阅读说明：本技术 一种草甘膦异丙胺盐水剂的制备方法 (Preparation method of glyphosate isopropylamine salt aqueous solution ) 是由 肖建中 于 2021-06-28 设计创作，主要内容包括：本发明公开一种草甘膦异丙胺盐水剂的制备方法,包括如下步骤：步骤1,将草甘膦原药、异丙胺、水混合搅拌,其中,草甘膦原药与异丙胺的摩尔比为1：1～1.2,草甘膦原药与异丙胺的混合物和水的重量比为1：3～5；步骤2,将步骤1得到的混合物倒出,过滤后再放入反应釜中；步骤3,继续向反应釜中加入助剂和水,此时加入的助剂和水与步骤2中混合物的质量比为1.5～3：7～10：1,搅拌得到草甘膦异丙胺盐水剂；其中,助剂是ST-90渗透剂或TAE表面活性剂。此种制备方法制备的草甘膦异丙胺盐水剂,具有较好的渗透性、保湿型、黏着性、附着性,从而提升产品综合药效。(The invention discloses a preparation method of glyphosate isopropylamine salt aqueous solution, which comprises the following steps: step 1, mixing and stirring a glyphosate technical, isopropylamine and water, wherein the molar ratio of the glyphosate technical to the isopropylamine is 1: 1-1.2, wherein the weight ratio of the mixture of glyphosate technical material and isopropylamine to water is 1: 3-5; step 2, pouring out the mixture obtained in the step 1, filtering and then putting into a reaction kettle; and 3, continuously adding the auxiliary agent and the water into the reaction kettle, wherein the mass ratio of the added auxiliary agent and the added water to the mixture in the step 2 is 1.5-3: 7-10: 1, stirring to obtain glyphosate isopropylamine salt aqueous solution; wherein the auxiliary agent is ST-90 penetrating agent or TAE surfactant. The glyphosate isopropylamine salt aqua prepared by the preparation method has better permeability, moisture retention, adhesion and adhesiveness, thereby improving the comprehensive drug effect of the product.)

1. A preparation method of glyphosate isopropylamine salt aqueous solution is characterized by comprising the following steps:

step 1, mixing and stirring a glyphosate technical, isopropylamine and water, wherein the molar ratio of the glyphosate technical to the isopropylamine is 1: 1-1.2, wherein the weight ratio of the mixture of glyphosate technical material and isopropylamine to water is 1: 3-5;

step 2, pouring out the mixture obtained in the step 1, filtering and then putting into a reaction kettle;

and 3, continuously adding the auxiliary agent and the water into the reaction kettle, wherein the mass ratio of the added auxiliary agent and the added water to the mixture in the step 2 is 1.5-3: 7-10: 1, stirring to obtain glyphosate isopropylamine salt aqueous solution; wherein the auxiliary agent is ST-90 penetrating agent or TAE surfactant.

2. The method of claim 1, wherein: in the step 1, all glyphosate raw pesticide and isopropylamine are added into a reaction kettle, and then all water is added into the reaction kettle.

3. The method of claim 2, wherein: in the step 1, part of glyphosate technical material, isopropylamine and water are added into a reaction kettle, mixed and stirred, and then the rest glyphosate technical material, isopropylamine and water are added, mixed and stirred.

4. The method of claim 1, wherein: in the step 1, all glyphosate technical and isopropylamine are added into a reaction kettle, part of water is added, and the mixture is mixed and stirred, then the rest water is added, and the mixture is mixed and stirred.

5. The method of any one of claims 2 to 4, wherein: in the step 1, the temperature of the reaction kettle is adjusted to 10-20 ℃ and kept for 20-45 min during mixing and stirring.

6. The method of claim 1, wherein: and in the step 2, filtering by adopting a filter screen of 100-180 meshes.

7. The method of claim 1, wherein: in the step 3, the stirring condition is that the temperature of the reaction kettle is 12-23 ℃, and the stirring is carried out for 5-10 min.

Technical Field

The invention belongs to the field of preparation processes of herbicides, and particularly relates to a preparation method of a glyphosate isopropylamine salt aqueous solution.

Background

The glyphosate is an efficient, low-toxicity and low-residue postemergence biocidal efficient herbicide, and the existing glyphosate production formulations mainly comprise 10% of glyphosate aqueous solution, 30% of glyphosate amine salt aqueous solution, 41% of glyphosate isopropylamine salt aqueous solution, 62% of glyphosate isopropylamine salt, 68% of glyphosate amine salt soluble granules, 50% of glyphosate ammonium salt soluble powder and the like in percentage by mass.

As is well known, the glyphosate salt has a good weeding effect by using ammonium salt and isopropylamine salt, but isopropylamine has a low boiling point, is flammable and volatile and belongs to a fire hazard class B, so that the preparation process has high requirements, and the prepared isopropylamine salt has poor performance and needs to be improved.

Disclosure of Invention

The invention aims to provide a preparation method of glyphosate isopropylamine salt aqueous solution, which has better permeability, moisture retention, adhesion and adhesiveness, thereby improving the comprehensive drug effect of the product.

In order to achieve the above purpose, the solution of the invention is:

a preparation method of glyphosate isopropylamine salt aqueous solution comprises the following steps:

step 1, mixing and stirring a glyphosate technical, isopropylamine and water, wherein the molar ratio of the glyphosate technical to the isopropylamine is 1: 1-1.2, wherein the weight ratio of the mixture of glyphosate technical material and isopropylamine to water is 1: 3-5;

step 2, pouring out the mixture obtained in the step 1, filtering and then putting into a reaction kettle;

and 3, continuously adding the auxiliary agent and the water into the reaction kettle, wherein the mass ratio of the added auxiliary agent and the added water to the mixture in the step 2 is 1.5-3: 7-10: 1, stirring to obtain glyphosate isopropylamine salt aqueous solution; wherein the auxiliary agent is ST-90 penetrating agent or TAE surfactant.

In the step 1, all glyphosate raw pesticide and isopropylamine are added into a reaction kettle, and then all water is added into the reaction kettle.

In the step 1, part of glyphosate technical material, isopropylamine and water are added into a reaction kettle, mixed and stirred, and then the rest glyphosate technical material, isopropylamine and water are added, mixed and stirred.

In the step 1, all glyphosate raw drug and isopropylamine are added into a reaction kettle, part of water is added, and the mixture is mixed and stirred, then the rest water is added, and the mixture is mixed and stirred.

In the step 1, the temperature of the reaction kettle is adjusted to 10-20 ℃ and kept for 20-45 min during mixing and stirring.

In the step 2, a filter screen with 100-180 meshes is adopted for filtering.

In the step 3, the stirring condition is that the temperature of the reaction kettle is 12-23 ℃, and the stirring is carried out for 5-10 min.

After the scheme is adopted, the invention has the following beneficial effects:

(1) according to the invention, through test analysis, proper auxiliary agents are screened, and the drug effect of the product is improved; experiments prove that the permeability, moisture retention, adhesion and adhesiveness of the product can be improved by adding auxiliary agents such as ST-90 penetrant (mainly 2040-X, namely polyester type multi-chain high-molecular polymer), TAE surfactant (TAE: buffer solution consisting of Tris base, acetic acid and Ethylene Diamine Tetraacetic Acid (EDTA)), and the like, so that the comprehensive efficacy of the product is improved;

(2) the invention adopts glyphosate technical as main raw material, the production process of the glyphosate technical of the applicant is stable in technology, skillful in experience, safe and controllable, DCS automatic operation and continuous production can be realized, the total yield of the product is far higher than the average level in the same industry, the content is higher, and high-quality, stable and sufficient raw materials are provided for the production of the product; meanwhile, the yield is improved, so that the production cost of the raw material glyphosate technical is further reduced, and the product has certain cost advantage;

(3) the glyphosate product is designed into an aqueous solution, and the aqueous solution is a novel environment-friendly preparation formulation which is environment-friendly, easy to transport and safe to use and accords with the national pesticide development direction;

(4) through sufficient tests, the invention adds selected additives according to the formula: firstly, penetrant ST-90, secondly surfactant TAE can prevent effectively that the glyphosate aqueous solution from decomposing, further promote product quality stability, not only reduced surface tension, improved the permeability, have good moist spreading power, adhesion and high-efficient osmotic force, improve solubility and the degree of consistency of glyphosate isopropylamine salt simultaneously, improve and knock down speed, strengthened the drug effect, and harmless to people and animals, pollution-free to the environment, to crops safe and reliable.

Drawings

FIG. 1 is a schematic diagram of the preparation of the present invention.

Detailed Description

The technical solution and the advantages of the present invention will be described in detail with reference to the accompanying drawings.

As shown in fig. 1, the present invention provides a preparation method of glyphosate isopropylamine salt aqueous solution, comprising the following steps:

step 1, mixing a mixture of 1: adding 1-1.2 glyphosate technical and isopropylamine into a reaction kettle, and adding water into the reaction kettle, wherein the weight ratio of the water to the mixture is (3-5): 1, after uniformly mixing and stirring, adjusting the temperature of a reaction kettle to 10-20 ℃, and keeping for 20-45 min;

in the step 1, all the ingredients can be mixed and stirred at one time or added in multiple times;

step 2, pouring the mixture obtained in the step 1 out, filtering the mixture through a filter screen of 100-180 meshes, and putting the filtered mixture into the reaction kettle;

and 3, continuously adding the auxiliary agent and the water into the reaction kettle, wherein the mass ratio of the added auxiliary agent to the added water to the mixture is 1.5-3: 7-10: 1, adjusting the temperature of a reaction kettle to 12-23 ℃, and stirring for 5-10min to obtain glyphosate isopropylamine salt aqua; wherein, the auxiliary agent can be ST-90 penetrating agent (mainly 2040-X, namely polyester type multi-chain polymer), TAE surfactant and other auxiliary agents, wherein, TAE refers to buffer solution composed of Tris (hydroxymethyl) aminomethane (Tris base), acetic acid (acetic acid) and Ethylene Diamine Tetraacetic Acid (EDTA).

Example 1

Step 1, mixing a mixture of 1: 1.1, adding glyphosate technical and isopropylamine into a reaction kettle at one time, and adding the mixture into the reaction kettle in a weight ratio of 3: 1, uniformly mixing and stirring the mixture, adjusting the temperature of the reaction kettle to 10 ℃, and keeping the temperature for 45 min;

step 2, pouring out the mixture obtained in the step 1, filtering the mixture through a 120-mesh filter screen, and putting the filtered mixture into the reaction kettle;

and 3, continuously adding the ST-90 penetrant and water into the reaction kettle, wherein the mass ratio of the added ST-90 penetrant and water to the mixture is 1.5: 8: 1, adjusting the temperature of the reaction kettle to 20 ℃, and stirring for 5min to obtain the glyphosate isopropylamine salt aqueous solution.

Example 2

Step 1, mixing a mixture of 1: adding glyphosate technical and isopropylamine into a reaction kettle, and adding the mixture into the reaction kettle in a weight ratio of 4: 1, uniformly mixing and stirring the mixture, adjusting the temperature of the reaction kettle to 12 ℃, and keeping the temperature for 40 min; then adding a mixture of the components in a molar ratio of 1: 1.15 glyphosate technical and isopropylamine, then adding the glyphosate technical and isopropylamine in a molar ratio of 1: 1.15 weight ratio of glyphosate technical to isopropylamine is 4: 1, keeping the temperature of the reaction kettle at 12 ℃ for 20 min;

step 2, pouring the mixture obtained in the step 1 out, filtering the mixture through a filter screen with 110 meshes, and putting the filtered mixture into the reaction kettle;

and 3, continuously adding the TAE surfactant and water into the reaction kettle, wherein the mass ratio of the added TAE surfactant and water to the mixture is 1.5: 10: 1, adjusting the temperature of the reaction kettle to 23 ℃, and stirring for 7min to obtain the glyphosate isopropylamine salt aqueous solution.

Example 3

Step 1, mixing a mixture of 1: 1.2, adding glyphosate technical and isopropylamine into a reaction kettle, and preparing the mixture according to the weight ratio of 5: 1, adding half water into a reaction kettle, mixing and stirring uniformly, adjusting the temperature of the reaction kettle to 20 ℃, and keeping for 15 min; then adding the rest half water, stirring, keeping the temperature of the reaction kettle at 20 ℃, and keeping for 20 min;

step 2, pouring out the mixture obtained in the step 1, filtering the mixture through a filter screen of 160 meshes, and putting the filtered mixture into the reaction kettle;

and 3, continuously adding the ST-90 penetrant and water into the reaction kettle, wherein the mass ratio of the added ST-90 penetrant and water to the mixture is 1.5: 4: 1, adjusting the temperature of the reaction kettle to 15 ℃, and stirring for 10min to obtain the glyphosate isopropylamine salt aqueous solution.

In summary, the preparation method of the glyphosate isopropylamine salt aqueous solution comprises the steps of reacting a glyphosate original drug with isopropylamine to prepare the glyphosate isopropylamine salt, adding an auxiliary agent and water to prepare the high-efficiency low-toxicity glyphosate isopropylamine salt aqueous solution, and adding auxiliary agents such as ST-90 penetrating agent, TAE surfactant and the like to improve the permeability, moisture retention, adhesion and adhesiveness of the product, so that the comprehensive drug effect of the product is improved.

The 41 percent glyphosate isopropylammonium aqua is an excellent biocidal high-efficiency herbicide and has been favored for a long time. The weeding composition has the characteristics of low toxicity, high weeding efficiency, strong destructive power on underground tissues of perennial deep-rooted weeds and capability of reaching the depth which is difficult to reach by common agricultural machinery, and the pesticide effect can be transferred to underground rhizomes within 24 hours, thus thoroughly eradicating the weeds. The glyphosate has good weeding effect, is widely used for preventing and controlling weeds in various crop fields, is a few excellent herbicide varieties at present, and can prevent and control monocotyledons, dicotyledons, annual and perennial plants, herbaceous plants, shrubs and other plants of more than 40 families. After entering the soil, the glyphosate is combined with metal ions such as iron, aluminum and the like to lose activity, has no adverse effect on seeds and soil microorganisms hidden in the soil, and has very wide market prospect because the product has stable dosage form, environmental protection, easy transportation and safe use.

At present, through market research, the market price of the 41 percent glyphosate isopropylammonium salt water agent is about 10500 yuan/ton. Because the glyphosate technical of our company has advanced production process, stable quality, high total yield and comprehensive cost lower than the average level of the industry, the quality and dosage of blending the 41 percent glyphosate isopropylammonium aqua can be ensured. Therefore, the product has strong competitive advantages in cost price and product quality, and can obtain higher market share.

The company predicts that 3000 tons of 41 percent glyphosate isopropylammonium aqua produced in 2017 can realize 3150 ten thousand yuan of zero-stock sales, 636 ten thousand yuan of profit and 120 ten thousand yuan of tax revenue.

The above embodiments are only for illustrating the technical idea of the present invention, and the protection scope of the present invention is not limited thereby, and any modifications made on the basis of the technical scheme according to the technical idea of the present invention fall within the protection scope of the present invention.