CN102585049B - Preparation method of emulsion type di-(2-ethylhexyl) peroxydicarbonate with mass fraction of 50 percent - Google Patents
Preparation method of emulsion type di-(2-ethylhexyl) peroxydicarbonate with mass fraction of 50 percent Download PDFInfo
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- CN102585049B CN102585049B CN201110442115.2A CN201110442115A CN102585049B CN 102585049 B CN102585049 B CN 102585049B CN 201110442115 A CN201110442115 A CN 201110442115A CN 102585049 B CN102585049 B CN 102585049B
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- ethylhexyl
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Abstract
The invention relates to a preparation method of emulsion type di-(2-ethylhexyl) peroxydicarbonate with a mass fraction of 50 percent. The preparation method is characterized in that the preparation method comprises the steps as follows: an alkaline liquor is mixed with an oxidant to react therewith; chloroformic acid 2-ethylhexyl is dripped into an obtained liquor; after the chloroformic acid 2-ethylhexyl is completely dripped, the obtained liquor is stirred; after the chloroformic acid 2-ethylhexyl reacts with the obtained liquor, the mother liquor is separated; deionized water, antifreeze, an emulsifier and a dispersant are evenly mixed, so as to obtain an aqueous phase liquor; an obtained reaction product is mixed with the obtained aqueous phase liquor; and after the temperature is reduced, the emulsion type di-(2-ethylhexyl) peroxydicarbonate is obtained. The prepared emulsion type di-(2-ethylhexyl) peroxydicarbonate overcomes the defects of a solvent type initiator that the energy consumption is high, the environmental protection is unavailable, and human bodies are easy to be injured in the production process, and simultaneously has the advantages of smooth polymerization reaction, stable product quality, little use amount, rapid initiation, even heat release, and the like of the solvent type initiator in a high polymer polymerization reaction.
Description
Technical field
The present invention relates to the method for making of a kind of emulsion-type massfraction 50% peroxy dicarbonate two (2-ethylhexyl), belong to the synthetic preparation method field with initiator of superpolymer.
Background technology
Along with the fast development of the synthetic industry of domestic superpolymer, superpolymer is synthetic to be promoted rapidly by kind and the demand of initiator.Emulsion-type peroxy dicarbonate two (2-ethylhexyl), synthesize and use efficient initiator as a kind of superpolymer, with solvent-borne type initiator initiator, compare, in the polymerization process of superpolymer, had the solvent-borne type initiator amount concurrently few, efficiency of initiation is high, the polyreaction heat release is even, be convenient to the advantage of controlling, after particularly water is cooked solvent, realize environmental protection, and effectively avoided the harm of flammable solvent to human body in production process, the products obtained therefrom excellent property is a kind of safety, environmental protection, the synthetic initiator of using of superpolymer 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 of a kind of emulsion-type massfraction 50% peroxy dicarbonate two (2-ethylhexyls) is provided, and 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 of a kind of emulsion-type massfraction 50% peroxy dicarbonate two (2-ethylhexyl) is provided, it is characterized in that following steps:
(1), by basic solution and oxygenant hybrid reaction, make the aqueous solution of superoxide;
(2) chloroformic acid 2-(ethyl hexyl) ester is added drop-wise in the solution of step (1) gained, stir on dropping limit, limit, temperature is controlled at 10～30 ℃, 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, then stirring reaction 60～90 minutes;
(4) reaction stops after finishing stirring, and standing 20～40 minutes, mother liquor is separated, resultant of reaction is washed till to pH value 5～7;
(5) by deionized water, frostproofer, emulsifying agent, dispersion agent in mass ratio 1: (0.26～0.47): (0.021～0.047): (0.021～0.047) mixes, and makes aqueous phase solution;
(6) resultant of reaction (oil phase) of step (4) gained is mixed with step (5) gained aqueous phase solution, both mass ratioes are 1: (0.9～1), stir under 0 ℃ that within 3～3.5 hours, to carry out emulsification synthetic;
(7) cooling obtains emulsion-type peroxy dicarbonate two (2-ethylhexyl) after-10 ℃～-15 ℃, and concentration is 49%～51%.
Basic solution in described step (1) is aqueous sodium hydroxide solution or potassium hydroxide aqueous solution, and its mass percent is 10%～20%;
Oxygenant in described step (1) is hydrogen peroxide, and the mass ratio of hydrogen peroxide and alkali is 1: 2.0～4.0.
Temperature in described step (2) is controlled at 20～30 ℃.
The stirring reaction time in described step (3) is 75～85 minutes.
Frostproofer in described step (5) is ethanol.
Emulsifying agent in described step (5) is milky white spirit.
Dispersion agent in described step (5) is polyvinyl alcohol.
The invention has the beneficial effects as follows: the emulsion-type peroxy dicarbonate of preparing two (2-ethylhexyl), overcome high, the not environmental protection, inflammable dangerous of solvent-borne type initiator power consumption, and easily cause shortcomings such as harms in process of production, in the superpolymer polyreaction, had solvent-borne type initiator stable polymerization reaction concurrently, the advantages such as constant product quality, consumption is few, initiation is quick, heat release is even, and environmental protection, avoided in the production process harm to human body.In addition, the method for preparing emulsion-type peroxy dicarbonate two (2-ethylhexyl) provided by the invention, simplified technical process, overcome the complicated requirement to conversion unit, reaction is carried out under gentle, safe environment, product content and yield increase substantially, and yield can reach more than 95%.Product stock, the convenient transportation of preparation, can be applicable to suitability for industrialized production in a large number.It is identical with same kind of products at abroad that product quality level can reach.
Product quality indicator is in Table 1:
Table 1
| Project | Index |
| Outward appearance | White emulsion |
| The active oxygen massfraction, % | 2.31±0.05 |
| The EHP massfraction, % | 50.0±1.0 |
| Chlorine (in Cl) massfraction, %≤ | 0.05 |
Embodiment
Below in conjunction with embodiment, the present invention is described further.
Embodiment mono-
The preparation process of emulsion-type peroxy dicarbonate two (2-ethylhexyl) is as follows:
(1) in the 500ml flask, add sodium hydroxide solution 100 grams that concentration is 25%, water 100 grams, stir and be cooled to 10 ℃;
(2) drip hydrogen peroxide 38 grams that content is 27.5% in the solution made to step (1), stirring reaction is made sodium peroxide solution;
(3) stir in backward flask and slowly drip chloroformic acid 2-(ethyl hexyl) ester 75 grams that concentration is 98%, temperature of reaction is controlled at 20～30 ℃, and 1.5 hours used times added, and adds after chloroformic acid 2-(ethyl hexyl) ester stirring reaction 30 minutes;
(4) reaction stops after finishing stirring, standing 20 minutes, reaction mother liquor is separated, by resultant of reaction wash to pH value be till 6, the peroxy dicarbonate pair (2-ethylhexyl) that makes content 98% totally 66.4 grams, yield is 98.5%;
(5) by deionized water, ethanol, milky white spirit, polyvinyl alcohol 1: 0.47: 0.047 in mass ratio: 0.021 mixes, and makes aqueous phase solution 65 grams;
(6) be the mass mixing of 1: 0.96 in mass ratio by the resultant of reaction of the aqueous phase solution of step (5) gained and step (4) gained, stir under 0 ℃ that within 3 hours, to carry out emulsification synthetic;
(7) obtain emulsion-type peroxy dicarbonate two (2-ethylhexyl) totally 130.1 grams after being cooled to-15 ℃, concentration is about 50%.All other indexs all reach the product quality indicator requirement.
| Project | Index |
| Outward appearance | White emulsion |
| The active oxygen massfraction, % | 2.33 |
| The EHP massfraction, % | 50.0 |
| Chlorine (in Cl) massfraction, % | 0.04 |
Embodiment bis-
The preparation process of emulsion-type peroxy dicarbonate two (2-ethylhexyl) is as follows:
(1) in the 500ml flask, add sodium hydroxide solution 100 grams that concentration is 25%, water 100 grams, stir and be cooled to 10 ℃;
(2) drip hydrogen peroxide 38 grams that content is 27.5%, stirring reaction is made sodium peroxide solution;
(3) stir in backward flask and slowly drip 98% chloroformic acid 2-(ethyl hexyl) ester 75 grams, temperature of reaction is controlled at 20～30 ℃, and 2 hours used times added, and adds after chloroformic acid 2-(ethyl hexyl) ester stirring reaction 30 minutes;
(4) reaction stops after finishing stirring, standing 40 minutes, reaction mother liquor is separated, by resultant of reaction wash to pH value be till 7, the peroxy dicarbonate pair (2-ethylhexyl) that makes content 98.7% totally 66.1 grams, yield is 98.8%;
(5) by deionized water, ethanol, milky white spirit, polyvinyl alcohol 1: 0.26: 0.021 in mass ratio: 0.047 mixes, and makes aqueous phase solution 65 grams;
(6) be the mass mixing of 1: 0.94 in mass ratio by the resultant of reaction of the aqueous phase solution of step (5) gained and step (4) gained, stir under 0 ℃ that within 3.5 hours, to carry out emulsification synthetic;
(7) obtain emulsion-type peroxy dicarbonate two (2-ethylhexyl) totally 127.9 grams after being cooled to-10 ℃, concentration is about 51%.All other indexs all reach the product quality indicator requirement.
| Project | Index |
| Outward appearance | White emulsion |
| The active oxygen massfraction, % | 2.30 |
| The EHP massfraction, % | 50.5 |
| Chlorine (in Cl) massfraction, % | 0.05 |
Claims (6)
1. the method for making of emulsion-type massfraction 50% peroxy dicarbonate two (2-ethylhexyl) is characterized in that following steps:
(1), by basic solution and oxygenant hybrid reaction, make the aqueous solution of superoxide;
(2) chloroformic acid 2-(ethyl hexyl) ester is added drop-wise in the solution of step (1) gained, stir on dropping limit, limit, temperature is controlled at 10～30 ℃, 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, then stirring reaction 60～90 minutes;
(4) reaction stops after finishing stirring, and standing 20～40 minutes, mother liquor is separated, resultant of reaction is washed till to pH value 5～7;
(5) by deionized water, frostproofer, emulsifying agent, dispersion agent 1:(0.26～0.47 in mass ratio): (0.021～0.047): (0.021～0.047) mixes, and makes aqueous phase solution;
(6) resultant of reaction of step (4) gained is mixed with the aqueous phase solution of step (5) gained, both mass ratioes are 1:(0.9～1), stir under 0 ℃ that within 3～3.5 hours, to carry out emulsification synthetic;
(7) obtain emulsion-type peroxy dicarbonate two (2-ethylhexyl) after being cooled to-10 ℃～-15 ℃, concentration is 49%～51%.
Basic solution in described step (1) is aqueous sodium hydroxide solution or potassium hydroxide aqueous solution, and its mass percent is 10%～20%;
Oxygenant in described step (1) is hydrogen peroxide, and the mass ratio of hydrogen peroxide and alkali is 1:2.0～4.0.
2. the method for making of emulsion-type massfraction 50% peroxy dicarbonate two (2-ethylhexyls) according to claim 1, is characterized in that, the temperature in described step (2) is controlled at 20～30 ℃.
3. the method for making of emulsion-type massfraction 50% peroxy dicarbonate two (2-ethylhexyls) according to claim 1, is characterized in that, the stirring reaction time in described step (3) is 75～85 minutes.
4. the method for making of emulsion-type massfraction 50% peroxy dicarbonate two (2-ethylhexyls) according to claim 1, is characterized in that, the frostproofer in described step (5) is ethanol.
5. the method for making of emulsion-type massfraction 50% peroxy dicarbonate two (2-ethylhexyls) according to claim 1, is characterized in that, the emulsion in described step (5) is milky white spirit.
6. the method for making of emulsion-type massfraction 50% peroxy dicarbonate two (2-ethylhexyls) according to claim 1, is characterized in that, the dispersion agent in described step (5) is polyvinyl alcohol.
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