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A kind of preparation method of herbicide saponin

A technology of sedge phosphorus and herbicide, which is applied in the field of preparation of herbicide sedge phosphate, can solve the problems of large particle size and uneven particle size distribution of the original drug of sedge phosphate, achieves safety and environmental protection in the preparation process, and improves the purity and yield. , to avoid the effect of the grinding process

Active Publication Date: 2022-01-25
潍坊新绿化工有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] The patent CN102260287B discloses a preparation method of the herbicide Saponin, which is specifically: using water as a solvent to prepare Saponin, adding an appropriate amount of phase transfer catalyst in the reaction, condensation and crystallization in one step, and cooling the reaction solution after the reaction , Saponin is directly precipitated and crystallized in water, and the product is obtained by filtering, washing, and drying; the deficiency of this patent is that the prepared Saponin original drug has a large particle size, and the particle size distribution is uneven

Method used

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  • A kind of preparation method of herbicide saponin

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Embodiment 1

[0030] A preparation method of herbicide saponin, specifically:

[0031] 1. Preparation of hollow microspheres: place X-type porous zeolite powder in a calcination furnace, control the temperature of the calcination furnace to 350°C, and obtain calcined X-type porous zeolite powder after calcination for 2 hours, and place 10 g of calcined X-type porous zeolite powder Zeolite powder is mixed with 35g of absolute ethanol, 1g of dimethyl diallyl ammonium chloride aqueous solution, 3g of acetic acid, and 1g of nickel nitrate before ultrasonic dispersion. The frequency of ultrasonic dispersion is controlled at 20kHz, and the time of ultrasonic dispersion is 20min. After the end, the dispersed raw material is obtained; the dispersed raw material is cooled to -20°C, frozen at -20°C for 30 minutes, then slowly heated to 90°C, and the temperature rise rate is controlled at 2°C / min, and the temperature is raised to 90°C to obtain The raw material after freezing treatment; then control t...

Embodiment 2

[0038] A preparation method of herbicide saponin, specifically:

[0039] 1. Preparation of hollow microspheres: Place X-type porous zeolite powder in a calciner, control the temperature of the calciner to 370°C, and calcined for 2.5 hours to obtain calcined X-type porous zeolite powder. The porous zeolite powder is mixed with 37g of absolute ethanol, 1.5g of dimethyl diallyl ammonium chloride aqueous solution, 4g of acetic acid, and 1.5g of nickel nitrate before ultrasonic dispersion. The frequency of ultrasonic dispersion is controlled at 25kHz, and the time of ultrasonic dispersion is 25min. , after the ultrasonic dispersion, the dispersed raw material was obtained; the dispersed raw material was cooled to -15°C, frozen at -15°C for 35 minutes, and then slowly raised to 95°C, controlled at a heating rate of 2.5°C / min, and then heated to 95 ℃, to obtain the raw material after freezing treatment; then control the temperature to 95 °C and stir the raw material after freezing tr...

Embodiment 3

[0046] A preparation method of herbicide saponin, specifically:

[0047] 1. Preparation of hollow microspheres: place X-type porous zeolite powder in a calciner, control the temperature of the calciner to 400°C, and obtain calcined X-type porous zeolite powder after calcining for 3 hours, and place 12 g of calcined X-type porous zeolite Zeolite powder is mixed with 40g of absolute ethanol, 2g of dimethyl diallyl ammonium chloride aqueous solution, 5g of acetic acid, and 2g of nickel nitrate before ultrasonic dispersion. The frequency of ultrasonic dispersion is controlled at 30kHz, and the time of ultrasonic dispersion is 30min. After the end, the dispersed raw material is obtained; the dispersed raw material is cooled to -10°C, frozen at -10°C for 40 minutes, then slowly heated to 100°C, and the heating rate is controlled to be 3°C / min, and the temperature is raised to 100°C to obtain Freezing the treated raw material; then controlling the temperature to 100° C. and stirring ...

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Abstract

The invention discloses a preparation method of the herbicide saponin, which comprises preparing hollow microspheres, preparing a catalyst, preparing N-chloroacetyl-N-isopropyl-p-chloroaniline, and preparing saponin; wherein, preparing hollow microspheres The microsphere step is to place X-type porous zeolite powder in a calciner, and after calcining to obtain calcined X-type porous zeolite powder, mix the calcined X-type porous zeolite powder with absolute ethanol, dimethyl diallyl Ammonium chloride, acetic acid, and nickel nitrate are mixed and ultrasonically dispersed, and dispersed raw materials are obtained after ultrasonic dispersion; the dispersed raw materials are frozen and then heated slowly, and then stirred at 90-100°C; The preparation method can increase the yield and purity of the saponin technical drug, reduce the particle size of the prepared savannyl phosphorus technical drug, and improve the uniformity of particle size distribution and fluidity.

Description

technical field [0001] The invention relates to a preparation method of a herbicide saponin, which belongs to the technical field of herbicides. Background technique [0002] The original drug of saponin is white or milky white powder, the content is 96%, the density is 1.4 (20 ℃), the melting point is 47-50 ℃, it decomposes at 150 ℃, it is not sensitive to light, at pH 5-9, temperature It is stable at 22°C, and its half-life in soil is 30-45 days (23°C). The appearance of its preparation is a brown liquid with a phosphate odor, and its storage stability at room temperature is 2 years. [0003] Phosphorus is mainly used in rice. It is an organophosphorus selective systemic herbicide. It is absorbed through the young shoots and underground stems of plants, inhibits cell fission and extension, makes it difficult for weeds to pull out new leaves, stops growth, and finally dies. The effect on weeds that are just sprouting is the best; the effect on weeds that have grown up is p...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/165B01J29/14B01J37/08B01J37/34C07C231/02C07C233/15
CPCC07F9/1651B01J29/143B01J37/08B01J37/343C07C231/02B01J2229/186C07C233/15
Inventor 王冕李军张玉雪崔卫涛马骏
Owner 潍坊新绿化工有限公司
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