Synthetic reaction device for producing p-toluenesulfonic acid
By introducing technical means such as fluid dispersers, liquid stabilizer layers and pressure balance pipes into the p-toluenesulfonic acid synthesis process, the problem of incomplete water is solved, efficient separation of toluene and the aqueous phase is achieved, and production efficiency and product quality are improved.
Patent Information
- Application Number
- CN202510120587.8
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-01-25
- Publication Date
- 2025-03-28
AI Technical Summary
In the prior art, the water with water in the p-toluenesulfonic acid synthesis process is not thorough, resulting in problems such as large loss of toluene, reverse reaction, low production efficiency and low product quality.
A continuous water distributor combination with a fluid disperser and a stable liquid layer is used, combined with a pressure balance tube and an aqueous phase self-flow controller, and a toluene aggregation column is set up to improve the separation efficiency of toluene and aqueous phase.
It effectively solves the problem of incomplete water carrying, reduces toluene loss, improves production efficiency and product quality, and is also beneficial to production safety and environmental protection.
Smart Images
Figure CN119701842A_ABST
Abstract
Description
Technical Field
[0001] The technical scheme of the present invention belongs to the technical field of chemical production combined device and p-toluenesulfonic acid synthesis process and device, and particularly relates to a synthesis reaction device for producing p-toluenesulfonic acid. Background Art
[0002] p-Toluenesulfonic acid, English abbreviation PTSA, molecular formula CH3C6H4SO3H, molecular weight 172, molecular weight 190 when containing 1 molecule of crystal water, melting point 38 ℃, white needle or powder crystals, easily soluble in water, very easy to deliquesce, easy to make cotton fabrics, wood, paper and other carbohydrates is a non-oxidizing organic strong acid. p-Toluenesulfonic acid is widely used in high-end electronics, synthetic medicine, pesticides, stabilizers for polymerization reactions and catalysts for organic synthesis, as intermediates for medicines and coatings and resin curing agents, and also as electroplating intermediates. It is an important basic chemical raw material.
[0003] p-Toluenesulfonic acid is synthesized by sulfonation reaction of toluene and concentrated sulfuric acid. From the perspective of the synthesis mechanism of p-toluenesulfonic acid, the reaction is to release one molecule of water, and the presence of water directly affects the degree of reaction and the content of p-toluenesulfonic acid. Therefore, it is necessary to continuously distill water and separate water from the reaction system to accelerate the synthesis reaction process of p-toluenesulfonic acid during the reaction process. Relative to the synthesis process of p-toluenesulfonic acid, whether the amount of water is completely taken is the key to the production process technology. The prior art usually uses the method of distilling a mixture of toluene and water to take water out of the reaction system, and then remove the water through a water separation process. Due to the defects in the design technology of the water separator in the process of taking water and separating water, the water separation will not be thorough, resulting in part of the water brought out returning to the synthesis reactor, which will cause the defects of reverse reaction, low production efficiency, large toluene loss and low product quality. Summary of the invention
[0004] In order to solve the above problems, the technical solution of the present invention discloses a synthetic reaction device for producing p-toluenesulfonic acid, and its innovative points include: 1. introducing a continuous water separator combination with a fluid disperser and a stable liquid layer, 2. introducing a pressure balance pipe, 3. introducing a water phase gravity controller, and 4. setting a toluene aggregation column on the top of the static water separator. It effectively solves the defects of incomplete water separation and large toluene loss in the prior art, and is very beneficial to safe production, environmental protection and improving production efficiency.
[0005] The invention discloses a synthesis reaction device for producing p-toluenesulfonic acid, comprising: a synthesis reaction kettle, a sulfuric acid feed port, a toluene feed port, an evaporation tube, a condenser assembly, a condensate pipeline, a continuous water separator assembly, a fluid disperser, a stable liquid layer, a pressure balance tube, an aqueous phase outlet pipe, an aqueous phase gravity controller, a siphon breaker, a static water separator A, a toluene aggregation column A, a static water separator B, a toluene aggregation column B, and a total water outlet, characterized in that an evaporation tube is installed just above the top of the synthesis reaction kettle, the evaporation tube is connected forwardly to the condenser assembly, and the condenser assembly is connected through the condensate pipeline. It is connected to a continuous water separator combination, which has two outlets, the upper outlet is connected to a pressure balance pipe, which is in turn connected to a synthesis reactor, the lower outlet of the continuous water separator combination is connected to a water phase gravity controller through a water phase outlet pipe, a siphon-breaking tube is provided on the top of the water phase gravity controller, the water phase gravity controller is downwardly connected to a static water separator A and a static water separator B respectively, a toluene aggregation column A is provided on the top of the static water separator A, a toluene aggregation column B is provided on the top of the static water separator B, and the lower parts of the static water separator A and the static water separator B are connected to the total water outlet through a pipeline.
[0006] Preferably, the synthesis reaction device for producing p-toluenesulfonic acid described in the technical solution of the present invention is characterized in that the condenser assembly is made of 904 stainless steel or titanium alloy or glass-lined material, and consists of two groups of heat exchange areas of 50-100m 2 The individual condensers are connected in series, with a total heat exchange area of 100-200m 2 The purpose of designing a condenser assembly with a large heat exchange area is to quickly condense the mixed gas evaporated from the synthesis reactor so as to minimize the solubility of toluene in water, thereby facilitating the separation of the toluene phase and the water phase.
[0007] Preferably, a synthetic reaction device for producing p-toluenesulfonic acid described in the technical solution of the present invention is characterized in that the continuous water separator combination is made of 904 stainless steel or glass-lined material or titanium alloy, and is composed of two continuous water separators with exactly the same diameter, height and internal structure combined in series, and the upper outlet of the continuous water separator combination is a toluene phase outlet, and the lower outlet is a water phase outlet.
[0008] Preferably, the synthesis reaction device for producing p-toluenesulfonic acid described in the technical solution of the present invention is characterized in that a stabilizing layer is installed at the upper and lower positions inside the continuous water separator assembly, and a fluid disperser is installed at the middle position, and the fluid disperser is connected to the condenser assembly through a condensate pipeline. The purpose of designing the fluid disperser and the stabilizing layer is to avoid or reduce the large fluctuation of the condensate entering the continuous water separator assembly, which is beneficial to the rapid separation of the toluene phase and the water phase.
[0009] Preferably, a synthetic reaction device for producing p-toluenesulfonic acid described in the technical solution of the present invention is characterized in that the fluid disperser consists of 1 main pipe and 2-4 branch pipes, the end of the main pipe is sealed, the branch pipes are perpendicular to the main pipe and are on the same plane, and the plane where the fluid disperser is located is parallel to the cross section of the oil-water phase separator.
[0010] Preferably, the synthetic reaction device for producing p-toluenesulfonic acid described in the technical solution of the present invention is characterized in that the fluid disperser is made of 904 stainless steel or titanium alloy or hard PP material, with a diameter of 25-50 mm, and 50-100 circular holes with a diameter of 5.0-10 mm are opened on the surface of the fluid disperser.
[0011] Preferably, a synthetic reaction device for producing p-toluenesulfonic acid described in the technical solution of the present invention is characterized in that the stable liquid layer is composed of two hard PP plates 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 plates. Each PP plate has 100-200 inclined holes with a diameter of 5.0-10.0 mm, and the inclination angle of the inclined holes is ∠30-60°.
[0012] Preferably, the synthesis reaction device for producing p-toluenesulfonic acid described in the technical solution of the present invention is characterized in that one end of the pressure balance pipe is connected to the toluene phase outlet on the upper part of the continuous water separator assembly, and the other end is connected to the synthesis reactor, and the horizontal height of the pipeline connected to the toluene phase outlet is 400-600mm higher than the height of the pipeline connected to one end of the synthesis reactor. Such a design is to facilitate the toluene phase from the continuous water separator assembly to flow smoothly into the synthesis reactor with a certain pressure.
[0013] Preferably, a synthetic reaction device for producing p-toluenesulfonic acid described in the technical solution of the present invention is characterized in that the height, diameter and internal structure of the static water separator A and the static water separator B are exactly the same, a water phase dispersion pipe is arranged in the middle position of the interior, and a wave-blocking plate is arranged in the upper position of the interior. The purpose of designing the alternately used static water separator A and static water separator B is to allow toluene sufficient time to separate from the water phase, and the purpose of designing the water phase dispersion pipe and the wave-blocking plate is to prevent the water phase combined from the continuous water separator from fluctuating when flowing into the static water separator A or the static water separator B, thereby making the toluene content in the toluene aggregation column relatively higher.
[0014] The synthetic reaction device for producing p-toluenesulfonic acid described in the technical solution of the present invention has obvious beneficial effects in the following aspects: (1) the condenser combination with a large heat exchange area can quickly condense the evaporated mixed gas, which is beneficial to the rapid separation of the toluene phase and the water phase; (2) the introduction of a continuous water separator combination designed with a fluid disperser and a stable liquid layer can effectively promote the rapid separation of the water phase and the toluene phase, which is very beneficial to improving production efficiency; (3) the provision of a pressure balance pipe can ensure that the toluene phase is smoothly returned to the synthetic reactor for reciprocating circulation with water operation; (4) the provision of a static water separator A and a static water separator B for alternate use can ensure that a small amount of toluene contained in the water phase is recycled and reused to the maximum extent, which is very beneficial to environmental protection and cost reduction. BRIEF DESCRIPTION OF THE DRAWINGS
[0015] In order to more clearly illustrate the embodiments of the technical solutions of the present invention or the technical solutions in the prior art, the drawings required for use in the embodiments or the description of the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention, and for ordinary technicians in this field, other drawings can also be obtained based on these drawings.
[0016] Figure 1 In the figure: synthesis reactor 01, sulfuric acid feed port 02, toluene feed port 03, evaporation tube 04, condenser assembly 05, condensate pipeline 51, continuous water separator assembly 06, fluid disperser 61, stable liquid layer 62, pressure balance tube 07, water phase outlet pipe 08, water phase gravity controller 09, siphon breaker 10, static water separator A11, toluene gathering column A12, water phase dispersion tube 13, wave blocking plate 14, venting tube 15, group A toluene collection port 16, static water separator B17, toluene gathering column B18, group B toluene collection port 19, total water outlet 20, steam inlet 21, steam trap 22. DETAILED DESCRIPTION
[0017] In order to make the purpose, technical solutions and advantages of the present invention clearer, the following Figure 1 This specific implementation example is further described.
[0018] A synthetic reaction device for producing p-toluenesulfonic acid described in an embodiment of the present specific implementation method comprises: a synthetic reaction kettle 01, a sulfuric acid feed port 02, a toluene feed port 03, an evaporation tube 04, a condenser assembly 05, a condensate pipeline 51, a continuous water separator assembly 06, a fluid disperser 61, a stable liquid layer 62, a pressure balance tube 07, an aqueous phase outlet pipe 08, an aqueous phase gravity controller 09, a siphon breaker 10, a stationary water separator A11, a toluene gathering column A12, an aqueous phase dispersion tube 13, a wave-blocking plate 14, a venting pipe 15, a group A toluene collection port 16, a stationary water separator B17, a toluene gathering column B18, a group B toluene collection port 19, a total water outlet 20, a steam inlet 21, and a steam trap 22.
[0019] Furthermore, a synthetic reaction device for producing p-toluenesulfonic acid described in the embodiment of the present specific implementation method is characterized in that an evaporation tube 04 is installed just above the top of the synthetic reaction kettle 01, and the evaporation tube 04 is connected to the condenser assembly 05 forward, and the condenser assembly 05 is connected to the continuous water separator assembly 06 through the condensate pipeline 51, and the continuous water separator assembly 06 is provided with two outlets, and the upper outlet is connected to the pressure balance pipe 07, and the pressure balance pipe 07 is connected to the synthetic reaction kettle 01, and the continuous water separator assembly 06 is provided with two outlets. The lower outlet of the device combination 06 is connected to the water phase gravity flow controller 09 through the water phase outlet pipe 08. A siphon breaking tube 10 is arranged on the top of the water phase gravity flow controller 09. The water phase gravity flow controller 09 is downwardly connected to the static water separator A11 and the static water separator B17 respectively. A toluene aggregation column A12 is arranged on the top of the static water separator A11. A toluene aggregation column B18 is arranged on the top of the static water separator B17. The lower parts of the static water separator A11 and the static water separator B17 are connected to the total water outlet 20 through a pipeline.
[0020] Furthermore, a synthetic reaction device for producing p-toluenesulfonic acid described in the embodiment of the present specific implementation method can be described in a simple manner as follows: first, a sufficient amount of sulfuric acid and toluene are added to the synthetic reactor 01 according to the proportion and the order of addition. After the reaction is started, water will be continuously generated, and the mixed vapor of toluene and water enters the condenser assembly 05 through the evaporation tube 04. After rapid condensation of the condenser assembly 05, the condensate enters the continuous water separator assembly 06 along the condensate pipeline 51 through the fluid disperser 61 and is quickly separated into a toluene phase and a water phase. The toluene phase rises and returns to the synthetic reactor 01 through the toluene phase outlet and the pressure balance pipe 07 to carry out reciprocating evaporation with water; the water phase flows downward and flows into the static water separator A11 and the static water separator B17 in turn, and is alternately left to stand for 24 hours, and then part of the separated toluene is released from the toluene aggregation columns at the top of the static water separator A11 and the static water separator B17 for recycling, and the separated water phase is transferred to the next process through the total water outlet 20 for harmless treatment.
[0021] Furthermore, the synthesis reaction device for producing p-toluenesulfonic acid described in the embodiment of this specific embodiment is characterized in that the condenser assembly is made of 904 stainless steel or titanium alloy or glass-lined material, and consists of two groups of heat exchange areas of 50-100m 2 The individual condensers are connected in series, with a total heat exchange area of 100-200m 2 The purpose of designing a condenser assembly with a large heat exchange area is to quickly condense the mixed gas evaporated from the synthesis reactor so as to minimize the solubility of toluene in water, thereby facilitating the separation of the toluene phase and the water phase.
[0022] Furthermore, a synthetic reaction device for producing p-toluenesulfonic acid described in an embodiment of this specific embodiment is characterized in that the continuous water separator combination is made of 904 stainless steel, glass-lined material or titanium alloy, and is composed of two continuous water separators with exactly the same diameter, height and internal structure combined in series, and the upper outlet of the continuous water separator combination is a toluene phase outlet, and the lower outlet is a water phase outlet.
[0023] Furthermore, a synthetic reaction device for producing p-toluenesulfonic acid described in the embodiment of the present specific implementation is characterized in that a stabilizing layer is installed at the upper and lower positions inside the continuous water separator assembly, and a fluid disperser is installed at the middle position, and the fluid disperser is connected to the condenser assembly through a condensate pipeline. The purpose of designing the fluid disperser and the stabilizing layer is to avoid or reduce the large fluctuation of the condensate entering the continuous water separator assembly, which is beneficial to the rapid separation of the toluene phase and the water phase.
[0024] Furthermore, a synthetic reaction device for producing p-toluenesulfonic acid described in an embodiment of this specific embodiment is characterized in that the fluid disperser consists of 1 main pipe and 2-4 branch pipes, the end of the main pipe is sealed, the branch pipe is perpendicular to the main pipe and on the same plane, and the plane where the fluid disperser is located is parallel to the cross section of the oil-water phase separator.
[0025] Furthermore, a synthetic reaction device for producing p-toluenesulfonic acid described in the embodiment of this specific implementation is characterized in that the fluid disperser is made of 904 stainless steel or titanium alloy or hard PP material, with a diameter of 25-50 mm, and 50-100 circular holes with a diameter of 5.0-10 mm are opened on the surface of the fluid disperser.
[0026] Furthermore, a synthetic reaction device for producing p-toluenesulfonic acid described in an embodiment of this specific embodiment is characterized in that the stabilizing liquid layer is composed of two hard PP plates 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 plates. Each PP plate has 100-200 inclined holes with a diameter of 5.0-10.0 mm, and the inclination angle of the inclined holes is ∠30-60°.
[0027] Furthermore, a synthetic reaction device for producing p-toluenesulfonic acid described in the embodiment of the present specific implementation is characterized in that one end of the pressure balance pipe is connected to the toluene phase outlet on the upper part of the continuous water separator assembly, and the other end is connected to the synthesis reactor, and the horizontal height of the pipeline connected to the toluene phase outlet is 400-600mm higher than the height of the pipeline connected to one end of the synthesis reactor. Such a design is to facilitate the toluene phase from the continuous water separator assembly to flow smoothly into the synthesis reactor with a certain pressure.
[0028] Furthermore, a synthetic reaction device for producing p-toluenesulfonic acid described in the embodiment of this specific embodiment is characterized in that the height, diameter and internal structure of the static water separator A and the static water separator B are exactly the same, a water phase dispersion pipe is arranged in the middle position of the interior, and a wave-blocking plate is arranged in the upper position of the interior. The purpose of designing the alternately used static water separator A and static water separator B is to allow toluene sufficient time to separate from the water phase, and the purpose of designing the water phase dispersion pipe and the wave-blocking plate is to prevent the water phase combined from the continuous water separator from fluctuating when flowing into the static water separator A or the static water separator B, thereby making the toluene content in the toluene aggregation column relatively higher.
[0029] Such a device, a synthesis reaction device for producing p-toluenesulfonic acid described in the technical solution of the present invention, has obvious beneficial effects in the following aspects: (1) the condenser combination with a large heat exchange area can quickly condense the evaporated mixed gas, which is beneficial to the rapid separation of the toluene phase and the water phase; (2) the introduction of a continuous water separator combination designed with a fluid disperser and a stable liquid layer can effectively promote the rapid separation of the water phase and the toluene phase, which is very beneficial to improving production efficiency; (3) the provision of a pressure balance pipe can ensure that the toluene phase is smoothly returned to the synthesis reactor for reciprocating circulation with water operation; (4) the provision of a static water separator A and a static water separator B for alternating use can ensure that the small amount of toluene contained in the water phase is recovered and reused to the maximum extent, which is very beneficial to environmental protection and cost reduction.
[0030] Such a device, a synthetic reaction device for producing p-toluenesulfonic acid described in the technical solution of the present invention, also has the characteristics of convenient operation, safety and reliability.
[0031] Any modification, equivalent substitution, improvement, etc. made within the spirit and principle of the present invention shall be included in the protection scope of the present invention. The protection scope of the present invention is to conform to the widest scope consistent with the principles and novel features described herein.
Claims
1. A synthesis reaction device for producing p-toluenesulfonic acid, comprising: A synthesis reactor, a sulfuric acid feed port, a toluene feed port, an evaporating tube, a condenser assembly, a condensate pipeline, a continuous water separator assembly, a fluid disperser, a stable liquid layer, a pressure balance tube, an aqueous phase outlet pipe, an aqueous phase gravity controller, a siphon breaker, a static water separator A, a toluene aggregation column A, a static water separator B, a toluene aggregation column B, and a total water outlet, characterized in that an evaporating tube is installed just above the top of the synthesis reactor, the evaporating tube is connected forwardly to the condenser assembly, the condenser assembly is connected to the continuous water separator assembly through a condensate pipeline, and the continuous water separator The device combination is provided with two outlets, the upper outlet is connected to the pressure balance pipe, the pressure balance pipe is connected to the synthesis reactor, the lower outlet of the continuous water separator combination is connected to the water phase gravity flow controller through the water phase outlet pipe, the top of the water phase gravity flow controller is provided with a siphon breaking tube, the water phase gravity flow controller is downwardly connected to the static water separator A and the static water separator B respectively, the top of the static water separator A is provided with a toluene aggregation column A, the top of the static water separator B is provided with a toluene aggregation column B, the lower parts of the static water separator A and the static water separator B are connected to the total water outlet through a pipeline.
2. A synthetic reaction device 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-lined material, and consists of two groups with a heat exchange area of 50-100m 2 The individual condensers are connected in series, with a total heat exchange area of 100-200m 2 .
3. A synthetic reaction device for producing p-toluenesulfonic acid according to claim 1, characterized in that: The continuous water separator combination is made of 904 stainless steel, glass-lined material or titanium alloy, and is composed of two continuous water separators with exactly the same diameter, height and internal structure combined in series. The upper outlet of the continuous water separator combination is the toluene phase outlet, and the lower outlet is the water phase outlet.
4. A synthetic reaction device for producing p-toluenesulfonic acid according to claim 1, characterized in that: The upper and lower positions inside the continuous water separator assembly are provided with stabilizing liquid layers, and the middle position is provided with a fluid disperser, which is externally connected to the condenser assembly through a condensate pipeline.
5. A synthetic reaction device for producing p-toluenesulfonic acid according to claim 1, characterized in that: The fluid disperser is composed of a main pipe and 2-4 branch pipes. The end of the main pipe is sealed. The branch pipes are perpendicular to the main pipe and are on the same plane. The plane where the fluid disperser is located is parallel to the cross section of the oil-water phase separator.
6. A synthetic reaction device for producing p-toluenesulfonic acid according to claim 1, characterized in that: The fluid disperser is made of 904 stainless steel or titanium alloy or hard PP material, with a diameter of 25-50 mm, and 50-100 circular holes with a diameter of 5.0-10 mm are opened on the surface of the fluid disperser.
7. A synthetic reaction device for producing p-toluenesulfonic acid according to claim 1, characterized in that: The stabilizing liquid layer is composed of two hard PP plates with a thickness of 5-10 mm, between which four PP support columns with a height of 50-100 mm are welded, and each PP plate has 100-200 inclined holes with a diameter of 5.0-10.0 mm, and the inclined hole inclination angle is ∠30-60°.
8. A synthetic reaction device 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 on the upper part of the continuous water separator assembly, and the other end is connected to the synthesis reactor. The horizontal height of the pipeline connected to the toluene phase outlet is 400-600mm higher than the horizontal height of the pipeline connected to one end of the synthesis reactor.
9. A synthetic reaction device for producing p-toluenesulfonic acid according to claim 1, characterized in that: The height, diameter and internal structure of the static water separator A are completely the same as those of the static water separator B. A water phase dispersion pipe is arranged in the middle of the interior, and a wave-blocking plate is arranged at the upper position of the interior.