CN102584665B - Method for preparing 75 mass percent solvent based cumyl peroxyneodecanoate - Google Patents
Method for preparing 75 mass percent solvent based cumyl peroxyneodecanoate Download PDFInfo
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Abstract
The invention relates to a method for preparing 75 mass percent solvent based cumyl peroxyneodecanoate and belongs to the field of preparation methods for initiators for synthesizing high polymers. The method is characterized by comprising the following steps of: adding cumene hydroperoxide into an alkaline solution; dripping neodecanoyl chloride into the obtained solution; after reaction, stopping stirring, and standing for 20 to 40 minutes, separating a mother solution, and washing a reaction product until pH value is 5 to 7; and adding an alkane solvent into the obtained reaction product, and stirring at the temperature of 0 DEG C for 1 hour; and thus obtaining the solvent based cumyl peroxyneodecanoate. According to the preparation method, a process is simplified, the complex requirements on reaction equipment are overcome, reaction is performed in a mild and safe environment, the quality and yield of the product are greatly improved, and the yield can reach over 95 percent. The quality level of the product is the same as that of products of the same kind in foreign countries.
Description
Technical field
The present invention relates to a kind of method for making of solvent-borne type massfraction 75% cumyl peroxyneodecanoate, belong to the field of the preparation method of superpolymer synthesis initiator.
Background technology
Along with the fast development of domestic superpolymer synthesis industry, kind and the demand of superpolymer synthesis initiator promote rapidly.Solvent type cumyl peroxyneodecanoate (CNP)-75 is as a kind of superpolymer synthesis higher effective initiator, in the course of the polymerization process, consumption is few, easily disperse in polymerization system, in polymerization, exothermic heat of reaction is even, and efficiency of initiation is higher, is convenient to control, products obtained therefrom excellent property is a kind of superpolymer synthesis initiator of safe, efficient, constant product quality.
Summary of the invention
According to the deficiencies in the prior art, the technical problem to be solved in the present invention is: the method for making providing a kind of solvent-borne type massfraction 75% cumyl peroxyneodecanoate, easy to operate, the process time is short and be suitable for industrial applications.
The technical solution adopted for the present invention to solve the technical problems is: the method for making providing a kind of solvent-borne type massfraction 75% cumyl peroxyneodecanoate, is characterized in that comprising step:
(1) add in basic solution by hydrogen phosphide cumene, the mass ratio of hydrogen phosphide cumene and alkali is 1: 0.27 ~ 0.54;
(2) be added drop-wise to by new decanoyl chloride in the solution of step (1) gained, dropping limit, limit is stirred, and new decanoyl chloride added in 2 hours at 40 minutes, and the mass ratio of the solution of new decanoyl chloride and step (1) gained is 1: 1.5 ~ 2.8;
(3) after new decanoyl chloride dropwises, then stirring reaction 30 ~ 50 minutes;
(4) reaction terminates standing 20 ~ 40 minutes of rear stopping stirring, is separated, till resultant of reaction being washed till pH value 5 ~ 7 by mother liquor;
(5) in the resultant of reaction of step (4) gained, add alkane solvent, stir 1 hour at temperature 0 DEG C; Obtain solvent type cumyl peroxyneodecanoate.
Basic solution in described step (1) is aqueous sodium hydroxide solution or potassium hydroxide aqueous solution, and its massfraction is 25% ~ 35%;
Temperature in described step (2) controls at 10 ~ 30 DEG C.
The stirring reaction time in described step (3) is 40 ~ 45 minutes.
The resultant of reaction of step (4) gained described in described step (5) and the mass ratio of alkane solvent are 1: 0.2 ~ 1: 0.25.
Solvent in described step (5) is solvent oil or Permethyl 99A..
The invention has the beneficial effects as follows:
(1) solvent type cumyl peroxyneodecanoate (CNP)-75, in superpolymer polyreaction, stable polymerization reaction, polymericular weight is even, reaction time shortens, constant product quality activity is high, consumption is few, initiation is quick, heat release uniform and stable, avoids the murder by poisoning to human body in production process, and can produce the higher more stable superpolymer product of quality.
(2) preparation method of solvent type cumyl peroxyneodecanoate provided by the invention (CNP)-75, simplify technical process, overcome the complicated requirement to conversion unit, reaction is carried out under gentle, safe environment, quality product and yield increase substantially, and yield can reach more than 95%.Product quality level can reach identical with same kind of products at abroad.
Product quality indicator is in table 1:
Table 1
| Project | Index |
| Outward appearance | Colourless transparent liquid, mechanical impurity |
| Colourity, Pt-Co≤ | 30 |
| Active oxygen massfraction, % | 3.92±0.05 |
| CNP massfraction, % | 75.0±1.0 |
| Chlorine (in Cl) massfraction, %≤ | 0.015 |
| Free acid (in neodecanoic acid)Massfraction, %≤ | 0.10 |
| Hydrogen base superoxide ( In CHP) massfraction, %≤ | 0.10 |
Embodiment
Below in conjunction with embodiment, the present invention is described further.
Embodiment one
The preparation process of solvent type cumyl peroxyneodecanoate (CNP)-75 is as follows:
(1) in 250ml flask, add 22.5 grams, the sodium hydroxide that content is 90%, 40 grams, water, stir and be cooled to 5 DEG C, make alkaline solution of sodium hydroxide, concentration is about 32.4%;
(2) in the obtained solution of step (1), drip the hydrogen phosphide cumene 47.9 grams that purity is 87.5%, react 30 minutes, temperature controls at 25-35 DEG C;
(3) stirring and slowly dripping concentration in backward flask is 80% new decanoyl chloride-solvent oil mixing solutions 55 grams, and temperature of reaction controls at 20 ~ 30 DEG C, and 2 hours used times added, and to add after new decanoyl chloride solution stirring reaction 30 minutes;
(4) reaction terminates rear stoppings and stirring, and leaves standstill 20 minutes, is separated by reaction mother liquor, resultant of reaction is washed to pH value be 5;
(5) obtained content is 80% cumyl peroxyneodecanoate (CNP) 84.8 grams, and yield is 95.9%;
(6) in obtained cumyl peroxyneodecanoate (CNP), add 19.5 grams of solvent oils, stir 1 hour at 0 DEG C, obtain solvent type cumyl peroxyneodecanoate (CNP), content is about 75.1%.All other indexs all reach product quality indicator requirement.
| Project | Index |
| Outward appearance | Colourless transparent liquid, mechanical impurity |
| Colourity, Pt-Co≤ | 30 |
| Active oxygen massfraction, % | 3.92±0.05 |
| CNP massfraction, % | 75.0±1.0 |
| Chlorine (in Cl) massfraction, %≤ | 0.015 |
| Free acid (in neodecanoic acid)Massfraction, %≤ | 0.10 |
| Hydrogen base superoxide ( In CHP) massfraction, %≤ | 0.10 |
Embodiment two
The preparation process of solvent type cumyl peroxyneodecanoate (CNP) is as follows:
(1) in 250ml flask, add 22.5 grams, the potassium hydroxide that content is 90%, 40 grams, water, stir and be cooled to 5 DEG C, make potassium hydroxide basic solution, concentration is about 32.4%;
(2) in the obtained solution of step (1), drip the hydrogen phosphide cumene 47.9 grams that concentration is 87.5%, react 30 minutes, temperature controls at 20-30 DEG C;
(3) stirring and slowly dripping concentration in backward flask is 80% new decanoyl chloride-Permethyl 99A. mixing solutions 55 grams, and temperature of reaction controls at 10 DEG C ~ 20 DEG C, and 40 minutes used times added, and to add after new decanoyl chloride solution stirring reaction 50 minutes;
(4) reaction terminates rear stoppings and stirring, and leaves standstill 40 minutes, is separated by reaction mother liquor, resultant of reaction is washed to pH value be 7;
(5) obtained content is 79.9% cumyl peroxyneodecanoate (CNP) 84.9 grams, and yield is 96%;
(6) in obtained cumyl peroxyneodecanoate (CNP), add 17.5 grams of Permethyl 99A.s, stir 1 hour in 0 DEG C, obtain solvent type cumyl peroxyneodecanoate (CNP), concentration is about 75.9%.All other indexs all reach product quality indicator requirement.
| Project | Index |
| Outward appearance | Colourless transparent liquid, mechanical impurity |
| Colourity, Pt-Co≤ | 30 |
| Active oxygen massfraction, % | 3.92±0.05 |
| CNP massfraction, % | 75.0±1.0 |
| Chlorine (in Cl) massfraction, %≤ | 0.015 |
| Free acid (in neodecanoic acid)Massfraction, %≤ | 0.10 |
| Hydrogen base superoxide ( In CHP) massfraction, %≤ | 0.10 |
Claims (2)
1. a method for making for solvent-borne type massfraction 75% cumyl peroxyneodecanoate, is characterized in that, comprise step:
(1) add in basic solution by hydrogen phosphide cumene, the mass ratio of hydrogen phosphide cumene and alkali is 2.07:1, step
(1) basic solution in is aqueous sodium hydroxide solution or potassium hydroxide aqueous solution, and its massfraction is 25% ~ 35%;
(2) be added drop-wise to by new decanoyl chloride in the solution of step (1) gained, dropping limit, limit is stirred, and new decanoyl chloride is little to 2 at 40 minutes
In time, interiorly adds, and the mass ratio of the solution of new decanoyl chloride and step (1) gained is 1:2.51, and temperature controls at 10 ~ 30 DEG C;
(3) after new decanoyl chloride dropwises, then stirring reaction 30 ~ 50 minutes;
(4) reaction terminates standing 20 ~ 40 minutes of rear stopping stirring, is separated, till resultant of reaction being washed till pH value 5 ~ 7 by mother liquor;
(5) in the resultant of reaction of step (4) gained, add alkane solvent, stir 1 hour at temperature 0 DEG C; Obtain solvent type cumyl peroxyneodecanoate, the resultant of reaction of described step (4) gained and the mass ratio of alkane solvent are 1:0.2 ~ 1:0.25, and the solvent in step (5) is solvent oil or Permethyl 99A..
2. the method for making of solvent-borne type massfraction 75% cumyl peroxyneodecanoate according to claim 1, is characterized in that the stirring reaction time in described step (3) is 40 ~ 45 minutes.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
| CN109134334A (en) * | 2018-09-11 | 2019-01-04 | 蓝凤祥 | A kind of Safe production technology of cumyl peroxyneodecanoate initiator |
| CN109400514A (en) * | 2018-10-30 | 2019-03-01 | 乌鲁木齐市华泰隆化学助剂有限公司 | A kind of preparation method of peroxidating (3,5,5 Trimethylhexanoic acid) tert-butyl ester |
| 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 |
| 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 |
| CN114031753B (en) * | 2020-12-31 | 2023-11-03 | 广东聚华印刷显示技术有限公司 | Organic polymers and their use |
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| CN1491210A (en) * | 2001-02-13 | 2004-04-21 | ���з��ɹ�˾ | Peroxyester preparation method |
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| US3624123A (en) * | 1968-05-01 | 1971-11-30 | Argus Chem | t-ALKYL PERESTERS OF t-HYDROPEROXIDES |
| US4075236A (en) * | 1976-09-30 | 1978-02-21 | Pennwalt Corporation | Continuous manufacture of peroxyesters |
| JPS56103159A (en) * | 1980-01-19 | 1981-08-18 | Nippon Oil & Fats Co Ltd | Preparation of novel peroxy ester |
| JPH05186511A (en) * | 1992-01-09 | 1993-07-27 | Nippon Oil & Fats Co Ltd | Method of polymerizing vinyl chloride monomer |
| US6995221B2 (en) * | 1999-11-04 | 2006-02-07 | Oxy Vinyls, L.P. | Method for producing organic peroxides and their use in the radical polymerization of monomers |
| EP1852418A1 (en) * | 2006-04-27 | 2007-11-07 | Arkema France | Process for synthesizing selected organic peroxides |
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| CN1491210A (en) * | 2001-02-13 | 2004-04-21 | ���з��ɹ�˾ | Peroxyester preparation method |
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| 《超高活性引发剂过氧化新癸酸异丙苯酯》;杨卫国;《精细与专用化学》;19981231(第14期);第11页左栏"二、生产原理"，第2-3行，第8-9行 * |
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Denomination of invention: Preparation method of 75% solvent based isopropyl decanoate peroxide Effective date of registration: 20230511 Granted publication date: 20141224 Pledgee: Zibo Linzi District sub branch of China Post Savings Bank Co.,Ltd. Pledgor: ZIBO ZHENGHUA AUXILIARY Co.,Ltd. Registration number: Y2023980040339 |