阅读说明：本技术 用于制备有机过氧化物的方法 (Process for preparing organic peroxides ) 是由 王子辉 邹杨 于 2021-08-02 设计创作，主要内容包括：本发明提供一种用于制备有机过氧化物的方法,涉及有机过氧化物制备领域。该用于制备有机过氧化物的方法,包括以下步骤：步骤一、进行挑选；步骤二、进行反应；步骤三、进行升温；步骤四、再次加温；步骤五、进行过滤；步骤六、进行清洗；步骤七、进行干燥。通过在反应结束后,对内部的剩余气体进行抽出,不仅完成了反应前的抽压,同时可以在后续的反应过程再次应用,从而使得到的产品率得到相应的提高,通过在反应过程中不服按加入过氧化物,提供相应反应物的浓度,使的反应物的反应程度较大,得到的成品较多,且添加的过氧化物,得到的氧气,在负压状态下通过催化剂易于进行反应,提高利用率。(The invention provides a method for preparing organic peroxide, and relates to the field of organic peroxide preparation. The method for preparing an organic peroxide comprises the following steps: step one, selecting; step two, carrying out reaction; step three, heating; step four, heating again; step five, filtering; step six, cleaning; and step seven, drying. Through after the reaction, take out inside residual gas, not only accomplished the take out pressure before the reaction, can use once more at subsequent reaction process simultaneously to make the product rate that obtains obtain corresponding improvement, through not obeying in the reaction process and pressing the peroxide of adding, provide the concentration of corresponding reactant, the reaction degree of the reactant that makes is great, the finished product that obtains is more, and the peroxide of adding, the oxygen that obtains easily reacts through the catalyst under negative pressure state, the increase of utilization ratio.)

1. A process for preparing an organic peroxide, characterized in that: the method comprises the following steps:

step one, selection: selecting proper reactants, inorganic peroxide, catalyst and filler;

step two, carrying out reaction: extracting air in a reaction kettle, and slowly adding an organic solvent, a reactant, inorganic peroxide, a catalyst and a filler into the reaction kettle in sequence;

step three, heating: when the temperature rises to 20-30 ℃, slowly adding sodium sulfate into the mixture, and reacting for 30-50 minutes;

step four, heating again: after the reaction is finished, heating to 40-50 ℃ again, then reacting for 30-60 minutes to the internal hydrogen peroxide solution;

step five, filtering: collecting oxygen and participating gas in the reaction kettle, and collecting the intercepted solid by filtering out an internal impurity solution of a product after the reaction is finished;

step six, cleaning: washing the obtained solid, and then soaking again;

step seven, drying: and drying the soaked solid at low temperature to obtain a corresponding finished product.

2. The process for producing an organic peroxide according to claim 1, wherein: the reactant is ketone or alcohol, and at least one tertiary alcohol group or tertiary ketone group is contained.

3. The process for producing an organic peroxide according to claim 1, wherein: the inorganic peroxide is one or more of sodium peroxide, sodium carbonate hydroperoxide and hydrogen peroxide.

4. The process for producing an organic peroxide according to claim 1, wherein: the catalyst is one or more of a solid acid catalyst, a cationic strong acid resin catalyst and a heteropoly acid catalyst.

5. The process for producing an organic peroxide according to claim 1, wherein: the filler is one or more of silicon dioxide, carbon black, calcium carbonate and kaolin.

6. The process for producing an organic peroxide according to claim 1, wherein: and the oxygen recollected in the step five can be used as inorganic peroxide to reenter the reaction kettle.

7. The process for producing an organic peroxide according to claim 1, wherein: and in the sixth step, the cleaning is to firstly wash twice by using plasma water with the pH of 8 and then wash by using plasma water with the pH of 7.

8. The process for producing an organic peroxide according to claim 1, wherein: the drying temperature in the seventh step is-2 ℃ to 2 ℃, and the drying time is 30 minutes to 50 minutes.

Technical Field

The invention relates to the technical field of organic peroxide preparation, in particular to a method for preparing organic peroxide.

Background

An organic compound containing a-O-peroxy functional group, wherein a hydrogen atom in hydrogen peroxide is replaced with an organic group such as an alkyl group, an acyl group, or an aromatic group. Is characterized in that the oxygen-containing free radical is generated by decomposition after being heated to exceed a certain temperature, and is unstable and easy to decompose. The organic peroxide in chemical production is mainly used as polymerization initiator and catalyst for synthetic resin. In the field of high molecular materials, it can be used as an initiator of free radical polymerization, an initiator of grafting reaction, a cross-linking agent of rubber and plastics, a curing agent of unsaturated polyester and a molecular weight and molecular weight distribution regulator in the preparation of spinning-grade polypropylene. The peroxyacyl nitrate compounds can be generated by the free radical reaction of polluted air in the environment under the action of light, and are one of the particles of photochemical oxidants.

The existing organic peroxide preparation methods are various, alkaline media are utilized to carry out catalytic reaction on silver ion activators, but materials are agglomerated, the yield is low, the production steps are complicated, and the reaction is carried out through strong acid, so that more heat is released in the reaction process, the produced organic peroxide is unstable and decomposed, and the yield is low.

Disclosure of Invention

Technical problem to be solved

Aiming at the defects of the prior art, the invention provides a method for preparing organic peroxide, which solves the problems of more complicated preparation steps and lower finished product in the prior art.

(II) technical scheme

In order to achieve the purpose, the invention is realized by the following technical scheme: a process for preparing an organic peroxide comprising the steps of:

step one, selection: selecting proper reactants, inorganic peroxide, catalyst and filler;

step two, carrying out reaction: extracting air in a reaction kettle, and slowly adding an organic solvent, a reactant, inorganic peroxide, a catalyst and a filler into the reaction kettle in sequence;

step three, heating: when the temperature rises to 20-30 ℃, slowly adding sodium sulfate into the mixture, and reacting for 30-50 minutes;

step four, heating again: after the reaction is finished, heating to 40-50 ℃ again, then reacting for 30-60 minutes to the internal hydrogen peroxide solution;

step five, filtering: collecting oxygen and participating gas in the reaction kettle, and collecting the intercepted solid by filtering out an internal impurity solution of a product after the reaction is finished;

step six, cleaning: washing the obtained solid, and then soaking again;

step seven, drying: and drying the soaked solid at low temperature to obtain a corresponding finished product.

Preferably, the reactant is a ketone or alcohol and has at least one tertiary alcohol or ketone group.

Preferably, the inorganic peroxide is one or more of sodium peroxide, sodium carbonate hydroperoxide and hydrogen peroxide.

Preferably, the catalyst is one or more of a solid acid catalyst, a cationic strong acid resin catalyst and a heteropolyacid catalyst.

Preferably, the filler is one or more of silica, carbon black, calcium carbonate and kaolin.

Preferably, the oxygen recollected in the fifth step can be used as inorganic peroxide to re-enter the reaction kettle.

Preferably, the cleaning in the sixth step is to wash twice with plasma water with pH 8, and then wash with plasma water with pH 7.

Preferably, the drying temperature in the seventh step is-2 ℃ to 2 ℃, and the drying time is 30 minutes to 50 minutes.

(III) advantageous effects

The present invention provides a process for preparing an organic peroxide. The method has the following beneficial effects:

1. according to the invention, before the reaction, air is pumped from the reaction kettle, so that the reactants in the reaction kettle are more pure and have higher concentration, and corresponding negative pressure is generated to promote molecular diffusion and accelerate the reaction.

2. According to the invention, after the reaction is finished, the residual gas in the reaction kettle is pumped out, so that the pumping pressure before the reaction is finished, and the residual gas can be reused in the subsequent reaction process, thereby correspondingly improving the product rate.

3. According to the invention, the peroxide is not added in the reaction process, so that the concentration of the corresponding reactant is provided, the reaction degree of the reactant is larger, more finished products are obtained, the added peroxide and the obtained oxygen are easy to react through the catalyst in a negative pressure state, and the utilization rate is improved.

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.

The first embodiment is as follows:

an embodiment of the present invention provides a method for preparing an organic peroxide, including the steps of:

step one, selection: selecting proper reactants, inorganic peroxide, catalyst and filler;

step two, carrying out reaction: extracting air in a reaction kettle, and slowly adding an organic solvent, a reactant, inorganic peroxide, a catalyst and a filler into the reaction kettle in sequence;

step three, heating: when the temperature rises to 20-30 ℃, slowly adding sodium sulfate into the mixture, and reacting for 30-50 minutes;

step four, heating again: after the reaction is finished, heating to 40-50 ℃ again, then reacting for 30-60 minutes to the internal hydrogen peroxide solution;

step five, filtering: collecting oxygen and participating gas in the reaction kettle, and collecting the intercepted solid by filtering out an internal impurity solution of a product after the reaction is finished;

step six, cleaning: washing the obtained solid, and then soaking again;

step seven, drying: and drying the soaked solid at low temperature to obtain a corresponding finished product.

The reactant is ketone or alcohol and at least has one tertiary alcohol group or tertiary ketone group, the catalyst is one or more of a solid acid catalyst, a cationic strong acid resin catalyst and a heteropoly acid catalyst, and the filler is one or more of silica, carbon black, calcium carbonate and kaolin.

And the oxygen recollected in the fifth step can be used as inorganic peroxide to re-enter the reaction kettle, the cleaning in the sixth step is to firstly wash twice by using plasma water with the pH of 8 and then wash by using plasma water with the pH of 7, the drying temperature in the seventh step is-2 ℃ to 2 ℃, and the drying time is 30 minutes to 50 minutes.

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.