CN219722906U - Continuous production device for 3,5, 6-trichloropyridine-2-sodium phenolate - Google Patents

Continuous production device for 3,5, 6-trichloropyridine-2-sodium phenolate Download PDF

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CN219722906U
CN219722906U CN202322262592.1U CN202322262592U CN219722906U CN 219722906 U CN219722906 U CN 219722906U CN 202322262592 U CN202322262592 U CN 202322262592U CN 219722906 U CN219722906 U CN 219722906U
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reaction chamber
shell
trichloropyridine
continuous production
tetrachloropyridine
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郭则续
贾如鹏
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Qian Cheng Industry & Trade Co ltd Shandong
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Qian Cheng Industry & Trade Co ltd Shandong
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Abstract

The utility model discloses a continuous production device of 3,5, 6-trichloropyridine-2-sodium phenolate, which comprises a liquid alkali storage tank and a tetrachloropyridine dissolution tank with heating equipment, wherein the liquid alkali storage tank and the tetrachloropyridine dissolution tank are connected with a reaction container through pipelines, the reaction container is a tangential flow tube type reactor, the tangential flow tube type reactor comprises a reaction chamber tube shell, heat exchange equipment is arranged outside the reaction chamber tube shell, and a stirring mechanism is arranged inside the reaction chamber tube shell. The utility model has the characteristics of short reaction time, high production efficiency and continuous production operation.

Description

Continuous production device for 3,5, 6-trichloropyridine-2-sodium phenolate
Technical Field
The utility model relates to the technical field of chemical synthesis equipment, in particular to a continuous production device of 3,5, 6-trichloropyridine-2-sodium phenolate.
Background
The 3,5, 6-trichloropyridine-2-phenol sodium is a white powdery solid which is slightly soluble in water, and is a key intermediate of novel pyridine heterocyclic pesticide chlorpyrifos. The traditional trichloroacetyl chloride and acrylonitrile addition ring compound is adopted in industry, and the problems are that more waste water is generated in the reaction, the residence time is long, the quality of the product is limited, and the production efficiency is low.
At present, a method for preparing 3,5, 6-trichloropyridine-2-sodium phenolate by taking tetrachloropyridine as a raw material through alkaline hydrolysis is gradually replacing the traditional production mode of a cyclization method, but most of the methods mainly adopt kettle type reactions, for example, a 3,5, 6-trichloropyridine-2-sodium phenolate synthesis device disclosed by CN211246583U, and a preparation method of hydrated trichloropyridine sodium phenolate disclosed by CN101045705A are all characterized in that a reaction kettle is taken as synthesis equipment, and the main method is that solid tetrachloropyridine is added into the reaction kettle, and reacts for 12-16 hours at 90-120 ℃ by adding alkali liquor with a certain concentration. The production method has low efficiency, high energy consumption and insignificant economic benefit.
Disclosure of Invention
The utility model provides a continuous production device for 3,5, 6-trichloropyridine-2-sodium phenolate, which is short in reaction time and capable of continuously producing, and aims to solve the problem of low efficiency of preparing 3,5, 6-trichloropyridine-2-sodium phenolate by a reaction kettle.
In order to solve the technical problems, the utility model comprises a liquid alkali storage tank and a tetrachloropyridine dissolution tank with heating equipment, wherein the liquid alkali storage tank and the tetrachloropyridine dissolution tank are connected with a reaction container through a pipeline, and the structure is characterized in that: the reactor is a tangential flow tube reactor, the tangential flow tube reactor comprises a reactor shell, heat exchange equipment is arranged outside the reactor shell, and a stirring mechanism is arranged inside the reactor shell.
After the structure is adopted, the solid raw material tetrachloropyridine is heated and melted in the tetrachloropyridine dissolution tank, liquid alkali is added into the liquid alkali storage tank, the melted tetrachloropyridine and the liquid alkali enter the tangential flow tube type reactor through the pipeline, the tangential flow tube type reactor is suitable for liquid-liquid heterogeneous reaction, under the condition that the heat exchange equipment keeps the reaction temperature, the stirring mechanism continuously stirs the reaction materials, the tetrachloropyridine and the liquid alkali are promoted to be uniformly mixed, the reaction process is accelerated, the reaction time is shortened, the materials are different from the materials in the reaction kettle to be completely mixed, the raw materials are pushed to flow and advance in the tangential flow tube type reactor, and are discharged from the tangential flow tube type reactor after the reaction is finished, so that the continuous production operation is realized.
Further, the stirring mechanism comprises a stirring shaft which is inserted into the reaction chamber tube shell and extends along the length direction of the shell, at least one row of fixed stirring blades are arranged on the stirring shaft along the axial direction, at least one row of guide vanes which are fixed on the inner wall of the shell are arranged on the reaction chamber tube shell along the length direction of the shell, and the stirring shaft is driven by a speed reducer.
Furthermore, one end of the guide vane is fixed on the inner wall of the reaction chamber tube shell, and the other end is bent to the stirring shaft.
Further, the feed end of the reaction chamber tube shell is provided with a tetrachloropyridine feed inlet, a liquid alkali feed inlet and an emptying port, the discharge end of the reaction chamber tube shell is provided with a discharge port and a sampling port, and the sampling port is connected with a control valve.
Further, the discharge port is connected to the middle part of the gas-liquid separation tank through a pipeline, a gas outlet is formed in the top of the gas-liquid separation tank, and a product outlet is formed in the bottom of the gas-liquid separation tank.
Furthermore, a heat pump and a heating insulation layer are arranged on a pipeline connected with the tetrachloropyridine dissolution tank and the tetrachloropyridine feed inlet, and a metering pump is arranged on a pipeline connected with the liquid alkali storage tank and the liquid alkali feed inlet.
Further, the reaction chamber tube shell is provided with a pressure regulating tube orifice, the pressure regulating tube orifice is connected with a pressure balance tank, and the pressure balance tank is communicated with a nitrogen balance reactor.
Further, the heat exchange equipment is a heat exchange medium tube shell arranged outside the reaction chamber tube shell, and the heat exchange medium tube shell is provided with a heat exchange medium inlet and a heat exchange medium outlet.
According to the utility model, the tetrachloropyridine dissolving tank heats and melts the solid raw material tetrachloropyridine, the melted tetrachloropyridine and liquid alkali enter the tangential flow tube reactor from the feeding end, the liquid-liquid heterogeneous reaction is carried out by pushing flow, the heat exchange equipment provides temperature conditions for the reaction, the pressure balance tank and the nitrogen balance reactor provide pressure conditions for the reaction, the stirring mechanism promotes uniform mixing of materials, accelerates the reaction process, shortens the reaction time, and is discharged when the materials reach the discharging end of the tangential flow tube reactor, so that continuous production operation is realized. The continuous production device of 3,5, 6-trichloropyridine-2-sodium phenolate has the characteristics of short reaction time and continuous production operation.
Drawings
FIG. 1 is a schematic diagram of the structure of the present utility model;
FIG. 2 is a schematic structural view of a tangential flow pipe reactor of the present utility model;
FIG. 3 is a schematic cross-sectional view of A-A;
in the figure: a 1-tetrachloropyridine dissolution tank; 2-a liquid alkali storage tank; a 3-tangential flow tube reactor; 31-reaction chamber tube shell; 32-a heat exchange medium tube shell; 33-speed reducer; 34-stirring shaft; 301-tetrachloropyridine feed inlet; 302-liquid alkali feed inlet; 303-a discharge hole; 304-an evacuation port; 305-a heat exchange medium inlet; 306-a heat exchange medium outlet; 307-pressure regulating orifice; 308-controlling a valve; 309-stirring blades; 310-a deflector; 4-a pressure balancing tank; 5-a gas-liquid separation tank; 51-gas outlet; 52-a product discharge port; 6-a heat pump; 7-a metering pump; 8-nitrogen balance reactor; 9-heating the heat insulation layer.
Detailed Description
Referring to fig. 1-3, 5, 6-trichloropyridine-2-sodium phenolate continuous production device comprises a tetrachloropyridine dissolution tank 1, a liquid alkali storage tank 2 and a tangential flow pipe reactor 3, wherein the tetrachloropyridine dissolution tank 1 is provided with a heating hot standby for heating a solid powder raw material tetrachloropyridine (melting point 90.5 ℃) to melt, and a heating device can adopt a jacket, a heating coil, an electric heating belt and the like; the liquid caustic soda storage tank 2 is used for storing sodium hydroxide solution with the concentration of 40 g/L; the tangential flow pipe reactor 3 is a reaction vessel for generating 3,5, 6-trichloropyridine-2-sodium phenolate by reacting tetrachloropyridine with liquid alkali. The tangential flow tube reactor 3 comprises a reaction chamber tube shell 31, wherein a tetrachloropyridine feed inlet 301, a liquid caustic soda feed inlet 302 and an emptying port 304 are arranged at the feed end of the reaction chamber tube shell 31, a discharge port 303 and a sampling port are arranged at the discharge end, the sampling port is connected with a control valve 308, and raw materials are pushed to flow from the feed end to the discharge end after entering the reaction chamber tube shell 31.
Referring to fig. 1-3, a pipeline connected with a tetrachloropyridine feed inlet 301 of a tetrachloropyridine dissolution tank 1 is provided with a heat pump 6 and a heating heat-preserving layer 9, wherein the heat pump 6 is used for controlling the flow of raw material tetrachloropyridine, the heating heat-preserving layer 9 is used for preserving heat of the tetrachloropyridine in the pipeline, and the heating heat-preserving layer 9 can adopt jacket heat tracing, electric heat tracing and the like; the pipeline of the liquid alkali storage tank 2 connected with the liquid alkali feed inlet 302 is provided with a metering pump 7, and the metering pump 7 is used for controlling the adding amount of liquid alkali; the evacuation port 304 is used to evacuate the contents of the reactor vessel shell 31. The discharge port 303 is connected with the middle part of the gas-liquid separation tank 5 through a pipeline, the top of the gas-liquid separation tank 5 is provided with a gas discharge port 51, the bottom of the gas-liquid separation tank 5 is provided with a product discharge port 52, gas generated in the gas-liquid separation tank 5 is discharged through the gas discharge port 51, and the product 3,5, 6-trichloropyridine-2-sodium phenolate is discharged through the product discharge port 52. The product at the discharge end of the reaction chamber tube shell 31 is collected through a control valve 308 of a sampling port, and the content of each component in the product is measured by liquid chromatography. The stirring mechanism is arranged in the reaction chamber shell 31 and comprises a stirring shaft 34 inserted into the reaction chamber shell 31 and extending along the length direction of the shell, six rows of stirring blades 309 fixed on the stirring shaft 34 are arranged along the axial direction of the stirring shaft 34, six rows of guide vanes 310 fixed on the inner wall of the reaction chamber shell 31 are arranged along the axial direction of the reaction chamber shell 31, one end of each guide vane 310 is fixed on the inner wall of the reaction chamber shell 31, the other end of each guide vane is bent to the stirring shaft 34, the stirring shaft 34 is driven by a speed reducer 33 to rotate, the stirring blades 309 rotate along with the rotation, stirring is formed on materials in the reaction chamber shell 31, part of the materials are thrown to the inner wall of the reaction chamber shell 31, and the materials are deflected towards the center under the guide of the guide vanes 310, so that the mixing uniformity of the materials is promoted.
Referring to fig. 1-3, a heat exchange medium tube shell 32 is arranged outside the reaction chamber tube shell 31, a heat exchange medium inlet 305 is arranged near the feeding end of the reaction chamber tube shell 31, a heat exchange medium outlet 306 is arranged near the discharging end of the reaction chamber tube shell 31, and the heat exchange medium tube shell 32 is filled with a heat medium to preheat the reaction chamber tube shell 31 and maintain the reaction temperature. The reaction chamber shell 31 is further provided with a pressure regulating pipe orifice 307, the pressure regulating pipe orifice 307 is connected with the pressure balance tank 4 through a pipeline, the pressure balance tank 4 is communicated with the nitrogen balance reactor 8 through a pipeline, and the pressure in the pressure balance tank 4 is constant because the pressure in the nitrogen balance reactor 8 is constant, and the pressure balance tank 4 maintains the pressure in the reaction chamber shell 31 to be basically constant, so that pressure conditions are provided for the reaction.
3 tests were carried out with the apparatus for continuous production of 3,5, 6-trichloropyridin-2-ol sodium according to the utility model.
Test 1: preheating reaction chamber shell 31 to 130 ℃, melting 2,3,5, 6-tetrachloropyridine in a tetrachloropyridine dissolution tank 1 at 95 ℃, preparing sodium hydroxide solution with mass fraction of 40g/L, storing the sodium hydroxide solution in a liquid caustic soda storage tank 2, pumping the melted 2,3,5, 6-tetrachloropyridine into the reaction chamber shell 31 with effective volume of 1.4L at 1.5ml/min through a heat pump 6 (feed inlet 93 ℃ and feed pipeline 100 ℃), simultaneously pumping sodium hydroxide solution into the tangential flow pipe reactor 3 at 23.3ml/min through a metering pump 7, maintaining the pressure of about 0.3Mpa through a nitrogen balance reactor 8 by a pressure balance tank 4, introducing a heating medium into a heat exchange medium shell 32, maintaining the temperature of the reaction chamber shell 31 at about 130 ℃, keeping the raw material for 60min from the feed end to the discharge end of the reaction chamber shell 31, collecting reaction products (3, 5, 6-trichloropyridine-2-sodium phenolate solution) discharged from the discharge end of the reaction chamber shell 31 through a gas-liquid separation tank 5, filtering the collected reaction products, and cooling down the sodium 3,5, 6-trichloropyridine-2-sodium phenolate after filtering the collected reaction products. Sampling through a sampling port, and measuring the content of each component by liquid chromatography: the content of 3,5, 6-trichloropyridine-2-phenol sodium is 98.06%; the content of the 2,3,5, 6-tetrachloropyridine is 1.91 percent; the total of the remaining impurities was 0.03%.
Test 2: preheating reaction chamber shell 31 to 130 ℃, melting 2,3,5, 6-tetrachloropyridine in a tetrachloropyridine dissolution tank 1 at 130 ℃, preparing sodium hydroxide solution with mass fraction of 40g/L, storing the sodium hydroxide solution in a liquid caustic soda storage tank 2, pumping the melted 2,3,5, 6-tetrachloropyridine into the reaction chamber shell 31 with effective volume of 1.4L at 1.5ml/min through a heat pump 6 (feed inlet 120 ℃ and feed pipeline 100 ℃), simultaneously pumping sodium hydroxide solution into the tangential flow pipe reactor 3 at 23.3ml/min through a metering pump 7, maintaining the pressure of about 0.3Mpa through a nitrogen balance reactor 8 by a pressure balance tank 4, introducing a heating medium into a heat exchange medium shell 32, maintaining the temperature of the reaction chamber shell 31 at about 120 ℃, keeping the raw material for 60min from the feed end to the discharge end of the reaction chamber shell 31, collecting reaction products (3, 5, 6-trichloropyridine-2-sodium phenolate solution) discharged from the discharge end of the reaction chamber shell 31 through a gas-liquid separation tank 5, filtering the collected reaction products, and cooling down the sodium 3,5, 6-trichloropyridine-2-sodium phenolate after filtering the collected reaction products. Sampling through a sampling port, and measuring the content of each component by liquid chromatography: the content of 3,5, 6-trichloropyridine-2-phenol sodium is 96.56%; the content of the 2,3,5, 6-tetrachloropyridine is 2.85 percent; the total of the remaining impurities was 0.59%.
Test 3: preheating reaction chamber shell 31 to 130 ℃, melting 2,3,5, 6-tetrachloropyridine in a tetrachloropyridine dissolution tank 1 at 130 ℃, preparing sodium hydroxide solution with mass fraction of 40g/L, storing the sodium hydroxide solution in a liquid caustic soda storage tank 2, pumping the melted 2,3,5, 6-tetrachloropyridine into the reaction chamber shell 31 with effective volume of 1.4L at 1.5ml/min through a heat pump 6 (feed inlet 93 ℃ and feed pipeline 100 ℃), simultaneously pumping sodium hydroxide solution into the tangential flow pipe reactor 3 at 23.3ml/min through a metering pump 7, maintaining the pressure of about 0.3Mpa through a nitrogen balance reactor 8 by a pressure balance tank 4, introducing a heating medium into a heat exchange medium shell 32, maintaining the temperature of the reaction chamber shell 31 at about 130 ℃, keeping the raw material for 60min from the feed end to the discharge end of the reaction chamber shell 31, collecting reaction products (3, 5, 6-trichloropyridine-2-sodium phenolate solution) discharged from the discharge end of the reaction chamber shell 31 through a gas-liquid separation tank 5, filtering the collected reaction products, and cooling down the sodium 3,5, 6-trichloropyridine-2-sodium phenolate after filtering the collected reaction products. Sampling through a sampling port, and measuring the content of each component by liquid chromatography: 3,5, 6-trichloropyridine-2-phenol sodium content is 97.02%; the content of the 2,3,5, 6-tetrachloropyridine is 2.92 percent; the total of the remaining impurities was 0.06%.
By using the production device provided by the utility model, the content of 3,5, 6-trichloropyridine-2-sodium phenolate in the product after 1h of reaction can reach 98%, compared with the existing reaction time of kettle type reaction for 12-16h, the production device provided by the utility model has the advantages that the reaction time is obviously shortened, the production efficiency is improved, the raw materials push and flow in the tangential flow pipe reactor, continuous production operation can be realized, and the operation cost is reduced.

Claims (8)

1. The utility model provides a 3,5, 6-trichloropyridine-2-sodium phenolate serialization apparatus for producing, includes liquid alkali storage tank (2) and has heating device's tetrachloropyridine dissolving tank (1), liquid alkali storage tank (2) and tetrachloropyridine dissolving tank (1) are connected with the reaction vessel through the pipeline, characterized by: the reactor is a tangential flow tube reactor (3), the tangential flow tube reactor (3) comprises a reactor tube shell (31), heat exchange equipment is arranged outside the reactor tube shell (31), and a stirring mechanism is arranged inside the reactor tube shell.
2. The continuous production device of 3,5, 6-trichloropyridine-2-sodium phenolate according to claim 1, characterized in that: the stirring mechanism comprises a stirring shaft (34) which is inserted into the reaction chamber tube shell (31) and extends along the length direction of the shell, the stirring shaft (34) is provided with at least one row of fixed stirring blades (309) along the axial direction, the reaction chamber tube shell (31) is provided with at least one row of guide vanes (310) fixed on the inner wall of the shell along the length direction of the shell, and the stirring shaft (34) is driven by a speed reducer (33).
3. The continuous production device of 3,5, 6-trichloropyridine-2-sodium phenolate according to claim 2, characterized in that: one end of the guide vane (310) is fixed on the inner wall of the reaction chamber tube shell (31), and the other end is bent to the stirring shaft (34).
4. The continuous production device of 3,5, 6-trichloropyridine-2-sodium phenolate according to claim 1, characterized in that: the reaction chamber is characterized in that a tetrachloropyridine feed inlet (301), a liquid alkali feed inlet (302) and an emptying port (304) are arranged at the feed end of the reaction chamber tube shell (31), a discharge port (303) and a sampling port are arranged at the discharge end of the reaction chamber tube shell (31), and the sampling port is connected with a control valve (308).
5. The continuous production device of 3,5, 6-trichloropyridine-2-sodium phenolate according to claim 4, wherein the continuous production device comprises the following components: the discharging port (303) is connected to the middle part of the gas-liquid separation tank (5) through a pipeline, a gas outlet (51) is formed in the top of the gas-liquid separation tank (5), and a product outlet (52) is formed in the bottom of the gas-liquid separation tank (5).
6. The continuous production device of 3,5, 6-trichloropyridine-2-sodium phenolate according to claim 4, wherein the continuous production device comprises the following components: the pipeline that tetrachloropyridine dissolving tank (1) and tetrachloropyridine feed inlet (301) are connected is equipped with heat pump (6) and heating heat preservation (9), the pipeline that liquid alkali storage tank (2) and liquid alkali feed inlet (302) are connected is equipped with measuring pump (7).
7. The continuous production device of 3,5, 6-trichloropyridine-2-sodium phenolate according to claim 1, characterized in that: the reaction chamber shell (31) is provided with a pressure regulating pipe orifice (307), the pressure regulating pipe orifice (307) is connected with a pressure balance tank (4), and the pressure balance tank (4) is communicated with a nitrogen balance reactor (8).
8. The continuous production device of 3,5, 6-trichloropyridine-2-sodium phenolate according to claim 1, characterized in that: the heat exchange equipment is a heat exchange medium tube shell (32) arranged outside the reaction chamber tube shell (31), and the heat exchange medium tube shell (32) is provided with a heat exchange medium inlet (305) and a heat exchange medium outlet (306).
CN202322262592.1U 2023-08-23 2023-08-23 Continuous production device for 3,5, 6-trichloropyridine-2-sodium phenolate Active CN219722906U (en)

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CN202322262592.1U CN219722906U (en) 2023-08-23 2023-08-23 Continuous production device for 3,5, 6-trichloropyridine-2-sodium phenolate

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Application Number Priority Date Filing Date Title
CN202322262592.1U CN219722906U (en) 2023-08-23 2023-08-23 Continuous production device for 3,5, 6-trichloropyridine-2-sodium phenolate

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CN219722906U true CN219722906U (en) 2023-09-22

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