CN102659960A - Preparation method of solvent-type di-(2-ethylhexyl)peroxydicarbonate with mass fraction of 60% - Google Patents
Preparation method of solvent-type di-(2-ethylhexyl)peroxydicarbonate with mass fraction of 60% Download PDFInfo
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- CN102659960A CN102659960A CN201110442093XA CN201110442093A CN102659960A CN 102659960 A CN102659960 A CN 102659960A CN 201110442093X A CN201110442093X A CN 201110442093XA CN 201110442093 A CN201110442093 A CN 201110442093A CN 102659960 A CN102659960 A CN 102659960A
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Abstract
The invention relates to a preparation method of solvent-type di-(2-ethylhexyl)peroxydicarbonate with mass fraction of 60%, and belongs to the preparation method field of initiator used in synthesis of high polymer. The preparation method is characterized by: adding hydrogen peroxide into an alkaline solution; dropping 2-etylhexyl-chlorformiat into the obtained solution with stirring; carrying out a stirring reaction for 30-50 minutes after finishing dropping 2-etylhexyl-chlorformiat; stopping stirring after the reaction, separating mother liquor, washing reaction products till pH value ranges between 5-7; adding an alkane solvent into the obtained reaction products; and producing solvent-type di-(2-ethylhexyl)peroxydicarbonate. The prepared solvent-type di-(2-ethylhexyl)peroxydicarbonate is easily dispersible in a polymerization system and releases uniform heat in a polymerization reaction, has a high initiating efficiency and is easy to control, and assists in producing products of stable and decent performances. The prepared solvent-type di-(2-ethylhexyl)peroxydicarbonate is an initiator used in synthesis of high polymer, which is safe, highly efficient and has stable product quality, and can assist in producing high polymer products with better quality and stability.
Description
Technical field
The present invention relates to the method for making of a kind of solvent-borne type massfraction 60% peroxy dicarbonate two (2-ethylhexyl) ester, belong to the synthetic preparation method field of superpolymer with 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 peroxy dicarbonate two (2-ethylhexyl) ester (EHP)-60 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: the method for making of a kind of solvent-borne type massfraction 60% peroxy dicarbonate two (2-ethylhexyl) 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: the method for making of a kind of solvent-borne type massfraction 60% peroxy dicarbonate two (2-ethylhexyl) ester is provided, it is characterized in that following steps:
(1) hydrogen peroxide is added in the basic soln, the mass ratio of hydrogen peroxide and alkali is 1: 2.0～4.0;
(2) chloroformic acid 2-(ethyl hexyl) ester is added drop-wise in the solution of step (1) gained; Stir while dripping; Temperature is controlled at 20～30 ℃; Chloroformic acid 2-(ethyl hexyl) ester added in 2 hours at 40 minutes, and the mass ratio of the solution of chloroformic acid 2-(ethyl hexyl) ester and step (1) gained is 1: 1.3～4.0;
(3) after chloroformic acid 2-(ethyl hexyl) ester 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 1～3.5 hour down for 0 ℃ in temperature; Obtain solvent-borne type peroxy dicarbonate two (2-ethylhexyl) ester.
Basic soln in the said step (1) is aqueous sodium hydroxide solution or potassium hydroxide aqueous solution, and its mass percent is 10%～20%;
Temperature in the said step (2) is controlled at 20～30 ℃.
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: 0.5～1: 0.7.
Solvent in the said step (5) is solvent oil or Permethyl 99A..
The invention has the beneficial effects as follows:
(1) in polymerization system, be prone to disperse and in polyreaction heat release even; Efficiency of initiation is high, is convenient to control, products obtained therefrom stable performance, good; Being that a kind of superpolymer safe, efficient, constant product quality is synthetic uses initiator, and can produce the higher more stable superpolymer product of quality.
(2) preparation method of solvent-borne type peroxy dicarbonate two provided by the invention (2-ethylhexyl) ester; 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<= | 20 |
| The active oxygen massfraction, % | 2.77±0.05 |
| The EHP massfraction, % | 60.0±1.0 |
| Chlorine (in Cl) massfraction, %<= | 0.05 |
Embodiment
Below in conjunction with embodiment the present invention is done and to further describe.
Embodiment one
The preparation process of solvent-borne type peroxy dicarbonate two (2-ethylhexyl) ester is following:
(1) in the 500ml flask, adding content is 25% sodium hydroxide solution 100 grams, and water 100 grams stir and are cooled to 5 ℃;
(2) in the solution that step (1) makes, dripping purity is 27.5% hydrogen peroxide 38 grams, reacts 30 minutes, and temperature is controlled at 25 ℃;
(3) stir that in flask, slowly to drip concentration be 98% chloroformic acid 2-ethylhexyl ester solution, 75 grams in the back, temperature of reaction is controlled at 20～30 ℃, and 1.5 hours times spent added, and adds behind the chloroformic acid 2-ethylhexyl ester 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 5;
(5) making content is 98.87% peroxy dicarbonate two (2-ethylhexyl) ester, 65.8 grams, and yield is 98.5%;
(6) in the peroxy dicarbonate that makes two (2-ethylhexyl) ester, add 40.8 gram solvent oils, in 0 ℃ of stirring 3 hours, obtain solvent-borne type peroxy dicarbonate two (2-ethylhexyl) ester, concentration is about 61%.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 | 18 |
| The active oxygen massfraction, % | 2.74 |
| The EHP massfraction, % | 60.5 |
| Chlorine (in Cl) massfraction, % | 0.04 |
Embodiment two
The preparation process of solvent-borne type peroxy dicarbonate two (2-ethylhexyl) ester is following:
(1) in the 500ml flask, adding content is 25% Pottasium Hydroxide 100 grams, and water 100 grams stir and are cooled to 5 ℃;
(2) in the solution that step (1) makes, dripping concentration is 27.5% hydrogen peroxide 38 grams, reacts 30 minutes, and temperature is controlled at 25 ℃;
(3) stir that in flask, slowly to drip concentration be 98% chloroformic acid 2-ethylhexyl ester solution, 75 grams in the back, temperature of reaction is controlled at 20～30 ℃, and 2 hours times spent added, and adds behind the chloroformic acid 2-ethylhexyl ester 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 7;
(5) making content is 98.2% peroxy dicarbonate two (2-ethylhexyl) ester (EHP), 65.9 grams, and yield is 98%;
(6) in the peroxy dicarbonate that makes two (2-ethylhexyl) ester (EHP), add 38.6 gram Permethyl 99A.s, in 0 ℃ of stirring 3.5 hours, obtain solvent-borne type peroxy dicarbonate two (2-ethylhexyl) ester, concentration is about 61.93%.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 | 19 |
| The active oxygen massfraction, % | 2.80 |
| The EHP massfraction, % | 69.5 |
| Chlorine (in Cl) massfraction, % | 0.05 |
Claims (6)
1. the method for making of solvent-borne type massfraction 60% peroxy dicarbonate two (2-ethylhexyl) ester is characterized in that following steps:
(1) hydrogen peroxide is added in the basic soln, the mass ratio of hydrogen peroxide and alkali is 1: 2.0～4.0;
(2) chloroformic acid 2-(ethyl hexyl) ester is added drop-wise in the solution of step (1) gained; Stir while dripping; Temperature is controlled at 20～30 ℃; Chloroformic acid 2-(ethyl hexyl) ester added in 2 hours at 40 minutes, and the mass ratio of the solution of chloroformic acid 2-(ethyl hexyl) ester and step (1) gained is 1: 1.3～4.0;
(3) after chloroformic acid 2-(ethyl hexyl) ester 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 3～3.5 hours down for 0 ℃ in temperature; Obtain solvent-borne type peroxy dicarbonate two (2-ethylhexyl) ester.
2. according to the method for making of said solvent-borne type massfraction 60% peroxy dicarbonate two of claim 1 (2-ethylhexyl) ester; It is characterized in that the basic soln in the said step (1) is aqueous sodium hydroxide solution or potassium hydroxide aqueous solution, its mass percent is 10%～20%;
3. according to the method for making of said solvent-borne type massfraction 60% peroxy dicarbonate two of claim 1 (2-ethylhexyl) ester, it is characterized in that the temperature in the said step (2) is controlled at 20～30 ℃.
4. according to the method for making of said solvent-borne type massfraction 60% peroxy dicarbonate two of claim 1 (2-ethylhexyl) ester, 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 claim 1 a solvent-borne type massfraction 60% peroxy dicarbonate two (2-ethylhexyl) ester, 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: 0.5～1: 0.7.
6. according to the method for making of said solvent-borne type massfraction 60% peroxy dicarbonate two of claim 1 (2-ethylhexyl) ester, 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 (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104370789A (en) * | 2014-11-26 | 2015-02-25 | 淄博正华助剂股份有限公司 | Method for preparing peroxidized dicarbonate (2-ethylhexyl) ester (EHP) by continuous flow |
| CN109180549A (en) * | 2018-09-12 | 2019-01-11 | 蓝凤祥 | A kind of Safe production technology of dicetyl peroxydicarbonate ethylhexyl initiator |
| CN111548295A (en) * | 2020-04-02 | 2020-08-18 | 鄂尔多斯市瀚博科技有限公司 | Preparation method of di (2-ethylhexyl) peroxydicarbonate |
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| US2464062A (en) * | 1947-11-26 | 1949-03-08 | Pittsburgh Plate Glass Co | Polymerization with a peroxydicar-bonate catalyst |
| GB2024224A (en) * | 1978-06-30 | 1980-01-09 | Ppg Industries Inc | Production of peroxydicarbonates |
| CN1387511A (en) * | 1999-11-04 | 2002-12-25 | 氧化乙烯公司 | Method for producing peroxydicarbonates and their use in radical polymerization of monomers |
| 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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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US2464062A (en) * | 1947-11-26 | 1949-03-08 | Pittsburgh Plate Glass Co | Polymerization with a peroxydicar-bonate catalyst |
| GB2024224A (en) * | 1978-06-30 | 1980-01-09 | Ppg Industries Inc | Production of peroxydicarbonates |
| CN1387511A (en) * | 1999-11-04 | 2002-12-25 | 氧化乙烯公司 | Method for producing peroxydicarbonates and their use in radical polymerization of monomers |
| 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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| 吕海金: "过氧化二碳酸(2-乙基)己酯的合成研究", 《青岛职业技术学院学报》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104370789A (en) * | 2014-11-26 | 2015-02-25 | 淄博正华助剂股份有限公司 | Method for preparing peroxidized dicarbonate (2-ethylhexyl) ester (EHP) by continuous flow |
| CN109180549A (en) * | 2018-09-12 | 2019-01-11 | 蓝凤祥 | A kind of Safe production technology of dicetyl peroxydicarbonate ethylhexyl initiator |
| CN111548295A (en) * | 2020-04-02 | 2020-08-18 | 鄂尔多斯市瀚博科技有限公司 | Preparation method of di (2-ethylhexyl) peroxydicarbonate |
| CN111548295B (en) * | 2020-04-02 | 2022-03-01 | 鄂尔多斯市瀚博科技有限公司 | Preparation method of di (2-ethylhexyl) peroxydicarbonate |
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Denomination of invention: Preparation of 60% solvent based bis (2-ethylhexyl) peroxydicarbonate Effective date of registration: 20230511 Granted publication date: 20140820 Pledgee: Zibo Linzi District sub branch of China Post Savings Bank Co.,Ltd. Pledgor: ZIBO ZHENGHUA AUXILIARY Co.,Ltd. Registration number: Y2023980040339 |