Method for continuously producing glyphosate isopropylamine salt aqueous solution

Abstract

The invention discloses a method for continuously producing a glyphosate isopropylamine salt aqueous solution, and belongs to the technical field of pesticide preparation production. Compared with a traditional intermittent production process, the continuous production process has the advantages that equipment is intelligently upgraded, high-precision automatic metering equipment is controlled by adopting a DCS (Distributed Control System), flow speed is controlled to realize precise gradient feeding, and after strict quality inspection of reaction raw materials, continuous production is carried out in a stirred tank reactor provided with an anti-explosion system and a waste gas absorption device; the defect that quality control is difficult due to manual operation is overcome, and the danger that an operator is prone to poisoning, combustion and explosion due to the fact that isopropylamine is low in boiling point and drastically releases heat when reacting with glyphosate raw acid is avoided. The content of effective components of the prepared product is stabilized at 62% + / -0.5%, the product quality consistency is good, and the product better conforms to the general direction of modern green automatic intelligent manufacturing.

Description

Technical Field

[0001] The invention belongs to the technical field of pesticide preparation production, and specifically relates to a method for continuously producing glyphosate isopropylamine salt solution, and in particular to a production process innovation of 62% glyphosate isopropylamine salt solution. Background Art

[0002] Glyphosate is an effective active chemical ingredient in many widely used herbicides, used for chemical weed control in orchards, mulberry gardens, tea plantations, rubber plantations, forest firebreaks, railways, highways and no-till land.

[0003] Glyphosate API can be processed into 10% glyphosate aqueous solution, 41% glyphosate isopropylamine salt solution, and 62% glyphosate isopropylamine salt solution.

[0004] At present, there are many problems in the production of 62% glyphosate isopropylamine salt solution:

[0005] 1. Traditional intermittent production has obvious disadvantages: intermittent production requires repeated feeding, reaction, separation and other operations. The equipment preparation work before each production is cumbersome, the production cycle is long, the equipment utilization rate is low, and it cannot meet the large-scale market demand.

[0006] 2. Quality control difficulties: There are many manual operation links, and errors are prone to occur in material ratio, reaction temperature and time control, resulting in uneven product quality and large fluctuations in the content of effective ingredients, which affects the weed control effect and product reputation.

[0007] 3. High cost and environmental pressure: Frequent equipment start and stop increase energy consumption, material transfer process is prone to waste, and production cost is high. At the same time, improper treatment of waste gas and wastewater generated in the production process will pollute the environment.

[0008] In order to solve the above defects, a technical solution is now provided. Summary of the invention

[0009] In order to overcome the above technical problems, the purpose of the present invention is to provide a method for continuously producing glyphosate isopropylamine salt solution, and in particular to an innovative production process for 62% glyphosate isopropylamine salt solution.

[0010] Compared with the traditional intermittent production process, the present invention uses DCS to control high-precision automatic metering equipment through intelligent equipment upgrade, strictly follows the formula ratio, and accurately meters the feed; uses a stirred tank reactor for continuous reaction; the product after the reaction is filtered through a bag filter and a plate and frame filter in turn, effectively intercepting unreacted solid particles and mechanical impurities; the filtered glyphosate isopropylamine solution enters the preparation system, and according to the preset formula, water and additives are added to the DCS to adjust the content and pH to ensure that the product quality accurately meets the quality standard of 62% glyphosate isopropylamine salt solution. The present invention overcomes the defects of intermittent production that requires repeated feeding, reaction, separation and other operations, and manual operation quality control is difficult. The content of the active ingredient of the product prepared by the present invention is stable at 62% ± 0.5%, the product quality consistency is good, and the weed control effect is reliable.

[0011] To achieve the above objectives, the technical solution provided by the present invention is as follows:

[0012] A method for continuously producing glyphosate isopropylamine salt water agent comprises: using DCS to control high-precision automatic metering equipment, continuously feeding raw materials into a stirred tank reactor at a set flow rate according to the raw material formula, controlling the reaction temperature to be 65°C-85°C for continuous reaction; after the reaction is complete, the glyphosate isopropylamine salt water agent is obtained through salt formation, preparation and packaging processes.

[0013] In some embodiments, the raw material formula includes, by weight: 10-20 parts of glyphosate, 15-20 parts of isopropylamine, 10-20 parts of adjuvant and 30-40 parts of water;

[0014] In some embodiments, the flow rate is 1-10 L / min.

[0015] In some embodiments, the stirred tank reactor is equipped with an explosion-proof system and an exhaust gas absorption device.

[0016] In some embodiments, the method for continuously producing glyphosate isopropylamine salt solution comprises the following steps:

[0017] (1) Precision pretreatment of raw materials:

[0018] Adopt DCS to control high-precision automatic metering equipment, strictly follow the raw material formula ratio, and accurately meter the feeding of glyphosate technical, isopropylamine, water and additives;

[0019] (2) Continuous reaction intensification:

[0020] The original drug is continuously fed into the stirred tank reactor at a set flow rate for continuous reaction, and the reaction temperature is precisely controlled to be 65°C-85°C;

[0021] (3) Refining and impurity removal:

[0022] The reaction products are filtered through bag filters and plate and frame filters in turn;

[0023] (4) Preparation and quality control:

[0024] The filtered glyphosate isopropylamine solution enters the preparation system, and the additives and water are added according to the preset formula, and the pH is adjusted to obtain the glyphosate isopropylamine salt solution.

[0025] In some embodiments, the molar ratio of glyphosate to isopropylamine in the raw material formula of step (1) is 1:1.05-1:1.08.

[0026] In some embodiments, in step (1), the purity of glyphosate acid is ≥95%, and the water content of isopropylamine is ≤0.5%, so as to avoid the generation of impurities by side reactions. 2+ / Mg 2+ to prevent the formation of insoluble salts with glyphosate.

[0027] In some embodiments, the flow rate in step (2) is divided into two stages, each with an interval of 30-40 minutes, and the feed is added at a flow rate ratio of 1.2-1.8:1.

[0028] The inventors have found that step (2) can achieve full mixing and rapid reaction of materials with the help of an efficient mixing device in the reactor. The heat generated by the reaction maintains the temperature of the reaction system stable, thereby improving the reaction conversion rate and selectivity.

[0029] The inventors found that the reactor in step (2) is equipped with an explosion-proof system and a waste gas absorption device (activated carbon adsorption + alkaline solution washing), which further increases the safety of the reaction.

[0030] The inventors have found that the reaction product in step (3) is filtered through a bag filter and then a plate and frame filter, thereby effectively retaining unreacted solid particles and mechanical impurities, further improving the purity of the product and reducing the impurity content.

[0031] In some embodiments, the auxiliary agent in step (4) is selected from at least one of a nonionic surfactant, a cationic surfactant and an anionic surfactant.

[0032] In some embodiments, the auxiliary agent in step (4) is selected from at least one of a nonionic surfactant, a cationic surfactant and an anionic surfactant, preferably orange peel essential oil, betaine, alkyl polyglycoside APG0810, and methylated rapeseed oil.

[0033] The basic characteristic of the surfactant used in the present invention is that it helps glyphosate to be absorbed through the stems and leaves of plants and conducted to the point of action, thereby maximizing the efficacy of the drug while also taking into account increasingly stringent environmental protection requirements.

[0034] In some embodiments, the pH in step (4) is 4.5-5.

[0035] In some embodiments, the method further includes automated packaging and tracing: the formulated qualified products are packaged through an automated packaging production line, using quantitative filling equipment to ensure that the volume of each bottle of product is accurate and consistent; at the same time, a product QR code tracing system is introduced to mark the production batch and production date information on the packaging to facilitate product quality tracking and problem tracing.

[0036] In some embodiments, the formula of the glyphosate isopropylamine salt water agent includes:

[0037] Component content (w / w%),

[0038] Glyphosate isopropylamine salt (62%) 62.0,

[0039] Additive 10.0,

[0040] Ammonia (25%) adjusted to pH 4.5-5,

[0041] Deionized water is added to 100%,

[0042] Wherein, the auxiliary agent is selected from at least one of orange peel essential oil, betaine, alkyl polyglycoside APG0810 and methylated rapeseed oil.

[0043] On the other hand, the present invention also provides glyphosate isopropylamine salt water prepared by the above method.

[0044] In a third aspect, the present invention also provides the use of the above-mentioned glyphosate isopropylamine salt water agent.

[0045] Compared with the prior art, this application has the following beneficial effects:

[0046] (1) Compared with the traditional intermittent production process, the present invention adopts intelligent equipment upgrade, DCS-controlled high-precision automatic metering equipment, and equipped with a stirred tank reactor with an explosion-proof system and exhaust gas absorption device, and an automatic packaging production line for production, which is more in line with the general direction of modern green automated intelligent manufacturing.

[0047] (2) DCS-controlled high-precision automatic metering equipment can accurately feed materials. The raw materials are strictly quality inspected, and the production process parameters are optimized. Gradient feeding is adopted: divided into three stages, with a flow rate ratio of 3:5:1 and an interval of 30 minutes. The heat generated by the reaction can maintain the temperature of the reaction system stable, thereby improving the reaction conversion rate and selectivity.

[0048] (3) The continuous reaction is carried out in a stirred tank reactor equipped with an explosion-proof system and an exhaust gas absorption device to avoid the low boiling point of isopropylamine, which reacts violently with glyphosate acid to release heat, and the operator is very likely to be poisoned, burned, or exploded. At the same time, the continuous production mode eliminates the frequent start and stop of equipment and the waiting time in the intermediate links in intermittent production, and the production efficiency is increased by more than 40%, which can quickly respond to changes in market demand.

[0049] (4) The method of the present application has near-zero pollutant emissions, the content of active ingredients in the product is stable at 62%±0.5%, the product quality is consistent, and the weed control effect is reliable. DETAILED DESCRIPTION

[0050] For ease of understanding, the application will be described more fully below, and preferred embodiments of the application are provided. However, the application can be implemented in many different forms and is not limited to the embodiments described herein. On the contrary, the purpose of providing these embodiments is to make the understanding of the disclosure of the present invention more thorough and comprehensive. In the embodiment, if specific techniques or conditions are not indicated, the techniques or conditions described in the document in this area or according to the product specification are carried out. Reagents used or instruments that do not indicate manufacturers are conventional products that can be obtained through the market.

[0051] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as those commonly understood by those skilled in the art of the present invention. The terms used in the specification of the present invention herein are only for the purpose of describing specific embodiments and are not intended to limit the present invention.

[0052] In the present invention, the number of ingredients refers to the number of weight parts.

[0053] In the present invention, meeting the quality standard of 62% glyphosate isopropylamine salt solution means meeting the requirements of GB / T 20684-2017 Glyphosate Aqueous Solution, and the acute oral toxicity is low toxicity (LD50>5000mg / kg). The qualified dilution stability described in the present invention means meeting the requirements of GB / T 20684-2017 standard.

[0054] In the present invention, the continuous production of glyphosate isopropylamine salt solution comprises:

[0055] 1. Equipment selection, installation and commissioning: Based on the production scale and process requirements, select high-precision metering equipment, advanced reactors (preferably continuous stirred tank reactors), efficient plate and frame filtration, and DCS blending and packaging production lines.

[0056] During the installation process, strictly follow the equipment installation manual to ensure that the equipment layout is reasonable and the connection is tight. After the installation is completed, conduct comprehensive debugging, check the equipment operation status, calibrate the measuring instruments, test the functions of the automatic control system, and ensure the normal operation of the equipment.

[0057] 2. Raw material procurement and management: Establish a strict raw material supplier screening system to ensure the stable and reliable quality of glyphosate technical, isopropylamine and adjuvants.

[0058] After the raw materials arrive, they are strictly inspected for quality and can only be stored after they pass the inspection. During the storage process, measures such as moisture-proof, sun-proof, and fire-proof are taken to ensure the quality of the raw materials. Before use, the quality and quantity of the raw materials are checked again to ensure that they meet production requirements.

[0059] Among them, the purity of glyphosate acid is ≥95%, and the water content of isopropylamine is ≤0.5% to avoid the generation of impurities by side reactions. Avoid using products containing Ca 2+ / Mg 2+ to prevent the formation of insoluble salts with glyphosate.

[0060] 3. Production operation process:

[0061] 3.1 Start-up preparation: Check whether the equipment, pipelines, and valves are in normal condition, start the DCS control system, and perform parameter initialization settings. Turn on the delivery pump of the raw material storage tank, slowly deliver the raw materials to the metering device, and wait for production instructions.

[0062] 3.2 Continuous production: After the production order is issued, the DCS control system transports the raw materials to the reactor for reaction according to the preset valve logic and proportion. Monitor the changes in parameters such as reaction temperature to ensure the normal reaction. The reaction products go through the salt formation, blending and packaging processes in sequence. During the production process, the product quality indicators are monitored in real time, and the production parameters are adjusted in time according to the test results.

[0063] 3.3 Shutdown operation: After the production task is completed, stop the raw material delivery pump, shut down the reactor stirring, mixing kettle and packaging production line. Clean the equipment and pipelines, remove residual materials, prevent materials from clogging and corroding the equipment. Keep good production records and equipment maintenance records.

[0064] 4. Quality control and management: Establish a complete quality management system to monitor the quality of the entire process from raw material procurement, production process to product packaging. During the production process, regularly sample and test products, including active ingredient content, pH value, density, impurity content, etc. If any abnormality in product quality is found, immediately analyze the cause and take corresponding measures to make adjustments to ensure that product quality always meets standard requirements.

[0065] In the present invention, ND means not detected.

[0066] Example 1

[0067] A method for continuously producing glyphosate isopropylamine salt solution comprises the following process steps:

[0068] (1) Precision pretreatment of raw materials

[0069] Raw material testing: glyphosate acid purity ≥ 95%, isopropylamine water content ≤ 0.5%, use purified water as the water source.

[0070] Raw material preparation: Under stirring, isopropylamine is dissolved in water at 30°C to prepare an isopropylamine aqueous solution, which is placed in liquid storage tank A; Under stirring, ammonia water is added to glyphosate original acid to prepare a glyphosate ammonia aqueous solution, which is placed in liquid storage tank B; alkyl polyglycoside APG0810 is dissolved in water to prepare an APG0810 aqueous solution, which is placed in liquid storage tank C;

[0071] (2) Continuous reaction intensification

[0072] Start the DCS control system and perform parameter initialization settings. Turn on the delivery pump of the raw material storage tank to slowly deliver the raw material to the metering device. The DCS control system delivers the raw material to the stirred tank reactor equipped with an explosion-proof system and an exhaust gas absorption device at a set flow rate of 1-10L / min (gradient feeding: divided into two stages, at a flow rate ratio of 1.2-1.8:1, with an interval of 30min-40min) according to the molar ratio of glyphosate acid to isopropylamine of 1:1.05-1:1.08, and the reaction temperature is precisely controlled to be 65℃-85℃, and the target value is monitored by the conductivity meter at 1.5-2.0 mS / cm, and the material is discharged;

[0073] (3) Refining and impurity removal

[0074] The reaction products are filtered through bag filters and plate and frame filters in turn;

[0075] (4) Preparation and quality control

[0076] The filtered glyphosate isopropylamine solution enters the preparation system, and additives are added according to the preset formula. By adding water to the DCS, adjusting the content of the additives, and adjusting the pH to 4.5-5 with ammonia water, it is ensured that the product quality precisely meets the quality standard of 62% glyphosate isopropylamine salt solution.

[0077] (5) Automated packaging and traceability

[0078] Qualified products are packaged through an automated packaging production line, using quantitative filling equipment to ensure that the amount of product in each bottle is accurate and consistent. At the same time, a product QR code traceability system is introduced to mark the production batch and production date information on the packaging to facilitate product quality tracking and problem tracing.

[0079] According to the above method, 62% glyphosate isopropylamine salt solution was prepared, and its active ingredient content, pH value, dilution stability, and low temperature stability were tested to see if they met the quality standards. The results are shown in the following table.

[0080] Table 1

[0081] Example 2

[0082] Referring to the method in Example 1, No. 1-7, the impurities in the obtained 62% glyphosate isopropylamine salt solution were detected, and the results are as follows.

[0083] Table 2

[0084] Comparative Example 1

[0085] Referring to the method in Example 1, the glyphosate / isopropylamine molar ratio was fixed at 1:1.05, the flow rate was 5 L / min, the flow rate ratio was 1.2:1 (interval 30 min), the reaction temperature was changed, and the other conditions remained unchanged. The product quality of the glyphosate isopropylamine salt solution was investigated. The results are shown in the table.

[0086] Table 3

[0087] Comparative Example 2

[0088] Referring to the method in Example 1, the glyphosate / isopropylamine molar ratio was fixed at 1:1.05, the reaction temperature was 75°C, the flow rate and flow rate ratio were changed, and the other factors were kept unchanged. The impurities in the obtained glyphosate isopropylamine salt solution were investigated. The results are shown in the table.

[0089] Table 4

[0090] Example 3

[0091] Referring to the method of Example 1, No. 1-7, the herbicidal effect of the obtained 62% glyphosate isopropylamine salt water agent was evaluated.

[0092] Field efficacy test

[0093] Test reagent: 62% glyphosate isopropylamine saline solution prepared according to the method of Example 1, No. 1-7.

[0094] Control agent: 62% cyclohexane glyphosate isopropylamine saline (purchased from Lianyungang Liben Crop Science and Technology Co., Ltd.).

[0095] Target of control: Setaria viridis, Erigeron sphaerocephala, and Goosegrass.

[0096] Test area: 50m 2 .

[0097] Preparation dosage: 200ml / mu.

[0098] Water consumption: 25kg / mu.

[0099] Test method: According to the area of ​​the test plot, accurately weigh various pesticides, dilute with water, and spray evenly. When spraying, pay attention to spraying the liquid evenly in the test plot to avoid missing or overspraying. After the test, randomly select 100 plants of Setaria viridis, Erigeron sphaerocephala, and Eleocharis sphaerocephala with the same growth in each plot 14 days and 28 days after the spraying, weigh the fresh weight, and calculate the weed control effect.

[0100] Fresh mass control effect / %=[fresh mass of weeds in blank control area (strains)-fresh mass of weeds in application area (strains)] / fresh mass of weeds in blank control area (strains)×100%.

[0101] The test results are shown in the table below.

[0102] Table 5

[0103] The above-mentioned embodiments only express the implementation methods of the present application, and the descriptions thereof are relatively specific and detailed, but they cannot be understood as limiting the scope of the present application. It should be pointed out that, for a person of ordinary skill in the art, several modifications and improvements can be made without departing from the concept of the present application, and these all belong to the protection scope of the present application. Therefore, the protection scope of the present application shall be subject to the attached claims.

Claims

1. A method for continuously producing glyphosate isopropylamine salt solution, characterized in that: include: Using DCS to control high-precision automatic metering equipment, according to the raw material formula, the raw materials are continuously fed into the stirred tank reactor at a set flow rate, and the reaction temperature is controlled to be 65°C-85°C for continuous reaction; after the reaction is complete, the glyphosate isopropylamine salt solution is obtained through salt formation, preparation and packaging processes; The raw material formula, by weight, includes: 10-20 parts of glyphosate, 15-20 parts of isopropylamine, 10-20 parts of adjuvant and 30-40 parts of water; The flow rate is 1-10 L / min.

2. The method according to claim 1, characterized in that The stirred tank reactor is equipped with an explosion-proof system and an exhaust gas absorption device.

3. The method according to any one of claims 1-2, characterized in that: The following steps are involved: (1) Precision pretreatment of raw materials Adopt DCS to control high-precision automatic metering equipment, strictly follow the raw material formula ratio, and accurately meter the feeding of glyphosate technical, isopropylamine, water and additives; (2) Continuous reaction intensification The original drug is continuously fed into the stirred tank reactor at a set flow rate for continuous reaction, and the reaction temperature is precisely controlled to be 65°C-85°C; (3) Refining and impurity removal The reaction products are filtered through bag filters and plate and frame filters in turn; (4) Preparation and quality control The filtered glyphosate isopropylamine solution enters the preparation system, and the additives and water are added according to the preset formula, and the pH is adjusted to obtain the glyphosate isopropylamine salt solution.

4. The method according to claim 3, characterized in that The molar ratio of glyphosate to isopropylamine in the raw material formula of step (1) is 1:1.05-1:1.

08.

5. The method according to claim 3, characterized in that: The flow rate in step (2) is divided into two stages, each with an interval of 30-40 minutes, and the feed is added at a flow rate ratio of 1.2-1.8:

1.

6. The method according to claim 3, characterized in that In step (4), the auxiliary agent is selected from at least one of a nonionic surfactant, a cationic surfactant and an anionic surfactant.

7. The method according to claim 3, characterized in that The pH in step (4) is 4.5-5.

8. The method according to claim 3, characterized in that It also includes automated packaging and traceability: qualified products are packaged through an automated packaging production line, using quantitative filling equipment to ensure that the volume of each bottle of product is accurate and consistent; at the same time, a product QR code traceability system is introduced to mark the production batch and production date information on the packaging to facilitate product quality tracking and problem tracing.

9. The glyphosate isopropylamine salt water solution prepared according to the method of claim 1.

10. Use of the glyphosate isopropylamine salt water agent according to claim 9.

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