CN102443079A - Preparation method of solvent type cumyl peroxyneodecanoate (CNP) - Google Patents
Preparation method of solvent type cumyl peroxyneodecanoate (CNP) Download PDFInfo
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- CN102443079A CN102443079A CN2010105004180A CN201010500418A CN102443079A CN 102443079 A CN102443079 A CN 102443079A CN 2010105004180 A CN2010105004180 A CN 2010105004180A CN 201010500418 A CN201010500418 A CN 201010500418A CN 102443079 A CN102443079 A CN 102443079A
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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
The present invention relates to the synthetic preparation method of a kind of superpolymer, the preparation method of particularly a kind of solvent-borne type peroxo-neodecanoic acid isopropyl benzene ester (CNP) with initiator.
Background technology
Along with the fast development of the synthetic industry of domestic superpolymer, synthetic quality and the demand with initiator of superpolymer promotes rapidly.As everyone knows, azo-initiator uses as superpolymer such as SE building-up reactions initiator like Diisopropyl azodicarboxylate, ABVN (ABVN) for a long time.But azo-initiator has shortcomings such as activity is low, toxicity height, influenced the quality product of superpolymer such as SE, and toxic substance is serious to the murder by poisoning of human body in process of production.
Solvent-borne type peroxo-neodecanoic acid isopropyl benzene ester (CNP) is used efficient initiator as a kind of superpolymer is synthetic, compares with common azo-initiator; In the superpolymer polymerization process, consumption is few, and efficiency of initiation is high; The polyreaction heat release is even, is convenient to control, has effectively avoided the murder by poisoning to human body in the production process; The products obtained therefrom excellent property is the synthetic initiator of using of a kind of superpolymer safe, efficient, constant product quality.
Summary of the invention
The present invention has overcome the deficiency of prior art, provides a kind of easy to operate, process time short and be suitable for the preparation method of the solvent-borne type peroxo-neodecanoic acid isopropyl benzene ester (CNP) of industrial applications.
Technical scheme of the present invention is: the preparation method of a kind of solvent-borne type peroxo-neodecanoic acid isopropyl benzene ester (CNP) comprises step: (1) adds hydrogen phosphide cumene in the basic soln; (2) hot decanoyl chloride slowly is added drop-wise in the solution of step (1) gained, stirs while dripping, temperature is controlled at 10～40 ℃, and hot decanoyl chloride added in 2 hours at 40 minutes; (3) after hot decanoyl chloride dropwises, restir reaction 20～60 minutes; (4) stop to stir after reaction finishes, leave standstill, mother liquor is separated, resultant of reaction is washed till pH value 5～7 till; (5) in the resultant of reaction of step (4) gained, add alkane solvent, stir; (6) be cooled to 0 ℃, obtain solvent-borne type peroxo-neodecanoic acid isopropyl benzene ester (CNP).
Basic soln in the said step (1) is aqueous sodium hydroxide solution or potassium hydroxide aqueous solution.
Temperature control is preferably 25～35 ℃ in the said step (2).
The stirring reaction time is preferably 30～50 minutes in the said step (3).
The mass ratio of the resultant of reaction in alkane solvent described in the said step (5) and the said batching still is 1: 15～1: 20.
Solvent in the said step (5) is preferably solvent oil or Permethyl 99A..
Beneficial effect of the present invention is: (1) solvent-borne type peroxo-neodecanoic acid isopropyl benzene ester (CNP) has overcome the shortcoming that the azo-initiator activity is low, toxicity is big, in the superpolymer polyreaction; Stable polymerization reaction; Polymericular weight is even, and shorten reaction time, and the constant product quality activity is high, consumption is few, initiation is quick, the heat release uniform and stable; Avoided in the production process murder by poisoning, and can produce the higher more stable superpolymer product of quality human body.(2) preparation method of solvent-borne type peroxo-neodecanoic acid isopropyl benzene ester provided by the invention (CNP); Simplified technical process, overcome complicated requirement, made under the environment that is reflected at gentleness, safety and carry out conversion unit; Product content and yield increase substantially, and yield can reach more than 95%.
Embodiment
Embodiment one: the preparation process of solvent-borne type peroxo-neodecanoic acid isopropyl benzene ester (CNP) is following:
(1) in the 500ml flask, the adding mass content is 90% sodium hydroxide 22.5 grams, and water 40 grams stir and are cooled to 5 ℃, process alkaline solution of sodium hydroxide, and concentration is about 32%;
(2) in the solution that step (1) makes, dripping purity is 87.5% hydrogen phosphide cumene 38 grams, reacts 30 minutes, and temperature is controlled at 25 ℃;
(3) stir that in flask, slowly to drip concentration be 80% hot decanoyl chloride solution 55 grams in the back, temperature of reaction is controlled at 25 ℃～30 ℃, adds in 2 hours at 1.5 hours, adds behind the hot decanoyl chloride solution stirring reaction 60 minutes;
(4) stop to stir after reaction finishes, leave standstill, reaction mother liquor is separated, it is till 5～7 that resultant of reaction is washed with water to the pH value;
(5) making mass content is 96% peroxo-neodecanoic acid isopropyl benzene ester (CNP), 82 grams, and yield is 95%;
(6) in the peroxo-neodecanoic acid isopropyl benzene ester (CNP) that makes, add 2.5 gram solvent oils, stir, be cooled to 0 ℃, obtain solvent-borne type peroxo-neodecanoic acid isopropyl benzene ester (CNP), concentration is about 93%.
Embodiment two: the preparation process of solvent-borne type peroxo-neodecanoic acid isopropyl benzene ester (CNP) is following:
(1) in the 500ml flask, the adding mass content is 90% Pottasium Hydroxide 22.5 grams, and water 40 grams stir and are cooled to 5 ℃, process Pottasium Hydroxide alkalescence solution, and concentration is about 32%;
(2) in the solution that step (1) makes, dripping concentration is 87.5% hydrogen phosphide cumene 38 grams, reacts 30 minutes, and temperature is controlled at 25 ℃;
(3) stir that in flask, slowly to drip concentration be 80% hot decanoyl chloride solution 55 grams in the back, temperature of reaction is controlled at 25 ℃～30 ℃, adds in 2 hours at 1.5 hours, adds behind the hot decanoyl chloride solution stirring reaction 60 minutes;
(4) stop to stir after reaction finishes, leave standstill, reaction mother liquor is separated, it is till 5～7 that resultant of reaction is washed with water to the pH value;
(5) making mass content is 97% peroxo-neodecanoic acid isopropyl benzene ester (CNP), 83 grams, and yield is 98%;
(6) in the peroxo-neodecanoic acid isopropyl benzene ester (CNP) that makes, add 3.0 gram Permethyl 99A.s, stir, be cooled to 0 ℃, obtain solvent-borne type peroxo-neodecanoic acid isopropyl benzene ester (CNP), concentration is about 99.5%.
Claims (6)
1. the preparation method of a solvent-borne type peroxo-neodecanoic acid isopropyl benzene ester (CNP) is characterized in that, comprises step:
(1) hydrogen phosphide cumene is added in the basic soln;
(2) hot decanoyl chloride slowly is added drop-wise in the solution of step (1) gained, stirs while dripping, temperature is controlled at 10～40 ℃, and hot decanoyl chloride added in 2 hours at 40 minutes;
(3) after hot decanoyl chloride dropwises, restir reaction 20～60 minutes;
(4) stop to stir after reaction finishes, leave standstill, mother liquor is separated, resultant of reaction is washed till pH value 5～7 till;
(5) in the resultant of reaction of step (4) gained, add alkane solvent, stir;
(6) be cooled to 0 ℃, obtain solvent-borne type peroxo-neodecanoic acid isopropyl benzene ester (CNP).
2. according to the preparation method of the said solvent-borne type peroxo-of claim 1 neodecanoic acid isopropyl benzene ester (CNP), it is characterized in that the basic soln in the said step (1) is aqueous sodium hydroxide solution or potassium hydroxide aqueous solution.
3. according to the preparation method of the said solvent-borne type peroxo-of claim 1 neodecanoic acid isopropyl benzene ester (CNP), it is characterized in that the temperature in the said step (2) is controlled at 25～35 ℃.
4. according to the preparation method of the said solvent-borne type peroxo-of claim 1 neodecanoic acid isopropyl benzene ester (CNP), it is characterized in that the stirring reaction time in the said step (3) is 30～50 minutes.
5. according to the preparation method of the said solvent-borne type peroxo-of claim 1 neodecanoic acid isopropyl benzene ester (CNP), it is characterized in that the mass ratio of the resultant of reaction in said alkane solvent in the said step (5) and the said batching still is 1: 15～1: 20.
6. according to the preparation method of the said solvent-borne type peroxo-of claim 1 neodecanoic acid isopropyl benzene ester (CNP), it is characterized in that the solvent in the said step (5) is solvent oil or Permethyl 99A..
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010105004180A CN102443079A (en) | 2010-10-08 | 2010-10-08 | Preparation method of solvent type cumyl peroxyneodecanoate (CNP) |
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| CN2010105004180A CN102443079A (en) | 2010-10-08 | 2010-10-08 | Preparation method of solvent type cumyl peroxyneodecanoate (CNP) |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102963971A (en) * | 2012-11-20 | 2013-03-13 | 乌鲁木齐市华泰隆化学助剂有限公司 | Method for recycling potassium chloride and organisms from initiator production waste liquid |
| CN104496874A (en) * | 2014-11-26 | 2015-04-08 | 淄博正华助剂股份有限公司 | Method for continuous flow preparation of cumyl peroxyneodecanoate (CNP) |
| CN109134334A (en) * | 2018-09-11 | 2019-01-04 | 蓝凤祥 | A kind of Safe production technology of cumyl peroxyneodecanoate initiator |
| CN112608265A (en) * | 2020-12-03 | 2021-04-06 | 宁夏顺邦达新材料有限公司 | Production process of cumyl peroxyneodecanoate |
-
2010
- 2010-10-08 CN CN2010105004180A patent/CN102443079A/en active Pending
Non-Patent Citations (1)
| Title |
|---|
| 杨卫国: "超高活性引发剂过氧化新癸酸异丙苯酯", 《精细与专用化学品》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102963971A (en) * | 2012-11-20 | 2013-03-13 | 乌鲁木齐市华泰隆化学助剂有限公司 | Method for recycling potassium chloride and organisms from initiator production waste liquid |
| CN104496874A (en) * | 2014-11-26 | 2015-04-08 | 淄博正华助剂股份有限公司 | Method for continuous flow preparation of cumyl peroxyneodecanoate (CNP) |
| CN109134334A (en) * | 2018-09-11 | 2019-01-04 | 蓝凤祥 | A kind of Safe production technology of cumyl peroxyneodecanoate initiator |
| CN112608265A (en) * | 2020-12-03 | 2021-04-06 | 宁夏顺邦达新材料有限公司 | Production process of cumyl peroxyneodecanoate |
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Application publication date: 20120509 |