CN102442932A - Preparation method of solvent type bis-(2-ethoxy)ethyl peroxydicarbonate (EEP) - Google Patents
Preparation method of solvent type bis-(2-ethoxy)ethyl peroxydicarbonate (EEP) Download PDFInfo
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- CN102442932A CN102442932A CN2010105004284A CN201010500428A CN102442932A CN 102442932 A CN102442932 A CN 102442932A CN 2010105004284 A CN2010105004284 A CN 2010105004284A CN 201010500428 A CN201010500428 A CN 201010500428A CN 102442932 A CN102442932 A CN 102442932A
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Abstract
The invention relates to an initiator for the synthesis of a high polymer, and specifically relates to a preparation method of solvent type bis-(2-ethoxy)ethyl peroxydicarbonate (EEP). The technical scheme comprises the following steps: mixing 2-ethoxyethyl chloroformate and an alkaline solution for reaction at 15-30 DEG C; washing the reaction product until the pH value is 5-7; pouring into a kettle at 5 DEG C; carrying out deep freezing at -18 DEG C for 11-12 hours; and adding a right amount of solvent to obtain the solvent type EEP. The preparation method of solvent type EEP simplifies the process flow, overcomes the complex requirements for reaction equipment, enables the reaction to be carried out in a moderate and safe environment, greatly improves the content and yield of the product and ensures that the yield can be up to 95% or above.
Description
Technical field
The present invention relates to the synthetic initiator of using of a kind of superpolymer, the preparation method of two (2-oxyethyl group) ethyl esters (EEP) of particularly a kind of solvent-borne type peroxy dicarbonate.
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.
Two (2-oxyethyl group) ethyl esters (EEP) of peroxy dicarbonate are used efficient initiator as a kind of superpolymer is synthetic, compare with common azo-initiator; In the superpolymer polymerization process, 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 two (2-oxyethyl group) ethyl esters (EEP) of peroxy dicarbonate of industrial applications.
Technical scheme of the present invention is: 1, the preparation method of two (2-oxyethyl group) ethyl esters (EEP) of a kind of solvent-borne type peroxy dicarbonate, and comprise step: (1) is with being cooled to 5～15 ℃ in the basic soln suction reaction kettle; (2) with in the slow dropwise reaction still of carbonochloridic acid 2-ethoxy ethyl ester, stir while dripping, temperature is controlled at 15～30 ℃, in 1.2～2 hours, adds; (3) stop to stir after reaction finishes, leave standstill, mother liquor is separated, resultant of reaction is washed till pH value 5～7 till; (4) falling behind the still dark freezing 11～12 hours under temperature-18 ℃ condition under 5 ℃ of conditions of temperature; (5) in the batching still, add solvent in the resultant of reaction with step (4) gained, under 0 ℃ of condition of temperature, stir; (6) obtain two (2-oxyethyl group) ethyl esters (EEP) of solvent-borne type peroxy dicarbonate.
In the said step (1) with being cooled to 10～12 ℃ in the basic soln suction reaction kettle.
Said step (1) neutral and alkali solution is that concentration is 10%～20% sodium hydroxide solution or potassium hydroxide solution.
Concentration is that the mass ratio of the carbonochloridic acid 2-ethoxy ethyl ester of 10%～20% basic soln and adding is 1.5: 1～2: 1 in the said step (2).
Solvent is a toluene in the said step (5).
Beneficial effect of the present invention is: two (2-oxyethyl group) ethyl esters (EEP) of the peroxy dicarbonate of preparing with method provided by the invention; Overcome the shortcoming that the azo-initiator activity is low, toxicity is big; 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.In addition; The preparation method of two (2-oxyethyl group) ethyl esters (EEP) of solvent-borne type peroxy dicarbonate provided by the invention; 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%.
Embodiment
Embodiment one: the preparation process of two (2-oxyethyl group) ethyl esters (EEP) of solvent-borne type peroxy dicarbonate is following:
(1) in the 500ml flask, adding concentration is 20% sodium hydroxide solution 100 grams, and water 100 grams stir and are cooled to 10 ℃, process alkaline solution of sodium hydroxide, and concentration is about 10%;
(2) in the solution that step (1) makes, slowly dripping purity is 97% carbonochloridic acid 2-ethoxy ethyl ester 55 grams, and temperature of reaction is controlled at 20 ℃～30 ℃, adds in 1 hour to 1.5 hours, adds the back stirring reaction 10 minutes;
(3) 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;
(4) falling behind the still dark freezing 11～12 hours under temperature-18 ℃ condition under 5 ℃ of conditions of temperature;
(5) in the batching still, add toluene 28 grams in the resultant of reaction of step (4) gained, under 0 ℃ of condition of temperature, stir.
(6) obtaining concentration is two (2-oxyethyl group) ethyl esters (EEP) 80 grams of 78% solvent-borne type peroxy dicarbonate, yield 95%.
Embodiment two: the preparation process of two (2-oxyethyl group) ethyl esters (EEP) of solvent-borne type peroxy dicarbonate is following:
(1) in the 500ml flask, adding concentration is 20% sodium hydroxide solution 100 grams, and water 40 grams stir and are cooled to 10 ℃, process alkaline solution of sodium hydroxide, and concentration is about 14.3%;
(2) in the solution that step (1) makes, slowly dripping purity is 97% carbonochloridic acid 2-ethoxy ethyl ester 55 grams, and temperature of reaction is controlled at 20 ℃～30 ℃, adds in 1 hour to 1.5 hours, adds the back stirring reaction 10 minutes;
(3) 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;
(4) falling behind the still dark freezing 11～12 hours under temperature-18 ℃ condition under 5 ℃ of conditions of temperature;
(5) in the batching still, add toluene 28 grams in the resultant of reaction of step (4) gained, under 0 ℃ of condition of temperature, stir.
(6) obtaining concentration is two (2-oxyethyl group) ethyl esters (EEP) 78 grams of 73% solvent-borne type peroxy dicarbonate, yield 92%.
Claims (5)
1. the preparation method of two (2-oxyethyl group) ethyl esters (EEP) of solvent-borne type peroxy dicarbonate is characterized in that, comprises step:
(1) with being cooled to 5～15 ℃ in the basic soln suction reaction kettle;
(2) with in the slow dropwise reaction still of carbonochloridic acid 2-ethoxy ethyl ester, stir while dripping, temperature is controlled at 15～30 ℃, in 1.2～2 hours, adds;
(3) stop to stir after reaction finishes, leave standstill, mother liquor is separated, resultant of reaction is washed till pH value 5～7 till;
(4) falling behind the still dark freezing 11～12 hours under temperature-18 ℃ condition under 5 ℃ of conditions of temperature;
(5) in the batching still, add solvent in the resultant of reaction with step (4) gained, under 0 ℃ of condition of temperature, stir;
(6) obtain two (2-oxyethyl group) ethyl esters (EEP) of solvent-borne type peroxy dicarbonate.
2. according to the preparation method of two (2-oxyethyl group) ethyl esters (EEP) of the said solvent-borne type peroxy dicarbonate of claim 1, it is characterized in that, in the said step (1) with being cooled to 10～12 ℃ in the basic soln suction reaction kettle.
3. according to the preparation method of two (2-oxyethyl group) ethyl esters (EEP) of the said solvent-borne type peroxy dicarbonate of claim 1, it is characterized in that said step (1) neutral and alkali solution is that concentration is 10%～20% sodium hydroxide solution or potassium hydroxide solution.
4. according to the preparation method of two (2-oxyethyl group) ethyl esters (EEP) of the said solvent-borne type peroxy dicarbonate of claim 3; It is characterized in that concentration is that the mass ratio of the carbonochloridic acid 2-ethoxy ethyl ester of 10%～20% basic soln and adding is 1.5: 1～2: 1 in the said step (2).
5. according to the preparation method of two (2-oxyethyl group) ethyl esters (EEP) of the said solvent-borne type peroxy dicarbonate of claim 1, it is characterized in that solvent is a toluene in the said step (5).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010105004284A CN102442932A (en) | 2010-10-08 | 2010-10-08 | Preparation method of solvent type bis-(2-ethoxy)ethyl peroxydicarbonate (EEP) |
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| Application Number | Priority Date | Filing Date | Title |
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| CN2010105004284A CN102442932A (en) | 2010-10-08 | 2010-10-08 | Preparation method of solvent type bis-(2-ethoxy)ethyl peroxydicarbonate (EEP) |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| US20040249097A1 (en) * | 1999-11-04 | 2004-12-09 | Cozens Ross J. | Method for producing organic peroxides and their use in the radical polymerization of monomers |
| AU2005202336A1 (en) * | 2005-05-30 | 2006-12-14 | Oxy Vinyls Lp | Method for producing organic peroxides and their use in the radical polymerization of monomers |
-
2010
- 2010-10-08 CN CN2010105004284A patent/CN102442932A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| US20040249097A1 (en) * | 1999-11-04 | 2004-12-09 | Cozens Ross J. | Method for producing organic peroxides and their use in the radical polymerization of monomers |
| AU2005202336A1 (en) * | 2005-05-30 | 2006-12-14 | Oxy Vinyls Lp | Method for producing organic peroxides and their use in the radical polymerization of monomers |
Non-Patent Citations (2)
| Title |
|---|
| "过氧化二碳酸二苯氧乙基酯合成的研究", 《聚氯乙烯》 * |
| 李焕生: "在分散体系中合成引发剂过氧化二碳酸二(2-苯氧乙基)酯", 《塑料工业》 * |
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Application publication date: 20120509 |