Production device for producing dimethyl sulfoxide by hydrogen peroxide method

Abstract

The utility model provides a production device for producing dimethyl sulfoxide by a hydrogen peroxide method, and belongs to the technical field of chemical reaction devices. The production device comprises a thioether buffer tank, a hydrogen peroxide buffer tank and a plurality of reaction zones connected in series. According to the scheme, the reaction heat of each main reactor is reduced by feeding dispersed hydrogen peroxide into the plurality of reaction units for reaction, and meanwhile, the material temperature is reduced in the auxiliary reactor, so that the condition that the feeding is influenced by unstable reactor pressure caused by gasification of raw materials in the reactors is prevented.

Description

Technical Field

[0001] This utility model belongs to the technical field of chemical reaction equipment, specifically relating to a production equipment for producing dimethyl sulfoxide by the hydrogen peroxide method. Background Technology

[0002] Dimethyl sulfoxide is an important chemical product widely used in fluorochloroaniline, acrylic fiber, aromatic hydrocarbon extraction, external medicines, nicotinic acid inositol ester, antioxidant 1010, esterification accelerator, traditional Chinese medicine extractant, water-based paint antifreeze, capacitors, tumor treatment, paint remover, trifluoronitrobenzene, sucrose stearate, chlorofiber, paraffin refining, automotive antifreeze in cold regions, autoclave cleaning agents, and pesticide synergists.

[0003] The main production facilities for dimethyl sulfoxide in China use the NO2 oxidation process. This method involves a violent reaction, high energy consumption, and produces sodium nitrate and sodium sulfate as byproducts. Considering the safety issues of transporting N2O4, most companies also have their own NO2 production facilities, making the process cumbersome.

[0004] Traditional hydrogen peroxide oxidation methods mostly use reaction vessels as reactors. This reaction method has a long reaction time, the reaction temperature is difficult to control, and the reaction is incomplete, which brings certain risks to the subsequent distillation process. Utility Model Content

[0005] The purpose of this invention is to provide a production apparatus for producing dimethyl sulfoxide using the hydrogen peroxide method, in order to solve the problems in the prior art.

[0006] This utility model is achieved through the following technical solution:

[0007] A production apparatus for producing dimethyl sulfoxide using the hydrogen peroxide method includes a sulfide buffer tank, a hydrogen peroxide buffer tank, and multiple reaction zones connected in series. Each reaction zone includes a main feed inlet and a main discharge outlet, as well as a main reactor and a secondary reactor connected in series. The inlet of the main reactor is connected to the main feed inlet, and the outlet of the main reactor is connected to the inlet of the secondary reactor. The outlet of the secondary reactor is connected to the main discharge outlet.

[0008] The main feed inlet of the reaction zone is connected to the sulfide buffer tank or the main discharge outlet of the previous reaction zone; the main discharge outlet of the last reaction zone is connected to the discharge cooler.

[0009] The hydrogen peroxide buffer tanks are connected to the main reactors of each reaction zone via hydrogen peroxide booster pumps.

[0010] Furthermore: a sulfide cooler is installed downstream of the sulfide buffer tank; the outlet of the discharge cooler is connected to the sulfide recovery system.

[0011] Furthermore: Cooling systems are installed on both the main reactor and the auxiliary reactor.

[0012] Furthermore, the main reactor and the auxiliary reactor are respectively a microchannel reactor, a tubular reactor, or a fixed-bed reactor.

[0013] The beneficial effects of this utility model are:

[0014] 1. This structure can disperse hydrogen peroxide into multiple reaction units for reaction, reducing the heat of reaction in each reaction unit, ensuring a complete and continuous reaction.

[0015] 2. In this structure, the reactor is divided into three different reaction zones according to the cooling medium. Each reaction zone has a different temperature. The reaction temperature is gradually increased as the concentration of sulfoxide in the product increases, so as to ensure the reaction rate, improve the conversion rate of raw materials, and make the reaction more complete. Attached Figure Description

[0016] Figure 1 This is a schematic diagram of the overall structure of this utility model;

[0017] Figure 2 This is a schematic diagram of the reaction zone structure;

[0018] Figure 3 This is a schematic diagram of the embodiment.

[0019] The numbers in the diagram are explained as follows: 1 is the main feed inlet, 2 is the main discharge outlet, 3 is the hydrogen peroxide booster pump, 4 is the sulfide cooler, 5 is the reaction zone, 6 is the discharge cooler, 7 is the cooling system, 8 is the main reactor, 9 is the auxiliary reactor, 10 is the sulfide buffer tank, 11 is the hydrogen peroxide buffer tank, 12 is the sulfide recovery system, 13 is fresh methyl sulfide, 14 is excess methyl sulfide, and 15 is hydrogen peroxide. Detailed Implementation

[0020] Reference Appendix Figure 1-3 This utility model discloses a production apparatus for producing dimethyl sulfoxide by hydrogen peroxide method, including a sulfide buffer tank 10, a hydrogen peroxide buffer tank 11, and multiple reaction zones 5 connected in series; the reaction zone 5 includes a main feed inlet 1 and a main discharge outlet 2, and also includes a main reactor 8 and a secondary reactor 9 connected in series, the inlet of the main reactor 8 is connected to the main feed inlet, the outlet is connected to the inlet of the secondary reactor 9, and the outlet of the secondary reactor 9 is connected to the main discharge outlet;

[0021] The main feed inlet of the reaction zone is connected to the sulfide buffer tank 10 or the main discharge outlet of the previous reaction zone; the main discharge outlet of the last reaction zone is connected to the discharge cooler 6.

[0022] The hydrogen peroxide buffer tank 11 is connected to the main reactor 8 of each reaction zone via the hydrogen peroxide booster pump 3.

[0023] Preferably, a sulfide cooler 4 is provided downstream of the sulfide buffer tank 10; the outlet of the discharge cooler 6 is connected to the sulfide recovery system 12.

[0024] Preferably, a cooling system 7 is provided on both the main reactor 8 and the auxiliary reactor 9.

[0025] This invention is used to prepare dimethyl sulfoxide by reacting dimethyl sulfide with hydrogen peroxide. In the preparation process, the raw material sulfide is pressurized by a sulfide booster pump in a sulfide buffer tank 10 and then enters a sulfide cooler. After cooling, it enters the reaction zone 5. The raw material hydrogen peroxide is pressurized by a hydrogen peroxide booster pump in a hydrogen peroxide buffer tank 11 and then enters the main reactor of each reaction zone 5.

[0026] The molar ratio of the raw material dimethyl sulfide to the total feed of hydrogen peroxide is 10~1.01:1;

[0027] The raw material sulfide is pressurized by a pump to a pressure of 0.3~3 MPa.G, and its temperature is 0~25℃ after passing through a cooler;

[0028] Reaction temperature: 0~120℃.

[0029] Preferably, the hydrogen peroxide 15 is an aqueous solution of 27.5% to 35% hydrogen peroxide.

[0030] Preferably, the methyl sulfide consists of two parts: fresh methyl sulfide 13 from the front-end process and excess methyl sulfide 14 recovered from the subsequent process.

[0031] Preferably, the amount of hydrogen peroxide added to each reaction zone increases incrementally, and the amount added to the later reaction zone is 1.25-1.5 times that of the previous reaction zone.

[0032] Preferably, the main reactor and the auxiliary reactor are microchannel reactors, tubular reactors, or fixed-bed reactors, respectively.

[0033] Example: This utility model provides a production apparatus for producing dimethyl sulfoxide using the hydrogen peroxide method. By dispersing hydrogen peroxide and feeding it into multiple reaction units, the heat of reaction in each reaction unit is reduced. At the same time, a multi-stage mixer and cooler are used to ensure rapid reaction while removing the heat of reaction, thus better controlling the reaction process.

[0034] The apparatus includes a sulfide buffer tank, a hydrogen peroxide buffer tank, and a sulfoxide reactor. The sulfoxide reactor is a skid-mounted integrated structure, internally containing a sulfide booster pump, a hydrogen peroxide booster pump, a sulfide cooler, three reaction zones, and an outlet cooler. The reaction zones are differentiated according to different reaction temperatures, with each zone consisting of one to four reaction units. Each reaction unit comprises one main reactor and one auxiliary reactor connected in series. A cooling system is installed within each reaction zone to regulate temperature and remove reaction heat. The cooling system can be circulated with various cooling media, including but not limited to chilled water, cryogenic water, circulating water, hot water, and steam.

[0035] The sulfoxide is produced by the reaction of dimethyl sulfide and hydrogen peroxide. The raw material sulfide is pressurized from a sulfide buffer tank by a sulfide booster pump and then enters the sulfide cooler inside the reactor. After cooling, it enters the mixer. The raw material hydrogen peroxide is pressurized from a hydrogen peroxide buffer tank by a hydrogen peroxide booster pump and then enters the reactor according to the sulfide to hydrogen peroxide feed ratio. The sulfide buffer tank and the hydrogen peroxide buffer tank are connected to the sulfoxide reaction unit via a distillation ether booster pump and a hydrogen peroxide booster pump, respectively. The sulfoxide reaction unit is connected to the sulfide recovery system via pipelines.

[0036] The production method of the production device of this utility model includes the following steps:

[0037] S1. The raw material sulfide is pumped to a pressure of 0.3~3 MPa.G and then fed into the sulfide cooler of the sulfoxide reaction unit. After reaching a temperature of 0~25℃, it enters the first-stage main reactor in the first reaction zone. The raw material hydrogen peroxide is pumped to a pressure of 0.3~3 MPa.G and then fed into all the main reactors in the first reaction zone. The amount of hydrogen peroxide entering the main reactors in the first reaction zone accounts for 10~90% of the total hydrogen peroxide feed, and is adjusted according to the different temperatures of each main reactor. The reaction pressure of the main reactors in the first reaction zone is 0.3~3 MPa.G, and the temperature is 10~100℃.

[0038] S2. The material from the first-stage main reactor in the first reaction zone reacts with the raw material hydrogen peroxide and then enters the first-stage auxiliary reactor in the first reaction zone to continue the reaction (reaction pressure 0.3~3Mpa.G, temperature 0~100℃).

[0039] S3. The material from the first-stage auxiliary reactor in the first reaction zone enters the subsequent reaction unit in the first reaction zone, and the above process is repeated until it enters the second reaction zone.

[0040] S4. The operation of the first reaction zone is repeated in the second reaction zone. The amount of hydrogen peroxide entering the main reactor of the second reaction zone accounts for 10-90% of the total hydrogen peroxide feed. The amount is adjusted according to the different temperatures of each main reactor. The reaction pressure of the main reactor in the second reaction zone is 0.3-3 MPa.G and the temperature is 10-100℃. The reaction pressure of the auxiliary reactor is 0.3-3 MPa.G and the temperature is 10-100℃.

[0041] S5. The operation of the first and second reaction zones is repeated in the third reaction zone. The amount of hydrogen peroxide entering the main reactor of the third reaction zone accounts for 10-90% of the total hydrogen peroxide feed. The amount is adjusted according to the different temperatures of each main reactor. The reaction pressure of the main reactor in the third reaction zone is 0.3-3 MPa.G and the temperature is 10-100℃. The reaction pressure of the auxiliary reactor is 0.3-3 MPa.G and the temperature is 10-100℃.

[0042] S6. The material from the third reaction zone enters the discharge cooler at a pressure of 0.3~3 MPa.G and a temperature of 10~100℃, and then goes to the sulfide recovery system.

[0043] Preferably, the sulfoxide reaction apparatus is connected to a utility system, and a regulating valve is provided on the utility pipeline of the reactor within the reaction unit to control the reaction temperature.

[0044] Preferably, the sulfoxide reaction device is connected to a safety relief system, and a safety valve is provided in the reaction unit to ensure reaction safety.

[0045] Preferably, the sulfoxide reaction apparatus is equipped with an internal online detection device to monitor the reaction degree.

[0046] Preferably, in the sulfoxide reaction apparatus, the feed ratio (molar) of the raw material dimethyl sulfide to hydrogen peroxide is (10~1.01):1; the operating temperature is 0~120℃; and the operating pressure is 0.1~5 MPaG.

[0047] Preferably, the methyl sulfide consists of two parts: fresh methyl sulfide from the front-end process and excess methyl sulfide recovered in the subsequent process, and the hydrogen peroxide is an aqueous solution of 27.5% to 35% hydrogen peroxide.

[0048] This invention significantly reduces the heat of reaction in each main reactor by dispersing hydrogen peroxide into multiple reaction units, while simultaneously lowering the material temperature in the auxiliary reactors to prevent the raw materials from vaporizing in the reactors, which could lead to unstable reactor pressure and affect the feeding process.

[0049] By connecting the main reactor and auxiliary reactor in series, the conversion rate within a single reaction unit can be effectively improved, the material temperature reduced, and precise temperature and reaction degree facilitated, effectively solving the problems in existing technologies and ensuring stable load on the reaction unit. Stepped feed rates can effectively guarantee the reaction conversion rate.

Claims

1. A production device for producing dimethyl sulfoxide by hydrogen peroxide method, characterized in that: it comprises a sulfide buffer tank (10), a hydrogen peroxide buffer tank (11) and a plurality of reaction zones (5) connected in series; the reaction zone (5) comprises a main feed port and a main discharge port, and further comprises a main reactor (8) and a secondary reactor (9) connected in series, the inlet of the main reactor (8) is communicated with the main feed port, the outlet is communicated with the inlet of the secondary reactor (9), and the outlet of the secondary reactor (9) is communicated with the main discharge port; the main feed port of the reaction zone is communicated with the sulfide buffer tank (10) or the main discharge port of the previous reaction zone; the main discharge port of the last reaction zone is communicated with a discharge cooler (6); the hydrogen peroxide buffer tank (11) is communicated with the main reactor (8) of each reaction zone through a hydrogen peroxide booster pump (3). A sulfide cooler (4) is arranged downstream of the sulfide buffer tank (10); the outlet of the discharge cooler (6) is communicated with a sulfide recovery system (12). Cooling systems are respectively arranged on the main reactor (8) and the secondary reactor (9). The main reactor and the secondary reactor are respectively micro-channel reactors, tubular reactors or fixed bed reactors.

2. The apparatus for producing dimethyl sulfoxide by hydrogen peroxide method according to claim 1, characterized in that:

2. The production device according to claim 1, characterized in that: the main reactor (8) and the secondary reactor (9) are respectively micro-channel reactors.

3. The apparatus for producing dimethyl sulfoxide by hydrogen peroxide method according to claim 1, characterized in that:

3. The production device according to claim 1, characterized in that: the main reactor (8) and the secondary reactor (9) are respectively tubular reactors.

4. The apparatus for producing dimethyl sulfoxide by hydrogen peroxide method according to claim 1, characterized in that:

4. The production device according to claim 1, characterized in that: the main reactor (8) and the secondary reactor (9) are respectively fixed bed reactors.

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