阅读说明：本技术 一种烯草酮锂盐标样的制备方法 (Preparation method of clethodim lithium salt standard sample ) 是由 董红波 邹淑芳 褚国忠 周红英 陈树辉 于 2020-05-21 设计创作，主要内容包括：本发明涉及一种烯草酮锂盐标样的制备方法,包括以下步骤：(1)以丙酮为溶剂,向丙酮中加入烯草酮和无水氢氧化锂,烯草酮与氢氧化锂的物质的量之比为1.1-1.3：1；(2)搅拌并升温至30℃-60℃,反应8-12小时；(3)自然冷却至10℃-15℃后析出结晶,过滤后得到结晶体,并用丙酮洗涤；(4)对结晶体真空干燥后粉碎、过筛得到最终标样。本发明简单易操作,制备的标样含量高,稳定性好,不宜结块。(The invention relates to a preparation method of clethodim lithium salt standard sample, which comprises the following steps: (1) adding clethodim and anhydrous lithium hydroxide into acetone by taking acetone as a solvent, wherein the mass ratio of clethodim to lithium hydroxide is 1.1-1.3: 1; (2) stirring and heating to 30-60 ℃, and reacting for 8-12 hours; (3) naturally cooling to 10-15 ℃, separating out crystals, filtering to obtain crystals, and washing with acetone; (4) and drying the crystals in vacuum, crushing and sieving to obtain the final standard sample. The method is simple and easy to operate, and the prepared standard sample has high content and good stability and is not easy to agglomerate.)

1. A preparation method of clethodim lithium salt standard samples is characterized by comprising the following steps: the method comprises the following steps:

(1) Adding clethodim and anhydrous lithium hydroxide into acetone by taking acetone as a solvent, wherein the mass ratio of clethodim to lithium hydroxide is 1.1-1.3: 1;

(2) Stirring and heating to 30-60 ℃, and reacting for 8-12 hours;

(3) Naturally cooling to 10-15 ℃, separating out crystals, filtering to obtain crystals, and washing with acetone;

(4) And drying the crystals in vacuum, crushing and sieving to obtain the final standard sample.

2. The process for preparing a clethodim lithium salt standard according to claim 1, wherein: in the step (4), the drying temperature is 30 ℃ to 50 ℃, and the vacuum degree is-0.08 MPa to-0.09 MPa.

3. The process for preparing a clethodim lithium salt standard according to claim 1, wherein: acetone is analytically pure 99% content acetone.

Technical Field

The invention relates to the technical field of chemical preparation, and particularly relates to a preparation method of a clethodim lithium salt standard sample.

Background

The clethodim lithium salt is a standard sample for quantitative analysis of clethodim technical materials, and the clethodim lithium salt obtained by the conventional synthesis method at present has the defects of low content, short storage time, poor stability, easiness in caking and the like.

Disclosure of Invention

Aiming at the defects of the prior art, the invention provides the preparation method of the clethodim lithium salt standard sample, which is simple and easy to operate, and the prepared standard sample has high purity and good stability.

The invention is realized by the following technical scheme:

The preparation method of the clethodim lithium salt standard sample comprises the following steps:

(1) Adding clethodim and anhydrous lithium hydroxide into acetone by taking acetone as a solvent, wherein the mass ratio of clethodim to lithium hydroxide is 1.1-1.3: 1;

(2) Stirring and heating to 30-60 ℃, and reacting for 8-12 hours;

(3) Naturally cooling to 10-15 ℃, separating out crystals, filtering to obtain crystals, and washing with acetone;

(4) And drying the crystals in vacuum, crushing and sieving to obtain the final standard sample.

Further, in the step (4), the drying temperature is 30 ℃ to 50 ℃, and the vacuum degree is-0.08 MPa to-0.09 MPa.

Further, acetone is analytically pure 99% content acetone.

The invention has the beneficial effects that:

The synthesis conditions of the clethodim lithium salt are improved and adjusted, so that the content yield of the clethodim lithium salt is increased, the stability is improved, the storage time is prolonged, and the product is not easy to agglomerate and is easy to crush.

Detailed Description

In order to clearly illustrate the technical features of the present solution, the present solution is explained below by way of specific embodiments.

A preparation method of clethodim lithium salt standard samples comprises the following steps:

(1) Acetone is used as a solvent, the acetone is used as acetone with the content of 99% of analytical purity, clethodim and anhydrous lithium hydroxide are added into the acetone, and the mass ratio of the clethodim to the lithium hydroxide is 1.1-1.3: 1;

(2) Stirring and heating to 30-60 ℃, and reacting for 8-12 hours;

(3) Naturally cooling to 10-15 ℃, separating out crystals, filtering to obtain crystals, and washing with acetone;

(4) And drying the crystals in vacuum, crushing and sieving to obtain the final standard sample.

Further, in the step (4), the drying temperature is 30 ℃ to 50 ℃, and the vacuum degree is-0.08 MPa to-0.09 MPa.