooler and a quench tank respectively, and the quench tank is provided with a Claus liquid sulfur inlet, a discharge port and a circulating cooling device.

[0018] Preferably, an ultrasonic descaling component is also provided on the pipeline of the circulating cooling device.

[0019] The invention provides a method for preparing insoluble sulfur by using Claus liquid sulfur, which comprises the following steps: rapidly cooling the Claus liquid sulfur to obtain insoluble sulfur.

[0020] Compared with the prior art, the present invention has the following beneficial effects:

[0021] The present invention utilizes Claus liquid sulfur to prepare insoluble sulfur. The quality of the prepared insoluble sulfur is equivalent to that of the insoluble sulfur prepared by the existing melting method, and low-cost preparation of insoluble sulfur is achieved, which saves energy and provides a new and more cost-effective option for related factories and enterprises that utilize the Claus method to recover sulfur without affecting the original production line.

[0022] The present invention also provides a device for preparing insoluble sulfur by using Claus liquid sulfur. A branch pipeline for directly flowing out high-temperature liquid sulfur is added to the pipeline from the outlet gas of the Claus reactor to the process gas cooler, and the high-temperature liquid sulfur is directly cooled to a quench tank to be prepared into insoluble sulfur. When sulfur needs to be prepared, the Claus liquid sulfur inlet can be directly closed, and ordinary sulfur can continue to be prepared by using the Claus process. A circulating cooling device is arranged in the quench tank, so that the quench medium evaporated by cooling the high-temperature liquid sulfur returns to the quench tank, and the temperature in the quench tank is maintained within a certain range, and the heat generated by the high-temperature cooling is recycled, thereby further reducing the cost. BRIEF DESCRIPTION OF THE DRAWINGS

[0023] Figure 1 The invention discloses a device for preparing insoluble sulfur by using Claus liquid sulfur, wherein 1 is a combustion furnace, 2 is a Claus furnace, 3 is a process gas cooler, 4 is a Claus reactor, 5 is a discharge port, 6 is a circulating cooling device, 7 is a quench tank, and 8 is a Claus liquid sulfur inlet. DETAILED DESCRIPTION

[0024] The invention provides a method for preparing insoluble sulfur by using Claus liquid sulfur, which comprises the following steps: rapidly cooling the Claus liquid sulfur to obtain insoluble sulfur.

[0025] In the present invention, the temperature of the Claus liquid sulfur is preferably 200-350°C, specifically 200, 250, 300 or 350°C.

[0026] The present invention has no particular limitation on the source of the Claus liquid sulfur, and the liquid stream obtained by the Claus process well known to those skilled in the art can be used.

[0027] In the present invention, the quenching temperature is preferably 0-60°C, specifically 0, 10, 20, 25, 30, 40, 45, 50 or 60°C, and the cooling rate of the quenching is preferably 5-50°C / min, specifically 5, 10, 20, 30, 40 or 50°C / min.

[0028] In the present invention, the temperature of the quenching medium is preferably not higher than 90°C.

[0029] In the present invention, the quenching medium is preferably water.

[0030] In the present invention, the mass ratio of the Claus liquid sulfur to the quenching medium is preferably 1:5 to 1:35, specifically 1:5, 1:15, 1:25 or 1:35.

[0031] In the present invention, a stabilizer is preferably added during the rapid cooling, and the stabilizer is preferably diphenylethylene or decabromodiphenylethane; the stabilizer can improve the conversion rate and stability of insoluble sulfur.

[0032] In the present invention, the mass ratio of the Claus liquid sulfur to the stabilizer is preferably 100:0.15-0.6, specifically 100:0.15, 100:0.25, 100:0.35, 100:0.45, 100:0.55 or 100:0.6.

[0033] In the present invention, the final temperature of the rapid cooling is preferably room temperature.

[0034] In the present invention, after the rapid cooling, the process preferably further comprises extracting and separating the obtained solid (the solid includes insoluble sulfur and soluble sulfur, which is a mixture) to obtain the insoluble sulfur.

[0035] In the present invention, the extractant for extraction and separation preferably includes CS2, and the mass ratio of the solid to the extractant is preferably 1:1 to 1:25, specifically 1:1, 1:3, 1:6, 1:9, 1:12 or 1:25.

[0036] In the present invention, the extraction and separation temperature is preferably 0-30°C, specifically 0, 10, 20 or 30°C, and the extraction and separation time is preferably 20-80 min, specifically 20, 40, 60 or 80 min.

[0037] In the present invention, the extraction and separation preferably also include solidification and pulverization in sequence, the solidification temperature is preferably 30-100°C, the time is preferably 10-40min, specifically 10, 20, 30 or 40min, the solidification is preferably carried out in a vacuum drying oven; the particle size after pulverization is preferably 0.2mm, and the pulverization is preferably carried out with a wall breaking machine.

[0038] In the present invention, the solid is preferably transported away, more preferably scraped away, and the scraping away is preferably carried out using a scraper conveyor, and the speed of the scraper conveyor is preferably 0.03 m / min.

[0039] In the present invention, the rapid cooling is preferably carried out in a rapid cooling tank equipped with a circulating cooling device.

[0040] The present invention also provides a device for preparing insoluble sulfur using Claus liquid sulfur, comprising:

[0041] A combustion furnace, a Claus furnace, a process gas cooler and a Claus reactor connected in sequence;

[0042] The outlet of the Claus reactor is communicated with a process gas cooler and a quench tank respectively, and the quench tank is provided with a Claus liquid sulfur inlet, a discharge port and a circulating cooling device.

[0043] Figure 1The present invention is a device for preparing insoluble sulfur using Claus liquid sulfur, wherein 1 is a combustion furnace, 2 is a Claus furnace, 3 is a process gas cooler, 4 is a Claus reactor, 5 is a discharge port, 6 is a circulating cooling device, 7 is a quench tank, and 8 is a Claus liquid sulfur inlet. Figure 1 The device of the present invention will be described.

[0044] The device of the present invention comprises a combustion furnace 1, a Claus furnace 2, a process gas cooler 3 and a Claus reactor 4 which are connected in sequence. The combustion furnace 1, the Claus furnace 2, the process gas cooler 3 and the Claus reactor 4 are all devices for preparing ordinary sulfur by the Claus process and do not affect the original production line.

[0045] The device of the present invention comprises a quench tank 7, wherein the quench tank 7 is provided with a Claus liquid sulfur inlet 8, a discharge port 5 and a circulating cooling device 6, wherein the circulating cooling device 6 is used to maintain the temperature in the quench tank 7 and to recycle the heat generated by high-temperature cooling.

[0046] In the present invention, the rapid cooling is performed in the rapid cooling tank 7 .

[0047] In the present invention, the quenching tank 7 is filled with a cooling medium.

[0048] The present invention adds a branch pipeline for direct outflow of high-temperature liquid sulfur to the pipeline from the outlet gas of the Claus reactor 4 to the process gas cooler 3 in the Claus sulfur production device, so that the high-temperature liquid sulfur enters the quench tank 7 from the Claus liquid sulfur inlet 8.

[0049] In the present invention, the quench tank 7 is preferably further provided with a stabilizer inlet.

[0050] In the present invention, an ultrasonic descaling component is preferably further provided on the pipeline of the circulating cooling device 6 to prevent the solid obtained after rapid cooling from adhering to the pipeline of the circulating cooling device 6.

[0051] In the present invention, the ultrasonic power of the ultrasonic descaling component is preferably 2-20 kW, specifically 2, 5, 7, 10, 15 or 20 kW.

[0052] In the present invention, a scraper conveyor is preferably also provided in the quenching tank 7 for transporting the solids away. The transport outlet of the scraper conveyor is connected to the discharge port. The scraper conveyor can transfer the quenched solids in time to prevent accumulation in the tank and affect the continuation of the condensation process.

[0053] In the present invention, the speed of the scraper conveyor is preferably 0.03 m / min.

[0054] The technical solutions in the present invention will be described clearly and completely below in conjunction with the embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, not all of them. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0055] The embodiments of the present invention are Figure 1 In the device shown, the quench tank 7 is also provided with a stabilizer inlet and a scraper conveyor, and an ultrasonic descaling component is also provided on the pipeline of the circulating cooling device 6. The ultrasonic power of the ultrasonic descaling component is 7kW, and the speed of the scraper conveyor is 0.03m / min.

[0056] Examples 1 to 12

[0057] Taking Claus high-temperature liquid sulfur as an example, the valve of the branch pipe at the outlet gas of the Claus reactor installed in the Claus sulfur production unit leading to the process gas cooler is opened, so that the high-temperature liquid sulfur is directly passed through the pipe into the quench tank with a circulating water device and a scraper conveyor. The circulating water device will transfer the heat of the quench in time for other channels. The scraper conveyor runs at a speed of 0.03m / min. Add the stabilizer diphenylethylene to the quench tank, control the mass ratio of high-temperature liquid sulfur and cooling water, dry and solidify the obtained mixture of insoluble sulfur and soluble sulfur in a vacuum drying oven at 60℃, and then crush it into particles with an average particle size of 0.2mm using a wall breaker, and then extract and separate it with CS2 to obtain insoluble sulfur.

[0058] The influencing factors of insoluble sulfur content were investigated by orthogonal experiment, and the specific parameters are shown in Table 1. In Table 1, IS content refers to the mass percentage of insoluble sulfur in the mixture. It can be seen that the present invention uses Claus liquid sulfur to prepare insoluble sulfur, realizes the preparation of low-cost insoluble sulfur, saves energy, and provides a new and more efficient option for related factories and enterprises that use Claus process to recover sulfur without affecting the original production line.

[0059] Table 1 Process parameters and test results of Examples 1 to 16

[0060]

[0061]

[0062] The above description is only a preferred embodiment of the present invention and does not limit the present invention in any form. It should be pointed out that for ordinary technicians in this technical field, several improvements and modifications can be made without departing from the principle of the present invention, and these improvements and modifications should also be regarded as the protection scope of the present invention.

Claims

1. A method for preparing insoluble sulfur using Claus liquid sulfur, characterized in that: The following steps are involved: Claus liquid sulfur is quenched to obtain insoluble sulfur.

2. The method according to claim 1, characterized in that The temperature of the Claus liquid sulfur is 200-350°C.

3. The method according to claim 1, characterized in that The rapid cooling temperature is 0-60°C, and the rapid cooling temperature reduction rate is 5-50°C / min.

4. The method according to claim 1 or 3, characterized in that The temperature of the quenching medium is not higher than 90°C.

5. The method according to claim 4, characterized in that The quenching medium is water.

6. The method according to claim 1, characterized in that During the rapid cooling, a stabilizer is added, wherein the stabilizer is diphenylethylene or decabromodiphenylethane.

7. The method according to claim 6, characterized in that The mass ratio of the Claus liquid sulfur to the stabilizer is 100:0.15-0.

6.

8. The method according to claim 1, characterized in that After the rapid cooling, the obtained solid is subjected to extraction and separation, the extractant for the extraction and separation comprises CS2, and the mass ratio of the solid to the extractant is 1:1 to 1:

25.

9. A device for preparing insoluble sulfur using Claus liquid sulfur, characterized in that: include: A combustion furnace, a Claus furnace, a process gas cooler and a Claus reactor connected in sequence; The outlet of the Claus reactor is communicated with a process gas cooler and a quench tank respectively. The quench tank is provided with a Claus liquid sulfur inlet, a discharge port and a circulating cooling device.

10. The device according to claim 9, characterized in that An ultrasonic descaling component is also provided on the pipeline of the circulating cooling device.

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