阅读说明：本技术 一种氯氨吡啶酸钾盐原料药的制备方法 (Preparation method of picloram potassium salt bulk drug ) 是由 宋国云 钟国宁 杨娇娇 于 2020-12-25 设计创作，主要内容包括：本发明涉及一种氯氨吡啶酸钾盐原料药的制备方法,主要包括以下步骤：将氯氨吡啶酸原粉与碳酸氢钾按照1:1-1.1的摩尔比投入捏合机中,25℃混合15min后,升温并保持温度40-80℃,然后加入水,继续混合搅拌反应60-120min。反应完成后,烘干,得到氯氨吡啶酸钾盐原料药。优点：整个生产过程物料始终保持固体状态,无需后续结晶过滤工序,没有三废产生,生产工艺安全、经济环保,对环境污染较小。(The invention relates to a preparation method of a raw material drug of picloram potassium salt, which mainly comprises the following steps: adding aminopyralid raw powder and potassium bicarbonate into a kneader according to the molar ratio of 1:1-1.1, mixing for 15min at 25 ℃, heating and keeping the temperature at 40-80 ℃, then adding water, and continuously mixing, stirring and reacting for 60-120 min. And after the reaction is finished, drying to obtain the raw material medicament of the chloropyridyl acid potassium salt. The advantages are that: the materials are always kept in a solid state in the whole production process, a subsequent crystallization and filtration process is not needed, three wastes are not generated, and the production process is safe, economical, environment-friendly and less in environmental pollution.)

1. A preparation method of a raw material drug of picloram potassium salt is characterized by comprising the following steps:

(1) putting the aminopyralid raw powder and potassium bicarbonate into a kneader according to a molar ratio of 1:1-1.1, mixing for 15-30min at 24.5-25.5 ℃, heating, keeping the temperature at 30-50 ℃, adding water, wherein the water amount is 1-8% of the mass of the aminopyralid raw powder, and kneading for 60-120 min;

(2) and after the reaction is finished, drying in a drying device at 65-100 ℃ to obtain the aminopyralid potassium salt raw material medicine.

2. The method for preparing the raw material drug of the potassium aminopyralid according to claim 1, which is characterized in that: the mol ratio of the aminopyralid to the potassium bicarbonate is 1:1-1.1, preferably 1: 1.04.

3. The method for preparing a potassium aminopyralid drug substance according to claim 1 or 2, characterized in that: the mol ratio of the aminopyralid to the potassium bicarbonate is 1: 1.04.

4. The method for preparing the raw material drug of the potassium aminopyralid according to claim 1, which is characterized by comprising the following steps: the solid aminopyralid and the potassium bicarbonate are premixed for 15-30min at the room temperature of 25 ℃, and then the temperature is raised to the reaction temperature for solid-solid reaction.

5. The method for preparing a potassium aminopyralid drug substance according to claim 1 or 4, which is characterized by comprising the following steps: the solid aminopyralid and the potassium bicarbonate are premixed for 20-25min at the room temperature of 25 ℃, and then the temperature is raised to the reaction temperature for solid-solid reaction.

6. The method for preparing the raw material drug of the potassium aminopyralid according to claim 1, which is characterized in that: the reaction temperature of the aminopyralid raw powder and the potassium bicarbonate is 40-80 ℃.

7. The method for preparing a potassium aminopyralid drug substance according to claim 1 or 6, characterized in that: the reaction temperature of the aminopyralid raw powder and the potassium bicarbonate is 60-70 ℃.

8. The method for preparing the raw material drug of the potassium aminopyralid according to claim 1, which is characterized in that: the reaction time of the aminopyralid raw powder and the potassium bicarbonate is 60-120min, preferably 90-120 min.

9. The method for preparing a potassium aminopyralid drug substance according to claim 1 or 8, characterized in that: the reaction time of the aminopyralid raw powder and the potassium bicarbonate is 90-120 min.

10. The method for preparing the raw material drug of the potassium aminopyralid according to claim 1, which is characterized in that: the drying mode in the drying device is drying in an oven, and the drying temperature is 65-100 ℃ or 80 ℃.

Technical Field

The invention relates to a preparation method of a picloram potassium salt raw material medicine, which has the advantages of safe and simple process, high product utilization rate, low cost and environmental friendliness, and belongs to the field of herbicide manufacture.

Background

Aminopyralid, also called amfenadine, chemical name 4-amino-3, 5, 6-trichloropyridine carboxylic acid, is a pyridine carboxylic acid novel herbicide developed by the agricultural department of pottery, and is widely used for weed control in mountainous regions, grasslands, planting lands and uncultivated areas. The aminopyralid belongs to a synthetic hormone type herbicide, can be quickly absorbed by stems, leaves and roots of plants, induces the plants to generate partial sexual reaction in sensitive plants, thereby leading the growth of the plants to be stagnated and the plants to rapidly die, has good systemic property, has the characteristics of low toxicity, high efficiency, no teratogenicity, low toxicity of mutagenicity to human beings and the like, and is researched and developed to be applied to the fields of rape and cereal crops to prevent and kill weeds. The method has the following defects: the aminopyralid needs to be prepared into a preparation for use when in use, the common preparation at present is a water aqua, and the water aqua has low mass concentration, so that the storage and transportation cost is high. Secondly, the conventional method for preparing the raw material drug of the picloram potassium salt is to react the picloram raw material drug with potassium hydroxide in a liquid phase, and then obtain the raw material drug through the working procedures of concentration, cooling, alcohol precipitation, suction filtration, drying and the like. The liquid phase method preparation process has the disadvantages of complex process, use of a large amount of organic solvent, generation of more waste water and the like.

Disclosure of Invention

The design purpose is as follows: the defects in the background technology are avoided, and the preparation method of the raw material drug of the picloram potassium salt is designed, wherein the product does not need concentration, crystallization, filtration and washing, can ensure the required quality concentration, and has the advantages of simple production process, low storage and transportation cost and almost no generation of three wastes.

The design scheme is as follows: in order to achieve the above design objectives. The picloram is prepared into the potassium salt bulk drug, and the picloram bulk drug is soluble in water, so that the picloram bulk drug is prepared into soluble powder or soluble granules, and the storage and transportation cost can be greatly reduced. Secondly, the preparation method adopts solid-solid reaction in the production process, the product does not need concentration, crystallization, filtration and washing, and the three wastes are hardly generated, so that the production process is simpler, the requirement on equipment is low, and the safety is greatly improved.

The technical scheme is as follows: a preparation method of a picloram potassium salt raw material medicine comprises the following steps of (1) putting picloram raw powder and potassium bicarbonate into a kneader according to a molar ratio of 1:1-1.1, mixing for 15-30min at 24.5-25.5 ℃, heating, keeping the temperature at 30-50 ℃, adding water, wherein the water amount is 1-8% of the mass of the picloram raw powder, and kneading for 60-120 min. (2) And after the reaction is finished, drying in a drying device at 65-100 ℃ to obtain the aminopyralid potassium salt raw material medicine.

Compared with the background technology, firstly, the solid-solid reaction is adopted in the production process, the product does not need to be concentrated, crystallized, filtered and washed, the three wastes are hardly generated, the production process is simpler, and the requirement on equipment is low; secondly, the storage and transportation cost is low, the safety is good, the utilization rate is high, and the manufacturing cost is low.

Detailed Description

A preparation method of aminopyralid raw material medicine comprises the following steps:

adding the aminopyralid raw powder and the potassium bicarbonate into a kneader according to the molar ratio of 1:1-1.1, mixing for 15-30min at 25 ℃, heating, keeping the temperature at 30-50 ℃, adding a proper amount of water, wherein the added amount of water is 1-8% of the mass of the aminopyralid raw powder, reacting for 60-120min, and sending into an oven for drying after the reaction is finished to obtain the aminopyralid raw material medicine.

In the reaction step, a kneader plays a role in extruding, stirring and mixing, a proper amount of water is added to initiate reaction, so that reactants are contacted more uniformly and the reaction is more complete, the reaction rate is increased by properly increasing the reaction temperature, and the reaction time is shortened.

The molar ratio of aminopyralid to potassium bicarbonate in the above preparation method is 1:1-1.1, preferably 1: 1.04.

In the preparation method, the solid aminopyralid and the potassium bicarbonate are firstly premixed at the room temperature of 25 ℃ for 15-30min, preferably 20-25min, and then heated to the reaction temperature for reaction.

In the preparation method, the reaction temperature of the aminopyralid raw powder and the potassium bicarbonate is 40-80 ℃, and the preferable temperature is 60-70 ℃.

In the preparation method, the reaction time of the aminopyralid raw powder and the potassium bicarbonate is 60-120min, preferably 90-120 min.

In the preparation method, the drying mode is drying in an oven, the drying temperature is 65-100 ℃, and the preferable temperature is 80 ℃.

Example 1: the preparation method of the potassium aminopyralid comprises the following steps: 1000g of aminopyralid raw powder (with the purity of 95%) and 482g of potassium bicarbonate (with the purity of 99%) are put into a kneader with the capacity of 2L together, premixed for 20min under the conditions of normal temperature and normal pressure, heated to 60 ℃, added with 50g of water at a constant speed, stirred and kneaded continuously, and sampled after 90min to detect the reaction condition of the materials, wherein detection shows that the materials can be completely dissolved in water, no bubble is generated in the dissolving process, and the reaction of the aminopyralid and the potassium bicarbonate is completely finished. The materials are sent into an oven and dried at 80 ℃ to obtain 1168g of the picloram chloride dry product, the content of the picloram chloride is detected to be 95.1%, and the yield is 99.1%.

Example 2: the preparation method of the potassium aminopyralid comprises the following steps: 300Kg of aminopyralid raw powder (with the purity of 95%) and 144.8Kg of potassium bicarbonate (with the purity of 99%) are put into a kneader with the capacity of 500L together, premixed for 20min under the conditions of normal temperature and normal pressure, heated to 60 ℃, added with 3Kg of water at uniform speed, stirred and kneaded continuously, and sampling is carried out after 90min to detect the reaction condition of the materials, and the detection shows that the materials can be completely dissolved in water, and no bubble is generated in the dissolving process, which indicates that the aminopyralid raw powder is completely converted into the potassium aminopyralid. The materials are sent into an oven and dried at 80 ℃ to obtain 351Kg of dry product of the aminopyralid, the content of the aminopyralid is detected to be 95.3 percent, and the yield is 99.2 percent.

Example 3: the preparation method of the potassium aminopyralid comprises the following steps: 1200Kg of aminopyralid raw powder (with the purity of 95 percent) and 579.2Kg of potassium bicarbonate (with the purity of 99 percent) are put into a kneader with the capacity of 2000L together, premixed for 25min under the conditions of normal temperature and normal pressure, heated to 60 ℃, added with 10Kg of water at uniform speed, continuously stirred and mixed, and sampled after 100min to detect the reaction condition of the materials, the detection shows that the materials can be completely dissolved in water, and no bubble is generated in the dissolving process, which indicates that the aminopyralid raw powder is completely converted into the potassium aminopyralid. The materials are sent into an oven and dried at the temperature of 80 ℃ to obtain 1410Kg of a dried product of the aminopyralid potassium salt, the content of the aminopyralid potassium salt is detected to be 95.1 percent, and the yield is 99.4 percent.

The product performance obtained in examples 1 to 3 is tested, namely the test result of the performance of the raw material drug of the picloram chloride potassium salt

It is to be understood that: although the above embodiments have described the design idea of the present invention in more detail, these descriptions are only simple descriptions of the design idea of the present invention, and are not limitations of the design idea of the present invention, and any combination, addition, or modification without departing from the design idea of the present invention falls within the scope of the present invention.