Synthetic reaction device for producing p-toluenesulfonic acid

Abstract

The utility model discloses a synthetic reaction device for producing p-toluenesulfonic acid, and belongs to the technical field of chemical production combination devices and p-toluenesulfonic acid synthesis processes and devices. The device is formed by combining a synthesis reaction kettle, an evaporation pipe, a condenser combination, a continuous water segregator combination, a water phase self-flow controller, a standing water segregator and the like. According to the technical scheme, the synthesis reaction device for producing p-toluenesulfonic acid is characterized in that continuous water separation technologies such as a continuous water separator and a water-phase self-flow controller are introduced in the production process; the standing water segregators which can alternately distribute water and are connected in parallel are designed; according to the technical scheme, the synthetic reaction device for producing the p-toluenesulfonic acid effectively solves the problem of low production efficiency caused by slow water carrying in the process of synthesizing the p-toluenesulfonic acid, and solves the problem of low toluene recovery rate; the device also has the characteristics of convenient operation, safety and reliability.

Description

Technical Field

[0001] This utility model relates to the technical field of chemical production combined equipment and p-toluenesulfonic acid synthesis process and equipment, and in particular to a synthesis reaction device for producing p-toluenesulfonic acid. Background Technology

[0002] p-Toluenesulfonic acid, abbreviated as PTSA, has the molecular formula CH3C6H4SO3H, a molecular weight of 172 (190 when containing one molecule of water of crystallization), and a melting point of 38°C. It is a white, needle-like or powdery crystal, readily soluble in water, extremely deliquescent, and readily decomposes in cotton fabrics, wood, paper, and other carbohydrates. It is a non-oxidizing strong organic acid. p-Toluenesulfonic acid is widely used in high-end electronics, synthetic pharmaceuticals, pesticides, as a stabilizer in polymerization reactions, and as a catalyst in organic synthesis. It is also used as an intermediate in pharmaceuticals and coatings, a resin curing agent, and an electroplating intermediate, making it an important basic chemical raw material.

[0003] p-Toluenesulfonic acid is synthesized from toluene and concentrated sulfuric acid through a sulfonation reaction. From the perspective of the p-toluenesulfonic acid synthesis mechanism, the reaction releases one molecule of water, and the presence of water directly affects the extent of the reaction and the content of p-toluenesulfonic acid. Therefore, during the reaction process, it is necessary to continuously remove and separate water from the reaction system through distillation to accelerate the synthesis of p-toluenesulfonic acid. For the p-toluenesulfonic acid synthesis process, the thoroughness of water removal is crucial to the production process technology. Existing technologies typically use distillation of a toluene-water mixture to remove water from the reaction system, followed by a water separation process. However, due to design flaws in the water separators used in the water removal and separation processes, incomplete water separation can occur, causing some of the removed water to return to the synthesis reactor. This leads to reverse reaction, low production efficiency, high toluene loss, and poor product quality. Summary of the Invention

[0004] To address the aforementioned problems, this utility model discloses a synthetic reaction apparatus for producing p-toluenesulfonic acid. Its innovations include: 1) the introduction of a continuous water separator combination with a fluid disperser and a stabilizing liquid layer; 2) the introduction of a pressure balancing pipe; 3) the introduction of a self-flowing aqueous phase controller; and 4) the installation of a toluene aggregation column at the top of the static water separator. This effectively solves the defects of incomplete water separation in existing technologies and the problem of high toluene loss, which is highly beneficial for safe production, environmental protection, and improved production efficiency.

[0005] The present invention relates to a synthetic reaction apparatus for producing p-toluenesulfonic acid, comprising: a synthetic reaction vessel, a sulfuric acid inlet, a toluene inlet, an evaporator tube, a condenser assembly, a condensate pipeline, a continuous water separator assembly, a fluid disperser, a stabilizing layer, a pressure balancing pipe, an aqueous phase outlet pipe, an aqueous phase gravity flow controller, a siphon breaking pipe, a static water separator A, a toluene aggregation column A, a static water separator B, a toluene aggregation column B, and a main outlet. The evaporator tube is installed directly above the top of the synthetic reaction vessel, and is connected forward to the condenser assembly. The condenser assembly is connected to the condensate pipeline via the condensate pipeline. The system connects to a continuous water distributor assembly, which has two outlets. The upper outlet is connected to a pressure balance pipe, which in turn connects to the synthesis reactor. The lower outlet of the continuous water distributor assembly is connected to a water phase gravity flow controller via a water phase outlet pipe. The top of the water phase gravity flow controller is equipped with a siphon breaking pipe. The water phase gravity flow controller is connected downwards to static water distributors A and B. The top of static water distributor A is equipped with a toluene aggregation column A, and the top of static water distributor B is equipped with a toluene aggregation column B. The lower parts of static water distributors A and B are connected to the main outlet via pipes.

[0006] Preferably, the synthetic reaction apparatus for producing p-toluenesulfonic acid described in this utility model is characterized in that the condenser assembly is made of 904 stainless steel, titanium alloy, or glass-lined material, and consists of two sets of heat exchangers with a heat exchange area of ​​50-100 m². 2 The individual condensers are combined in series, with a total heat exchange area of ​​100-200 m². 2 The purpose of this condenser assembly with a large heat exchange area is to rapidly condense the mixed gas evaporated from the synthesis reactor, thereby minimizing the solubility of toluene in water and facilitating the separation of the toluene phase from the aqueous phase.

[0007] Preferably, the synthetic reaction apparatus for producing p-toluenesulfonic acid described in this utility model is characterized in that the continuous water separator assembly is made of 904 stainless steel, glass-lined material, or titanium alloy, and is composed of two continuous water separators with identical diameter, height, and internal structure connected in series. The upper outlet of the continuous water separator assembly is the toluene phase outlet, and the lower outlet is the aqueous phase outlet.

[0008] Preferably, the synthetic reaction apparatus for producing p-toluenesulfonic acid described in this utility model is characterized in that a liquid stabilizing layer is installed at the upper and lower parts of the continuous water separator assembly, and a fluid disperser is installed in the middle position. The fluid disperser is connected to the condenser assembly externally through a condensate pipe. This design of the fluid disperser and liquid stabilizing layer aims to avoid or reduce large fluctuations in the condensate entering the continuous water separator assembly, thereby facilitating the rapid separation of the toluene phase and the aqueous phase.

[0009] Preferably, the synthetic reaction apparatus for producing p-toluenesulfonic acid described in this utility model is characterized in that the fluid disperser consists of one main pipe and two to four branch pipes, the end of the main pipe is sealed, the branch pipes are perpendicular to the main pipe and on the same plane, and the plane in which the fluid disperser is located is parallel to the cross-section of the oil-water phase separator.

[0010] Preferably, the synthetic reaction apparatus for producing p-toluenesulfonic acid described in this utility model is characterized in that the fluid disperser is made of 904 stainless steel, titanium alloy, or rigid PP material, with a diameter of 25-50 mm, and the surface of the fluid disperser has 50-100 circular holes with a diameter of 5.0-10 mm.

[0011] Preferably, the synthetic reaction apparatus for producing p-toluenesulfonic acid described in this utility model is characterized in that the stabilizing layer is composed of two rigid PP sheets with a thickness of 5-10mm, and four PP support columns with a height of 50-100mm are welded between the two PP sheets. Each PP sheet has 100-200 oblique holes with a diameter of 5.0-10.0mm and an inclination angle of ∠30-60°.

[0012] Preferably, the synthetic reaction apparatus for producing p-toluenesulfonic acid described in this utility model is characterized in that one end of the pressure balance pipe is connected to the toluene phase outlet at the top of the continuous water separator assembly, and the other end is connected to the synthesis reactor. The horizontal height of the pipe connecting to the toluene phase outlet is 400-600 mm higher than the height of the pipe connecting to the synthesis reactor. This design is to facilitate the smooth flow of the toluene phase from the continuous water separator assembly into the pressurized synthesis reactor.

[0013] Preferably, the synthetic reaction apparatus for producing p-toluenesulfonic acid described in this utility model is characterized in that the height, diameter, and internal structure of the settling separator A and settling separator B are identical, with an aqueous phase dispersion tube located in the middle and a wave-damping plate located near the top. The purpose of designing the settling separators A and B for alternating use is to allow sufficient time for toluene to separate from the aqueous phase. The purpose of designing the aqueous phase dispersion tube and the wave-damping plate is to prevent fluctuations in the aqueous phase flowing from the continuous separator assembly into settling separator A or settling separator B, thereby resulting in a relatively higher toluene content in the toluene aggregation column.

[0014] The synthetic reaction apparatus for producing p-toluenesulfonic acid described in this utility model has the following significant beneficial effects: (1) The combination of condensers with a large heat exchange area can quickly condense the evaporated mixed gas, which is more conducive to the rapid separation of the toluene phase and the aqueous phase; (2) The introduction of a continuous water separator with a fluid disperser and a stable liquid layer can effectively promote the rapid separation of the aqueous phase and the toluene phase, which is very beneficial to improving production efficiency; (3) The pressure balance pipe can ensure that the toluene phase is smoothly returned to the synthesis reactor for reciprocating circulation with water; (4) The alternating use of static water separator A and static water separator B can ensure that the small amount of toluene contained in the aqueous phase is recovered and reused to the maximum extent, which is very beneficial to environmental protection and cost reduction. Attached Figure Description

[0015] To more clearly illustrate the technical solutions in the embodiments of this utility model or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments of this utility model. For those skilled in the art, other drawings can be obtained based on these drawings.

[0016] Figure 1 This is a schematic diagram of the structure and process of a synthetic reaction apparatus for producing p-toluenesulfonic acid, as described in an embodiment of the present invention.

[0017] Figure 1 In the middle section: Synthesis reactor 01, sulfuric acid inlet 02, toluene inlet 03, evaporation tube 04, condenser assembly 05, condensate pipeline 51, continuous water separator assembly 06, fluid disperser 61, liquid stabilizer 62, pressure balance tube 07, aqueous phase outlet tube 08, aqueous phase gravity flow controller 09, siphon breaking tube 10, static water separator A11, toluene aggregation column A12, aqueous phase dispersion tube 13, wave-damping plate 14, venting pipe 15, A group toluene collection port 16, static water separator B17, toluene aggregation column B18, B group toluene collection port 19, main outlet 20, steam inlet 21, steam trap 22. Detailed Implementation

[0018] To make the objectives, technical solutions, and advantages of this utility model clearer, the following description is provided in conjunction with... Figure 1 The specific embodiments of this implementation will be further described.

[0019] The specific embodiment of this invention describes a synthetic reaction apparatus for producing p-toluenesulfonic acid, comprising: a synthetic reaction vessel 01, a sulfuric acid inlet 02, a toluene inlet 03, an evaporation pipe 04, a condenser assembly 05, a condensate pipe 51, a continuous water separator assembly 06, a fluid disperser 61, a liquid stabilizer 62, a pressure balancing pipe 07, an aqueous phase outlet pipe 08, an aqueous phase gravity flow controller 09, a siphon breaking pipe 10, a static water separator A11, a toluene aggregation column A12, an aqueous phase dispersion pipe 13, a wave-damping plate 14, a vent pipe 15, a group A toluene collection port 16, a static water separator B17, a toluene aggregation column B18, a group B toluene collection port 19, a main outlet 20, a steam inlet 21, and a steam trap 22.

[0020] Furthermore, in the specific embodiment of this invention, the synthetic reaction apparatus for producing p-toluenesulfonic acid is characterized in that an evaporation tube 04 is installed directly above the top of the synthetic reaction vessel 01. The evaporation tube 04 is connected forward to a condenser assembly 05. The condenser assembly 05 is connected to a continuous water separator assembly 06 via a condensate pipe 51. The continuous water separator assembly 06 has two outlets, with the upper outlet connected to a pressure balancing pipe 07. The pressure balancing pipe 07 is then connected to the synthetic reaction vessel 01, continuously separating water... The lower outlet of the device assembly 06 is connected to the water phase gravity flow controller 09 via the water phase outlet pipe 08. The top of the water phase gravity flow controller 09 is equipped with a siphon breaking pipe 10. The water phase gravity flow controller 09 is connected downward to the static water distributor A11 and the static water distributor B17 respectively. The top of the static water distributor A11 is equipped with a toluene aggregation column A12, and the top of the static water distributor B17 is equipped with a toluene aggregation column B18. The lower parts of the static water distributor A11 and the static water distributor B17 are connected to the main outlet 20 through pipes.

[0021] Furthermore, the synthetic reaction apparatus for producing p-toluenesulfonic acid described in this specific embodiment can be simply described as follows: First, sufficient sulfuric acid and toluene are added to the synthesis reactor 01 according to the proportion and feeding sequence. After the reaction starts, water is continuously generated. The mixed vapor of toluene and water enters the condenser assembly 05 through the evaporator pipe 04. After rapid condensation by the condenser assembly 05, the condensate enters the continuous water separator assembly 06 through the condensate pipe 51 and the fluid disperser 61, and is rapidly separated into toluene phase and water phase. The toluene phase rises and returns to the synthesis reactor 01 through the toluene phase outlet and the pressure balance pipe 07 for repeated evaporation and water removal. The water phase flows downward and flows into the settling water separator A11 and settling water separator B17 in sequence, and is alternately settling for 24 hours. Then, part of the separated toluene is released from the toluene collection column at the top of the settling water separator A11 and settling water separator B17 for recycling. The water phase after separation is transferred to the next process for harmless treatment through the main outlet 20.

[0022] Furthermore, the synthetic reaction apparatus for producing p-toluenesulfonic acid described in this specific embodiment is characterized in that the condenser assembly is made of 904 stainless steel, titanium alloy, or glass-lined material, and consists of two sets of heat exchangers with a heat exchange area of ​​50-100 m². 2 The individual condensers are combined in series, with a total heat exchange area of ​​100-200 m². 2 The purpose of this condenser assembly with a large heat exchange area is to rapidly condense the mixed gas evaporated from the synthesis reactor, thereby minimizing the solubility of toluene in water and facilitating the separation of the toluene phase from the aqueous phase.

[0023] Furthermore, the synthetic reaction apparatus for producing p-toluenesulfonic acid described in this specific embodiment is characterized in that the continuous water separator assembly is made of 904 stainless steel, glass-lined material, or titanium alloy, and is composed of two continuous water separators with identical diameter, height, and internal structure connected in series. The upper outlet of the continuous water separator assembly is the toluene phase outlet, and the lower outlet is the aqueous phase outlet.

[0024] Furthermore, the synthetic reaction apparatus for producing p-toluenesulfonic acid described in this specific embodiment is characterized in that a liquid stabilizing layer is installed at the upper and lower parts of the continuous water separator assembly, and a fluid disperser is installed in the middle position. The fluid disperser is connected to the condenser assembly externally through a condensate pipe. This design of the fluid disperser and liquid stabilizing layer aims to avoid or reduce large fluctuations in the condensate entering the continuous water separator assembly, thereby facilitating the rapid separation of the toluene phase and the aqueous phase.

[0025] Furthermore, the synthetic reaction apparatus for producing p-toluenesulfonic acid described in this specific embodiment is characterized in that the fluid disperser consists of one main pipe and two to four branch pipes, the end of the main pipe is sealed, the branch pipes are perpendicular to the main pipe and on the same plane, and the plane in which the fluid disperser is located is parallel to the cross-section of the oil-water phase separator.

[0026] Furthermore, the synthetic reaction apparatus for producing p-toluenesulfonic acid described in this specific embodiment is characterized in that the fluid disperser is made of 904 stainless steel, titanium alloy, or rigid PP material, with a diameter of 25-50 mm, and the surface of the fluid disperser has 50-100 circular holes with a diameter of 5.0-10 mm.

[0027] Furthermore, the synthetic reaction apparatus for producing p-toluenesulfonic acid described in this specific embodiment is characterized in that the stabilizing layer is composed of two rigid PP sheets with a thickness of 5-10 mm, and four PP support columns with a height of 50-100 mm are welded between the two PP sheets. Each PP sheet has 100-200 oblique holes with a diameter of 5.0-10.0 mm and an inclination angle of ∠30-60°.

[0028] Furthermore, in the specific embodiment of this invention, the synthetic reaction apparatus for producing p-toluenesulfonic acid is characterized in that one end of the pressure balance pipe is connected to the toluene phase outlet at the top of the continuous water separator assembly, and the other end is connected to the synthesis reactor. The horizontal height of the pipe connected to the toluene phase outlet is 400-600 mm higher than the height of the pipe connected to the synthesis reactor. This design is to facilitate the smooth flow of the toluene phase from the continuous water separator assembly into the pressurized synthesis reactor.

[0029] Furthermore, the synthetic reaction apparatus for producing p-toluenesulfonic acid described in this specific embodiment is characterized in that the height, diameter, and internal structure of the settling separator A and settling separator B are identical, with an aqueous phase dispersion tube located in the middle and a wave-damping plate located near the top. The purpose of designing the settling separators A and B for alternating use is to allow sufficient time for toluene to separate from the aqueous phase. The purpose of designing the aqueous phase dispersion tube and the wave-damping plate is to prevent fluctuations in the aqueous phase flowing from the continuous separator assembly into settling separator A or settling separator B, thereby resulting in a relatively higher toluene content in the toluene aggregation column.

[0030] The present invention provides a synthetic reaction apparatus for producing p-toluenesulfonic acid, which has the following significant beneficial effects: (1) The combination of condensers with a large heat exchange area enables the evaporated mixed gas to condense quickly, which is beneficial for the rapid separation of the toluene phase and the aqueous phase; (2) The introduction of a continuous water separator with a fluid disperser and a liquid stabilizer can effectively promote the rapid separation of the aqueous phase and the toluene phase, which is very beneficial for improving production efficiency; (3) The pressure balance pipe can ensure that the toluene phase is smoothly returned to the synthesis reactor for reciprocating circulation with water; (4) The alternating use of static water separator A and static water separator B can ensure that the small amount of toluene contained in the aqueous phase is recovered and reused to the maximum extent, which is very beneficial for environmental protection and cost reduction.

[0031] This device, the synthetic reaction apparatus for producing p-toluenesulfonic acid described in this utility model, is also characterized by convenient operation and safety and reliability.

[0032] Any modifications, equivalent substitutions, or improvements made within the spirit and principles of this utility model shall be included within the protection scope of this utility model. The protection scope of this utility model shall conform to the widest range consistent with the principles and novel features described herein.

Claims

1. A synthetic reaction apparatus for producing p-toluenesulfonic acid, comprising: The reactor comprises a synthesis reactor, a sulfuric acid inlet, a toluene inlet, an evaporator tube, a condenser assembly, a condensate pipeline, a continuous water separator assembly, a fluid disperser, a stabilizing layer, a pressure balancing pipe, an aqueous phase outlet pipe, an aqueous phase gravity flow controller, a siphon breaking pipe, a static water separator A, a toluene agglomerating column A, a static water separator B, a toluene agglomerating column B, and a main outlet. The evaporator tube is installed directly above the top of the synthesis reactor, and it connects forward to the condenser assembly. The condenser assembly is connected to the continuous water separator assembly via a condensate pipeline, continuously distributing water... The unit assembly has two outlets. The upper outlet is connected to a pressure balance pipe, which is then connected to the synthesis reactor. The lower outlet of the continuous water separator assembly is connected to a water phase gravity flow controller via a water phase outlet pipe. A siphon breaking pipe is installed at the top of the water phase gravity flow controller. The water phase gravity flow controller is connected downwards to static water separator A and static water separator B. Toluene aggregation column A is installed at the top of static water separator A, and toluene aggregation column B is installed at the top of static water separator B. The lower parts of static water separator A and static water separator B are connected to the main outlet via pipes.

2. The synthetic reaction apparatus for producing p-toluenesulfonic acid according to claim 1, characterized in that, The condenser assembly is made of 904 stainless steel, titanium alloy, or glass enameling, and consists of two sets of heat exchangers with a heat exchange area of ​​50-100 m². 2 The individual condensers are combined in series, with a total heat exchange area of ​​100-200 m². 2 .

3. The synthetic reaction apparatus for producing p-toluenesulfonic acid according to claim 1, characterized in that, The continuous water distributor assembly is made of 904 stainless steel, glass-lined glass, or titanium alloy. It consists of two continuous water distributors with identical diameter, height, and internal structure connected in series. The upper outlet of the continuous water distributor assembly is the toluene phase outlet, and the lower outlet is the aqueous phase outlet.

4. A synthetic reaction apparatus for producing p-toluenesulfonic acid according to claim 1, characterized in that, The continuous water distributor assembly is equipped with a liquid stabilizing layer at the upper and lower parts, and a fluid disperser at the middle position. The fluid disperser is connected to the condenser assembly through a condensate pipe.

5. The synthetic reaction apparatus for producing p-toluenesulfonic acid according to claim 1, characterized in that, The fluid disperser consists of one main pipe and two to four branch pipes. The end of the main pipe is sealed, and the branch pipes are perpendicular to the main pipe and on the same plane. The plane in which the fluid disperser is located is parallel to the cross-section of the oil-water phase separator.

6. The synthetic reaction apparatus for producing p-toluenesulfonic acid according to claim 1, characterized in that, The fluid disperser is made of 904 stainless steel, titanium alloy, or rigid PP material, with a diameter of 25-50mm. The surface of the fluid disperser has 50-100 circular holes with a diameter of 5.0-10mm.

7. A synthetic reaction apparatus for producing p-toluenesulfonic acid according to claim 1, characterized in that, The liquid-stabilizing layer consists of two rigid PP sheets with a thickness of 5-10mm. Four PP support columns with a height of 50-100mm are welded between the two PP sheets. Each PP sheet has 100-200 oblique holes with a diameter of 5.0-10.0mm and an inclination angle of ∠30-60°.

8. A synthetic reaction apparatus for producing p-toluenesulfonic acid according to claim 1, characterized in that, One end of the pressure balance pipe is connected to the toluene phase outlet at the top of the continuous water separator assembly, and the other end is connected to the synthesis reactor. The horizontal height of the pipe connected to the toluene phase outlet is 400-600mm higher than the horizontal height of the pipe connected to the synthesis reactor.

9. A synthetic reaction apparatus for producing p-toluenesulfonic acid according to claim 1, characterized in that, The static water distributor A and static water distributor B are exactly the same in height, diameter and internal structure. A water phase dispersion pipe is set in the middle of the interior and a wave-damping plate is set in the upper part of the interior.

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