Glyphosate salt aqueous solution production system and method

Abstract

The application discloses a glyphosate salt aqueous solution production system and method, and belongs to the field of pesticides. The system comprises a raw pesticide feeding hopper, a mixing kettle, a tubular reactor, a material conveying pump, a cooling device, a receiving kettle, a water storage tank, an alkali liquor storage tank and an additive storage tank. Glyphosate raw pesticide and water are mixed in the mixing kettle to obtain a solid-liquid mixture slurry, which is then conveyed into the tubular reactor by the material conveying pump to react with alkali liquor to obtain a reaction liquid, and finally, the reaction liquid is conveyed into the receiving kettle to realize complete reaction of one batch and addition of additives. The application realizes continuous production through the alternating use of the mixing kettle, the conveying pump, the tubular reactor and multiple receiving kettles, the flow of the material conveying pump determines the production capacity, the production capacity of the glyphosate salt aqueous solution is greatly improved, the problem of tail gas absorption such as ammonia gas is avoided, the production environment is improved, safety and environmental protection are realized, the input and output of each batch and the quality of the product can be accurately controlled, and the product quality is fully ensured.

Description

Technical Field

[0001] This invention relates to the field of pesticide technology, and in particular to a glyphosate salt aqueous solution production system and method. Background Technology

[0002] Glyphosate aqueous solution is one of the most widely used herbicides. It is a systemic, transgenic, non-selective post-emergence foliar herbicide used for weed control in dryland areas. Global glyphosate technical grade production capacity is approximately 1.1 million tons. Glyphosate technical grade is insoluble in water and needs to be neutralized with appropriate alkalis to form salts before further processing to prepare various water-soluble glyphosate salts. These water-soluble glyphosate salts mainly include glyphosate ammonium salts, isopropylamine salts, dimethylamine salts, ethanolamine salts, and potassium salts, among others.

[0003] For a long time, glyphosate aqueous solution production has been intermittent. The production equipment consists of multiple independent salt-forming reactors. Each reactor is equipped with a glyphosate technical feed hopper, water addition device, alkali addition device, adjuvant addition device, filtration device, finished product storage tank, and tail gas absorption device. During production, a fixed amount of glyphosate technical is added to the salt-forming reactor, followed by a fixed amount of water and alkali. The alkali and glyphosate technical undergo an acid-base neutralization reaction within the reactor. Then, a fixed amount of adjuvants is added to produce the glyphosate aqueous solution. In this production method, the material needs to remain in the salt-forming reactor for 1-3 hours before it can be emptied for the next batch, thus enabling intermittent production.

[0004] As mentioned above, the intermittent production method of glyphosate aqueous solution means that the production capacity depends on the number and size of the salt-forming reactors. Increasing or expanding capacity requires either increasing the number of reactors or enlarging their volume. For large customer orders, such as 3000KL or 5000KL, requiring delivery in large packaging sizes within a short timeframe, existing equipment and production processes are difficult to meet. Furthermore, the salt-forming reactors require emptying, cleaning, or cooling operations after each batch, further reducing production efficiency and resulting in significant energy losses.

[0005] Chinese patent document CN109221243A discloses a continuous production process for glyphosate liquid formulations. Glyphosate technical powder, alkali solution, and water are continuously fed into an intermediate tank at a molar ratio of 1:0.9–2:4–20. Water and alkali solution are continuously fed into the intermediate tank via flow meters, while glyphosate is continuously fed into the intermediate tank via a screw conveyor and weighing process. After pre-reaction in the intermediate tank, the mixture is conveyed to a pipeline static mixer for continuous reaction, yielding an acid-base reaction solution, thus achieving continuous production. However, actual testing revealed the following problems:

[0006] 1. The key to continuous production in CN109221243A is the precise control and continuous feeding of glyphosate technical, water, and alkali solution. It has been proven that it is difficult to achieve the same level of precision in continuous feeding of glyphosate technical as it is in the case of water or alkali solution, which can be controlled by flow meters. This is because glyphosate technical is a solid powder with varying particle sizes and bulk densities, making it difficult to achieve continuous and precise feeding of glyphosate technical. As a result, it is difficult to achieve the precise and continuous feeding of glyphosate technical powder, alkali solution, and water in a molar ratio of 1:0.9 to 2:4 to 20 into the intermediate tank in CN109221243A.

[0007] CN109221243A describes a pre-reaction of glyphosate technical with alkali solution in an intermediate tank. The reaction is exothermic. When the added alkali solution is a solution of ammonia or amine, some of the unreacted ammonia or amine will evaporate. The hot water vapor from the intermediate tank and the evaporated ammonia or amine will enter the glyphosate technical feeding device, causing the glyphosate technical to clump in the feeding device, resulting in blockage and poor flow. This makes it more difficult to accurately feed glyphosate technical continuously.

[0008] Because the input of glyphosate technical grade cannot be precisely controlled, the material ratio is unbalanced, making it difficult to accurately control product quality and production costs, resulting in defects such as excessively low product content. Therefore, the continuous production method described in CN109221243A is difficult to achieve.

[0009] 2. In batch production, the liquid alkali pipe in the salt-forming reactor is inserted 1.0 to 1.5 meters below the liquid surface to prevent ammonia or amine gas from escaping through a liquid seal. Even so, some incompletely reacted ammonia or amine gas may still escape. CN109221243A, however, uses an intermediate tank for pre-reaction with alkali solution. This intermediate tank is similar to the salt-forming reactor in a batch production unit. The bottom material in the intermediate tank is 200 kg, and the liquid seal level is much lower than that in the batch production method. Ammonia or amine gas will easily escape, causing significant difficulties in tail gas absorption.

[0010] 3. In CN109221243A, the glyphosate technical grade is added at a rate of 200–1000 kg / h, which is faster than the existing batch production method for single 10 glyphosate technical grade ... 3 The capacity of the salt-forming reactor is still low, and it has no practical value for industrial production. Summary of the Invention

[0011] To address the shortcomings of existing technologies, this invention provides a glyphosate salt aqueous solution production system and method, which enables continuous production of glyphosate salt aqueous solutions and greatly improves production capacity.

[0012] The technical solution provided by this invention is as follows:

[0013] A glyphosate salt aqueous solution production system includes a technical grade feed hopper, a mixing vessel, a tubular reactor, a material conveying pump, a cooling device, a receiving vessel, a water storage tank, an alkali storage tank, and an adjuvant storage tank, wherein:

[0014] The mixing vessel is equipped with a mixing vessel agitator. The raw material feeding hopper is connected to the raw material inlet of the mixing vessel. The water storage tank is connected to the water inlet of the mixing vessel through a water supply pipe. The discharge port of the mixing vessel is connected to the slurry inlet of the tubular reactor through a solid-liquid slurry conveying pipe. The alkali storage tank is connected to the alkali inlet of the tubular reactor through an alkali pipe.

[0015] The number of receiving vessels is at least two, and each receiving vessel is equipped with a receiving vessel agitator. The reaction liquid outlet of the tubular reactor is connected in parallel to the reaction liquid inlet of each receiving vessel through a reaction liquid delivery pipeline. The auxiliary agent storage tank is connected in parallel to the auxiliary agent inlet of each receiving vessel through an auxiliary agent pipeline.

[0016] The material conveying pump is installed on the solid-liquid mixture conveying pipeline or the reaction liquid conveying pipeline, and the cooling device is installed on the tubular reactor and / or the reaction liquid conveying pipeline;

[0017] The raw material feeding hopper is equipped with a feeding device and a metering device. The water supply pipe is equipped with a water inlet valve and a water flow meter. The alkali solution pipe is equipped with an alkali solution inlet valve and an alkali solution flow meter. The reaction liquid conveying pipe is equipped with a reaction liquid inlet valve for each receiving vessel. The auxiliary agent pipe is equipped with an auxiliary agent inlet valve and an auxiliary agent flow meter for each receiving vessel. The discharge port of the mixing vessel is equipped with a discharge port control valve.

[0018] Furthermore, a compressed air pipeline is connected to the solid-liquid mixture slurry conveying pipeline, the compressed air pipeline is connected to an air source, and an air control valve is installed on the compressed air pipeline.

[0019] Furthermore, the alkali solution pipeline is connected to the solid-liquid mixture slurry conveying pipeline through an alkali solution branch pipe, and a branch pipe alkali solution valve is provided on the alkali solution branch pipe.

[0020] Furthermore, the material conveying pump is installed on the solid-liquid mixture conveying pipeline and close to the tubular reactor side, the connection between the alkali branch pipe and the solid-liquid mixture conveying pipeline is close to the mixing vessel side, and the connection between the compressed air pipeline and the solid-liquid mixture conveying pipeline is located before the material conveying pump.

[0021] Furthermore, the solid-liquid mixture slurry conveying pipeline is inclined downwards at a certain slope in accordance with the conveying direction of the solid-liquid mixture slurry.

[0022] Furthermore, the reaction liquid delivery pipeline is connected to the return port of the mixing vessel via a return liquid pipeline, and the return liquid pipeline is equipped with a return liquid valve and a return liquid flow meter.

[0023] Furthermore, the connection between the return liquid pipe and the reaction liquid delivery pipe is located after the cooling device.

[0024] Furthermore, the cooling device includes a cooler, which is installed on the reaction liquid delivery pipeline. The reaction liquid outlet of the tubular reactor is connected to the reaction liquid inlet of the cooler through one section of the reaction liquid delivery pipeline, and the reaction liquid outlet of the cooler is connected in parallel to the reaction liquid inlet of each receiving vessel through the other section of the reaction liquid delivery pipeline.

[0025] Furthermore, the cooling device includes a cooling sleeve that is fitted over the outside of the tubular reactor, and the cooling sleeve has a coolant inlet and a coolant outlet.

[0026] Furthermore, the tubular reactor includes a tubular shell, a mixing unit is disposed inside the tubular shell, the slurry inlet and the reaction liquid outlet are respectively disposed at both ends of the tubular shell, and the alkali inlet of the tubular reactor is located on the side of the tubular shell near the slurry inlet.

[0027] Furthermore, the end of the alkali pipe is inserted into the tubular shell through the alkali inlet, and the direction of alkali outflow from the end of the alkali pipe is opposite to the direction of conveying the solid-liquid mixture slurry inside the tubular shell.

[0028] Furthermore, the end of the alkali solution pipeline has a beveled cut, the orientation of which is opposite to the conveying direction of the solid-liquid mixture slurry;

[0029] Alternatively, the end of the alkali pipe may be bent in the opposite direction to the conveying direction of the solid-liquid mixture slurry.

[0030] Furthermore, the mixing component unit includes one or more of the following: an externally powered mixing device, a fluid-driven mixing device, and a stationary mixing device.

[0031] Furthermore, the externally powered mixing device includes a stirring blade, which is axially or vertically installed inside the tubular housing and connected to an external power source outside the tubular housing.

[0032] The fluid-driven mixing device includes a rotating propeller blade, which is installed inside the tubular housing via a rotating bearing and a support frame, and the rotating propeller blade is installed in an alternating manner of forward and reverse rotation.

[0033] The fixed mixing device includes a fixed spiral blade, which is fixedly installed inside the tubular housing. The fixed spiral blade is installed in an alternating manner of left-hand and right-hand rotation.

[0034] A method for producing glyphosate salt aqueous solutions, the method comprising:

[0035] S1: Calculate the ratio of glyphosate technical and water according to the requirements of the finished glyphosate salt aqueous solution. Open the technical feed hopper and water inlet valve. Continuously add the glyphosate technical from the technical feed hopper and the water from the water storage tank into the mixing vessel at the addition rate corresponding to the calculated ratio. Turn on the agitator of the mixing vessel to form a solid-liquid slurry under the action of agitation.

[0036] S2: When the solid-liquid mixture slurry in the mixing vessel accumulates to the minimum set amount, the discharge port control valve, the material conveying pump, and the reaction liquid feed valve of one of the idle receiving vessels are opened, and the solid-liquid mixture slurry is conveyed to the tubular reactor through the material conveying pump;

[0037] Simultaneously, the alkali feed valve is opened, and the alkali in the alkali storage tank is continuously added to the tubular reactor at a set addition rate. The solid-liquid mixture slurry reacts with the alkali in the tubular reactor to generate a reaction liquid.

[0038] S3: Turn on the cooling device to cool the reaction liquid to the set temperature and then transport it into the receiving vessel with the reaction liquid feed valve opened;

[0039] S4: Turn on the agitator of the receiving vessel to ensure that the reaction solution reacts completely and mixes evenly in the receiving vessel;

[0040] S5: After the set batch of glyphosate technical, water, and alkali solution has been used up, close the technical feed hopper, water feed valve, and alkali solution feed valve. Use the material conveying pump to transport all the materials that can be conveyed in the mixing tank, solid-liquid mixture conveying pipeline, tubular reactor, and reaction liquid conveying pipeline into the receiving tank. Close the open reaction liquid feed valve and open the reaction liquid feed valve of the remaining empty receiving tank to start the next batch of production.

[0041] At the same time, open the auxiliary agent feed valve corresponding to the receiving vessel used in this batch, add the set amount of auxiliary agent into the receiving vessel, and transfer the finished product after it is stirred evenly and the sample analysis is qualified.

[0042] Furthermore, when a compressed air pipeline is connected to the solid-liquid mixture slurry conveying pipeline, step S5 includes:

[0043] Once the set batch of glyphosate technical, water, and alkali solution has been used up, close the technical feed hopper, water inlet valve, and alkali solution inlet valve. Use the material pump to transfer all transportable materials from the mixing vessel, solid-liquid slurry conveying pipeline, tubular reactor, and reaction liquid conveying pipeline into the receiving vessel. Close the outlet control valve and open the air control valve to blow any remaining material from the solid-liquid slurry conveying pipeline, tubular reactor, and reaction liquid conveying pipeline into the receiving vessel using compressed air. Close the opened reaction liquid inlet valve and open the reaction liquid inlet valve of the remaining empty receiving vessel to begin production for the next batch.

[0044] Simultaneously, open the auxiliary agent feed valve corresponding to the receiving vessel used in this batch, add the set amount of auxiliary agent into the receiving vessel, and after stirring evenly and sampling analysis is qualified, transfer the obtained glyphosate salt aqueous solution product.

[0045] Furthermore, when the reaction liquid delivery pipeline is connected to the return port of the mixing vessel via a return liquid pipeline, step S2 further includes:

[0046] If the ratio of glyphosate technical and water results in a solid-liquid ratio in the solid-liquid mixture that is greater than a set value, the return valve is opened to return the reaction liquid in the reaction liquid delivery pipeline to the mixing vessel at a set flow rate.

[0047] Furthermore, the minimum set amount of the solid-liquid mixture slurry is the minimum amount required to ensure that the material conveying pump does not run dry during normal conveying.

[0048] The present invention has the following beneficial effects:

[0049] 1. This invention mixes glyphosate technical grade and water in a mixing vessel to obtain a solid-liquid slurry. This slurry is then pumped to a tubular reactor via a material transfer pump to react with an alkaline solution, yielding a reaction solution. Finally, the solution is transferred to a receiving vessel to complete the reaction of one batch and add adjuvants. Through the alternating use of the mixing vessel, transfer pump, tubular reactor, and multiple receiving vessels, continuous production using the mixing vessel is achieved. This invention represents a significant breakthrough in the production capacity of glyphosate salt aqueous solutions. Production output is no longer limited by the capacity of existing salt-forming vessels but is determined by the flow rate of the material transfer pump; that is, the production capacity is directly proportional to the output flow rate of the material transfer pump. When capacity needs to be expanded, only the flow rate of the material transfer pump needs to be increased, without increasing the number of salt-forming vessels. This completely changes the original production model. One production system can not only meet the production capacity of multiple independent salt-forming vessels but also meet the delivery requirements of large orders within a short timeframe, with low operating costs.

[0050] 2. The neutralization reaction of glyphosate technical with alkaline solution takes place in a tubular reactor. The tubular reactor is sealed, and the inlet and outlet are connected to sealed pipes. The liquid inside the tubular reactor and the liquid inside the pipes are equivalent to a liquid seal, which makes the liquid level of the liquid seal very high. The glyphosate acid reacts fully with the alkaline substances, and there is no amine or ammonia odor overflow. This avoids the problem of tail gas absorption, improves the production environment, and is safe and environmentally friendly.

[0051] 3. Within a single batch, the entire process from material input to finished product output is continuously automated. Two receiving vessels are set up for batch switching, and the input, output, and product quality of each batch are precisely controlled, thus fully ensuring product quality. Attached Figure Description

[0052] Figure 1 This is a schematic diagram of the glyphosate salt aqueous solution production system of the present invention;

[0053] Figure 2 Example of a tubular reactor Figure 1 ;

[0054] Figure 3 for Figure 2 Sectional view along axis AA;

[0055] Figure 4 for Figure 2 A schematic diagram of a fixed spiral blade, wherein (a) is a schematic diagram of a right-hand spiral blade, (b) is a schematic diagram of a left-hand spiral blade, and (c) is a schematic diagram of a left-hand spiral blade rotated 90°;

[0056] Figure 5 Example of a tubular reactor Figure 2 ;

[0057] Figure 6 for Figure 5 A schematic diagram of the stirring blades;

[0058] Figure 7 Example of a tubular reactor Figure 3 ;

[0059] Figure 8 for Figure 7 A schematic diagram of rotating propeller blades;

[0060] Figure 9 Example of a tubular reactor Figure 4 ;

[0061] Figure 10 for Figure 9 A schematic diagram of rotating propeller blades;

[0062] Figure 11 Example of a tubular reactor Figure 5 . Detailed Implementation

[0063] To make the technical problems, technical solutions, and advantages of this invention clearer, the technical solutions of this invention will be clearly and completely described below in conjunction with the accompanying drawings and specific embodiments. Obviously, the described embodiments are only a part of the embodiments of this invention, and not all of them. The components of the embodiments of this invention described and shown in the accompanying drawings can generally be arranged and designed in various different configurations. Therefore, the following detailed description of the embodiments of the invention provided in the accompanying drawings is not intended to limit the scope of the claimed invention, but merely to illustrate selected embodiments of the invention. All other embodiments obtained by those skilled in the art based on the embodiments of this invention without inventive effort are within the scope of protection of this invention.

[0064] This invention provides a glyphosate salt aqueous solution production system, such as... Figure 1 As shown, it includes a raw material feeding hopper 1, a mixing vessel 2, a tubular reactor 3, a material conveying pump 4, a cooling device 5 and / or 6, a receiving vessel 7, a water storage tank 8, an alkali storage tank 9, and an auxiliary agent storage tank 10, wherein:

[0065] The mixing vessel 2 is equipped with a mixing vessel agitator 11, which is driven by an external motor or other drive mechanism to stir the materials inside the mixing vessel 2. The top of the mixing vessel 2 is equipped with a raw material inlet 12 and a water inlet 14, and the bottom is equipped with a discharge outlet 15, which is equipped with a discharge outlet control valve 34.

[0066] The technical grade feed hopper 1 is positioned above the mixing vessel 2. The feed hopper 1 is equipped with a feeding device 26 and a metering device. The feeding device 26 can be a variable frequency screw feeder, installed at the bottom outlet of the feed hopper 1. The bottom outlet of the feed hopper 1 is connected to the technical grade inlet 12 of the mixing vessel 2; the connection can be a flexible connection or similar structure. The metering device can be a weighing module, used to weigh the remaining glyphosate technical grade in the feed hopper 1 in real time. The weighing module works in conjunction with the variable frequency screw feeder, and under the control of the controller, allows the glyphosate technical grade in the feed hopper 1 to be continuously fed into the mixing vessel 2 at a certain speed. Please note that because glyphosate technical grade is a solid powder, its particle size and bulk density are not entirely uniform; therefore, continuous feeding of glyphosate technical grade can only guarantee approximate accuracy, not continuous and precise feeding.

[0067] The water storage tank 8 is connected to the water inlet 14 of the mixing vessel 2 via the water supply pipe 13. The water supply pipe 13 is equipped with a water inlet valve 27 and a water flow meter 28. The water inlet valve 27 is a flow valve that can automatically adjust the flow rate. The water inlet valve 27, the water flow meter 28, and the related pump work together to feed water (preferably deionized water) from the water storage tank 8 into the mixing vessel 2 at a certain speed under the control of the controller.

[0068] After glyphosate technical and water are added to mixing vessel 2, a solid-liquid slurry is formed under the stirring action of mixing vessel agitator 11.

[0069] The tubular reactor 3 includes a slurry inlet 17, a reaction liquid outlet 18, and an alkali inlet 20. The discharge port 15 of the mixing vessel 2 is connected to the slurry inlet 17 of the tubular reactor 3 through a solid-liquid mixed slurry conveying pipe 16. Under the action of the material conveying pump 4, the solid-liquid mixed slurry enters the tubular reactor 3 through the slurry inlet 17.

[0070] The alkali storage tank 9 is connected to the alkali inlet 20 of the tubular reactor 3 via an alkali pipeline 19. An alkali feed valve 29 and an alkali flow meter 30 are installed on the alkali pipeline 19. The alkali feed valve 29 is an automatically adjustable flow valve. The alkali feed valve 29, the alkali flow meter 30, and the corresponding pump work together, and under the control of the controller, the alkali in the alkali storage tank 9 can be continuously and accurately fed into the tubular reactor 3 at a certain speed.

[0071] In this invention, the alkaline solution can be one or more of liquid ammonia, ammonia water, isopropylamine, monoethanolamine, potassium hydroxide, sodium hydroxide, dimethylamine, or other organic and inorganic bases.

[0072] The solid-liquid mixture and the alkaline solution undergo a neutralization reaction within the tubular reactor 3. This reaction is exothermic and extremely rapid. The solid-liquid mixture of glyphosate technical and water instantly transforms into a transparent liquid upon contact with the alkaline solution, dissolving the glyphosate technical and generating a reaction solution, i.e., a glyphosate salt solution. The generated reaction solution, driven by the material transfer pump 4, enters the reaction solution transfer pipe 22 from the reaction solution outlet 18, and then flows into the receiving vessel 7. The flow velocity of the material in the tubular reactor 4 can be 0.5–2.0 m / s, preferably 0.7–1.0 m / s.

[0073] In this invention, the material conveying pump 4 can be selected from those with variable frequency motors, allowing adjustment of the motor frequency to increase or decrease the pump flow rate based on changes in production capacity. For example, an open impeller centrifugal pump can be selected, preferably a slurry pump or a mortar pump, which performs well when the solid-liquid ratio of glyphosate technical and water is 1.3:1 to 1:1. More preferably, the mortar pump is a UHB-ZK series model. Furthermore, the flow rate and head of the material conveying pump 4 can be selected with a margin based on the required production capacity and operating conditions. That is, the actual output flow rate of the material conveying pump 4 is selected according to the required production capacity, and the head of the material conveying pump 4 is selected based on the pipeline resistance and the height of the receiving vessel 7. Flow rates of 5 to 300 m³ / h can be selected. 3 / h, with a head of 30-100m.

[0074] During the neutralization reaction in the tubular reactor 3, heat is released. In order to cool the reaction liquid, the present invention provides a cooling device on the tubular reactor 3 and / or the reaction liquid conveying pipeline 22 to cool the reaction liquid to below the set temperature before it enters the receiving vessel 7.

[0075] There are at least two receiving vessels 7, and each receiving vessel 7 is equipped with a receiving vessel agitator 21. The receiving vessel agitator 21 is driven by an external motor or other drive mechanism to agitate the material in the receiving vessel 7. The receiving vessel 7 is provided with a reaction liquid inlet 23 and an auxiliary agent inlet 25 at the top, and a finished product outlet 35 at the bottom.

[0076] The reaction liquid outlet 18 of the tubular reactor 3 is connected in parallel to the reaction liquid inlet 23 of each receiving vessel 7 via reaction liquid delivery pipes 22. Each receiving vessel 7 is equipped with a reaction liquid feed valve 31 on the reaction liquid delivery pipes 22. In one configuration, the reaction liquid delivery pipes 22 can be multiple parallel pipes, with the tubular reactor 3 connected to multiple receiving vessels 7 via these multiple pipes. In this case, the reaction liquid feed valves 31 are installed on each of the reaction liquid delivery pipes 22. In another configuration, the reaction liquid delivery pipes 22 consist of a single pipe at the beginning and branch pipes at the end, with each branch pipe connected to multiple receiving vessels 7. In this case, the reaction liquid feed valves 31 are installed on each branch pipe.

[0077] The additive storage tank 10 is connected in parallel to the additive inlet 25 of each receiving vessel 7 via additive pipelines 24. Each receiving vessel 7 is equipped with an additive feed valve 32 and an additive flow meter 33 on the additive pipeline 24. Under the control of the controller and the action of the corresponding pump, the additive in the additive storage tank 10 can be accurately fed into the receiving vessel 7. Similar to the reaction liquid conveying pipeline 22, the additive pipeline 24 can be multiple pipelines that are completely parallel, or it can be in the form of a single pipeline at the beginning and multiple branch pipes at the end.

[0078] This invention employs a continuous production method. Glyphosate technical, water, and alkali solution are continuously fed into the reactor, and the resulting reaction solution continuously enters a receiving vessel 7. At this time, the reaction solution inlet valve 31 of this receiving vessel 7 is open, while the reaction solution inlet valves 31 of the other receiving vessels 7 are closed. When a batch of glyphosate technical, water, and alkali solution is used up, all the reaction solutions produced in that batch enter a receiving vessel 7 for further mixing and complete reaction. Then, adjuvants are added, and the mixture is thoroughly mixed within the receiving vessel 7. After a period of time, the finished product is obtained. The finished product can be transferred to a finished product tank through the finished product outlet 35 for packaging and transportation.

[0079] Meanwhile, mixing vessel 2 begins production for the next batch. Since the current receiving vessel 7 is still adding additives to prepare the finished product, to avoid the still-in-use receiving vessel 7 affecting the continuous production of mixing vessel 2, the produced reaction liquid is transferred to another receiving vessel 7. In other words, mixing vessel 2 of this invention produces continuously, while multiple receiving vessels 7 are used alternately to achieve batch-by-batch continuous production of glyphosate salt aqueous solutions.

[0080] In the production of this invention, production needs to be carried out in batches. Before producing a batch, the proportions of glyphosate technical, water, alkali solution, and adjuvants must first be calculated according to the requirements of the finished glyphosate salt aqueous solution, and the total yield of this batch must be determined. Correspondingly, the total amounts of glyphosate technical, water, alkali solution, and adjuvants used are also determined. In practical applications, the total yield of each batch can be set to be the same, thus allowing for repeated control without changing the parameters.

[0081] When adding glyphosate technical and water into mixing vessel 2, the glyphosate technical and water should be continuously added to the mixing vessel according to the calculated ratio. Since the continuous feeding of glyphosate technical is not precise, it cannot be guaranteed that the ratio of glyphosate technical and water in mixing vessel 2 is completely consistent with the calculated ratio, but can only be roughly accurate.

[0082] The solid-liquid mixture of glyphosate technical and water reacts with alkali solution in tubular reactor 3. While the alkali solution can be continuously and precisely fed, the glyphosate technical is not continuously and precisely fed. Therefore, complete reaction cannot be achieved in tubular reactor 3, requiring all materials from a batch to be transferred to receiving vessel 7. Although the glyphosate technical cannot be continuously and precisely fed, the total amount of glyphosate technical in a batch can be precisely measured. Therefore, after all materials enter receiving vessel 7, the amounts of glyphosate technical, water, and alkali solution in receiving vessel 7 are accurate and conform to the calculated ratios, allowing for complete reaction in receiving vessel 7. Even if there is an imbalance in the material ratio during the reaction in tubular reactor 3, it will eventually reach equilibrium in receiving vessel 7. Then, the precisely calculated amount of adjuvants is added to receiving vessel 7 to obtain the finished glyphosate salt aqueous solution that meets quality requirements.

[0083] After one batch of production is completed, mixing vessel 2 becomes idle and can continue producing the next batch. However, receiving vessel 7 is not yet idle and requires further reaction and the addition of additives. To prevent receiving vessel 7 from affecting the continuous production of mixing vessel 2, this invention uses multiple receiving vessels 7. After mixing vessel 2 completes the production of the previous batch, it continues to produce the current batch using other receiving vessels 7. After mixing vessel 2 completes the production of the current batch, the receiving vessel 7 from the previous batch becomes idle again. This alternating use of receiving vessels 7 achieves continuous production of glyphosate salt aqueous solutions. Moreover, this invention does not require a large number of reaction vessels; only one mixing vessel and at least two receiving vessels are needed to achieve continuous production.

[0084] The present invention has the following beneficial effects:

[0085] 1. This invention mixes glyphosate technical grade and water in a mixing vessel to obtain a solid-liquid slurry. This slurry is then pumped to a tubular reactor via a material transfer pump to react with an alkaline solution, yielding a reaction solution. Finally, the solution is transferred to a receiving vessel to complete the reaction of one batch and add adjuvants. Through the alternating use of the mixing vessel, transfer pump, tubular reactor, and multiple receiving vessels, continuous production using the mixing vessel is achieved. This invention represents a significant breakthrough in the production capacity of glyphosate salt aqueous solutions. Production output is no longer limited by the capacity of existing salt-forming vessels but is determined by the flow rate of the material transfer pump; that is, the production capacity is directly proportional to the output flow rate of the material transfer pump. When capacity needs to be expanded, only the flow rate of the material transfer pump needs to be increased, without increasing the number of salt-forming vessels. This completely changes the original production model. One production system can not only meet the production capacity of multiple independent salt-forming vessels but also meet the delivery requirements of large orders within a short timeframe, with low operating costs.

[0086] 2. The neutralization reaction of glyphosate technical with alkaline solution takes place in a tubular reactor. The tubular reactor is sealed, and the inlet and outlet are connected to sealed pipes. The liquid inside the tubular reactor and the liquid inside the pipes are equivalent to a liquid seal, which makes the liquid level of the liquid seal very high. The glyphosate acid reacts fully with the alkaline substances, and there is no amine or ammonia odor overflow. This avoids the problem of tail gas absorption, improves the production environment, and is safe and environmentally friendly.

[0087] 3. Within a single batch, the entire process from material input to finished product output is continuously automated. Two receiving vessels are set up for batch switching, and the input, output, and product quality of each batch are precisely controlled, thus fully ensuring product quality.

[0088] In this invention, after a batch of production is completed in the mixing vessel 2, all materials in the mixing vessel 2, the solid-liquid mixture conveying pipeline 16, the tubular reactor 3, and the reaction liquid conveying pipeline 22 need to be conveyed to the receiving vessel 7 by the material conveying pump 4 to achieve precise control of the quality of a batch of products. To prevent the material conveying pump 4 from failing to empty all materials and convey them to the receiving vessel 7, resulting in residual materials in the solid-liquid mixture conveying pipeline, the tubular reactor, and the reaction liquid conveying pipeline, which would affect the quality of a batch of products, this invention connects a compressed air pipeline 36 to the solid-liquid mixture conveying pipeline 16. The compressed air pipeline 36 is connected to an external air source, which can be a compressed air tank or an air compressor, etc. An air control valve 37 is installed on the compressed air pipeline 36.

[0089] After a batch of mixing tank 2 is completed and the mixing tank 2 is emptied, the feed valves of each raw material are closed, the discharge control valve 34 is closed, and the air control valve 37 is opened. Compressed air is used to blow the remaining material in the solid-liquid mixture slurry conveying pipeline 16, tubular reactor 3, material conveying pump 4, and reaction liquid conveying pipeline 22 into the receiving tank 7 to prevent material residue from causing the product quality in the receiving tank 7 to be unable to be accurately controlled.

[0090] The solid-liquid mixture slurry conveying pipeline 16 is inclined downwards at a certain slope according to the conveying direction of the solid-liquid mixture slurry, so that the pipeline does not accumulate material and the glyphosate technical grade does not precipitate at a material flow velocity of 0.5-1.5 m / s. For example, the inclination angle is A, tanA = 1:2000.

[0091] To further prevent blockage of the solid-liquid mixture slurry conveying pipeline 16, the alkali pipeline 19 is connected to the solid-liquid mixture slurry conveying pipeline 16 through the alkali branch pipe 42. The alkali branch pipe 42 is equipped with a branch alkali valve 43. When the solid-liquid mixture slurry conveying pipeline 16 is blocked, a small amount of alkaline substance is added through the alkali branch pipe 42 to dissolve the glyphosate technical and eliminate the blockage.

[0092] In this invention, the material transfer pump 4 can be installed on the solid-liquid mixture slurry conveying pipeline 16, pumping the solid-liquid mixture slurry into the tubular reactor 3 via positive pressure pumping. Alternatively, the material transfer pump 4 can be installed on the reaction liquid conveying pipeline 22, pumping the solid-liquid mixture slurry via negative pressure adsorption. Preferably, the material transfer pump 4 is installed on the solid-liquid mixture slurry conveying pipeline 16. Compared to installing the material transfer pump 4 on the reaction liquid conveying pipeline 22, the positive pressure pumping provides a higher liquid conveying pressure to the tubular reactor 3. Furthermore, the positive pressure in the tubular reactor 3 can provide a better liquid seal, preventing ammonia or amine gas from escaping.

[0093] The material conveying pump 4 can be located on the solid-liquid mixture conveying pipeline 16 near the tubular reactor 3. The connection between the alkali branch pipe 42 and the solid-liquid mixture conveying pipeline 16 is close to the mixing vessel 2. This can eliminate blockages in various parts of the solid-liquid mixture conveying pipeline 16. The connection between the compressed air pipeline 36 and the solid-liquid mixture conveying pipeline 16 is located before the material conveying pump 4, or more specifically, close to the mixing vessel 2, which makes it easier to blow out the material in the solid-liquid mixture conveying pipeline 16.

[0094] Currently, the solid-liquid ratio of glyphosate technical and water-liquid mixture in the produced products is between 0.5:1 and 2.75:1. Existing technology CN109221243A involves adding alkali solution for pre-reaction in an intermediate tank. For high-content glyphosate aqueous solutions, when the weight ratio of glyphosate technical to water is greater than 2.6, the amount of water is very small while the amount of glyphosate technical is very large. Directly adding alkali solution for reaction causes problems with mass and heat transfer, resulting in localized high concentrations of glyphosate salts and glyphosate salt crystallization blockage at the discharge port, making it impossible to produce high-content glyphosate salts.

[0095] In this invention, glyphosate technical and water form a solid-liquid slurry in mixing vessel 2, which is then transported by material transfer pump 4. When the solid-liquid ratio of the slurry is between 0.5:1 and 1.2:1, pumping is relatively convenient. For products with higher solid-liquid ratios, to prevent difficulties in transport by material transfer pump 4 and in stirring within mixing vessel 2, this invention connects the reaction liquid transport pipe 22 to the return port 39 of mixing vessel 2 via a return liquid pipe 38. The return liquid pipe 38 is equipped with a return liquid valve 40 and a return liquid flow meter 41. By returning the reaction liquid to mixing vessel 2, the solid-liquid ratio of the slurry is reduced. The return flow rate of the reaction liquid is equal to the glyphosate technical flow rate minus the water flow rate.

[0096] Preferably, the connection between the return liquid pipe 38 and the reaction liquid delivery pipe 22 can be located after the cooling device, so that the reaction liquid is cooled and then returned to the mixing vessel 2.

[0097] The present invention does not limit the specific implementation of the cooling device. In one example, the cooling device includes a cooler 6, which is installed on the reaction liquid conveying pipeline 22. The reaction liquid outlet 18 of the tubular reactor 3 is connected to the reaction liquid inlet of the cooler 6 through a section of the reaction liquid conveying pipeline 22. The reaction liquid outlet of the cooler 6 is connected in parallel to the reaction liquid inlet 23 of each receiving vessel 7 through the other section of the reaction liquid conveying pipeline 22.

[0098] Cooler 6 can be a shell-and-tube cooler with a cooling area of ​​50–500 m². 2 Preferably 100-300m 2 The reaction liquid enters the tube, and the coolant enters the space between the tubes.

[0099] In another example, the cooling device includes a cooling sleeve 5, which is fitted over the outside of the tubular reactor 3, and has a coolant inlet 44 and a coolant outlet 45.

[0100] Furthermore, the cooling sleeve 5 can be used in conjunction with the cooler 6. The cooling sleeve 5 can be used to initially cool the reaction liquid after neutralization to 50-65°C, and then the liquid can be cooled to 35-45°C by the cooler 6.

[0101] like Figure 2-11 As shown, the tubular reactor 3 of the present invention includes a tubular shell 46 with flanges at both ends for easy connection to upstream and downstream pipes. A mixing unit is provided inside the tubular shell 46. A slurry inlet 17 and a reaction liquid outlet 18 are respectively located at both ends of the tubular shell 46. The alkali inlet 20 of the tubular reactor 3 is located on the side of the tubular shell 46 near the slurry inlet 17.

[0102] The end of the alkali pipe 19 is inserted into the tubular shell 46 through the alkali inlet 20. The direction of alkali flow at the end of the alkali pipe 19 is opposite to the direction of solid-liquid mixture conveying inside the tubular shell 46. The alkali fluid forms a vortex here to promote uniform mixing and full reaction of the materials.

[0103] For example, the alkali pipe 19 is vertically inserted into the center or near the center of the tubular housing 46. The end of the alkali pipe 19 has a beveled cut at an acute angle to the axis of the alkali pipe 19, for example, 30 degrees. The beveled cut is oriented in the opposite direction to the conveying direction of the solid-liquid mixture slurry, so that the alkali outflow direction is opposite to the conveying direction of the solid-liquid mixture slurry.

[0104] Alternatively, the end of the alkali pipe 19 is bent in the opposite direction to the conveying direction of the solid-liquid mixture slurry, so that the alkali outflow direction is opposite to the conveying direction of the solid-liquid mixture slurry.

[0105] The mixing unit is used to ensure thorough mixing of materials within the tubular reactor 3. The mixing unit may include an externally powered mixing device 47 or 48 (e.g., Figure 5 , 11 (as shown), fluid-driven mixing device 49 (e.g.) Figure 7 , 9 (as shown) and fixed mixing device 50 (e.g.) Figure 2 , 5 One or more of the following (as shown in Figures 7 and 11). The number of hybrid component units can be multiple, and they can be installed individually or in combination.

[0106] Externally powered hybrid devices 47 or 48 are devices driven by external power sources such as motors, for example... Figure 5 , 11As shown, it includes a stirring blade 51, which is axially or vertically installed inside the tubular housing 46, and the stirring blade 51 is connected to an external power source 52 outside the tubular housing 46.

[0107] For example, such as Figure 5 , 6 As shown, the stirring blade 51 is an open turbine blade or a helical propulsion blade, which is axially installed on the tubular shell 46, so that the fluid moves radially while moving axially, promoting uniform mixing and full reaction of materials.

[0108] For example, the externally powered mixing device can be an electric vertical small reactor with an open turbine impeller; or the externally powered mixing device can be a vertical or horizontal pipeline pump 53, such as... Figure 11 As shown, the impeller of the pipeline pump 53 is an open turbine blade.

[0109] The fluid-driven mixing device 49 is a device that requires no external power and is driven to rotate solely by the liquid within the tubular housing 46, such as... Figure 7-10 As shown, it includes rotating propeller blades 54, which can be manufactured with a helix angle of 30-40°, and 3-6 blades are evenly distributed to form the propeller. Two rotating bearings are installed at the center of the propeller shaft. Figure 8 , 10 As shown, a support frame is provided inside the tubular housing 46. Rotating propeller blades 54 are mounted inside the tubular housing 46 via rotating bearings 55 and the support frame 56. Multiple rotating propeller blades 54 are installed alternately in forward and reverse rotation. When the fluid flows axially, it drives the propeller blades to rotate, causing the fluid to move radially while moving axially, promoting uniform mixing and thorough reaction of the materials.

[0110] The stationary mixing device 50 is a device that remains stationary, such as... Figure 2-5 As shown in Figures 7 and 11, it includes fixed spiral plates 57 and 58, which are fixedly installed inside the tubular housing 46. The fixed spiral plates 57 and 58 are installed in an alternating manner of left-hand and right-hand rotation.

[0111] For example, the fixed spiral blades 57 and 58 can be selected as SK, SL, or SX types. Figure 4 As shown, the SK-type spiral blade, which is a rotating blade twisted 180°, is divided into right-hand and left-hand spiral blades. During installation, right-hand spiral blades 57 and left-hand spiral blades 58 are installed alternately. Left-hand blades should be rotated 90° before welding for better cutting effect. According to the diameter of the tubular shell 46, four spiral blades with the same rotation direction are selected and welded together as a group. Each group of spiral blades is fixed inside the tubular shell 46 with opposite rotation directions.

[0112] In this invention, in addition to the valves and flow meters mentioned above, corresponding valves and flow meters can be installed on various pipelines not mentioned above as needed.

[0113] This invention also provides a production method for the aforementioned glyphosate salt aqueous solution production system, the method comprising:

[0114] S1: Calculate the ratio of glyphosate technical and water according to the requirements of glyphosate salt aqueous solution. Open the technical feed hopper 1 and the water feed valve 27. Continuously add the glyphosate technical in the technical feed hopper 1 and the water in the water storage tank 8 into the mixing vessel 2 at the addition rate corresponding to the calculated ratio. Turn on the mixing vessel agitator 11 to form a solid-liquid mixture slurry under the action of agitation.

[0115] S2: When the solid-liquid mixture slurry in the mixing vessel 2 accumulates to the minimum set amount, the discharge port control valve 34, the material conveying pump 4, and the reaction liquid feed valve 31 of one of the idle receiving vessels 7 are opened, and the solid-liquid mixture slurry is conveyed to the tubular reactor 3 by the material conveying pump 4.

[0116] At the same time, the alkali feed valve 29 is opened, and the alkali in the alkali storage tank 9 is continuously added to the tubular reactor 3 at the set addition rate. The solid-liquid mixture slurry and the alkali react in the tubular reactor 3 to generate a reaction liquid.

[0117] S3: Turn on the cooling device to cool the reaction liquid to the set temperature and then transport it into the receiving vessel 7 with the reaction liquid feed valve 31 turned on.

[0118] S4: Turn on the agitator 21 in the receiving vessel to ensure that the reaction liquid reacts completely and mixes evenly in the receiving vessel 7.

[0119] S5: After the set batch of glyphosate technical, water, and alkali solution has been used up, close the technical feed hopper 1, water feed valve 27, and alkali feed valve 29. Use the material pump 4 to transfer all transportable materials from the mixing vessel 1, solid-liquid mixture conveying pipeline 16, tubular reactor 3, and reaction liquid conveying pipeline 22 into the receiving vessel 7. Close the open reaction liquid feed valve 31 and open the remaining empty receiving vessel's reaction liquid feed valve to begin the next batch of production.

[0120] At the same time, open the auxiliary agent feed valve 32 corresponding to the receiving vessel used in this batch, add the set amount of auxiliary agent, dye paste, etc. into the receiving vessel 7, and after stirring evenly and sampling analysis is qualified, transfer the finished product to the finished product vessel through the filter.

[0121] As an improvement, when a compressed air pipe 36 is connected to the solid-liquid mixture conveying pipe 16, S5 includes:

[0122] Once the set batch of glyphosate technical, water, and alkali solution has been used up, close the technical feed hopper 1, water feed valve 27, and alkali feed valve 29. Use the material pump 4 to transfer all transportable materials from the mixing vessel 2, solid-liquid mixture conveying pipe 16, tubular reactor 3, and reaction liquid conveying pipe 22 into the receiving vessel 7. Close the discharge control valve 34 and open the air control valve 37. Use compressed air to blow any remaining material from the solid-liquid mixture conveying pipe 16, tubular reactor 3, and reaction liquid conveying pipe 22 into the receiving vessel 7. Close the opened reaction liquid feed valve and open the remaining empty receiving vessel's reaction liquid feed valve to begin the next batch of production.

[0123] At the same time, open the auxiliary agent feed valve 32 corresponding to the receiving vessel used in this batch, add the set amount of auxiliary agent, dye paste, etc. into the receiving vessel 7, and after stirring evenly and sampling analysis is qualified, transfer the finished product to the finished product vessel through the filter.

[0124] As another improvement, when the reaction liquid delivery pipe 22 is connected to the return port 39 of the mixing vessel 2 via the return pipe 38, S2 further includes:

[0125] If the ratio of glyphosate technical and water causes the solid-liquid ratio of the solid-liquid mixture to be greater than the set ratio, the return valve 40 is opened to return the reaction liquid in the reaction liquid delivery pipeline 22 to the mixing vessel 2 at the set flow rate. The return flow of the reaction liquid to the mixing vessel 2 reduces the solid-liquid ratio of the solid-liquid mixture. The return flow rate of the reaction liquid is equal to the flow rate of glyphosate technical minus the flow rate of water.

[0126] The aforementioned minimum set amount of solid-liquid mixture slurry is the minimum amount to ensure that the material conveying pump 4 does not run dry during normal conveying. The cumulative amount in the mixing tank can be controlled between 2000 and 5000 kg.

[0127] The method of the present invention is illustrated below with several detailed test examples. In each test example, a mortar pump of model 80UHB-50-50 with a flow rate of 50 m³ / h was used as the material conveying pump 4. 3 / h, with a head of 50m. Tubular reactor 4 is selected with... Figure 2 The structure shown has a diameter of 200mm and a length of 2075mm. It contains 14 sets of fixed spiral blades, each set of which is installed alternately in opposite directions of rotation inside the tube. Each set of fixed spiral blades consists of 4 SK-type rotating spiral blades twisted 180°.

[0128] Experimental Example 1:

[0129] 360a.eg / L glyphosate isopropylamine salt.

[0130] Calculated batch feed amounts: 10800 kg of 95% glyphosate technical grade, 5850 kg of 70% isopropylamine, 13140 kg of deionized water, and 3300 kg of adjuvants. The solid-liquid ratio of glyphosate technical grade to water is 0.82:1. The addition rate of glyphosate technical grade is 16200 kg / h, and the addition rate of deionized water is 19710 kg / h.

[0131] Turn on the cooling equipment, turn on the mixer 11 and the receiving tank mixer 21; turn on the water inlet valve 27 and the raw material feeding hopper 1 to add deionized water and glyphosate technical into the mixing tank 2. Under the action of stirring, the water and glyphosate technical are mixed into a solid-liquid mixture.

[0132] When the mixing vessel 2 contains a certain amount of solid-liquid mixture, the discharge control valve 34 is opened, the isopropylamine feed valve 29 is opened, the isopropylamine addition rate is 8775 kg / h, and the material conveying pump 4 is started. The solid-liquid mixture from the mixing vessel 2 undergoes a neutralization reaction with isopropylamine in the tubular reactor 3 via the material conveying pump 4. The exothermic neutralization reaction of the reaction liquid passes through the cooler 6, and the temperature is controlled to ≤40℃ before entering the receiving vessel 7, where the reaction liquid further undergoes complete reaction and homogenization. During the conveying process, the solid-liquid mixture completes the neutralization reaction in the tubular reactor 3, and the material is transformed into a clear and transparent liquid.

[0133] Once the raw and auxiliary materials for this batch have been used up, close all raw and auxiliary material feed valves. Empty the material in mixing vessel 2 using material transfer pump 4, and close the discharge control valve 34 of mixing vessel 2. Blow out any remaining material in the pipeline with compressed air by opening air control valve 37, and the material enters receiving vessel 7. Repeat the above steps for the next batch of production, switching the reactants to another receiving vessel.

[0134] After the materials in receiving vessel 7 are thoroughly mixed and reacted, the auxiliary agent is added through auxiliary agent inlet valve 32, and water is added through the deionized water flow regulating valve. The approved reaction liquid weight is 33096 kg. The required dye is then added, stirred thoroughly, and sampled for analysis and testing. The analysis shows a content of 31.2%, density of 1.16, pH value of 5.1, and a clear, transparent liquid appearance, indicating the product is qualified. The product is then filtered and transferred to the finished product storage tank for packaging into finished products.

[0135] Another sample was refrigerated at 0-5℃ for 7 days: it passed the test.

[0136] Samples were stored at 54℃ for 14 days: qualified.

[0137] The material conveying pump 4 of this batch runs for about 40 minutes, and the production capacity of 360a.eg / L glyphosate isopropylamine salt is 33096kg.

[0138] Experimental Example 2:

[0139] 33% glyphosate ammonium salt.

[0140] Calculated batch feed amounts: 10800 kg of 95% glyphosate technical grade, 1725 kg of 100% ammonia, 18255 kg of deionized water, and 3420 kg of adjuvants. The solid-liquid ratio of glyphosate technical grade to water is 0.59:1. The addition rates of glyphosate technical grade are 16200 kg / h, deionized water is 27382 kg / h, and ammonia is 2588 kg / h.

[0141] The specific process is similar to that of Experiment 1 and will not be repeated here. The final approved reaction solution weight was 34,200 kg. The required dye was added, stirred thoroughly, and then a sample was taken for analysis and testing. The analysis showed a content of 30.0%, a density of 1.19, a pH value of 5.1, and a clear, transparent appearance, indicating the product was qualified. It was then filtered and transferred to a finished product storage tank for packaging into the final product.

[0142] Another sample was refrigerated at 0-5℃ for 7 days: it passed the test.

[0143] Samples were stored at 54℃ for 14 days: qualified.

[0144] The material conveying pump 4 for this batch runs for approximately 40 minutes, with a production capacity of 34,200 kg of 33% glyphosate ammonium salt.

[0145] Experimental Example 3:

[0146] 540a.eg / L glyphosate potassium salt.

[0147] Calculated batch feed amounts: 16200 kg of 95% glyphosate technical grade, 12900 kg of 48% potassium hydroxide, 6750 kg of deionized water, and 3990 kg of adjuvants. The glyphosate technical grade is added at a rate of 16200 kg / h, and the deionized water is added at a rate of 6750 kg / h. Since the solid-liquid ratio of glyphosate technical grade to water is 2.4:1, which is relatively high, a portion of the reaction solution needs to be refluxed back into mixing vessel 2. The reflux flow rate is equal to the glyphosate technical grade flow rate minus the deionized water flow rate, i.e., the reflux flow rate is 9450 kg / h.

[0148] Turn on the cooling equipment, and turn on the agitator 11 of the mixing vessel and the agitator 21 of the receiving vessel. Open the water inlet valve 27 and the technical material feeding hopper 1 to add deionized water and glyphosate technical material into the mixing vessel 2. Under the action of stirring, the water and glyphosate technical material are mixed into a solid-liquid mixture. When there is a certain amount of solid-liquid mixture in the mixing vessel 2, open the return valve 40, and part of the reaction liquid returns to the mixing vessel 2, while part of the reaction liquid enters the receiving vessel 7. Open the isoalkali inlet valve 29, and add potassium hydroxide at a rate of 12900 kg / h. Turn on the material conveying pump 4. The solid-liquid mixture from the mixing vessel 2 undergoes a neutralization reaction with potassium hydroxide in the tubular reactor 3 via the material conveying pump 4. The neutralization reaction of the reaction liquid is exothermic. After passing through the cooler 6, the temperature is controlled to be ≤40℃. Part of the reaction liquid returns to the mixing vessel 2 to maintain a certain solid-liquid ratio, while part of the reaction liquid enters the receiving vessel 7, where the reaction liquid is further completely reacted and mixed evenly. During the transport process, the solid-liquid mixture undergoes a neutralization reaction within the tubular reactor 3, transforming the material into a clear and transparent liquid.

[0149] After the raw and auxiliary materials for this batch have been used up, close all raw and auxiliary material feed valves and close the return valve 40. All reaction liquid will then enter the receiving vessel 7. The material transfer pump 4 will evacuate the material from the mixing vessel 2, and the discharge control valve 34 of the mixing vessel 2 will be closed. Any remaining material in the pipeline will be blown out with compressed air by opening the air control valve 37, and the material will then enter the receiving vessel 7. Repeat the above steps for the next batch of production, switching the reaction material to another receiving vessel.

[0150] After the materials in receiving vessel 7 have been thoroughly mixed and reacted, 3990 kg of additives are added through additive feed valve 32, and water is added through deionized water flow regulating valve to bring the approved reaction liquid weight to 39870 kg. Brown dye is then added, stirred thoroughly, and sampled for analysis. Analysis shows a content of 38.6%, density of 1.40, pH of 5.3, and an appearance of a clear, brown liquid, indicating the product is qualified. The product is then filtered and transferred to the finished product storage tank for packaging into finished products.

[0151] Another sample was refrigerated at 0-℃ for 7 days: qualified.

[0152] Samples were stored at 54℃ for 14 days: qualified.

[0153] The material conveying pump 4 in this batch runs for about 60 minutes, and the production capacity of 540a.eg / L glyphosate potassium salt is 39870kg.

[0154] Experimental Example 4:

[0155] 608 g / L glyphosate dimethylamine salt.

[0156] Calculated batch feed amounts: 14400 kg of 95% glyphosate technical grade, 11100 kg of 40% dimethylamine, 5280 kg of deionized water, and 3420 kg of adjuvants. The addition rates of glyphosate technical grade are 21600 kg / h, deionized water is 7920 kg / h, and dimethylamine is 16650 kg / h. Since the solid-liquid ratio of glyphosate technical grade to water is 2.73:1, this high ratio necessitates partial reflux of the reaction mixture into mixing vessel 2. The reflux flow rate is equal to the glyphosate technical grade flow rate minus the deionized water flow rate, i.e., a reflux flow rate of 13680 kg / h.

[0157] The specific process is similar to that of Experiment 3 and will not be repeated here. Finally, 3420 kg of additive was added through additive feed valve 32. Appropriate amounts of water were added by adjusting the deionized water flow rate, and the approved reaction solution weight was 34200 kg. Yellow dye was added, stirred thoroughly, and then a sample was taken for analysis and testing. The analysis showed a content of 39.1%, a density of 1.23, a pH value of 4.9, and an appearance of a clear, transparent yellow liquid, indicating the product was qualified. The product was then filtered and transferred to a finished product storage tank for packaging into finished products.

[0158] Another sample was refrigerated at 0-℃ for 7 days: qualified.

[0159] Samples were stored at 54℃ for 14 days: qualified.

[0160] The material conveying pump 4 of this batch runs for about 40 minutes, and the production capacity of 608g / L glyphosate dimethyl salt is 34,200kg.

[0161] Finally, it should be noted that the above-described embodiments are merely specific implementations of the present invention, used to illustrate the technical solutions of the present invention, and not to limit it. The scope of protection of the present invention is not limited thereto. Although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that any person skilled in the art can still modify or easily conceive of changes to the technical solutions described in the foregoing embodiments within the scope of the technology disclosed in the present invention, or make equivalent substitutions for some of the technical features; and these modifications, changes, or substitutions do not cause the essence of the corresponding technical solutions to deviate from the spirit and scope of the technical solutions of the embodiments of the present invention. All should be covered within the scope of protection of the present invention. Therefore, the scope of protection of the present invention should be determined by the scope of the claims.

Claims

1. A glyphosate salt aqueous solution production system, characterized in that, It includes a raw material feeding hopper, a mixing vessel, a tubular reactor, a material conveying pump, a cooling device, a receiving vessel, a water storage tank, an alkali storage tank, and an auxiliary agent storage tank, wherein: The mixing vessel is equipped with a mixing vessel agitator. The raw material feeding hopper is connected to the raw material inlet of the mixing vessel. The water storage tank is connected to the water inlet of the mixing vessel through a water supply pipe. The discharge port of the mixing vessel is connected to the slurry inlet of the tubular reactor through a solid-liquid slurry conveying pipe. The alkali storage tank is connected to the alkali inlet of the tubular reactor through an alkali pipe. The number of receiving vessels is at least two, and each receiving vessel is equipped with a receiving vessel agitator. The reaction liquid outlet of the tubular reactor is connected in parallel to the reaction liquid inlet of each receiving vessel through a reaction liquid delivery pipeline. The auxiliary agent storage tank is connected in parallel to the auxiliary agent inlet of each receiving vessel through an auxiliary agent pipeline. The material conveying pump is installed on the solid-liquid mixture slurry conveying pipeline, and the cooling device is installed on the tubular reactor and / or the reaction liquid conveying pipeline; The raw material feeding hopper is equipped with a feeding device and a metering device; the water supply pipe is equipped with a water inlet valve and a water flow meter; the alkali solution pipe is equipped with an alkali solution inlet valve and an alkali solution flow meter; the reaction liquid conveying pipe is equipped with a reaction liquid inlet valve for each receiving vessel; the auxiliary agent pipe is equipped with an auxiliary agent inlet valve and an auxiliary agent flow meter for each receiving vessel; and the discharge port of the mixing vessel is equipped with a discharge port control valve. The solid-liquid mixture slurry conveying pipeline is connected to a compressed air pipeline, which is connected to an air source and is equipped with an air control valve. The alkali pipeline is connected to the solid-liquid mixture slurry conveying pipeline through an alkali branch pipe, and a branch pipe alkali valve is provided on the alkali branch pipe. The reaction liquid delivery pipeline is connected to the return port of the mixing vessel through a return liquid pipeline, and the return liquid pipeline is equipped with a return liquid valve and a return liquid flow meter.

2. The glyphosate salt aqueous solution production system according to claim 1, characterized in that, The material conveying pump is installed on the solid-liquid mixture conveying pipeline and close to the tubular reactor. The connection between the alkali branch pipe and the solid-liquid mixture conveying pipeline is close to the mixing vessel. The connection between the compressed air pipeline and the solid-liquid mixture conveying pipeline is located before the material conveying pump.

3. The glyphosate salt aqueous solution production system according to claim 1, characterized in that, The solid-liquid mixture slurry conveying pipeline is inclined downwards at a certain slope in accordance with the conveying direction of the solid-liquid mixture slurry.

4. The glyphosate salt aqueous solution production system according to claim 1, characterized in that, The connection between the return liquid pipeline and the reaction liquid delivery pipeline is located after the cooling device.

5. The glyphosate salt aqueous solution production system according to claim 1, characterized in that, The cooling device includes a cooler, which is installed on the reaction liquid delivery pipeline. The reaction liquid outlet of the tubular reactor is connected to the reaction liquid inlet of the cooler through a section of the reaction liquid delivery pipeline, and the reaction liquid outlet of the cooler is connected in parallel to the reaction liquid inlet of each receiving vessel through the other section of the reaction liquid delivery pipeline.

6. The glyphosate salt aqueous solution production system according to claim 1 or 5, characterized in that, The cooling device includes a cooling sleeve that is fitted over the outside of the tubular reactor. The cooling sleeve has a coolant inlet and a coolant outlet.

7. The glyphosate salt aqueous solution production system according to any one of claims 1-3, characterized in that, The tubular reactor includes a tubular shell, inside which a mixing unit is disposed. The slurry inlet and the reaction liquid outlet are respectively disposed at both ends of the tubular shell, and the alkali inlet of the tubular reactor is located on the side of the tubular shell near the slurry inlet.

8. The glyphosate salt aqueous solution production system according to claim 7, characterized in that, The end of the alkali pipe is inserted into the tubular shell through the alkali inlet, and the direction of alkali outflow from the end of the alkali pipe is opposite to the direction of conveying the solid-liquid mixture slurry inside the tubular shell.

9. The glyphosate salt aqueous solution production system according to claim 8, characterized in that, The end of the alkali solution pipeline has a beveled cut, the direction of which is opposite to the conveying direction of the solid-liquid mixture slurry; Alternatively, the end of the alkali pipe may be bent in the opposite direction to the conveying direction of the solid-liquid mixture slurry.

10. The glyphosate salt aqueous solution production system according to claim 7, characterized in that, The mixing unit includes one or more of the following: an externally powered mixing device, a fluid-driven mixing device, and a stationary mixing device.

11. The glyphosate salt aqueous solution production system according to claim 10, characterized in that, The externally powered mixing device includes a stirring blade, which is axially mounted inside the tubular housing and connected to an external power source outside the tubular housing. The fluid-driven mixing device includes a rotating propeller blade, which is installed inside the tubular housing via a rotating bearing and a support frame, and the rotating propeller blade is installed in an alternating manner of forward and reverse rotation. The fixed mixing device includes a fixed spiral blade, which is fixedly installed inside the tubular housing. The fixed spiral blade is installed in an alternating left-handed and right-handed manner.

12. A method for producing glyphosate salt aqueous solution according to any one of claims 1-11, characterized in that, The method includes: S1: Calculate the ratio of glyphosate technical and water according to the requirements of the finished glyphosate salt aqueous solution. Open the technical feed hopper and water inlet valve. Continuously add the glyphosate technical from the technical feed hopper and the water from the water storage tank into the mixing vessel at the addition rate corresponding to the calculated ratio. Turn on the agitator of the mixing vessel to form a solid-liquid slurry under the action of agitation. S2: When the solid-liquid mixture slurry in the mixing vessel accumulates to the minimum set amount, the discharge port control valve, the material conveying pump, and the reaction liquid feed valve of one of the idle receiving vessels are opened, and the solid-liquid mixture slurry is conveyed to the tubular reactor through the material conveying pump; Simultaneously, the alkali feed valve is opened, and the alkali in the alkali storage tank is continuously added to the tubular reactor at a set addition rate. The solid-liquid mixture slurry reacts with the alkali in the tubular reactor to generate a reaction liquid. S3: Turn on the cooling device to cool the reaction liquid to the set temperature and then send it into the receiving vessel of the opened reaction liquid feed valve; S4: Turn on the agitator of the receiving vessel to ensure that the reaction solution reacts completely and mixes evenly in the receiving vessel; S5: After the set batch of glyphosate technical, water, and alkali solution has been used up, close the technical feed hopper, water feed valve, and alkali solution feed valve. Use the material conveying pump to transport all the materials that can be conveyed in the mixing tank, solid-liquid mixture conveying pipeline, tubular reactor, and reaction liquid conveying pipeline into the receiving tank. Close the open reaction liquid feed valve and open the reaction liquid feed valve of the remaining empty receiving tank to start the next batch of production. At the same time, open the auxiliary agent feed valve corresponding to the receiving vessel used in this batch, add the set amount of auxiliary agent into the receiving vessel, and transfer the finished product after it is stirred evenly and the sample analysis is qualified.

13. The method according to claim 12, characterized in that, S5 includes: Once the set batch of glyphosate technical, water, and alkali solution has been used up, close the technical feed hopper, water inlet valve, and alkali solution inlet valve. Use the material pump to transfer all transportable materials from the mixing vessel, solid-liquid slurry conveying pipeline, tubular reactor, and reaction liquid conveying pipeline into the receiving vessel. Close the outlet control valve and open the air control valve to blow any remaining material from the solid-liquid slurry conveying pipeline, tubular reactor, and reaction liquid conveying pipeline into the receiving vessel using compressed air. Close the opened reaction liquid inlet valve and open the reaction liquid inlet valve of the remaining empty receiving vessel to begin production for the next batch. Simultaneously, open the auxiliary agent feed valve corresponding to the receiving vessel used in this batch, add the set amount of auxiliary agent into the receiving vessel, and after stirring evenly and sampling analysis is qualified, transfer the obtained glyphosate salt aqueous solution product.

14. The method according to claim 13, characterized in that, S2 further includes: If the ratio of glyphosate technical and water results in a solid-liquid ratio in the solid-liquid mixture that is greater than a set value, the return valve is opened to return the reaction liquid in the reaction liquid delivery pipeline to the mixing vessel at a set flow rate.

15. The method according to any one of claims 12-14, characterized in that, The minimum set quantity of the solid-liquid mixture slurry is the minimum quantity that ensures the material conveying pump does not run dry during normal conveying.

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