阅读说明：本技术 一种邻乙基苯胺生产制备方法 (Production and preparation method of o-ethylaniline ) 是由 林瑜琨 马俊 于 2020-12-30 设计创作，主要内容包括：本发明公开了一种邻乙基苯胺生产制备方法,包括原料邻硝基,其特征在于：在原料邻硝基中加入催化剂,经过加氢反应得到邻乙基苯胺。所述催化剂为雷尼镍催化剂,含量为1％。本发明的制备方法,提取的邻乙基苯胺纯度高,利用率高,工艺先进。水汽蒸馏可以使得催化剂与混合产物很好的分离,不产生有害的副产品,绿色环保。(The invention discloses a method for preparing o-ethylaniline, which comprises a raw material o-nitro, and is characterized in that: adding a catalyst into the raw material o-nitro, and carrying out hydrogenation reaction to obtain o-ethylaniline. The catalyst is a Raney nickel catalyst, and the content of the catalyst is 1%. The preparation method of the invention has the advantages of high purity of the extracted o-ethylaniline, high utilization rate and advanced process. The steam distillation can ensure that the catalyst and the mixed product are well separated, no harmful by-product is generated, and the method is green and environment-friendly.)

1. The production and preparation method of o-ethylaniline comprises a raw material o-nitro group, and is characterized in that: adding a catalyst into the raw material o-nitro, and carrying out hydrogenation reaction to obtain o-ethylaniline.

2. The method for preparing o-ethylaniline according to claim 1, which is characterized in that: the catalyst is a Raney nickel catalyst.

3. The method for preparing o-ethylaniline according to claim 1, which is characterized in that: the method comprises the following steps:

the method comprises the following steps: and (3) putting the o-nitro into a reaction kettle according to the proportion.

Step two: adding Raney nickel catalyst into a reaction kettle, and fully stirring the reaction mixture at the reaction temperature of 100-150 DEG C

Step three: filling hydrogen into the reaction kettle until the hydrogen is fully mixed with the mixture, wherein the hydrogen pressure is 3-3.5 MPa.

Step four: and (3) carrying out steam distillation on the reacted mixed product, cooling to room temperature, and standing to obtain colorless oily liquid for later use.

Step five: the colorless oily liquid was dried and filtered to give o-ethylaniline.

4. The method for preparing o-ethylaniline according to claim 3, which is characterized in that: and the stirring speed in the second step is 1500 r/min.

5. The method for preparing o-ethylaniline according to claim 3, which is characterized in that: and the content of the Raney nickel catalyst in the second step is 1%.

6. The method for preparing o-ethylaniline according to claim 1, which is characterized in that: in the third step, a small amount of hydrogen is required to be filled into the reaction kettle for multiple times, so that the catalytic reaction of the ortho-nitro is uniform.

7. The method for preparing o-ethylaniline according to claim 1, which is characterized in that: said step five uses anhydrous magnesium sulfate as a drying agent.

Technical Field

The invention belongs to the technical field of pesticide preparation, and particularly relates to a method for producing o-ethylaniline.

Background

O-ethylaniline is an important pesticide, dye and medical intermediate, and is a key intermediate for synthesizing novel insecticides in the aspect of pesticides. After N-alkylation reaction of o-ethylaniline and 2-bromopropane, the weedicide can be prepared, and is a pre-emergence selective herbicide with good effect on removing grassy weeds and some broad-leaved weeds. O-ethylaniline is also a raw material for the herbicide imazamox and the insecticide ethyl chlordimeform. In the dye industry, the product can be used for preparing the sulfur light-fast blue.

The o-ethylaniline produced by the current enterprises has low utilization rate, is easy to generate harmful byproducts, and the discharged waste gas and waste water have great influence on the environment, so that the o-ethylaniline production preparation method is provided.

Disclosure of Invention

The invention aims to provide a method for producing o-ethylaniline, which aims to solve the problems that the o-ethylaniline produced by the existing enterprises in the background technology is low in utilization rate, harmful byproducts are easy to generate, and the discharged waste gas and waste water have great influence on the environment.

In order to achieve the purpose, the invention provides the following technical scheme: the production and preparation method of o-ethylaniline comprises a raw material o-nitro group, and is characterized in that: adding a catalyst into the raw material o-nitro, and carrying out hydrogenation reaction to obtain o-ethylaniline.

Preferably, the catalyst is a raney nickel catalyst.

Also comprises the following steps:

the method comprises the following steps: and (3) putting the o-nitro into a reaction kettle according to the proportion.

Step two: adding Raney nickel catalyst into a reaction kettle, and fully stirring the reaction mixture at the reaction temperature of 100-150 DEG C

Step three: filling hydrogen into the reaction kettle until the hydrogen is fully mixed with the mixture, wherein the hydrogen pressure is 3-3.5 MPa.

Step four: and (3) carrying out steam distillation on the reacted mixed product, cooling to room temperature, and standing to obtain colorless oily liquid for later use.

Step five: the colorless oily liquid was dried and filtered to give o-ethylaniline.

Preferably, the stirring speed in the second step is 1500 r/min.

Preferably, the content of the raney nickel catalyst in the second step is 1%.

Preferably, the hydrogen in the third step needs to be filled into the reaction kettle for a plurality of times in a small amount, so that the o-nitro catalytic reaction is uniform.

Preferably, said step five uses anhydrous magnesium sulfate as a drying agent.

Compared with the prior art, the invention has the beneficial effects that:

(1) the preparation method of the invention has the advantages of high purity of the extracted o-ethylaniline, high utilization rate and advanced process.

(2) Steam distillation allows good separation of the catalyst from the product mixture without the production of harmful by-products.

Detailed Description

The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.

Example 1

The invention provides a technical scheme that: the production and preparation method of o-ethylaniline comprises a raw material o-nitro group, and is characterized in that: adding a catalyst into the raw material o-nitro, and carrying out hydrogenation reaction to obtain o-ethylaniline.

In this embodiment, the preferred catalyst is a raney nickel catalyst.

The Raney nickel catalyst has the advantages of simple preparation, low preparation cost and high activity, and can greatly improve the hydrogenation reaction speed and effectively improve the production efficiency.

The anhydrous magnesium sulfate is a neutral compound, has no chemical reaction on various organic matters, has the performance of quick water absorption, and is used as a drying agent to dry colorless oily liquid for later use.

The method comprises the following steps:

the method comprises the following steps: and (3) putting the o-nitro into a reaction kettle according to the proportion.

Step two: adding Raney nickel catalyst into a reaction kettle, and fully stirring the reaction mixture at the reaction temperature of 100-150 DEG C

Step three: filling hydrogen into the reaction kettle until the hydrogen is fully mixed with the mixture, wherein the hydrogen pressure is 3-3.5 MPa.

Step four: and (3) carrying out steam distillation on the reacted mixed product, cooling to room temperature, and standing to obtain colorless oily liquid for later use.

Step five: the colorless oily liquid was dried and filtered to give o-ethylaniline.

Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.