CN102584665A - 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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- CN102584665A CN102584665A CN201110441702XA CN201110441702A CN102584665A CN 102584665 A CN102584665 A CN 102584665A CN 201110441702X A CN201110441702X A CN 201110441702XA CN 201110441702 A CN201110441702 A CN 201110441702A CN 102584665 A CN102584665 A CN 102584665A
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- neodecanoic acid
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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% peroxo-neodecanoic acid isopropyl benzene ester, belong to superpolymer and synthesize field with the preparation method of initiator.
Background technology
Along with the fast development of the synthetic industry of domestic superpolymer, synthetic kind and the demand with initiator of superpolymer promotes rapidly.Solvent-borne type peroxo-neodecanoic acid isopropyl benzene ester (CNP)-75 is used efficient initiator as a kind of superpolymer is synthetic, and in polymerization process, consumption is few; In polymerization system, disperse easily; Exothermic heat of reaction is even in polymerization, and efficiency of initiation is higher, is convenient to control; 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
According to the deficiency of prior art, the technical problem that the present invention will solve is: a kind of method for making of solvent-borne type massfraction 75% peroxo-neodecanoic acid isopropyl benzene ester is provided, and easy to operate, process time is short and be suitable for industrial applications.
The technical solution adopted for the present invention to solve the technical problems is: a kind of method for making of solvent-borne type massfraction 75% peroxo-neodecanoic acid isopropyl benzene ester is provided, it is characterized in that comprising step:
(1) hydrogen phosphide cumene is added in the basic soln, the mass ratio of hydrogen phosphide cumene and alkali is 1: 0.27～0.54;
(2) new decanoyl chloride is added drop-wise in the solution of step (1) gained, stirs while dripping, 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, restir reaction 30～50 minutes;
(4) stop to stir after reaction finishes and left standstill 20～40 minutes, 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, stirred 1 hour down for 0 ℃ in temperature; Obtain solvent-borne type peroxo-neodecanoic acid isopropyl benzene ester.
Basic soln in the said step (1) is aqueous sodium hydroxide solution or potassium hydroxide aqueous solution, and its massfraction is 25%～35%;
Temperature in the said step (2) is controlled at 10～30 ℃.
The stirring reaction time in the said step (3) is 40～45 minutes.
The resultant of reaction of the gained of step (4) described in the said step (5) and the mass ratio of alkane solvent are 1: 0.2～1: 0.25.
Solvent in the said step (5) is solvent oil or Permethyl 99A..
The invention has the beneficial effects as follows:
(1) solvent-borne type peroxo-neodecanoic acid isopropyl benzene ester (CNP)-75; In the superpolymer polyreaction, stable polymerization reaction, polymericular weight is even; Shorten reaction time; Constant product quality is active high, consumption is few, initiation is quick, the heat release uniform and stable, has avoided in the production process murder by poisoning to human body, and can produce the higher more stable superpolymer product of quality.
(2) preparation method of solvent-borne type peroxo-neodecanoic acid isopropyl benzene ester provided by the invention (CNP)-75; Simplified technical process, overcome complicated requirement, made under the environment that is reflected at gentleness, safety and carry out conversion unit; Quality product and yield increase substantially, and yield can reach more than 95%.It is identical with external like product that product quality level can reach.
Product quality indicator is seen table 1:
Table 1
| Project | Index |
| Outward appearance | Colourless transparent liquid does not have mechanical impurity |
| Colourity, Pt-Co<= | 30 |
| The active oxygen massfraction, % | 3.92±0.05 |
| The 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 done and to further describe.
Embodiment one
The preparation process of solvent-borne type peroxo-neodecanoic acid isopropyl benzene ester (CNP)-75 is following:
(1) in the 250ml flask, adding 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 32.4%;
(2) in the solution that step (1) makes, dripping purity is 87.5% hydrogen phosphide cumene 47.9 grams, reacts 30 minutes, and temperature is controlled at 25-35 ℃;
(3) stir that in flask, slowly to drip concentration be that 80% new decanoyl chloride-solvent oil mixing solution 55 restrains in the back, temperature of reaction is controlled at 20～30 ℃, and 2 hours times spent added, and adds behind the new decanoyl chloride solution stirring reaction 30 minutes;
(4) stop to stir after reaction finishes, left standstill 20 minutes, reaction mother liquor is separated, with resultant of reaction wash to the pH value be till 5;
(5) making content is 80% peroxo-neodecanoic acid isopropyl benzene ester (CNP), 84.8 grams, and yield is 95.9%;
(6) in the peroxo-neodecanoic acid isopropyl benzene ester (CNP) that makes, add 19.5 gram solvent oils, stirred 1 hour down in 0 ℃, obtain solvent-borne type peroxo-neodecanoic acid isopropyl benzene ester (CNP), content is about 75.1%.All other indexs all reach the product quality indicator requirement.
| Project | Index |
| Outward appearance | Colourless transparent liquid does not have mechanical impurity |
| Colourity, Pt-Co<= | 30 |
| The active oxygen massfraction, % | 3.92±0.05 |
| The 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-borne type peroxo-neodecanoic acid isopropyl benzene ester (CNP) is following:
(1) in the 250ml flask, adding 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 32.4%;
(2) in the solution that step (1) makes, dripping concentration is 87.5% hydrogen phosphide cumene 47.9 grams, reacts 30 minutes, and temperature is controlled at 20-30 ℃;
(3) stir that in flask, slowly to drip concentration be that 80% new decanoyl chloride-Permethyl 99A. mixing solutions 55 restrains in the back, temperature of reaction is controlled at 10 ℃～20 ℃, and 40 minutes times spent added, and adds behind the new decanoyl chloride solution stirring reaction 50 minutes;
(4) stop to stir after reaction finishes, left standstill 40 minutes, reaction mother liquor is separated, with resultant of reaction wash to the pH value be till 7;
(5) making content is 79.9% peroxo-neodecanoic acid isopropyl benzene ester (CNP), 84.9 grams, and yield is 96%;
(6) in the peroxo-neodecanoic acid isopropyl benzene ester (CNP) that makes, add 17.5 gram Permethyl 99A.s, in 0 ℃ of stirring 1 hour, obtain solvent-borne type peroxo-neodecanoic acid isopropyl benzene ester (CNP), concentration is about 75.9%.All other indexs all reach the product quality indicator requirement.
| Project | Index |
| Outward appearance | Colourless transparent liquid does not have mechanical impurity |
| Colourity, Pt-Co<= | 30 |
| The active oxygen massfraction, % | 3.92±0.05 |
| The 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 (6)
1. the method for making of solvent-borne type massfraction 75% a peroxo-neodecanoic acid isopropyl benzene ester is characterized in that, comprises step:
(1) hydrogen phosphide cumene is added in the basic soln, the mass ratio of hydrogen phosphide cumene and alkali is 1: 0.27～0.54;
(2) hot decanoyl chloride is added drop-wise in the solution of step (1) gained, stirs while dripping, hot 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, restir reaction 30～50 minutes;
(4) stop to stir after reaction finishes and left standstill 20～40 minutes, 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, stirred 1 hour down for 0 ℃ in temperature; Obtain solvent-borne type peroxo-neodecanoic acid isopropyl benzene ester.
2. according to the method for making of the said solvent-borne type massfraction 75% peroxo-neodecanoic acid isopropyl benzene ester of claim 1, it is characterized in that the basic soln in the said step (1) is aqueous sodium hydroxide solution or potassium hydroxide aqueous solution, its massfraction is 25%～35%;
3. according to the method for making of the said solvent-borne type massfraction 75% peroxo-neodecanoic acid isopropyl benzene ester of claim 1, it is characterized in that the temperature in the said step (2) is controlled at 10～30 ℃.
4. according to the method for making of the said solvent-borne type massfraction 75% peroxo-neodecanoic acid isopropyl benzene ester of claim 1, it is characterized in that the stirring reaction time in the said step (3) is 40～45 minutes.
5. according to the method for making of the said solvent-borne type massfraction 75% peroxo-neodecanoic acid isopropyl benzene ester of claim 1, it is characterized in that the resultant of reaction of the gained of step (4) described in the said step (5) and the mass ratio of alkane solvent are 1: 0.2～1: 0.25.
6. according to the method for making of the said solvent-borne type massfraction 75% peroxo-neodecanoic acid isopropyl benzene ester of claim 1, it is characterized in that the solvent in the said step (5) is solvent oil or Permethyl 99A..
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN114031753A (en) * | 2020-12-31 | 2022-02-11 | 广东聚华印刷显示技术有限公司 | Organic polymer and application thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN114031753A (en) * | 2020-12-31 | 2022-02-11 | 广东聚华印刷显示技术有限公司 | Organic polymer and application thereof |
| 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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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 |