CN102585048A - Preparation method of 70% mass fraction of solvent type cumyl peroxyneodecanoate - Google Patents
Preparation method of 70% mass fraction of solvent type cumyl peroxyneodecanoate Download PDFInfo
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- CN102585048A CN102585048A CN2011104417034A CN201110441703A CN102585048A CN 102585048 A CN102585048 A CN 102585048A CN 2011104417034 A CN2011104417034 A CN 2011104417034A CN 201110441703 A CN201110441703 A CN 201110441703A CN 102585048 A CN102585048 A CN 102585048A
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- neodecanoic acid
- acid isopropyl
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Abstract
The invention relates to a preparation method of 70% mass fraction of solvent type cumyl peroxyneodecanoate, belonging to the field of a preparation method of an initiator for synthesizing high polymers. The preparation method is characterized by comprising the following steps: adding cumyl hydroperoxide into alkaline solution; dropping neodecanoyl chloride into the obtained solution, stirring simultaneously when dropping; after the dropping of the neodecanoyl chloride, stirring again and reacting for 30-50min; after the reaction, stopping stirring, separating mother liquor, washing a reaction product until the pH value of the reaction product is 5-7; adding an alkane solvent into the reaction product, stirring for 30min at the temperature of 0 DEG C; and obtaining the solvent type cumyl peroxyneodecanoate. According to the preparation method provided by the invention, the process flow is simplified, the complicated requirements on a reaction device can be met, the reaction is conducted under the moderate and safe environment, the content and the yield of the product are improved greatly, and the yield is more than 95%. The quality of the product is the same as that of the abroad similar products.
Description
Technical field
The present invention relates to a kind of method for making of peroxo-neodecanoic acid isopropyl benzene ester of solvent-borne type massfraction 70%, 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)-70 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 peroxo-neodecanoic acid isopropyl benzene ester of solvent-borne type massfraction 70% 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 peroxo-neodecanoic acid isopropyl benzene ester of solvent-borne type massfraction 70% is provided, it is characterized in that following steps:
(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, 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 30 minutes 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: 0.25～1: 0.35.
Alkane solvent in the said step (5) is solvent oil or Permethyl 99A..
The invention has the beneficial effects as follows:
(1) the solvent-borne type peroxo-neodecanoic acid isopropyl benzene ester of preparing with method provided by the invention (CNP)-70; 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)-70; 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%.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, % | 70.0±1.0 |
| Chlorine (in Cl) massfraction, %<= | 0.05 |
| 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 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 25～30 ℃;
(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 50 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 7;
(5) making content is 80.5% peroxo-neodecanoic acid isopropyl benzene ester totally 85 grams, and yield is 96.7%;
(6) in the peroxo-neodecanoic acid isopropyl benzene ester that makes, add 31.4 gram solvent oils, in 0 ℃ of stirring 30 minutes, obtain solvent-borne type peroxo-neodecanoic acid isopropyl benzene ester, concentration is about 71%.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 | 28 |
| The active oxygen massfraction, % | 3.97 |
| The CNP massfraction, % | 70.8 |
| Chlorine (in Cl) massfraction, % | 0.04 |
| Free acid (in neodecanoic acid)Massfraction, % | 0.10 |
| Hydrogen base superoxide ( In CHP) massfraction, % | 0.09 |
Embodiment two
The preparation process of solvent-borne type peroxo-neodecanoic acid isopropyl benzene ester 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 10～20 ℃;
(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 20 ℃～30 ℃, adds at 40 minutes, adds behind the new decanoyl chloride solution stirring reaction 30 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 5;
(5) making content is 80.3% peroxo-neodecanoic acid isopropyl benzene ester totally 84 grams, and yield is 95.4%;
(6) in the peroxo-neodecanoic acid isopropyl benzene ester that makes, add 22.4 gram Permethyl 99A.s, in 0 ℃ of stirring 30 minutes, obtain solvent-borne type peroxo-neodecanoic acid isopropyl benzene ester, concentration is about 70%.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 | 29 |
| The active oxygen massfraction, % | 3.90 |
| The CNP massfraction, % | 70.0 |
| Chlorine (in Cl) massfraction, % | 0.05 |
| Free acid (in neodecanoic acid)Massfraction, % | 0.10 |
| Hydrogen base superoxide ( In CHP) massfraction, % | 0.08 |
Claims (6)
1. the method for making of the peroxo-neodecanoic acid isopropyl benzene ester of a solvent-borne type massfraction 70% is characterized in that following steps:
(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, 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 30 minutes for 0 ℃ in temperature; Obtain solvent-borne type peroxo-neodecanoic acid isopropyl benzene ester.
2. according to the method for making of the peroxo-neodecanoic acid isopropyl benzene ester of the said solvent-borne type massfraction 70% 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 peroxo-neodecanoic acid isopropyl benzene ester of the said solvent-borne type massfraction 70% 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 peroxo-neodecanoic acid isopropyl benzene ester of the said solvent-borne type massfraction 70% 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 peroxo-neodecanoic acid isopropyl benzene ester of the said solvent-borne type massfraction 70% 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: 0.25～1: 0.35.
6. according to the method for making of the peroxo-neodecanoic acid isopropyl benzene ester of the said solvent-borne type massfraction 70% of claim 1, it is characterized in that the alkane solvent in the said step (5) is solvent oil or Permethyl 99A..
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Cited By (5)
| 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 |
| CN105693584A (en) * | 2016-03-17 | 2016-06-22 | 乌鲁木齐市华泰隆化学助剂有限公司 | Peroxided neodecanoic acid isopropyl phenyl ester and method for preparing peroxided neodecanoic acid isopropyl phenyl ester through phase transfer catalyst |
| CN107827801A (en) * | 2017-11-16 | 2018-03-23 | 展红明 | The preparation method of the type tert-butyl peroxyneo-caprate of solvent-borne type mass fraction 75% |
| 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 |
-
2011
- 2011-12-26 CN CN2011104417034A patent/CN102585048A/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 (5)
| 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 |
| CN105693584A (en) * | 2016-03-17 | 2016-06-22 | 乌鲁木齐市华泰隆化学助剂有限公司 | Peroxided neodecanoic acid isopropyl phenyl ester and method for preparing peroxided neodecanoic acid isopropyl phenyl ester through phase transfer catalyst |
| CN107827801A (en) * | 2017-11-16 | 2018-03-23 | 展红明 | The preparation method of the type tert-butyl peroxyneo-caprate of solvent-borne type mass fraction 75% |
| 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: 20120718 |