Continuous reaction device for tetrakis hydroxymethyl phosphonium sulfate

By designing a continuous reaction device for tetrahydroxymethylphosphate, the problems of low reaction efficiency and low product yield are solved, continuous production is achieved, and production efficiency and product purity are improved.

CN223288038UActive Publication Date: 2025-09-02CHANGSHU NEW TECH CHEM
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Patent Information

Application Number
CN202422726016.2
Authority / Receiving Office
CN · China
Patent Type
Utility models(China)
Current Assignee / Owner
Filing Date
2024-11-08
Publication Date
2025-09-02
Estimated Expiration
2034-11-08

AI Technical Summary

Technical Problem

The current tetrahydroxymethylphosphate production has low reaction efficiency, low product yield and purity, making it difficult to achieve continuous production.

Method used

A continuous reaction device of tetrahydroxymethylphosphate phosphorus sulfate including a reactor, a jet pump, a gas-liquid mixing pipeline and a circulation outlet pipeline is designed to increase the gas-liquid contact time and contact area through the gas-liquid mixing pipeline, and to achieve continuous feeding and discharge using the circulation outlet pipeline.

Benefits of technology

The production efficiency and product purity of tetrahydroxymethyl sulfate are improved, continuous production is achieved, and the practicality of production is enhanced.

✦ Generated by Eureka AI based on patent content.

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Abstract

The utility model discloses a continuous reaction device for tetrakis hydroxymethyl phosphonium sulfate. The continuous reaction device comprises a reaction kettle, an injection pump, a gas-liquid mixing pipeline and a circulating liquid outlet pipeline, a feeding hole of the reaction kettle is respectively connected with a formaldehyde feeding pipe, a sulfuric acid solution feeding pipe and a discharging hole of the injection pump; a gas phase inlet of the injection pump is connected with a first phosphine inlet pipe; one end of the gas-liquid mixing pipeline and one end of the circulating liquid outlet pipeline are respectively connected with a discharge hole of the reaction kettle, and the other end of the gas-liquid mixing pipeline and the other end of the circulating liquid outlet pipeline are respectively connected with a liquid phase inlet of the injection pump. Due to the design of the gas-liquid mixing pipeline and the circulating discharging pipe, on one hand, the contact time of gas and liquid phases is prolonged, the absorption amount and the absorption rate of the liquid phases to hydrogen phosphide gas are improved, and therefore the production efficiency of tetrakis hydroxymethyl phosphonium sulfate is improved; on the other hand, on the premise that the production efficiency and quality of tetrakis hydroxymethyl phosphonium sulfate are guaranteed, continuous feeding and continuous discharging are achieved, the purpose of continuous production is achieved, and practicability is high.
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Description

Technical Field

[0001] The utility model relates to the field of chemical production equipment, in particular to a tetrakis (hydroxymethyl)phosphonium sulfate continuous reaction device. Background Art

[0002] Tetrakis (hydroxymethyl)phosphonium sulfate is typically produced by reacting formaldehyde, sulfuric acid solution, and phosphine gas. This reaction is a gas-liquid mixing reaction. Existing reactors use gas and liquid to mix and react within the reactor. However, this reaction is limited by the mixing time and contact area, resulting in low reaction efficiency, low product yield and purity, and difficulty in continuous production. Utility Model Content

[0003] The utility model can solve the above problems existing in the existing tetrakis (hydroxymethyl) phosphonium sulfate production by providing a tetrakis (hydroxymethyl) phosphonium sulfate continuous reaction device.

[0004] In order to solve the above technical problems, the utility model provides a tetrakis (hydroxymethyl) phosphonium sulfate continuous reaction device, comprising: a reactor, a jet pump, a gas-liquid mixing pipeline and a circulating liquid outlet pipeline;

[0005] The feed port of the reactor is connected to the formaldehyde feed pipe, the sulfuric acid solution feed pipe and the discharge port of the jet pump respectively;

[0006] The gas phase inlet of the jet pump is connected to the first phosphine inlet pipe;

[0007] One end of the gas-liquid mixing pipeline and the circulating liquid outlet pipeline are respectively connected to the discharge port of the reactor, and the other end thereof are respectively connected to the liquid phase inlet of the jet pump.

[0008] In a preferred embodiment of the present invention, a gas-liquid mixed flow pump is installed on the gas-liquid mixing pipeline.

[0009] In a preferred embodiment of the present invention, a static mixer is installed on the gas-liquid mixing pipeline, and the static mixer is located on the pipeline between the gas-liquid mixed flow pump and the jet pump.

[0010] In a preferred embodiment of the present invention, the feed port of the gas-liquid mixed flow pump is also connected to the second phosphine inlet pipe.

[0011] In a preferred embodiment of the present invention, the top of the reactor is provided with a gas outlet, and the gas outlet is connected to the gas phase inlet of the jet pump through a pipeline.

[0012] In a preferred embodiment of the present invention, the circulating liquid outlet pipeline includes a circulating pipe, a discharge pipe, a circulating pump and a mass flow meter;

[0013] The circulation pump and the mass flow meter are installed on the circulation pipe;

[0014] One end of the discharge pipe is connected to the circulation pipe; and a discharge flow valve is provided on the discharge pipe.

[0015] In a preferred embodiment of the present invention, the device further comprises a program controller; a circulation flow valve is installed on the circulation pipe between the discharge pipe and the injection pump;

[0016] The mass flow meter is connected to the program controller via a signal, and is linked to the circulation flow valve and the discharge flow valve through the program controller for control.

[0017] In a preferred embodiment of the present invention, the formaldehyde feed pipe and the sulfuric acid solution feed pipe are respectively provided with a formaldehyde flow valve and a sulfuric acid solution flow valve; the program controller is connected to the formaldehyde flow valve and the sulfuric acid solution flow valve.

[0018] The beneficial effects of the utility model are as follows: the utility model provides a tetrakis (hydroxymethyl) phosphonium sulfate continuous reaction device, which, through the design of the gas-liquid mixing pipeline and the circulating discharge pipe, increases the contact time of the gas-liquid two phases, improves the absorption amount and absorption rate of the liquid phase to phosphine gas, and thus increases the production efficiency of the tetrakis (hydroxymethyl) phosphonium sulfate; on the other hand, while ensuring the production efficiency and quality of the tetrakis (hydroxymethyl) phosphonium sulfate, realizes continuous feeding and continuous discharging, achieves the purpose of continuous production, and has strong practicality. BRIEF DESCRIPTION OF THE DRAWINGS

[0019] Figure 1 This is a schematic diagram of the three-dimensional structure of a preferred embodiment of a tetrakis (hydroxymethyl)phosphonium sulfate continuous reaction device of the present invention;

[0020] The markings of the components in the accompanying drawings are as follows:

[0021] 10. Reactor, 11. Formaldehyde inlet, 12. Sulfuric acid solution inlet, 13. Mixed liquid inlet, 14. Mixed liquid outlet, 15. Circulating liquid outlet, 16. Gas outlet;

[0022] 20. Jet pump, 21. Liquid phase inlet, 22. Discharge port, 23. Gas phase inlet;

[0023] 30. Formaldehyde feed pipe, 31. Formaldehyde flow valve;

[0024] 40. Sulfuric acid solution feed pipe, 41. Sulfuric acid solution flow valve;

[0025] 51. First phosphine inlet pipe, 52. Second phosphine inlet pipe;

[0026] 61. Gas-liquid mixed flow pump, 62. Static mixer;

[0027] 71. Circulation pipe, 72. Discharge pipe, 73. Circulation pump, 74. Mass flow meter, 75. Circulation flow valve, 76. Discharge flow valve. DETAILED DESCRIPTION

[0028] The preferred embodiments of the present invention are described in detail below in conjunction with the accompanying drawings so that the advantages and features of the present invention can be more easily understood by those skilled in the art, thereby making a clearer and more precise definition of the protection scope of the present invention.

[0029] See also Figure 1 , the embodiments of the present utility model include:

[0030] Example 1

[0031] The utility model discloses a tetrakis (hydroxymethyl)phosphonium sulfate continuous reaction device, comprising a reaction kettle 10, a jet pump 20, a gas-liquid mixing pipeline and a circulating liquid outlet pipeline.

[0032] The top of the jet pump 20 is a liquid phase inlet 21 , the bottom is a discharge port 22 , and the side is provided with a gas phase inlet 23 ; the gas phase inlet 23 of the jet pump 20 is connected to the first phosphine inlet pipe 51 .

[0033] The reactor 10 has feed ports at the top, including a formaldehyde inlet 11, a sulfuric acid solution inlet 12, and a mixed feed port 13; and discharge ports at the bottom, including a mixed liquid discharge port 14 and a circulating liquid discharge port 15. Furthermore, a gas discharge port 16 is provided at the top of the reactor 10.

[0034] Specifically, the formaldehyde feeding pipe 30 is connected to the reactor 10 through the formaldehyde inlet 11 , and is used to continuously introduce liquid-phase raw material formaldehyde into the reactor 10 .

[0035] The sulfuric acid solution feed pipe 40 is connected to the reactor 10 through the sulfuric acid solution inlet 12 and is used to continuously introduce the liquid phase raw sulfuric acid solution into the reactor 10 .

[0036] The discharge port 22 of the jet pump 20 is connected to the reactor 10 through the mixing inlet 13 , and is used to continuously introduce phosphine gas or a mixture of phosphine gas, formaldehyde and sulfuric acid solution into the reactor 10 .

[0037] The gas outlet 16 is connected to the gas phase inlet 23 of the jet pump 20 through a pipeline, and is used to pump the phosphine gas that has not been absorbed by the liquid phase in the reactor 10 back into the reactor 10 through the jet pump 20, so that the phosphine gas can be reused and the utilization rate of the gas raw material can be improved.

[0038] One end of the gas-liquid mixing pipeline is connected to the mixed liquid discharge port 14 of the reactor 10 , and the other end thereof is connected to the liquid phase inlet 21 of the jet pump 20 .

[0039] Specifically, a gas-liquid mixing pump 61 and a static mixer 62 are sequentially installed along the direction of material flow in the gas-liquid mixing pipeline. Two static mixers 62 are connected in series to the gas-liquid mixing pipeline, and their model is SV-5 / 80. The design of the gas-liquid mixing pipeline increases the contact time and area between the phosphine gas, formaldehyde, and sulfuric acid solution, improving the absorption rate and amount of phosphine gas, thereby effectively increasing the yield of tetrakis(hydroxymethyl)phosphonium sulfate without increasing the volume of the reactor 10.

[0040] In addition, the feed port of the gas-liquid mixed flow pump 61 is also connected to the second phosphine inlet pipe 52 for replenishing fresh phosphine gas into the gas-liquid mixed pipeline, thereby increasing the phosphine gas content in the gas-liquid mixed pipeline and increasing the amount of phosphine gas dissolved in the formaldehyde and sulfuric acid solution, thereby further improving the yield of tetrakis(hydroxymethyl)phosphonium sulfate.

[0041] The circulating liquid outlet pipeline includes a circulating pipe 71 , a discharge pipe 72 , a circulating pump 73 , a mass flow meter 74 and a circulating flow valve 75 .

[0042] Specifically, one end of the circulation pipe 71 is connected to the circulating liquid discharge port 15 of the reactor 10 , and the other end thereof is connected to the liquid phase inlet 21 of the jet pump 20 .

[0043] One end of the discharge pipe 72 is connected to the circulation pipe 71 , and the other end thereof leads to a subsequent process. A discharge flow valve 76 is installed on the discharge pipe 72 .

[0044] The circulation pump 73 and the mass flow meter 74 are sequentially installed on the circulation pipe 71 between the reactor 10 and the discharge pipe 72. The circulation flow valve 75 is installed on the circulation pipe 71 between the discharge pipe 72 and the jet pump 20.

[0045] The mass flowmeter 74 is used to monitor the density of the reaction liquid flowing out of the reactor 10 in real time, and to detect the content of the product tetrakis(hydroxymethyl)phosphonium sulfate) by density. When the density test passes, the discharge flow valve 76 is opened to allow the reaction liquid to be discharged through the discharge pipe 72. The reflux and discharge rates of the material are controlled by adjusting the openings of the circulation flow valve 75 and the discharge valve 76.

[0046] Furthermore, the device also includes a program controller.

[0047] The formaldehyde feed pipe 30 is provided with a formaldehyde flow valve 31 ; the sulfuric acid feed pipe 40 is connected with a sulfuric acid solution flow valve 41 .

[0048] The mass flow meter 74 is connected to the program controller and, through the program controller, is linked to the circulation flow valve 75, the discharge flow valve 76, the formaldehyde flow valve 31, and the sulfuric acid solution flow valve 41 for interlocking control. Specifically, the mass flow meter 74 detects the level of tetrakis(hydroxymethyl)phosphonium sulfate generated in the reactor and adjusts the openings of the circulation flow valve 75, the discharge flow valve 76, the formaldehyde flow valve 31, and the sulfuric acid solution flow valve 41 to control the ratio of the feed and discharge amounts. This balances the total feed amount of formaldehyde and sulfuric acid solution with the discharge amount of the reacted material, thereby achieving continuous feeding and discharging and achieving the goal of continuous production.

[0049] The utility model provides a tetrakis (hydroxymethyl) phosphonium sulfate continuous reaction device, which has the following advantages:

[0050] The design of a gas-liquid mixed flow pump and a static mixer on the gas-liquid mixing pipeline increases the contact time between the gas and liquid phases, improves the absorption capacity and absorption rate of phosphine gas by the liquid phase, and thus increases the production efficiency of tetrakis(hydroxymethyl)phosphonium sulfate.

[0051] Based on the design of the circulating liquid outlet pipeline, through the design of the mass flow meter, discharge pipe, discharge flow valve and circulating flow valve on the circulating pipeline, continuous feeding and continuous discharging are realized while ensuring the production efficiency and quality of tetrakis (hydroxymethyl) phosphonium sulfate, achieving the goal of continuous production.

[0052] The above description is merely an embodiment of the present invention and does not limit the patent scope of the present invention. Any equivalent structure or equivalent process transformation made by using the contents of the description and drawings of the present invention, or directly or indirectly applied in other related technical fields, are also included in the patent protection scope of the present invention.

Claims

1. A tetrakis (hydroxymethyl)phosphonium sulfate continuous reaction device, characterized in that: include: Reactor, jet pump, gas-liquid mixing pipeline and circulating liquid outlet pipeline; The feed port of the reactor is connected to the formaldehyde feed pipe, the sulfuric acid solution feed pipe and the discharge port of the jet pump respectively; The gas phase inlet of the jet pump is connected to the first phosphine inlet pipe; One end of the gas-liquid mixing pipeline and the circulating liquid outlet pipeline are respectively connected to the discharge port of the reactor, and the other ends thereof are respectively connected to the liquid phase inlet of the jet pump.

2. A tetrakis (hydroxymethyl) phosphonium sulfate continuous reaction device according to claim 1, characterized in that: A gas-liquid mixed flow pump is installed on the gas-liquid mixing pipeline.

3. A tetrakis (hydroxymethyl) phosphonium sulfate continuous reaction device according to claim 2, characterized in that: A static mixer is installed on the gas-liquid mixing pipeline, and the static mixer is located on the pipeline between the gas-liquid mixed flow pump and the jet pump.

4. A tetrakis (hydroxymethyl) phosphonium sulfate continuous reaction device according to claim 3, characterized in that: The feed port of the gas-liquid mixed flow pump is also connected to the second phosphine inlet pipe.

5. A tetrakis (hydroxymethyl) phosphonium sulfate continuous reaction device according to claim 1, characterized in that: The top of the reactor is provided with a gas outlet, which is connected to the gas phase inlet of the jet pump through a pipeline.

6. A tetrakis (hydroxymethyl) phosphonium sulfate continuous reaction device according to claim 1, characterized in that: The circulating liquid outlet pipeline includes a circulating pipe, a discharge pipe, a circulating pump and a mass flow meter; The circulation pump and the mass flow meter are installed on the circulation pipe; One end of the discharge pipe is connected to the circulation pipe; and a discharge flow valve is provided on the discharge pipe.

7. A tetrakis (hydroxymethyl) phosphonium sulfate continuous reaction device according to claim 6, characterized in that: The device also includes a program controller; a circulation flow valve is installed on the circulation pipe between the discharge pipe and the injection pump; The mass flow meter is connected to the program controller via a signal, and is linked to the circulation flow valve and the discharge flow valve through the program controller for control.

8. The tetrakis(hydroxymethyl)phosphonium sulfate continuous reaction device according to claim 7, characterized in that: The formaldehyde feed pipe and the sulfuric acid solution feed pipe are respectively provided with a formaldehyde flow valve and a sulfuric acid solution flow valve; the program controller is connected with the formaldehyde flow valve and the sulfuric acid solution flow valve.