Dimethyl sulfate synthesis system

By using liquid alkali to react with crude dimethyl ether in a tubular reactor to produce methanol and sodium carboxylate, the problem of equipment blockage caused by formaldehyde polymerization was solved, and the production of high-purity dimethyl ether and process stability were achieved.

CN223717091UActive Publication Date: 2025-12-26HUBEI YUANDA FUCHI PHARMA CHEM +1
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Patent Information

Application Number
CN202422646534.3
Authority / Receiving Office
CN · China
Patent Type
Utility models(China)
Current Assignee / Owner
Filing Date
2024-10-30
Publication Date
2025-12-26
Estimated Expiration
2034-10-30

AI Technical Summary

Technical Problem

In existing technologies, formaldehyde produced during the dehydration of methanol to generate crude dimethyl ether is prone to polymerization, leading to equipment blockage and decreased purity, which affects the stability and continuity of the production process.

Method used

In a tubular reactor, crude dimethyl ether is reacted with liquid alkali to produce methanol and sodium carboxylate. The methanol and sodium carboxylate are then separated by distillation to obtain high-purity dimethyl ether.

Benefits of technology

It effectively removes formaldehyde, improves the purity of dimethyl ether, avoids equipment blockage, and ensures the stability and continuity of the production process.

✦ Generated by Eureka AI based on patent content.

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Abstract

The utility model relates to a system for converting formaldehyde in crude dimethyl ether and a dimethyl sulfate synthesis system, the system comprises a crude dimethyl ether transfer tank, the output end of the crude dimethyl ether transfer tank is provided with a delivery pump; a metering pump is mounted at the output end of the liquid caustic soda tank; and the output end of the tubular reactor is communicated with the delivery pump and the metering pump. In the tubular reactor, formaldehyde in the crude dimethyl ether is effectively disproportionated to generate methanol and sodium carboxylate, high-purity dimethyl ether can be obtained through a subsequent rectification step, and methanol and sodium carboxylate are separated at the same time, so that effective treatment of the crude dimethyl ether and pure extraction of the product are realized. The tubular reactor plays a crucial role, not only provides places and conditions required by disproportionation reaction, but also ensures effective generation and separation of products, and provides powerful support for subsequent dimethyl ether rectification and dimethyl sulfate synthesis.
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Description

TECHNICAL FIELD

[0001] The present application relates to the chemical industry field, in particular to a methanol conversion system in crude dimethyl ether and a dimethyl sulfate synthesis system. BACKGROUND

[0002] Dimethyl sulfate is an organic compound with the chemical formula (CH3O)2SO2, which is a colorless or light yellow transparent liquid, slightly soluble in water, soluble in ethanol, diethyl ether, acetone, etc., mainly used as a methylation reagent, solvent, and also used in organic synthesis of medicine, pesticide, dye, and perfume. The common production process of dimethyl sulfate is the synthesis of dimethyl ether and sulfur trioxide, that is, methanol is first dehydrated to generate dimethyl ether, and then dimethyl ether reacts with sulfur trioxide to synthesize crude dimethyl sulfate, and then refined to obtain dimethyl sulfate product.

[0003] In the related art, methanol is dehydrated to generate crude dimethyl ether, which produces methanol as a byproduct. Methanol is prone to polymerization to form polyformaldehyde, which affects the purity of dimethyl ether and subsequent application. Polyformaldehyde will gradually accumulate and block the condenser and other key equipment. This not only increases the difficulty and cost of equipment maintenance, but also affects the stability and continuity of the entire production process. SUMMARY

[0004] The present application provides a methanol conversion system in crude dimethyl ether and a dimethyl sulfate synthesis system. In the tubular reactor, the methanol in the crude dimethyl ether is effectively disproportionated to generate methanol and sodium carboxylate. Through subsequent rectification steps, high-purity dimethyl ether can be obtained, and methanol and sodium carboxylate can be separated, realizing effective treatment of crude dimethyl ether and pure extraction of products.

[0005] In a first aspect, the embodiments of the present application provide a methanol conversion system in crude dimethyl ether, which comprises:

[0006] A crude dimethyl ether transfer tank, wherein the output end of the crude dimethyl ether transfer tank is provided with a delivery pump;

[0007] A liquid alkali tank, wherein the output end of the liquid alkali tank is provided with a metering pump;

[0008] A tubular reactor, wherein the output end of the tubular reactor is in communication with the delivery pump and the metering pump.

[0009] In a second aspect, the embodiments of the present application provide a dimethyl sulfate synthesis system, which comprises the methanol conversion system in crude dimethyl ether as described above.

[0010] In combination with the second aspect, in an implementation manner, the dimethyl sulfate synthesis system comprises:

[0011] A dimethyl ether rectification column, wherein the input end of the dimethyl ether rectification column is in communication with the output end of the tubular reactor;

[0012] A dimethyl ether condenser, wherein the input end of the dimethyl ether condenser is connected to the output end of the dimethyl ether distillation column;

[0013] The dimethyl ether transfer tank has its input end connected to the output end of the dimethyl ether condenser.

[0014] The container is connected to the output end of the dimethyl ether transfer tank.

[0015] In conjunction with the second aspect, in one embodiment, the container includes:

[0016] Diester tank container;

[0017] The first delivery pipeline has one end connected to the input end of the diester tank container and the other end connected to the output end of the dimethyl ether transfer tank.

[0018] In conjunction with the second aspect, in one embodiment, the delivery pipeline is equipped with a first air-opening valve.

[0019] In conjunction with the second aspect, in one embodiment, the number of the first air-opening valves is three, and the three first air-opening valves are connected in series sequentially.

[0020] In conjunction with the second aspect, in one embodiment, the container includes:

[0021] Ester tank container;

[0022] The second conveying pipeline has one end connected to the input end of the first ester tank container, and the other end connected to the side wall of the first conveying pipeline.

[0023] In conjunction with the second aspect, in one embodiment, the second delivery pipeline is equipped with a second air-opening valve.

[0024] In conjunction with the second aspect, in one embodiment, the container includes:

[0025] Two-suction container;

[0026] The third conveying pipeline has one end connected to the input end of the second suction container, and the other end connected to the side wall of the second conveying pipeline.

[0027] In conjunction with the second aspect, in one embodiment, the delivery pipeline is equipped with a third air-opening valve.

[0028] The beneficial effects of the technical solutions provided in this application include:

[0029] The crude dimethyl ether is stably transported to the tubular reactor by the conveying pump after the crude dimethyl ether transfer tank, the liquid alkali is accurately added into the tubular reactor by the metering pump after the liquid alkali tank, the tubular reactor provides an efficient reaction environment, so that the crude dimethyl ether and the liquid alkali occur disproportionation reaction in the tubular reactor, the formaldehyde in the crude dimethyl ether is effectively disproportionated to generate methanol and sodium carboxylate, high-purity dimethyl ether can be obtained through subsequent rectification steps, and the methanol and the sodium carboxylate are separated, so that the effective treatment of the crude dimethyl ether and the pure extraction of the product are realized. The tubular reactor plays a crucial role, which not only provides a place and conditions required by the disproportionation reaction, but also ensures the effective generation and separation of the product, thereby providing strong support for subsequent dimethyl ether rectification and dimethyl sulfate synthesis. BRIEF DESCRIPTION OF DRAWINGS

[0030] In order to more clearly illustrate the technical solutions in the embodiments of the present application, the following will briefly introduce the drawings needed to be used in the embodiment description. Obviously, the drawings in the following description are only some embodiments of the present application, and other drawings can be obtained by those skilled in the art without any creative effort.

[0031] Figure 1 The structure diagram of the dimethyl sulfate synthesis system.

[0032] In the figure: 1, crude dimethyl ether transfer tank; 2, conveying pump; 3, liquid alkali tank; 4, metering pump; 5, tubular reactor; 6, dimethyl ether rectification column; 7, dimethyl ether condenser; 8, dimethyl ether transfer tank; 9, container; 91, diester tank container; 92, conveying pipeline I; 93, first gas valve; 94, monoester tank container; 95, conveying pipeline II; 96, second gas valve; 97, diabsorption tank container; 98, conveying pipeline III; 99, third gas valve. DETAILED DESCRIPTION

[0033] In order to make the personnel in the technical field better understand the present application, the technical solutions in the embodiments of the present application will be described clearly and completely in the following with reference to the drawings in the embodiments of the present application. Obviously, the described embodiments are only some embodiments of the present application, not all the embodiments. Based on the embodiments in the present application, all other embodiments obtained by those skilled in the art without any creative effort belong to the scope of protection of the present application.

[0034] The crude dimethyl ether methanol conversion system and the dimethyl sulfate synthesis system provided by the embodiments of the present application can effectively convert the methanol in the crude dimethyl ether into methanol and sodium carboxylate in the tubular reactor, high-purity dimethyl ether can be obtained through subsequent rectification steps, and the methanol and the sodium carboxylate are separated, so that the effective treatment of the crude dimethyl ether and the pure extraction of the product are realized.

[0035] Firstly, such as Figure 1 As shown in the figure, this application provides a formaldehyde conversion system in crude dimethyl ether, which includes: a crude dimethyl ether transfer tank 1, the output end of which is equipped with a transfer pump 2; a liquid alkali tank 3, the output end of which is equipped with a metering pump 4; and a tubular reactor 5, the input end of which is connected to the transfer pump 2 and the metering pump 4.

[0036] In this embodiment, crude dimethyl ether is stably delivered to tubular reactor 5 via transfer pump 2 after crude dimethyl ether transfer tank 1. Metering pump 4 after liquid alkali tank 3 ensures that liquid alkali is precisely added to tubular reactor 5 as needed. Tubular reactor 5 provides a highly efficient reaction environment, allowing crude dimethyl ether and liquid alkali to undergo a disproportionation reaction. In tubular reactor 5, formaldehyde in crude dimethyl ether is effectively disproportionated to produce methanol and sodium carboxylate. Through subsequent distillation steps, high-purity dimethyl ether can be obtained, while methanol and sodium carboxylate are separated, achieving efficient processing of crude dimethyl ether and pure extraction of the product. Tubular reactor 5 plays a crucial role, not only providing the necessary environment and conditions for the disproportionation reaction but also ensuring the effective generation and separation of the product, providing strong support for subsequent dimethyl ether distillation and dimethyl sulfate synthesis.

[0037] Secondly, such as Figure 1 As shown in the embodiments of this application, a dimethyl sulfate synthesis system is provided, which includes the formaldehyde conversion system in crude dimethyl ether as described above.

[0038] In conjunction with the second aspect, in one embodiment, the dimethyl sulfate synthesis system includes: a dimethyl ether distillation column 6, the input end of which is connected to the output end of the tubular reactor 5;

[0039] Dimethyl ether condenser 7, the input end of which is connected to the output end of the dimethyl ether distillation column 6; dimethyl ether transfer tank 8, the input end of which is connected to the output end of the dimethyl ether condenser 7; container 9, the container 9 being connected to the output end of the dimethyl ether transfer tank 8.

[0040] In this embodiment, the dimethyl ether distillation column 6 separates dimethyl ether based on the difference in volatility of the substances. Sodium carboxylate and methanol are retained in the bottom residue to ensure product concentration. The dimethyl ether condenser 7 condenses gaseous dimethyl ether into a liquid state for easy storage and transportation. The dimethyl ether transfer tank 8 serves as a temporary storage container to ensure the purity and safety of dimethyl ether. Container 9 is used to receive and store dimethyl ether output from the dimethyl ether transfer tank. This improves the purity of dimethyl ether, meeting subsequent production needs. It ensures the safe storage and transportation of dimethyl ether, reducing environmental pollution. It provides high-quality dimethyl ether feedstock for the synthesis of dimethyl sulfate.

[0041] In combination with the second aspect, in an embodiment, the container 9 comprises: a diester tank container 91; a first conveying pipeline 92, one end of the first conveying pipeline 92 is in communication with the input end of the diester tank container 91, and the other end is in communication with the output end of the dimethyl ether transfer tank 8.

[0042] In this embodiment, the diester tank container 91 is used to store dimethyl ether or other related fluids delivered by the dimethyl ether transfer tank 8. The first conveying pipeline 92 connects the dimethyl ether transfer tank 8 and the diester tank container 91, ensuring smooth delivery of fluids. Through the first conveying pipeline 92, dimethyl ether can be efficiently delivered from the dimethyl ether transfer tank 8 to the diester tank container 91, ensuring the continuity of the production process. The diester tank container 91 provides a safe storage environment for dimethyl ether, preventing fluid leakage and the mixing of external impurities, ensuring product quality. The coordinated operation of the entire system, including the delivery and storage of dimethyl ether, helps to improve production efficiency and reduce production costs.

[0043] In combination with the second aspect, in an embodiment, the first conveying pipeline 92 is installed with a first gas opening valve 93.

[0044] In this embodiment, the first gas opening valve 93 is installed on the first conveying pipeline 92 to control the opening and closing of the pipeline. Through the first gas opening valve 93, the opening and closing of the first conveying pipeline 92 can be easily controlled, and thus the delivery of dimethyl ether can be controlled. In an emergency, the delivery of dimethyl ether can be quickly cut off by closing the first gas opening valve 93 to prevent the accident from expanding. The addition of the first gas opening valve 93 makes the entire conveying system more flexible, and the working state of the conveying pipeline can be adjusted according to production needs.

[0045] In combination with the second aspect, in an embodiment, the number of first gas opening valves 93 is three, and the three first gas opening valves 93 are sequentially connected in series.

[0046] In this embodiment, three first gas opening valves 93 are sequentially connected in series in the first conveying pipeline 92. The series connection of multiple valves can achieve more precise control of fluid flow, and each valve can be independently adjusted to open, thereby more accurately controlling the flow. If one of the valves fails, the other valves can still work, ensuring the continuous operation of the system and improving the reliability of the system. The series connection allows each valve to be independently maintained and replaced, reducing maintenance difficulty and cost.

[0047] In combination with the second aspect, in an embodiment, the container 9 comprises: a monoester tank container 94; a second conveying pipeline 95, one end of the second conveying pipeline 95 is in communication with the input end of the monoester tank container 94, and the other end is in communication with the side wall of the first conveying pipeline 92.

[0048] In this embodiment, the ester tank container 94 is another container for storing fluid, similar to the diester tank container 91. The delivery pipeline two 95 is connected to the input end of the ester tank container 94 at one end and to the side wall of the existing delivery pipeline one 92 at the other end. By adding the ester tank container 94, the system can store more fluid, improving storage capacity and flexibility. The connection of the delivery pipeline two 95 with the delivery pipeline one 92 allows the system to allocate fluid as needed, for example, to deliver dimethyl ether from one pipeline to the container connected by the other pipeline. If the ester tank container 94 stores fluid that reacts or mixes with dimethyl ether, this design can facilitate the mixing of the two fluids, improving production efficiency. When the production process or product formula needs to be changed, this design makes it easier for the system to adapt to new requirements.

[0049] In combination with the second aspect, in an embodiment, the delivery pipeline two 95 is installed with a second gas opening valve 96.

[0050] In this embodiment, the installation of the second gas opening valve 96 allows precise control of the flow of fluid in the delivery pipeline two 95. By adjusting the opening of the valve, the flow rate and flow velocity of the fluid can be adjusted to meet the specific needs of the production process. In emergency situations such as fluid leakage, abnormal pressure, etc., the second gas opening valve 96 can be quickly closed to shut off the fluid flow, preventing the accident from expanding and ensuring the safe operation of the system.

[0051] By reasonably controlling the opening of the second gas opening valve 96, unnecessary fluid waste can be avoided, energy consumption can be reduced, and production efficiency can be improved. The installation position of the second gas opening valve 96 is convenient for inspection and maintenance, and once problems are found, they can be treated in a timely manner to ensure the stable operation of the system. The addition of the second gas opening valve 96 makes the entire fluid delivery system more flexible, allowing the adjustment of the fluid delivery path and flow according to production needs, improving the adaptability and adjustability of the system.

[0052] In combination with the second aspect, in an embodiment, the container 9 comprises: a di- suction tank container 97; a delivery pipeline three 98, one end of the delivery pipeline three 98 is in communication with the input end of the di-suction tank container 97, and the other end is in communication with the side wall of the delivery pipeline two 95.

[0053] In this embodiment, the second suction tank container 97 is a newly added container in the system, used to store fluids for different process stages. The third delivery pipeline 98 is connected to the input end of the second suction tank container 97 at one end, and connected to the side wall of the existing second delivery pipeline 95 at the other end. This design allows fluid to flow between the second suction tank container 97 and the second delivery pipeline 95. By adding the second suction tank container 97, the system can store more types of fluids, or perform different treatments on the fluids, such as cooling, heating, mixing, etc., thereby increasing the functionality and flexibility of the system. The addition of the third delivery pipeline 98 allows fluid to flow between different containers and pipelines, optimizing the fluid flow path and reducing unnecessary delivery distance and energy consumption.

[0054] If the material processed in the second suction tank container 97 is related to the fluid in the second delivery pipeline 95, this design can conveniently combine the two fluids for use, improving production efficiency. The newly added container and pipeline provide a foundation for future expansion of the system, and if more fluid processing or storage functions are needed, they can be easily expanded on this basis.

[0055] In combination with the second aspect, in an embodiment, the third delivery pipeline 98 is installed with a third gas valve 99.

[0056] In this embodiment, the installation of the third gas valve 99 allows the fluid flow in the third delivery pipeline 98 to be precisely controlled. By adjusting the opening of the valve, the flow rate and flow velocity of the fluid can be accurately adjusted to meet specific process requirements. In emergency situations such as fluid leakage, overpressure or underpressure, the third gas valve 99 can respond quickly to shut off the fluid flow, preventing accidents and ensuring safe operation of the system. By properly controlling the opening of the third gas valve 99, waste of fluid can be avoided, energy consumption can be reduced, and the energy efficiency ratio of the entire system can be improved. The installation location of the third gas valve 99 is convenient for workers to perform daily inspection and maintenance. Once the valve fails or needs to be adjusted, it can be promptly handled to ensure normal operation of the system. The addition of the third gas valve 99 makes the fluid delivery system more flexible and variable. According to production needs, the fluid delivery path and flow rate can be flexibly adjusted to improve the adaptability and adjustability of the system. The third gas valve 99 can be connected to an automatic control system to achieve remote control and automatic operation. This not only improves production efficiency, but also reduces errors and risks caused by human operation.

[0057] In the description of the present application, it should be noted that the terms "upper", "lower", and the like are used for indicating the orientation or positional relationship shown in the drawings, and are only for the convenience of describing the present application and simplifying the description, and do not indicate or imply that the devices or elements referred to must have a particular orientation, be constructed and operated in a particular orientation, and therefore cannot be understood as limiting the present application. Unless otherwise explicitly specified and limited, the terms "mounting", "connection", "connecting" should be interpreted broadly, for example, can be fixed connection, can also be detachable connection, or integrally connected; can be mechanical connection, can also be electrical connection; can be directly connected, can also be indirectly connected through an intermediate medium, can be the internal communication of two elements. For those skilled in the art, the specific meaning of the above terms in the present application can be understood according to the specific circumstances.

[0058] It should be noted that in the present application, relational terms such as "first" and "second", and the like are used only to distinguish one entity or operation from another entity or operation, and do not necessarily require or imply that there is any such actual relationship or order between these entities or operations. Moreover, the terms "comprising", "including" or any other variant thereof are intended to cover non-exclusive inclusion, so that a process, method, article or apparatus including a series of elements includes not only those elements, but also other elements not explicitly listed, or other elements inherent in such a process, method, article or apparatus. Without more limitations, the element defined by the statement "comprising a" does not exclude the presence of other identical elements in the process, method, article or apparatus including the element.

[0059] The above is only a specific embodiment of the present application, which enables those skilled in the art to understand or implement the present application. Various modifications to these embodiments will be apparent to those skilled in the art, and the general principles defined herein can be implemented in other embodiments without departing from the spirit or scope of the present application. Therefore, the present application will not be limited to these embodiments shown herein, but will conform to the widest scope consistent with the principles and novel features applied herein.

Claims

1. A dimethyl sulfate synthesis system characterized by, It includes a formaldehyde conversion system in the crude dimethyl ether; The formaldehyde conversion system in the crude dimethyl ether includes, A crude dimethyl ether transfer tank (1) is provided with a delivery pump (2) at its output end; A liquid alkali tank (3) is provided with a metering pump (4) at its output end; A tubular reactor (5) is in communication with the delivery pump (2) and the metering pump (4) at its input end; The dimethyl sulfate synthesis system includes: A dimethyl ether rectification tower (6) is in communication with the output end of the tubular reactor (5) at its input end; A dimethyl ether condenser (7) is in communication with the output end of the dimethyl ether rectification tower (6) at its input end; A dimethyl ether transfer tank (8) is in communication with the output end of the dimethyl ether condenser (7) at its input end; A container (9) is in communication with the output end of the dimethyl ether transfer tank (8).

2. The dimethyl sulfate synthesis system according to claim 1, wherein The container (9) includes: A diester tank container (91); A delivery pipeline I (92) is in communication with the input end of the diester tank container (91) at one end and with the output end of the dimethyl ether transfer tank (8) at the other end.

3. The dimethyl sulfate synthesis system according to claim 2, wherein The delivery pipeline I (92) is provided with a first air opening valve (93).

4. The dimethyl sulfate synthesis system according to claim 3, wherein The number of the first air opening valves (93) is three, and the three first air opening valves (93) are in series communication.

5. The dimethyl sulfate synthesis system according to claim 2, wherein The container (9) includes: A monoester tank container (94); A delivery pipeline II (95) is in communication with the input end of the monoester tank container (94) at one end and with the side wall of the delivery pipeline I (92) at the other end.

6. The dimethyl sulfate synthesis system according to claim 5, wherein The delivery pipeline II (95) is provided with a second air opening valve (96).

7. The dimethyl sulfate synthesis system according to claim 5, wherein The container (9) includes: A di-suction tank container (97); A delivery pipeline III (98) is in communication with the input end of the di-suction tank container (97) at one end and with the side wall of the delivery pipeline II (95) at the other end.

8. The dimethyl sulfate synthesis system according to claim 7, wherein The delivery pipeline III (98) is provided with a third air opening valve (99).