CN102442933A - Preparation method of solvent type tert-butyl peroxyneo-caprate (BNP) - Google Patents
Preparation method of solvent type tert-butyl peroxyneo-caprate (BNP) Download PDFInfo
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- CN102442933A CN102442933A CN2010105001267A CN201010500126A CN102442933A CN 102442933 A CN102442933 A CN 102442933A CN 2010105001267 A CN2010105001267 A CN 2010105001267A CN 201010500126 A CN201010500126 A CN 201010500126A CN 102442933 A CN102442933 A CN 102442933A
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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 tert-butyl peroxyneo-caprate (BNP). According to the technical scheme of the invention, the preparation method of the solvent type BNP comprises the following steps of: mixing octyl decanoyl chloride with an alkaline solution and tert-butyl hydrogen peroxide, stirring and reacting at the temperature of 10-40 DEG C; separating a mother liquor; and washing a reaction product to the neutral state and adding an alkane solvent to obtain the solvent type BNP. Due to the adoption of the method for preparing the solvent type BNP provided by the invention, the process flow is simplified, the complex requirements on reaction equipment are eliminated, a reaction is undergone in the mild and safe environment, the product content and yield are 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 special butyl ester of solvent-borne type peroxo-neodecanoic acid (BNP) 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 unsurmountable activity is low, toxicity height, influenced superpolymer such as polyvinyl chloride product quality, and toxic substance is serious to the murder by poisoning of human body in process of production.
The special butyl ester (BNP) of solvent-borne type peroxo-neodecanoic acid is used efficient initiator as a kind of superpolymer is synthetic, compares with common azo-initiator; The special butyl ester of solvent-borne type peroxo-neodecanoic acid is in the superpolymer polymerization process, and 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 method for preparing the special butyl ester of solvent-borne type peroxo-neodecanoic acid (BNP) of industrial applications.
Technical scheme of the present invention is: 1, the preparation method of the special butyl ester of a kind of solvent-borne type peroxo-neodecanoic acid (BNP), and comprise step: (1) adds tertbutyl peroxide 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 the special butyl ester (BNP) of solvent-borne type peroxo-neodecanoic acid.
Basic soln in the said step (1) is aqueous sodium hydroxide solution or potassium hydroxide aqueous solution.
Temperature in the said step (2) is controlled at 25～35 ℃.
The stirring reaction time in the said step (3) is 30～50 minutes.
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.
Solvent in the said step (5) is solvent oil or Permethyl 99A..
Beneficial effect of the present invention is: the special butyl ester (BNP) of solvent-borne type peroxo-neodecanoic acid so that method provided by the invention is prepared 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.In addition, the method for preparing the special butyl ester of solvent-borne type peroxo-neodecanoic acid (BNP) provided by the invention has been simplified technical process; Overcome complicated requirement to conversion unit; Make under the environment that is reflected at gentleness, safety and carry out, product content and yield increase substantially, and yield can reach more than 95%.
Embodiment
Embodiment one: the preparation process of the special butyl ester of solvent-borne type peroxo-neodecanoic acid (BNP) 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 70.5% tertbutyl peroxide 28 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 50 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 the special butyl ester of 97% peroxo-neodecanoic acid (BNP) 83 grams, and yield is 93%;
(6) in the special butyl ester of the peroxo-neodecanoic acid that makes (BNP), add 5 gram Permethyl 99A.s, stir, be cooled to 0 ℃, obtain the special butyl ester (BNP) of solvent-borne type peroxo-neodecanoic acid, concentration is about 91%.
Embodiment two: the preparation process of the special butyl ester of solvent-borne type peroxo-neodecanoic acid (BNP) 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 70.5% tertbutyl peroxide 28 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 50 grams in the back, temperature of reaction is controlled at 25 ℃～35 ℃, 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 the special butyl ester of 97% peroxo-neodecanoic acid (BNP) 83 grams, and yield is 95%;
(6) in the special butyl ester of the peroxo-neodecanoic acid that makes (BNP), add 4 gram solvent oils, stir, be cooled to 0 ℃, obtain the special butyl ester (BNP) of solvent-borne type peroxo-neodecanoic acid, concentration is about 92.5%.
Claims (6)
1. the preparation method of the special butyl ester of solvent-borne type peroxo-neodecanoic acid (BNP) is characterized in that, comprises step:
(1) tertbutyl peroxide 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 the special butyl ester (BNP) of solvent-borne type peroxo-neodecanoic acid.
2. according to the preparation method of the special butyl ester of the said solvent-borne type peroxo-of claim 1 neodecanoic acid (BNP), 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 special butyl ester of the said solvent-borne type peroxo-of claim 1 neodecanoic acid (BNP), 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 special butyl ester of the said solvent-borne type peroxo-of claim 1 neodecanoic acid (BNP), 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 special butyl ester of the said solvent-borne type peroxo-of claim 1 neodecanoic acid (BNP), 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 special butyl ester of the said solvent-borne type peroxo-of claim 1 neodecanoic acid (BNP), 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 |
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| CN2010105001267A CN102442933B (en) | 2010-10-08 | 2010-10-08 | Preparation method of solvent type tert-butyl peroxyneo-caprate (BNP) |
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| CN2010105001267A CN102442933B (en) | 2010-10-08 | 2010-10-08 | Preparation method of solvent type tert-butyl peroxyneo-caprate (BNP) |
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| CN102442933B CN102442933B (en) | 2013-11-06 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104592080A (en) * | 2014-11-26 | 2015-05-06 | 淄博正华助剂股份有限公司 | Method for preparing tert-butyl peroxyneodecanoate (BNP) through continuous flow |
| CN105646315A (en) * | 2015-10-30 | 2016-06-08 | 乌鲁木齐市华泰隆化学助剂有限公司 | Preparation method of solvent type 1,1,3,3-tertramethylbutyl peroxy neo-caprate |
| CN109678773A (en) * | 2018-12-13 | 2019-04-26 | 乌鲁木齐市华泰隆化学助剂有限公司 | A kind of preparation method of peroxide -2-ethyl hexanoic acid tert-butyl |
Citations (4)
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| CN1335326A (en) * | 2000-07-26 | 2002-02-13 | 阿托费纳公司 | Improved process for producing polyvinyl chloride |
| WO2004078800A1 (en) * | 2003-03-06 | 2004-09-16 | Basell Polyolefine Gmbh | Regulation of the continuous ethylene polymerization process in a high-pressure reactor |
| WO2008006666A1 (en) * | 2006-07-12 | 2008-01-17 | United Initiators Gmbh & Co. Kg | Continuous method for producing acyl peroxides |
| CN101287704A (en) * | 2005-10-14 | 2008-10-15 | 埃尔费尔德微技术Bts有限责任公司 | Method for the production of organic peroxides by means of a microreaction technique |
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2010
- 2010-10-08 CN CN2010105001267A patent/CN102442933B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1335326A (en) * | 2000-07-26 | 2002-02-13 | 阿托费纳公司 | Improved process for producing polyvinyl chloride |
| WO2004078800A1 (en) * | 2003-03-06 | 2004-09-16 | Basell Polyolefine Gmbh | Regulation of the continuous ethylene polymerization process in a high-pressure reactor |
| CN101287704A (en) * | 2005-10-14 | 2008-10-15 | 埃尔费尔德微技术Bts有限责任公司 | Method for the production of organic peroxides by means of a microreaction technique |
| WO2008006666A1 (en) * | 2006-07-12 | 2008-01-17 | United Initiators Gmbh & Co. Kg | Continuous method for producing acyl peroxides |
Non-Patent Citations (1)
| Title |
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| 赵玉英: "过氧化新癸酸叔丁酯（BNP）的合成", 《浙江化工》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104592080A (en) * | 2014-11-26 | 2015-05-06 | 淄博正华助剂股份有限公司 | Method for preparing tert-butyl peroxyneodecanoate (BNP) through continuous flow |
| CN105646315A (en) * | 2015-10-30 | 2016-06-08 | 乌鲁木齐市华泰隆化学助剂有限公司 | Preparation method of solvent type 1,1,3,3-tertramethylbutyl peroxy neo-caprate |
| CN109678773A (en) * | 2018-12-13 | 2019-04-26 | 乌鲁木齐市华泰隆化学助剂有限公司 | A kind of preparation method of peroxide -2-ethyl hexanoic acid tert-butyl |
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