Dimethyl sulfoxide preparation device capable of removing anions

Abstract

The utility model discloses a dimethyl sulfoxide preparation device capable of removing anions, which comprises a reaction unit, a rectification unit and an ion exchange unit, the ion exchange unit comprises a crude sulfoxide buffer tank and a plurality of groups of ion exchangers which are arranged in parallel; a feed port of the ion exchanger is communicated with the crude sulfoxide buffer tank through a crude sulfoxide feeding pump, and a discharge port of the ion exchanger is communicated with the rectification unit; the device further comprises a regenerated liquid buffer tank for containing regenerated liquid. According to the scheme, trace phosphoric acid, nitric acid and sulfate ions contained in the crude sulfoxide prepared by a method for adsorbing hydrogen peroxide through substances such as ion exchange resin, activated carbon and a molecular sieve reduce corrosion to rectification equipment, meanwhile, byproduct sulfone can be further purified in a subsequent rectification system, raw material consumption is reduced, and energy consumption is reduced.

Description

Technical Field

[0001] This utility model belongs to the field of chemical technology, specifically relating to an apparatus for preparing dimethyl sulfoxide. 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, synthetic berberine, 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] Hydrogen peroxide itself is chemically unstable and easily decomposes. Phosphoric acid can react with metal ions (such as iron, copper, and manganese) in hydrogen peroxide to form complexes, thereby reducing the catalytic effect of these metal ions on the decomposition of hydrogen peroxide, allowing hydrogen peroxide to exist more stably and extending its shelf life.

[0004] Phosphoric acid can help control the pH value of hydrogen peroxide systems. A suitable pH range helps hydrogen peroxide perform at its best and can further enhance its stability.

[0005] To improve the stability of hydrogen peroxide and prevent its decomposition, stabilizers containing phosphate or its salts may be added during the production process. These stabilizers can combine with impurities such as metal ions in hydrogen peroxide, inhibiting its decomposition. However, they also leave a certain amount of phosphate, nitric acid, and sulfate ions in the hydrogen peroxide. In the production of dimethyl sulfoxide, these ionic groups not only corrode equipment during distillation, but the high boiling points of the ionic compounds also cause these substances to accumulate in the byproduct dimethyl sulfoxide, making the byproduct difficult to purify and resulting in high raw material consumption. Utility Model Content

[0006] The purpose of this invention is to provide a dimethyl sulfoxide preparation apparatus capable of removing anions, thereby solving the problems in the prior art.

[0007] This utility model is achieved through the following technical solution: a dimethyl sulfoxide preparation device capable of removing anions, comprising a reaction unit and a distillation unit, characterized in that: it further comprises an ion exchange unit; the ion exchange unit includes a crude sulfoxide buffer tank connected to the reaction unit or the distillation unit, and also includes several groups of ion exchangers arranged in parallel; the inlet of the ion exchanger is connected to the crude sulfoxide buffer tank through a crude sulfoxide feed pump, and the outlet of the ion exchanger is connected to the distillation unit; it also includes a regenerated liquid buffer tank for holding the regenerated liquid, the regenerated liquid buffer tank being connected to the regenerated liquid inlet of the ion exchanger through a regenerated liquid feed pump, and the regenerated liquid outlet of the ion exchanger being connected to a wastewater treatment system.

[0008] Furthermore: the ion exchanger has two sets.

[0009] Furthermore, the ion exchanger is internally provided with a filling material for adsorbing ions, which is one or a mixture of ion exchange resin, activated carbon, molecular sieve, activated alumina, and silica gel.

[0010] Furthermore, the regeneration solution is a sodium hydroxide solution or water.

[0011] Furthermore: the distillation unit includes two or more distillation columns.

[0012] Furthermore, the reaction unit includes multiple reactors, which are one of the following: tubular reactors, batch reactors, and microchannel reactors.

[0013] The advantages of this utility model are: 1. Removing trace amounts of phosphoric acid, nitric acid, and sulfate ions from the raw material hydrogen peroxide before distillation reduces corrosion to the distillation equipment;

[0014] 2. Remove trace amounts of phosphoric acid, nitric acid, and sulfate ions from the raw hydrogen peroxide, further purify the by-product sulfone, reduce raw material consumption, and lower energy consumption;

[0015] 3. Using ion exchange resins, activated carbon, and molecular sieves to adsorb phosphate, nitrate, and sulfate ions without introducing other substances reduces the difficulty of purification and waste emissions. Attached Figure Description

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

[0017] Figure 2 This is a schematic diagram of the deionization unit within the distillation unit. Detailed Implementation

[0018] As attached Figure 1-2 As shown, this utility model discloses a dimethyl sulfoxide preparation device capable of removing anions, including a reaction unit 1 and a distillation unit 3, and also includes an ion exchange unit 1;

[0019] The ion exchange unit 2 includes a crude sulfoxide buffer tank 21 connected to the reaction unit or the distillation unit, and also includes several sets of ion exchangers 23 arranged in parallel; the feed inlet of the ion exchanger is connected to the crude sulfoxide buffer tank through a crude sulfoxide feed pump 22, and the discharge outlet of the ion exchanger is connected to the distillation unit.

[0020] It also includes a regenerated liquid buffer tank 24 for holding the regenerated liquid, which is connected to the regenerated liquid inlet of the ion exchanger via a regenerated liquid feed pump 25, and the regenerated liquid outlet of the ion exchanger is connected to the wastewater treatment system.

[0021] Preferably, the ion exchanger has two or three sets, so that while one set is in use, at least one set is in a regeneration or fully regenerated state, ensuring that it can be replaced at any time.

[0022] Preferably, the ion exchanger is provided with a filling material for adsorbing ions, and the filling material is one or a mixture of ion exchange resin, activated carbon, molecular sieve, activated alumina, and silica gel.

[0023] Preferably, the regeneration solution is a sodium hydroxide solution or water, which can neutralize the anions adsorbed by the filler to achieve the regeneration effect.

[0024] Preferably, the distillation unit includes two or more distillation columns, which are connected in series to separate byproducts in the product step by step.

[0025] Preferably, the reaction unit includes multiple reactors, which are one of the following: tubular reactors, batch reactors, microchannel reactors, and other types of reactors.

[0026] The method of using this utility model includes a reaction step, a deionization step, and a distillation step;

[0027] The reaction steps are carried out in the reaction unit, as detailed below:

[0028] S11. The raw materials hydrogen peroxide and sulfide are pumped to a pressure of 0.1~3 MPa.G and then fed into the sulfoxide reaction unit. The reaction pressure is 0.1~3 MPa.G and the temperature is 10~100℃.

[0029] The ion exchange step:

[0030] S21: Crude sulfoxide enters the crude sulfoxide buffer tank, and after being pressurized by the crude sulfoxide feed pump, it enters the ion exchanger;

[0031] S22: Crude sulfoxide undergoes ion exchange with the packing material in the ion exchanger, and the deionized crude sulfoxide after ion exchange is sent to the subsequent process.

[0032] S23: When the crude sulfoxide after passing through the ion exchanger is found to still contain anions such as phosphate, nitrate and sulfate exceeding the specified value, it proves that the packing material in the ion exchanger needs to be regenerated. At this time, the regenerated liquid in the regenerated liquid buffer tank is pressurized by the regenerated liquid feed pump and pumped into the ion exchanger to regenerate the ion exchanger.

[0033] The distillation step:

[0034] S31: Crude sulfoxide is distilled in a sulfoxide delight removal tower. The recovered sulfide obtained at the top of the tower is dehydrated in a three-stage sulfide dehydration tank. The organic phase is returned to the refined sulfide buffer tank and then reintroduced into the reactor to participate in the reaction. The aqueous phase enters the sulfoxide wastewater to the sulfoxide wastewater tower. The concentrated sulfoxide at the bottom of the tower is sent to the sulfoxide dehydration tower for further distillation.

[0035] S32: The sulfoxide dehydration tower top sulfoxide distillation wastewater is sent to the external pipeline network, while the concentrated sulfoxide at the bottom of the tower enters the sulfoxide distillation tower for further distillation.

[0036] S33: Sulfoxide distillation column: Sulfoxide at the top of the column is sent to the finished product storage tank, and sulfoxide at the bottom of the column is sent to the sulfone crystallization vessel.

[0037] S34: The top of the sulfoxide wastewater tower recovers sulfide and sends it to the sulfide buffer tank; the bottom of the tower sends sulfoxide distillation wastewater to the external pipeline network.

[0038] 35: The sulfone solution containing sulfoxide from the bottom of the sulfoxide distillation column is cooled in a sulfoxide crystallizer to precipitate crystals, and then enters a sulfoxide centrifuge. The dimethyl sulfone obtained by centrifugation is bagged, and the mother liquor is sent to a mother liquor storage tank and then pumped to a crude sulfoxide buffer tank. The sulfone solution containing sulfoxide from the bottom of the sulfoxide distillation column can be centrifuged as needed, or it can be used directly as a byproduct without centrifugation.

[0039] Wherein: the ion exchanger operates at a temperature of 10~150℃ and a pressure of 0.1~2 MPaG.

[0040] It should be noted that the structures of the reaction unit and distillation unit in this scheme are existing technologies, and the parts not described in detail are common knowledge. In this scheme, the connections between the various parts are preferably made through pipelines, and necessary control valves and sampling ports are installed on each pipeline.

[0041] In this design, a deionization device is installed after the reactor. Specifically, the deionization device can be installed as needed before distillation (after the reaction unit), between distillation columns (between two adjacent distillation columns), after distillation, and before or after centrifugation (before or after the centrifuge, where the centrifuge is located after the distillation column in the distillation unit). Passing the crude sulfoxide through this device before or during distillation effectively removes trace amounts of phosphoric acid, nitric acid, and sulfate ions introduced by the hydrogen peroxide feedstock. This effectively reduces corrosion of the distillation equipment during the reaction process, lowers the corrosion resistance requirements of the equipment, extends its service life, and reduces the impurity content in the product. The deionization device removes trace amounts of phosphoric acid, nitric acid, and sulfate ions from the reaction products, further purifying the byproduct sulfone, reducing raw material consumption during distillation, lowering energy consumption, and significantly reducing the difficulty of the distillation process. Furthermore, the deionization device uses ion exchange resins, activated carbon, and molecular sieves as packing materials, which adsorb phosphoric acid, nitric acid, and sulfate ions without introducing other substances, reducing purification difficulty and waste emissions.

Claims

1. A dimethyl sulfoxide preparation apparatus capable of removing anions, comprising a reaction unit and a distillation unit, characterized in that: It also includes ion exchange units; The ion exchange unit includes a crude sulfoxide buffer tank connected to the reaction unit or the distillation unit, and also includes several sets of ion exchangers arranged in parallel; the inlet of the ion exchanger is connected to the crude sulfoxide buffer tank through a crude sulfoxide feed pump, and the outlet of the ion exchanger is connected to the distillation unit. It also includes a regenerated liquid buffer tank for holding the regenerated liquid, which is connected to the regenerated liquid inlet of the ion exchanger via a regenerated liquid feed pump, and the regenerated liquid outlet of the ion exchanger is connected to the wastewater treatment system.

2. The apparatus for preparing dimethyl sulfoxide capable of removing anions according to claim 1, characterized in that: There are two sets of ion exchangers.

3. The apparatus for preparing dimethyl sulfoxide capable of removing anions according to claim 1, characterized in that: The ion exchanger is internally filled with a packing material for adsorbing ions, which is one or a mixture of ion exchange resin, activated carbon, molecular sieve, activated alumina, and silica gel.

4. The apparatus for preparing dimethyl sulfoxide capable of removing anions according to claim 1, characterized in that: The regeneration solution is a sodium hydroxide solution or water.

5. The apparatus for preparing dimethyl sulfoxide capable of removing anions according to claim 1, characterized in that: The reaction unit includes multiple reactors, which are one of the following: tubular reactor, batch reactor, and microchannel reactor.

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