A water washing device for triethyl phosphite synthesis

CN224686851UActive Publication Date: 2026-08-28LUOHE XINWANG CHEM CO LTD
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Patent Information

Application Number
CN202521145811.0
Authority / Receiving Office
CN · China
Patent Type
Utility models(China)
Current Assignee / Owner
Filing Date
2025-06-06
Publication Date
2026-08-28
Estimated Expiration
2035-06-06

AI Technical Summary

Technical Problem

[0003]目前,传统的水洗设备大多采用简单的搅拌反应釜式结构,在水洗过程中,存在着以下问题:首先,合成完的物料水洗因为涉及到缚酸剂的盐酸盐与碱的反应会产生大量放热现象,会造成亚磷酸三乙酯的水解;其次,合成完的物料与碱水的混合不均匀,导致水洗效率低下,难以充分去除杂质;再次,水洗后水相和有机相的分离效果不佳,容易造成产品的损失和后续干燥处理需要大量的干燥剂的困难

Benefits of technology

本实用新型使用高效的水洗反应器水洗,传热效果好,能够使物料与水充分混合,提高水洗效率,能尽量少地防止亚磷酸三乙酯的水解,同时也确保杂质得到充分去除。进一步地,本实用新型使用高效的离心分液设备进行水相和有机相的分离,相较于传统的静置分液罐和分液塔能更好地分离水相,减少后续干燥剂的用量,从而整体提升亚磷酸三乙酯合成过程中水洗工序的效率和质量。

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Abstract

The utility model discloses a purpose lies in provide a kind of for triethyl phosphite synthesis's washing device, the washing device includes washing reactor and centrifugal liquid separation equipment, and the washing reactor is connected with centrifugal liquid separation equipment by pipeline connection. Through optimized equipment structure, improve the efficiency of alkali washing, while reducing the decomposition of material washing whole process, enhance the separation effect of aqueous phase and organic phase, reduce the dosage of drying agent, to improve the efficiency and quality of washing process in triethyl phosphite synthesis as a whole.
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Description

Technical Field

[0001] This utility model relates to the field of chemical equipment technology, specifically to a water washing device for the synthesis of triethyl phosphite. Background Technology

[0002] Triethyl phosphite is an important organic chemical raw material and intermediate with wide applications in pesticides, pharmaceuticals, dyes, and other fields. In the synthesis of triethyl phosphite, water washing is a crucial post-treatment step, its purpose being to remove residual catalysts, impurities, and unreacted raw materials such as phosphorus trichloride and ethanol from the reaction products using alkaline water.

[0003] Currently, most traditional water washing equipment adopts a simple stirred reaction vessel structure. During the water washing process, the following problems exist: First, the washing of the synthesized material involves a large amount of exothermic reaction between the hydrochloride salt of the acid-binding agent and the alkali, which can cause hydrolysis of triethyl phosphite. Second, the uneven mixing of the synthesized material and the alkaline water leads to low washing efficiency and difficulty in fully removing impurities. Third, the separation of the aqueous and organic phases after washing is poor, easily causing product loss and requiring large amounts of desiccant for subsequent drying. Therefore, there is an urgent need to design a new type of water washing device to meet the demand for efficient water washing in the synthesis of triethyl phosphite. Utility Model Content

[0004] The purpose of this invention is to provide a water washing device for the synthesis of triethyl phosphite, which improves the uniformity of material washing, reduces hydrolysis of the material during the washing process, enhances the separation effect between the material and water, and reduces the amount of desiccant used subsequently. The technical solution is as follows: A water washing apparatus for the synthesis of triethyl phosphite includes a water washing reactor and a centrifugal separator, wherein the water washing reactor and the centrifugal separator are connected by pipelines.

[0005] Preferably, the water washing reactor consists of a set of pipeline reactors, including an outer shell, a stirring shaft with a built-in circulating chilled brine cooling system, and a jacket, wherein the stirring rod on the stirring shaft is configured as a straight line.

[0006] Preferably, the outer shell is provided with an inlet for the initial material, an inlet for the dilute alkali solution, an outlet for the washed material, and a vent.

[0007] Preferably, the material outlet and vent after washing are located above the outer casing, with the vent higher than the material outlet after washing.

[0008] Preferably, the inlet for the initial material and the inlet for the dilute alkali solution are located below the outer casing, with the inlet for the dilute alkali solution slightly lower than the inlet for the initial material.

[0009] Preferably, the centrifugal separator is provided with baffles for the aqueous phase, baffles for the triethyl phosphite feed solution, and baffles for the feed solution, arranged from top to bottom inside.

[0010] The water washing apparatus for the synthesis of triethyl phosphite of this invention has the following beneficial effects: This invention utilizes a highly efficient water washing reactor with excellent heat transfer, ensuring thorough mixing of materials and water, thus improving washing efficiency and minimizing the hydrolysis of triethyl phosphite while ensuring complete removal of impurities. Furthermore, this invention employs a highly efficient centrifugal separator to separate the aqueous and organic phases. Compared to traditional settling tanks and separatory towers, this method achieves better separation of the aqueous phase, reducing the amount of desiccant required and thereby improving the overall efficiency and quality of the water washing process in the synthesis of triethyl phosphite. Attached Figure Description

[0011] Figure 1 This is a schematic diagram of the water washing reactor in the water washing apparatus for the synthesis of triethyl phosphite according to this utility model. Figure 2 This is a schematic diagram of the centrifugal separation device in the water washing apparatus for the synthesis of triethyl phosphite according to this utility model.

[0012] Symbol markings: 1-Stirring motor, 2 and 10-Inlet and outlet of chilled brine on the stirring shaft, respectively, 3 and 8-Inlet and outlet of chilled brine in the outer jacket, respectively, 4-Vent port, 5-Outlet of material after washing, 6-Stirring rod, 7-Initial material inlet, 9-Inlet of dilute alkali solution, 11-Drum motor, 12-Baffle of aqueous phase after separation, 13-Aqueous phase outlet, 14-Baffle of triethyl phosphite solution after separation, 15-Outlet of triethyl phosphite solution, 16-Baffle of solution, 17-Outer shell, 18-Material inlet. Detailed Implementation

[0013] The synthesis of triethyl phosphite requires the addition of an acid-binding agent to bind the generated hydrogen chloride gas and thus prevent the excessive formation of byproducts. The initial material for the water washing process is a viscous liquid, necessitating a stirring device. The water washing process in triethyl phosphite synthesis is essentially a reaction between sodium hydroxide in a dilute alkaline solution and the hydrochloride salt of the acid-binding agent, producing sodium chloride and the corresponding acid-binding agent. This reaction generates a significant amount of heat that needs to be removed promptly. The water washing process must be completed below 10°C; otherwise, the triethyl phosphite will hydrolyze, generating the byproduct diethyl phosphite. The aforementioned water washing reactor significantly increases the heat exchange area, preventing the formation of side reactions due to temperature increases. The water washing reactor also increases the contact between the organic and aqueous phases, further ensuring uniform mixing. Simultaneously, the precise ratio of material to dilute alkaline solution contributes to a more homogeneous reaction process.

[0014] The present invention relates to a water washing apparatus for the synthesis of triethyl phosphite, comprising a water washing reactor and a centrifugal separator, wherein the water washing reactor and the centrifugal separator are connected by pipelines.

[0015] like Figure 1 As shown, the water washing reactor consists of a pipeline reactor, including an outer shell, a stirring shaft with a built-in circulating chilled brine cooling system, and a jacket. The stirring rod 6 on the stirring shaft is preferably configured in a straight line to prevent backmixing.

[0016] The outer casing is provided with an initial material inlet 7, a dilute alkali solution inlet 9, a washed material outlet 5, and a vent 4. The washed material outlet 5 and the vent 4 are located above the outer casing, with the vent 4 being higher than the washed material outlet 5.

[0017] The initial material inlet 7 and the dilute alkali solution inlet 9 are located below the outer shell, with the dilute alkali solution inlet 9 being slightly lower than the initial material inlet 7.

[0018] This invention relates to a centrifugal separation device that utilizes conventional centrifugal equipment. It comprises a static outer shell, a dynamically rotating drum, various baffles, and a drive motor. Its working principle relies primarily on the centrifugal force generated by high-speed rotation. This force, combined with the density difference between the liquid and liquid phases, effectively mixes and separates two immiscible liquids, thus achieving extraction. The device boasts high separation efficiency, simple operation, and a compact structure. The mixture of the material liquid and dilute alkaline water enters the drum through a channel connecting the annular gap to the inside of the drum, where centrifugal force facilitates the separation of the two phases. During separation, the denser, heavier phase is thrown to the inner wall of the drum, enters the heavy phase collection chamber through the heavy phase channel, and is finally discharged from the heavy phase outlet. The lighter phase, on the other hand, accumulates in the center of the drum, enters the light phase collection chamber through the light phase channel, and then flows out from the light phase outlet.

[0019] Figure 2 A specific example of a centrifugal separator is shown. During operation, the drum motor 11 drives the drum inside the outer casing 17 to rotate. The liquid, washed by the aforementioned water washing reactor, enters the drum through the material inlet 18 and then through the channel, where centrifugal force separates triethyl phosphite and water. The centrifugal separator has, from top to bottom, baffles 12 for the aqueous phase, baffles 14 for the triethyl phosphite liquid, and baffles 16 for the liquid. During separation, the denser triethyl phosphite is thrown to the inner wall of the drum, enters the heavy phase collection chamber through the heavy phase channel, and is finally discharged from the triethyl phosphite liquid outlet 15. Water, on the other hand, accumulates in the center of the drum, enters the light phase collection chamber through the light phase channel, and then flows out from the aqueous phase outlet 13.

[0020] This invention utilizes a highly efficient water washing reactor with excellent heat transfer, ensuring thorough mixing of materials and water, thus improving washing efficiency and minimizing the hydrolysis of triethyl phosphite while ensuring complete removal of impurities. Furthermore, the use of a highly efficient centrifugal separator for separating the aqueous and organic phases provides better separation of the aqueous phase compared to traditional settling tanks and separatory towers, reducing the amount of desiccant required and thereby improving the overall efficiency and quality of the water washing process in the synthesis of triethyl phosphite.

[0021] The specific embodiments described above further illustrate the purpose, technical solution, and beneficial effects of this utility model. It should be understood that the above description is only a specific embodiment of this utility model and is not intended to limit the scope of protection of this utility model. Any modifications, equivalent substitutions, improvements, etc., made within the concept and principles of this utility model should be included within the scope of protection of this utility model.

Claims

1. A water washing apparatus for the synthesis of triethyl phosphite, characterized in that, It includes a water washing reactor and a centrifugal separator, wherein the water washing reactor and the centrifugal separator are connected by pipelines.

2. The water washing apparatus for the synthesis of triethyl phosphite according to claim 1, characterized in that, The water washing reactor consists of a set of pipeline reactors, including an outer shell, a stirring shaft with a built-in circulating chilled brine cooling system, and a jacket. The stirring rod on the stirring shaft is configured as a straight line.

3. The water washing apparatus for the synthesis of triethyl phosphite according to claim 1, characterized in that, The outer casing is equipped with an inlet for the initial material, an inlet for the dilute alkali solution, an outlet for the washed material, and a vent.

4. The water washing apparatus for the synthesis of triethyl phosphite according to claim 1, characterized in that, The material outlet and vent after washing are located above the outer casing, with the vent higher than the material outlet after washing.

5. The water washing apparatus for the synthesis of triethyl phosphite according to claim 1, characterized in that, The inlet for the initial material and the inlet for the dilute alkali solution are located below the outer shell, with the inlet for the dilute alkali solution being lower than the inlet for the initial material.

6. The water washing apparatus for the synthesis of triethyl phosphite according to claim 1, characterized in that, The centrifugal separator is equipped with baffles for the aqueous phase, baffles for the triethyl phosphite feed solution, and baffles for the feed solution, arranged from top to bottom.