Sulfur trioxide assisted sulfonation forward reaction device

Abstract

The utility model relates to the technical field of chemical production devices, and discloses a sulfur trioxide-assisted sulfonation forward reaction device, which comprises a 98 acid storage tank and a refined naphthalene storage tank, the 98 acid storage tank and the refined naphthalene storage tank are connected with a wiped-film cooler, an outlet of the wiped-film cooler is connected with a sulfonation reaction tower, a bottom outlet of the sulfonation reaction tower is connected with a sulfonation liquid metering tank, and the sulfonation liquid metering tank is connected with a liquid storage tank. A sulfonation liquid metering tank is connected into a neutralization reaction kettle, the neutralization reaction kettle is connected with a trapping kettle through a Roots blower, an outlet of the trapping kettle is connected into a tube nest of a normal-pressure contact chamber, a tube nest outlet of the normal-pressure contact chamber is connected with a top inlet of the normal-pressure contact chamber, and a bottom outlet of the normal-pressure contact chamber is connected with an absorption tower. A top spray pipe of the absorption tower is connected with a first branch pipe, a bottom outlet of the absorption tower is connected with the intermediate tank, and the intermediate tank is connected with a top inlet of the sulfonation reaction tower. According to the device, resources can be fully utilized, and environmental pollution is reduced; the generated sulfuric acid can improve the reaction proceeding degree, the raw material conversion rate is increased, and the change of market requirements can be dealt with.

Description

Technical Field

[0001] The utility model relates to the technical field of chemical production devices, in particular to a device for sulfur trioxide-assisted sulfonation forward reaction. Background Art

[0002] The main reaction in the sulfonation section of the 2-naphthol production process is: at 110°C, refined naphthalene reacts with 98 sulfuric acid to produce naphthalenesulfonic acid and water. When the raw material ratio changes, it will affect the product ratio, but when the temperature changes, it has a greater impact on the product structure. For example, at a temperature of 170°C, the output of naphthalenesulfonic acid decreases, and naphthalene disulfonic acid is the main product.

[0003] Changing the reaction parameters can cause changes in product quality, but parameter adjustment has little effect on the raw material conversion rate. This is because the sulfonation reaction is a reversible reaction. Water will be generated during the reaction. On the one hand, the generated water will dilute the sulfuric acid in the reactants and reduce the reaction rate; on the other hand, as the reaction proceeds, the sulfuric acid is gradually reacted and the sulfuric acid concentration gradually decreases until it reaches the equilibrium concentration. The reaction no longer proceeds, resulting in an increase in product by-products and incomplete reaction.

[0004] To separate the reaction water from the product and increase the sulfuric acid concentration to ensure maximum reaction performance, attempts were made to operate the reaction in a negative pressure environment and also to use a dehydrator, but neither was effective. Therefore, sulfonation dehydration became a key point and a pain point in improving the raw material conversion rate. Summary of the Invention

[0005] In order to solve the problems in the current sulfonation process that the raw material conversion rate cannot be further improved by adjusting the reaction conditions, and that the water produced by the reaction is not conducive to the reaction proceeding in the production direction, the utility model provides a device for sulfur trioxide-assisted sulfonation forward reaction in order to further ensure the sulfuric acid concentration so that the reaction proceeds to the maximum extent.

[0006] The utility model is implemented by the following technical solutions:

[0007] A device for sulfur trioxide-assisted sulfonation forward reaction comprises a 98% acid storage tank for storing 98% concentrated sulfuric acid and a refined naphthalene storage tank, the 98% acid storage tank and the refined naphthalene storage tank being connected to a scraped film cooler via a first pipeline and a second pipeline respectively, the outlet of the scraped film cooler being connected to a sulfonation reaction tower, the bottom outlet of the sulfonation reaction tower being connected to a sulfonation liquid metering tank, the sulfonation liquid metering tank being connected to a neutralization reactor, the neutralization reactor being connected to a capture reactor via a Roots blower, the outlet of the capture reactor being connected to a tube array of a normal pressure contact chamber, the tube array outlet of the normal pressure contact chamber being connected to a top inlet of the normal pressure contact chamber, the bottom outlet of the normal pressure contact chamber being connected to an absorption tower, the top spray pipe of the absorption tower being connected to a first branch pipe connected to the first pipeline, the bottom outlet of the absorption tower being connected to an intermediate tank, and the intermediate tank being connected to the top inlet of the sulfonation reaction tower via a third pipeline.

[0008] During implementation, the method comprises a 98 acid storage tank and a refined naphthalene storage tank for storing 98% concentrated sulfuric acid, wherein the 98 acid storage tank and the refined naphthalene storage tank are connected to a scraped film cooler through a first pipeline and a second pipeline respectively, and a preliminary mixing reaction is carried out in the scraped film cooler, a first pump is installed on the first pipeline, the first pipeline is connected to a first branch pipe at the rear of the first pump, and a second pump is installed on the second pipeline; the outlet of the scraped film cooler is connected to a sulfonation reaction tower, specifically, the sulfonation reaction tower comprises a first sulfonation reaction tower and a second sulfonation reaction tower, the bottom outlet of the first sulfonation reaction tower is connected to an upper inlet of the second sulfonation reaction tower, and the bottom outlet of the second sulfonation reaction tower is connected to a sulfonation liquid metering tank; the bottom outlet of the sulfonation reaction tower is connected to a sulfonation liquid metering tank, the top of the sulfonation liquid metering tank is connected to a nitrogen pipe, the sulfonation liquid metering tank is connected to a neutralization reactor, and the neutralization reactor is connected to a Roots reactor. The fan is connected to the capturing kettle, the outlet of the capturing kettle is connected to the tubes of the normal pressure contact chamber, an oxygen branch is connected to the connecting pipeline between the capturing kettle and the tubes of the normal pressure contact chamber, and the tube heat exchange is used to improve the reaction process. The tube outlet of the normal pressure contact chamber is connected to the top inlet of the normal pressure contact chamber, and a catalyst layer is provided above and below the tubes outside the normal pressure contact chamber. The bottom outlet of the normal pressure contact chamber is connected to the absorption tower, and the top spray pipe of the absorption tower is connected to the first branch connected to the first pipeline. The bottom outlet of the absorption tower is connected to the intermediate tank for temporarily storing the fuming sulfuric acid produced in the absorption tower. The intermediate tank is connected to the top inlet of the sulfonation reaction tower through a third pipeline. The third pipeline is installed with an inlet valve. A pressure gauge is installed on the top of the sulfonation reaction tower. The pressure gauge is interlocked with the inlet valve, and the opening and closing of the inlet valve is controlled by monitoring the pressure.

[0009] During use, 98% concentrated sulfuric acid enters the scraped film cooler from the 98 acid storage tank through the first pipeline, and undergoes a preliminary mixing reaction with the refined naphthalene entering the scraped film cooler through the second pipeline. After mixing, it enters the sulfonation reaction tower. The sulfonated liquid after the reaction enters the sulfonation liquid metering tank, is pressed out by nitrogen, enters the neutralization reactor, and enters the neutralization section. The SO2 gas generated in the neutralization reactor is temporarily stored in the capture reactor through a Roots blower. After drying, the SO2 is sent from the bottom to the tubes of the normal pressure contact chamber together with the oxygen from the oxygen branch pipe. After being discharged from the tubes, it enters the top of the normal pressure contact chamber through a pipeline, passes through the catalyst layer located outside the tubes, reacts under the catalyst to generate SO3 and sinks. The reaction exotherm causes heat exchange inside and outside the tubes. In this way, the temperature of the SO2 and O2 entering the atmospheric contact chamber is increased, thereby accelerating the reaction rate, while the temperature of the SO3 decreases and it enters the absorption tower from the bottom. In the absorption tower, the SO3 contacts the 98% concentrated sulfuric acid sprayed from the top, and is reversely absorbed to form fuming sulfuric acid. The 98% concentrated sulfuric acid here comes from the first branch pipe connected to the first pipeline. The fuming sulfuric acid discharged from the bottom of the absorption tower is buffered in the intermediate tank. When the inlet valve interlocked with the sulfonation reaction tower is opened, the fuming sulfuric acid is pumped in from the top of the sulfonation reaction tower. The SO3 in the fuming sulfuric acid encounters the water in the sulfonation reaction tower to form sulfuric acid, thereby reducing the continuous decrease in sulfuric acid concentration. In addition, adjusting parameters such as temperature and raw material ratio is conducive to the forward reaction and the generation of ideal products. The reuse of SO2 ensures environmental protection while improving resource utilization. Converting it to SO3 can also increase the raw material conversion rate. In addition, the addition of DCS ensures the normal operation of industrial production.

[0010] Compared with the prior art, the present invention has the following beneficial effects:

[0011] The utility model provides a device for sulfur trioxide-assisted sulfonation forward reaction, effectively utilizing SO2 generated in the 2-naphthol neutralization stage to oxidize and produce SO3. The SO3 and 98 acid generate fuming sulfuric acid, which is then fed into a sulfonation reaction tower for dehydration to promote the forward reaction. This device cleverly utilizes SO2 to generate SO3, which reacts with the water generated by sulfonation to produce sulfuric acid. This not only fully utilizes resources and reduces environmental pollution, but also enhances the reaction rate and improves the raw material conversion rate. Adjusting parameters based on this can also change product specifications, facilitating responses to changing market demands. BRIEF DESCRIPTION OF THE DRAWINGS

[0012] Figure 1 A schematic structural diagram of the present invention is shown.

[0013] In the figure: 1-98 acid storage tank, 2-refined naphthalene storage tank, 3-first pump, 4-second pump, 5-wiped film cooler, 6-sulfonation reaction tower, 61-first sulfonation reaction tower, 62-second sulfonation reaction tower, 7-sulfonation liquid metering tank, 8-neutralization reactor, 9-Roots blower, 10-capture reactor, 11-normal pressure contact chamber, 111-catalyst layer, 12-absorption tower, 13-intermediate tank, 14-inlet valve; L1-first pipeline, L11-first branch pipe, L2-second pipeline, L3-third pipeline, L4-nitrogen pipe, L5-oxygen branch pipe. DETAILED DESCRIPTION

[0014] The specific embodiments of the present invention will be described below with reference to the accompanying drawings.

[0015] A device for sulfur trioxide-assisted sulfonation forward reaction, such as Figure 1 As shown: comprising a 98 acid storage tank 1 storing 98% concentrated sulfuric acid and a refined naphthalene storage tank 2, the 98 acid storage tank 1 and the refined naphthalene storage tank 2 are connected to a scraped film cooler 5 via a first pipeline L1 and a second pipeline L2, respectively, a preliminary mixing reaction is carried out in the scraped film cooler, a first pump 3 is installed on the first pipeline L1, the first pipeline L1 is connected to a first branch pipe L11 at the rear of the first pump, and a second pump 4 is installed on the second pipeline L2; the outlet of the scraped film cooler 5 is connected to a sulfonation reaction tower 6. In this embodiment, the sulfonation reaction The tower is provided with two, and multiple sulfonation reaction towers can also be connected in series. The sulfonation reaction tower 6 includes a first sulfonation reaction tower 61 and a second sulfonation reaction tower 62. The bottom outlet of the first sulfonation reaction tower 61 is connected to the upper inlet of the second sulfonation reaction tower 62, and the bottom outlet of the second sulfonation reaction tower 62 is connected to the sulfonation liquid metering tank 7; the bottom outlet of the sulfonation reaction tower 6 is connected to the sulfonation liquid metering tank 7, and the top of the sulfonation liquid metering tank 7 is connected to the nitrogen pipe L4. The sulfonation liquid metering tank 7 is connected to the neutralization reactor 8, and the neutralization reactor The reaction kettle 8 is connected to the capturing kettle 10 through a Roots blower 9. The outlet of the capturing kettle 10 is connected to the tubes of the normal pressure contact chamber 11. The connecting pipeline between the capturing kettle 10 and the tubes of the normal pressure contact chamber 11 is connected to an oxygen branch pipe L5. The tube heat exchange is used to improve the reaction process. The tube outlet of the normal pressure contact chamber 11 is connected to the top inlet of the normal pressure contact chamber 11. A catalyst layer 111 is provided above and below the tubes in the normal pressure contact chamber 11. The bottom outlet of the normal pressure contact chamber 11 is connected to the absorption tower 12. The top spray pipe of the absorption tower 12 is connected to the first branch pipe L11 connected to the first pipeline L1. The bottom outlet of the absorption tower 12 is connected to the intermediate tank 13 for temporarily storing the fuming sulfuric acid produced in the absorption tower 12. The intermediate tank 13 is connected to the top inlet of the sulfonation reaction tower 6 through the third pipeline L3. The third pipeline L3 is equipped with an inlet valve 14. A pressure gauge is installed on the top of the sulfonation reaction tower 6. The pressure gauge is interlocked with the inlet valve 14, and the opening and closing of the inlet valve 14 are controlled by monitoring the pressure.

[0016] During use, 98% concentrated sulfuric acid enters the scraped film cooler 5 from the 98 acid storage tank 1 through the first pipeline L1, and undergoes a preliminary mixed reaction with the refined naphthalene entering the scraped film cooler 5 through the second pipeline L2. After mixing, it enters the sulfonation reaction tower 6, and the sulfonated liquid after the reaction enters the sulfonated liquid metering tank 7, is pressed out by nitrogen, enters the neutralization reactor 8, and enters the neutralization section. The SO2 gas generated in the neutralization reactor 8 is temporarily stored in the capture reactor 10 through the Roots blower 9. After drying, the SO2 is sent to the tubes of the normal pressure contact chamber 11 from the bottom together with the oxygen from the oxygen branch pipe L5. After being discharged from the tubes, it enters from the top of the normal pressure contact chamber 11 through a pipeline, passes through the catalyst layer 111 outside the tubes, reacts to generate SO3 under the catalyst and sinks, and the exothermic heat of reaction causes the reaction inside and outside the tubes to Heat exchange occurs, raising the temperature of the SO₂ and O₂ entering atmospheric contact chamber 11, accelerating the reaction rate. The temperature of the SO₃ decreases, allowing it to enter the absorption tower from the bottom. In absorption tower 12, the SO₃ comes into contact with 98% concentrated sulfuric acid sprayed from the top, undergoing reverse absorption to form fuming sulfuric acid. The 98% concentrated sulfuric acid here originates from first branch pipe L11 connected to first pipeline L1. The fuming sulfuric acid discharged from the bottom of absorption tower 12 is buffered in intermediate tank 13. When inlet valve 14, interlocked with sulfonation reactor 6, is opened, fuming sulfuric acid is pumped in from the top of sulfonation reactor 6. The SO₃ in the fuming sulfuric acid reacts with water in sulfonation reactor 6 to form sulfuric acid, thereby reducing the continuous decrease in sulfuric acid concentration. Adjusting parameters such as temperature and raw material ratios facilitates the forward reaction and produces the desired product. SO₂ reuse ensures environmental protection while improving resource utilization, and its conversion to SO₃ also increases raw material conversion.

[0017] The scope of protection claimed by the present invention is not limited to the above specific embodiments. For those skilled in the art, the present invention may have various deformations and changes. Any modifications, improvements and equivalent substitutions made within the concept and principle of the present invention should be included in the scope of protection of the present invention.

Claims

1. A device for sulfur trioxide-assisted sulfonation forward reaction, characterized in that: The invention comprises a 98% acid storage tank (1) for storing 98% concentrated sulfuric acid and a refined naphthalene storage tank (2), wherein the 98% acid storage tank (1) and the refined naphthalene storage tank (2) are connected to a scraped film cooler (5) through a first pipeline (L1) and a second pipeline (L2), respectively, and the outlet of the scraped film cooler (5) is connected to a sulfonation reaction tower (6), and the bottom outlet of the sulfonation reaction tower (6) is connected to a sulfonation liquid metering tank (7), and the sulfonation liquid metering tank (7) is connected to a neutralization reactor (8), and the neutralization reactor (8) is connected to a capture reactor (10) through a Roots blower (9), and the capture reactor (10) is connected to the capture reactor (11). The outlet of the kettle (10) is connected to the tube array of the normal pressure contact chamber (11), the tube array outlet of the normal pressure contact chamber (11) is connected to the top inlet of the normal pressure contact chamber (11), the bottom outlet of the normal pressure contact chamber (11) is connected to the absorption tower (12), the top spray pipe of the absorption tower (12) is connected to the first branch pipe (L11) connected to the first pipeline (L1), the bottom outlet of the absorption tower (12) is connected to the intermediate tank (13), and the intermediate tank (13) is connected to the top inlet of the sulfonation reaction tower (6) through the third pipeline (L3).

2. The device for sulfur trioxide-assisted sulfonation forward reaction according to claim 1, characterized in that: An inlet valve (14) is installed on the third pipeline (L3), and a pressure gauge is installed on the top of the sulfonation reaction tower (6), and the pressure gauge is interlocked with the inlet valve (14).

3. The device for sulfur trioxide-assisted sulfonation forward reaction according to claim 1, characterized in that: A first pump (3) is installed on the first pipeline (L1), the first pipeline (L1) is connected to a first branch pipe (L11) behind the first pump, and a second pump (4) is installed on the second pipeline (L2).

4. The device for sulfur trioxide-assisted sulfonation forward reaction according to claim 1, characterized in that: The top of the sulfonated liquid metering tank (7) is connected to a nitrogen pipe (L4).

5. The device for sulfur trioxide-assisted sulfonation forward reaction according to claim 1, characterized in that: An oxygen branch pipe (L5) is connected to the connecting pipeline between the collection kettle (10) and the tube array of the normal pressure contact chamber (11).

6. The device for sulfur trioxide-assisted sulfonation forward reaction according to claim 1, characterized in that: Catalyst layers (111) are provided above and below the tubes in the atmospheric pressure contact chamber (11).

7. The device for sulfur trioxide-assisted sulfonation forward reaction according to claim 1, characterized in that: The sulfonation reaction tower (6) comprises a first sulfonation reaction tower (61) and a second sulfonation reaction tower (62), wherein the bottom outlet of the first sulfonation reaction tower (61) is connected to the upper inlet of the second sulfonation reaction tower (62), and the bottom outlet of the second sulfonation reaction tower (62) is connected to the sulfonation liquid metering tank (7).

Images