Ammonium glyphosate granule and preparation method thereof

Abstract

The invention discloses ammonium glyphosate granules and a preparation method thereof, and belongs to the technical field of pesticide preparation production. Various parameters in the production process are accurately controlled by adopting an automatic control system, a material transfer link is reduced by adopting granulation and drying integrated equipment, and the particle size of the product is 1.0-1.5 mm, the particle size distribution is uniform and the dust rate is low by virtue of collaborative optimization of a process, a formula and equipment in the production process; and the content of the effective components is stabilized in a range of 75.7% + / -2.5%, so that the quality consistency and the use effect of the product are improved, and the market competitiveness and the user satisfaction of the product are enhanced.

Description

Technical Field

[0001] The invention belongs to the technical field of pesticide preparation production, and specifically relates to a glyphosate ammonium salt granule and a preparation method thereof. Background Art

[0002] Glyphosate ammonium salt granules are a systemic, conductive herbicide that has significant control effects on perennial malignant weeds. However, the efficacy of glyphosate ammonium salt granules is not very stable. One of the important reasons is that the particle size is uneven, which leads to low product stability, poor solubility and unstable efficacy, which is also a technical difficulty of glyphosate ammonium salt granules.

[0003] At present, the production process of 75.7% glyphosate ammonium salt granules is mainly based on intermittent production. In traditional intermittent production, glyphosate technical, ammonium salt (such as liquid ammonia, ammonium bicarbonate, etc.) and additives (such as dispersants, binders, etc.) are first mixed and reacted in a reactor in a certain proportion. After the reaction is completed, the granule product is made through multiple processes such as drying, granulation, and screening. This production method has many shortcomings: 1. Low production efficiency: Each batch of production needs to go through multiple steps such as batching, reaction, drying, and granulation. Each step requires a certain amount of time for equipment preparation and operation. The production cycle is long and it is difficult to achieve large-scale industrial production. 2. Unstable quality: Manual batching and operation are prone to errors, resulting in large differences in the quality of different batches of products. For example, in the granulation process, it is difficult to keep the temperature, humidity and other conditions manually controlled accurately, which makes the shape, size and hardness of the particles uneven, affecting the solubility and efficacy of the product. 3. High energy consumption and large material loss: During intermittent production, equipment is frequently started and stopped, which increases energy consumption. At the same time, during material transfer and processing, material residue and loss are likely to occur, resulting in waste of resources.

[0004] Furthermore, the particle size of granules usually affects their dissolution rate, dispersibility, fluidity, anti-hygroscopicity and uniformity during application. Smaller particles may dissolve faster, but are prone to dust, affecting operational safety; larger particles may dissolve slower, but have better fluidity and are easier to spread mechanically. In addition, particle size distribution (uniformity) is also important, and too wide a distribution may lead to unstable performance.

[0005] Therefore, it is of great significance to develop an automated controlled and precisely regulated production process for 75.7% glyphosate ammonium salt granules to ensure the uniformity and stability of the granules. Summary of the invention

[0006] In order to overcome the above technical problems in the production process of the traditional 75.7% glyphosate ammonium salt granules, the purpose of the present invention is to provide a glyphosate ammonium salt granules and a preparation method thereof. The present invention adopts an automated control system to accurately control various parameters in the production process, and the integrated granulation and drying equipment reduces the material transfer link. The particle size of the obtained product is uniform, and the content of the active ingredient is stable within the range of 75.7% ± 2.5%, which improves the quality consistency and use effect of the product and enhances the market competitiveness of the product.

[0007] To achieve the above objectives, the technical solution provided by the present invention is as follows:

[0008] In one aspect, the present invention provides a glyphosate ammonium salt granule, wherein the formula of the glyphosate isopropylamine granule comprises: .

[0009] On the other hand, the present invention also provides a method for preparing glyphosate ammonium salt granules, comprising the following steps:

[0010] (1) Raw material pretreatment:

[0011] Measure glyphosate technical, ammonium bicarbonate, ammonium sulfate, and adjuvants respectively;

[0012] (2) Continuous reaction:

[0013] A high-speed mixing reaction device is used to continuously transport the metered glyphosate technical, ammonium bicarbonate, ammonium sulfate and adjuvant solution to the reaction device, and the reaction temperature is precisely controlled to be 50°C-60°C;

[0014] (3) Integration of granulation and drying:

[0015] The reacted glyphosate ammonium salt mixture directly enters the granulation equipment and then enters the continuous dryer;

[0016] (4) Screening and packaging:

[0017] The product after granulation and drying is monitored by an online particle size monitoring system, which provides real-time feedback of production parameters, and then sieved to obtain qualified particles, which are then automatically packaged to obtain glyphosate ammonium salt granules.

[0018] In some embodiments, the raw material glyphosate technical in step (1) needs to be crushed to a certain particle size so as to better participate in the reaction; and the auxiliary agent is dispersed according to the formula requirements and set aside.

[0019] In some embodiments, the raw material glyphosate in step (1) needs to pass through an 85-mesh sieve (particle size ≤ 180 μm) to ensure mixing uniformity.

[0020] In some embodiments, the auxiliary agent in step (1) is sodium tripolyphosphate, alkyl polyglycoside APG and nano-silicon dioxide or sodium tripolyphosphate, tallow amine polyoxyethylene ether and nano-silicon dioxide.

[0021] The present invention creatively combines alkyl polyglucosides APG or tallow amine polyvinyl ether with nano-silicon dioxide and applies it to glyphosate ammonium salt granules. The core concept is to systematically solve the technical bottlenecks of easy aggregation of active ingredients, uneven release of drug efficacy and poor target permeability in traditional granules through the synergistic cooperation of functional additives. Specifically: the surfactant system of alkyl polyglucosides APG or tallow amine polyvinyl ether not only significantly reduces the solid-liquid interfacial tension, but also adsorbs on the surface of glyphosate ammonium salt crystals through intermolecular hydrogen bonding, and forms a physical-chemical double coating layer with the mesoporous structure of nano-silicon dioxide. The composite coating layer not only utilizes the high specific surface area of ​​nano-silicon dioxide to achieve molecular-level dispersion of active ingredients, but also inhibits electrostatic adsorption between particles through the charge balance of surfactants, and can still maintain the integrity of the particle structure under wet and hot storage conditions. The synergistic effect of the two ultimately shortens the disintegration time of the granules, reduces the contact angle of the leaves, and the agglomeration rate is less than 1% after storage at 50°C for 6 months, overcoming the long-standing technical contradiction in the field that stability and rapidity are difficult to achieve at the same time.

[0022] In some embodiments, the equipment in step (3) is preferably a rotary granulator.

[0023] In some embodiments, the step (3) is performed using a continuous fluidized bed granulation dryer.

[0024] In some embodiments, the feed thickness in step (3) is 5-8 mm, the set temperature is 95-100° C., the insulation temperature is 75-80° C., and the moisture content is controlled to be ≤0.5%.

[0025] In some embodiments, in step (3), during the granulation drying process, hot air is used to dry the material, and the material is formed into particles under the action of the specific structure and airflow inside the equipment. By accurately controlling parameters such as drying temperature, feed rate and airflow rate, the size and shape of the particles are adjusted to ensure the uniformity and stability of the particles.

[0026] In some embodiments, in step (4), the granulated and dried product is sieved through a vibrating screen to separate large particles and small particles that do not meet the particle size requirements.

[0027] In some embodiments, in step (4), the particle size is acceptable if it is between 1.0 and 1.5 mm.

[0028] Furthermore, the large particles are crushed and returned to the granulation process, and the small particles are treated as defective products.

[0029] In some embodiments, in step (4), qualified particles are continuously packaged by automated packaging equipment, and the packaging weight and sealing quality are strictly controlled during the packaging process to ensure the packaging quality of the product.

[0030] In some embodiments, the above steps (1) to (4) are equipped with a PLC monitoring system.

[0031] In some embodiments, the PLC monitoring system monitors reaction temperature, current, and time period.

[0032] In some embodiments, the PLC monitoring system monitors the reaction temperature, current, time cycle and other parameters in real time through the sensor devices installed on each device and pipeline, and automatically adjusts the operating status of the equipment, such as the opening of the valve, the speed of the fan, the power of the heating device, etc., through the PLC system control parameter range, to achieve automatic control and precise adjustment of the production process. At the same time, the system also has data recording and analysis functions, which is convenient for tracing and optimizing the production process.

[0033] On the other hand, the present invention also provides glyphosate isopropylamine salt granules prepared by the above method.

[0034] In a third aspect, the present invention also provides the use of the above-mentioned glyphosate isopropylamine salt granules.

[0035] Compared with the prior art, this application has the following beneficial effects:

[0036] (1) Significant improvement in production efficiency: The continuous production process has achieved uninterrupted production from raw materials to finished products, increasing production capacity by 50%. The reaction time, which originally required stacking for 7 days, has been shortened to 1 hour, a 168-fold reduction in reaction time. This can meet the needs of large-scale industrial production and improve the company's market supply capacity.

[0037] (2) Stable and reliable product quality: The automated control system accurately controls various parameters in the production process. The integrated granulation and drying equipment reduces the material transfer process. Through the coordinated optimization of process-formula-equipment during the production process, the product particle size is ensured to be between 1.0 and 1.5 mm, with uniform particle size distribution (SPAN value reduced from 1.5 to 0.8) and low dust rate (<1%). The content of active ingredients is stable within the range of 75.7% ± 2.5%, which improves the quality consistency and use effect of the product and enhances the product's market competitiveness and user satisfaction.

[0038] (3) Reduced energy consumption and material loss: Continuous production avoids frequent start and stop of equipment and reduces energy consumption. At the same time, precise metering and automated material transportation and temperature control systems reduce material residue and loss, energy consumption is reduced by 25%, material loss is reduced by 2.3%, production costs are reduced, and the economic benefits of the enterprise are improved.

[0039] (4) The production process is more environmentally friendly: the integrated granulation and drying equipment reduces the material transfer process and reduces dust emissions; automated control reduces material leakage that may occur during manual operation, making the production process more environmentally friendly and in line with the requirements of sustainable development. DETAILED DESCRIPTION

[0040] 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.

[0041] 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.

[0042] In the present invention, a method for preparing glyphosate ammonium salt granules comprises:

[0043] 1. Equipment selection, installation and commissioning: According to the production scale and process requirements, select the appropriate type of high-speed mixing reaction device, continuous fluidized bed granulation dryer, vibrating screen, automatic packaging equipment, etc. During the equipment installation process, strictly follow the equipment installation instructions to ensure the installation accuracy and stability of the equipment. After the installation is completed, fully debug the equipment, check the operating status of the equipment, test the functions of the PLC monitoring system, and ensure that the system can accurately monitor and control various parameters in the production process.

[0044] 2. Raw material management: Establish strict raw material procurement standards and inspection systems to ensure that the quality of glyphosate technical, ammonium bicarbonate, ammonium sulfate and adjuvants meets production requirements. Classify and store the purchased raw materials to prevent them from getting damp and deteriorating. During the production process, pre-treat the raw materials according to the process requirements to ensure that the particle size and solubility of the raw materials meet the needs of continuous production.

[0045] 3. Production operation process:

[0046] 3.1 Start-up preparation: Check whether the equipment, pipelines, valves, etc. are in normal condition, start the PLC monitoring system, and perform system initialization settings. Start the preparation and measurement of raw and auxiliary materials, and wait for production instructions.

[0047] 3.2 Continuous production: After the production order is issued, the automatic control system controls the mixing reaction according to the preset parameters. The reacted materials enter the granulation and drying equipment for granulation and drying. During the production process, pay close attention to the various parameters displayed by the PLC monitoring system. If any abnormal parameters are found, adjust them in time. The qualified products after screening enter the packaging process for packaging, and the unqualified products are handled according to regulations.

[0048] 3.3 Shutdown operation: After the production task is completed, stop preparing materials, shut down the operation of the reaction device, granulation drying equipment, screening equipment and packaging equipment. Clean the equipment and pipelines, remove residual materials, and prevent materials from clogging pipelines and equipment. Shut down the PLC monitoring system and keep production records and equipment maintenance records.

[0049] 4. Quality control and management: During the production process, the product quality is regularly tested, and the test items include particle size, active ingredient content, moisture content, etc. According to the test results, the production parameters are adjusted in time to ensure that the product quality meets the standard requirements. A complete quality management system is established to monitor the quality of each link in the production process, from raw material procurement to product packaging, to achieve full process quality traceability, and ensure the stability and reliability of product quality.

[0050] In the present invention, the size of the particles is called the particle size, which can also be called the particle diameter. The particle size or particle diameter indicates the particle diameter. For non-spherical particles, the particle diameter is related to the measurement standard and statistical method, and the particle diameter can only be "equivalent", that is, when a certain physical property of a particle is the same or similar to that of a homogeneous spherical particle, we use the diameter of the spherical particle to represent the diameter of the actual particle, which is called the equivalent particle diameter.

[0051] The present invention calculates D10, D50, and D90 as the particle size of the particle size volume distribution, and D50 represents the average particle size of particles that account for 50% of the volume. The particle size distribution SPAN value is used to represent the width of the particle size distribution, and the SPAN value satisfies: SPAN=(D90-D10) / D50. A large SPAN value means a wide particle size distribution, and a small SPAN value means a narrow particle size distribution.

[0052] Example 1

[0053] Process:

[0054] (1) Raw material pretreatment

[0055] At room temperature, glyphosate technical, ammonium bicarbonate, ammonium sulfate, alkyl polyglycoside APG, and nano-silica are measured separately, and the pH is adjusted to 4.8 with sodium tripolyphosphate, a pH regulator; among them, the raw material glyphosate needs to pass through an 85-mesh sieve (particle size ≤ 180μm) to ensure mixing uniformity.

[0056] (2) Continuous reaction

[0057] A high-speed mixing reaction device is used to continuously transport the metered glyphosate technical, ammonium bicarbonate, ammonium sulfate and auxiliary agent solution to the reaction device, and the reaction temperature is precisely controlled to be 50°C-60°C.

[0058] (3) Integration of granulation and drying

[0059] The glyphosate ammonium salt mixture after the reaction directly enters the granulation equipment and then enters the continuous dryer; wherein, the feed thickness is 5-8mm, the set temperature is 95-100℃, the insulation temperature is 75-80℃, and the moisture content is controlled to ≤0.5%.

[0060] (4) Screening and packaging

[0061] The product after granulation and drying is passed through an online particle size monitoring system to provide real-time feedback of production parameters, and qualified particles are screened and automatically packaged to obtain glyphosate ammonium salt granules with an average particle size of 1.0-1.5 mm and a SPAN value of 0.8.

[0062] Example 2

[0063] Referring to the preparation method in Example 1, the ammonium bicarbonate content was changed to 40 (w / w%), and the other contents remained unchanged to obtain glyphosate ammonium salt granules with an average particle size of 1.0-1.5 mm and a SPAN value of 0.8.

[0064] Example 3

[0065] Referring to the preparation method in Example 1, the alkyl polyglycoside APG was replaced with tallow amine polyoxyethylene ether with the same content, and the other contents remained unchanged to obtain glyphosate ammonium salt granules with an average particle size of 1.0-1.5 mm and a SPAN value of 0.8.

[0066] According to the method described in Examples 1-3 above, 75.7% glyphosate isopropylamine granules were prepared, and various technical indicators of the product were tested. The results are shown in the following table.

[0067] Table 1

[0068] Comparative Example 1

[0069] Referring to the method in Example 1, the glyphosate ammonium salt granules were prepared by artificial feeding with other conditions unchanged.

[0070] Comparative Example 2

[0071] Referring to the method in Example 1, in step (3), the feed thickness is 5-8 mm, the set temperature is 90° C., the insulation temperature is 75-80° C., and the moisture content is controlled to be ≥ 2%.

[0072] Example 4

[0073] Referring to the method in Example 1, Comparative Example 3 did not add alkyl polyglycoside APG, Comparative Example 4 did not add nano silicon dioxide, and other conditions remained unchanged to prepare glyphosate ammonium salt granules. The test results are shown in the following table.

[0074] Table 2

[0075] Example 5

[0076] The efficacy comparison test of the 75.7% glyphosate ammonium salt granules prepared in Example 1, Example 2, Example 3 and Comparative Examples 1-2 and the 75.7% glyphosate ammonium salt granules sold on the market was conducted as follows:

[0077] Field efficacy test:

[0078] Test agent: 75.7% glyphosate ammonium salt granules prepared using Examples 1-3 and Comparative Examples 1-2.

[0079] Control agent: commercially available 75.7% glyphosate ammonium salt granules (purchased from Jema Chemical Co., Ltd.).

[0080] Target of control: foxtail grass, barnyard grass and thatch.

[0081] Test area: 50m 2 .

[0082] Dosage of preparation: 200g / mu.

[0083] Water consumption: 20kg / mu.

[0084] 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 into the test plot to avoid missing or overspraying. After the test, observe the weed death at 14 days and compare the herbicidal activity of various pesticides.

[0085] The herbicidal effects of the formulations of the present invention and the comparative agents are shown in the following table.

[0086] Table 3

[0087] The above-described 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 glyphosate ammonium salt granule, characterized in that: The formula of the glyphosate isopropylamine granules comprises: 。 2. The method for preparing the glyphosate ammonium salt granules according to claim 1, characterized in that: The following steps are involved: (1) Raw material pretreatment: Measure glyphosate technical, ammonium bicarbonate, ammonium sulfate, and adjuvants respectively; (2) Continuous reaction: A high-speed mixing reaction device is used to continuously transport the metered glyphosate technical, ammonium bicarbonate, ammonium sulfate and adjuvant solution to the reaction device, and the reaction temperature is precisely controlled to be 50°C-60°C; (3) Integration of granulation and drying: The reacted glyphosate ammonium salt mixture directly enters the granulation equipment and then enters the continuous dryer; (4) Screening and packaging: The product after granulation and drying is monitored by an online particle size monitoring system, which provides real-time feedback of production parameters, and then sieved to obtain qualified particles, which are then automatically packaged to obtain glyphosate ammonium salt granules.

3. The method according to claim 2, characterized in that In the step (1), the raw material glyphosate needs to pass through an 85-mesh sieve.

4. The method according to claim 2 or 3, characterized in that: The auxiliary agents in step (1) are sodium tripolyphosphate, alkyl polyglycoside APG and nano silicon dioxide or sodium tripolyphosphate, tallow amine polyoxyethylene ether and nano silicon dioxide.

5. The method according to claim 2, characterized in that: The granulation equipment in step (3) is a rotary granulator.

6. The method according to claim 2, characterized in that The step (3) is carried out using a continuous fluidized bed granulation dryer.

7. The method according to any one of claims 2 or 5-6, characterized in that: The feed thickness in step (3) is 5-8 mm, the set temperature is 95-100° C., the insulation temperature is 75-80° C., and the moisture content is controlled to be ≤0.5%.

8. The method according to claim 2, characterized in that: In the step (4), the granulated and dried product is screened by a vibrating screen to separate large particles and small particles that do not meet the particle size requirements. The particle size of 1.0-1.5 mm is qualified.

9. The method according to claim 2, characterized in that: The above steps (1) to (4) are all equipped with a PLC monitoring system.

10. The method according to claim 9, characterized in that The PLC monitoring system monitors reaction temperature, current, and time period.

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