Preparation method of solvent type cumyl peroxyneodecanoate (CNP)

Abstract

The invention relates to a preparation method of an initiator for synthesizing a high polymer, in particular to a preparation method of solvent type cumyl peroxyneodecanoate (CNP). According to the technical scheme of the invention, the preparation method of the solvent type CNP comprises the following steps of: mixing octyl decanoyl chloride with an alkaline solution and cumyl hydroperoxide, stirring and reacting at the temperature of 10-40 DEG C; and washing a reaction product to neutral, and adding an alkane solvent to obtain the solvent type CNP. Due to the adoption of the method for preparing the solvent type CNP provided by the invention, the process flow is simplified, the complex requirements on reaction equipment are eliminated, a reaction can be undergone in a mild and safe condition, the product content and yield can be increased greatly, and the yield can be over 95 percent.

Description

technical field

[0001] The invention relates to a preparation method of an initiator for polymer synthesis, in particular to a preparation method of solvent-type cumyl peroxyneodecanoate (CNP). Background technique

[0002] With the rapid development of the domestic polymer synthesis industry, the quality and demand of initiators for polymer synthesis have increased rapidly. As we all know, azo initiators, such as azobisisobutyronitrile and azobisisoheptanonitrile (ABVN), have long been used as initiators for the synthesis of high polymers such as polyvinyl chloride. However, azo initiators have disadvantages such as low activity and high toxicity, which affect the product quality of high polymers such as polyvinyl chloride, and the toxic substances in the production process are seriously harmful to the human body.

[0003] Solvent-based cumyl peroxyneodecanoate (CNP), as a high-efficiency initiator for high polymer synthesis, compared with ordinary azo initiators, in the p...

Examples

Embodiment 1

[0012] Embodiment one: the preparation steps of solvent type cumyl peroxyneodecanoate (CNP) are as follows:

[0013] (1) In a 500ml flask, add 22.5 grams of sodium hydroxide with a mass content of 90%, 40 grams of water, stir and cool to 5°C, and make a sodium hydroxide alkaline solution with a concentration of about 32%;

[0014] (2) 38 grams of cumene hydroperoxide with a purity of 87.5% were added dropwise to the solution prepared in step (1), reacted for 30 minutes, and the temperature was controlled at 25° C.;

[0015] (3) Slowly add 55 grams of 80% octadecanoyl chloride solution in the flask after stirring evenly, the reaction temperature is controlled at 25°C to 30°C, and the addition is completed within 1.5 hours to 2 hours. After adding the octadecanoyl chloride solution Stir the reaction for 60 minutes;

[0016] (4) Stop stirring after the reaction is over, let it stand, separate the reaction mother liquor, and wash the reaction product with water until the pH value...

Embodiment 2

[0019] Embodiment two: the preparation steps of solvent type cumyl peroxyneodecanoate (CNP) are as follows:

[0020] (1) In a 500ml flask, add 22.5 grams of potassium hydroxide with a mass content of 90%, 40 grams of water, stir and cool to 5°C, and make a potassium hydroxide alkaline solution with a concentration of about 32%;

[0021] (2) 38 grams of cumene hydroperoxide with a concentration of 87.5% were added dropwise to the solution prepared in step (1), reacted for 30 minutes, and the temperature was controlled at 25° C.;

[0022] (3) Slowly add 55 grams of 80% octadecanoyl chloride solution in the flask after stirring evenly, the reaction temperature is controlled at 25°C to 30°C, and the addition is completed within 1.5 hours to 2 hours. After adding the octadecanoyl chloride solution Stir the reaction for 60 minutes;

[0023] (4) Stop stirring after the reaction is over, let it stand, separate the reaction mother liquor, and wash the reaction product with water until...

technical field

[0001] The invention relates to a preparation method of an initiator for polymer synthesis, in particular to a preparation method of solvent-type cumyl peroxyneodecanoate (CNP). Background technique

[0002] With the rapid development of the domestic polymer synthesis industry, the quality and demand of initiators for polymer synthesis have increased rapidly. As we all know, azo initiators, such as azobisisobutyronitrile and azobisisoheptanonitrile (ABVN), have long been used as initiators for the synthesis of high polymers such as polyvinyl chloride. However, azo initiators have disadvantages such as low activity and high toxicity, which affect the product quality of high polymers such as polyvinyl chloride, and the toxic substances in the production process are seriously harmful to the human body.

[0003] Solvent-based cumyl peroxyneodecanoate (CNP), as a high-efficiency initiator for high polymer synthesis, compared with ordinary azo initiators, in the p...

Examples

Embodiment 1

[0012] Embodiment one: the preparation steps of solvent type cumyl peroxyneodecanoate (CNP) are as follows:

[0013] (1) In a 500ml flask, add 22.5 grams of sodium hydroxide with a mass content of 90%, 40 grams of water, stir and cool to 5°C, and make a sodium hydroxide alkaline solution with a concentration of about 32%;

[0014] (2) 38 grams of cumene hydroperoxide with a purity of 87.5% were added dropwise to the solution prepared in step (1), reacted for 30 minutes, and the temperature was controlled at 25° C.;

[0015] (3) Slowly add 55 grams of 80% octadecanoyl chloride solution in the flask after stirring evenly, the reaction temperature is controlled at 25°C to 30°C, and the addition is completed within 1.5 hours to 2 hours. After adding the octadecanoyl chloride solution Stir the reaction for 60 minutes;

[0016] (4) Stop stirring after the reaction is over, let it stand, separate the reaction mother liquor, and wash the reaction product with water until the pH value...

Embodiment 2

[0019] Embodiment two: the preparation steps of solvent type cumyl peroxyneodecanoate (CNP) are as follows:

[0020] (1) In a 500ml flask, add 22.5 grams of potassium hydroxide with a mass content of 90%, 40 grams of water, stir and cool to 5°C, and make a potassium hydroxide alkaline solution with a concentration of about 32%;

[0021] (2) 38 grams of cumene hydroperoxide with a concentration of 87.5% were added dropwise to the solution prepared in step (1), reacted for 30 minutes, and the temperature was controlled at 25° C.;

[0022] (3) Slowly add 55 grams of 80% octadecanoyl chloride solution in the flask after stirring evenly, the reaction temperature is controlled at 25°C to 30°C, and the addition is completed within 1.5 hours to 2 hours. After adding the octadecanoyl chloride solution Stir the reaction for 60 minutes;

[0023] (4) Stop stirring after the reaction is over, let it stand, separate the reaction mother liquor, and wash the reaction product with water until...