CN102827051A - Method for synthesizing dicumyl peroxide - Google Patents
Method for synthesizing dicumyl peroxide Download PDFInfo
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- CN102827051A CN102827051A CN2012103567306A CN201210356730A CN102827051A CN 102827051 A CN102827051 A CN 102827051A CN 2012103567306 A CN2012103567306 A CN 2012103567306A CN 201210356730 A CN201210356730 A CN 201210356730A CN 102827051 A CN102827051 A CN 102827051A
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Abstract
The invention discloses a method for synthesizing dicumyl peroxide. The method comprises the steps of: firstly, measuring certain refined benzyl alcohol and certain oxidant solution in a measuring tank; then, stirring after a reaction kettle is opened, putting the measured refined benzyl alcohol into the reaction kettle via a vacuum system on the reaction kettle and adding a cocatalyst when the benzyl alcohol is added till 1/3 volume of the reaction kettle; after the refined benzyl alcohol is added completely, feeding all measured oxidant solution into the reaction kettle via the vacuum system on the reaction kettle; after feeding, starting a bottom bubble valve of the reaction kettle and adjusting the pressure at the bottom of the kettle to be at about -0.04MPa; and finally, controlling the temperature of the synthetic reaction to be at 43-45 DEG C via an adjusting valve of a hot water (less than or equal to 60 DEG C) reaction kettle jacket and an adjusting valve of a circulating water reaction kettle coil, wherein the reaction time is controlled within 5-6.5 hours per kettle; and byproducts of the reaction, such as phenol and acetone and the like after the reaction and are removed by fully stirring and mixing the reaction solution and alkali liquor (about 10wt% of sodium hydroxide solution) in a cleaning kettle based on a mass ratio of 1: 0.1.
Description
Technical field
The present invention relates to the working method of Di Cumyl Peroxide 99, relate in particular to a kind of compound method of Di Cumyl Peroxide 99.
Background technology
In existing Di Cumyl Peroxide 99 was synthetic, oxidation liquid and smart benzylalcohol added the heating of thermal recovery LP steam chuck at the synthesis reactor internal reaction, and reaction cooled adopts direct river cooling, and the temperature of reaction fluctuation is bigger, and general temperature controlling range is at 40～50 ℃.With this understanding, the by product that generates in the reaction process is more, and is up to about 20%, very big to isopropyl benzene consumption influence like content of by-products such as phenol, acetone.Make device running cost high.Influenced Enterprises'Competitiveness.Moreover reaction will be controlled at temperature between 40～50 ℃ direct river cooling that will be a large amount of.The energy consumption of device is very big, is unfavorable for cleaner production.Also have the original reactor vacuum system to be given by W type reciprocating vacuum pump, noise was bigger when this vacuum pump moved, and failure rate is higher in the operational process, and maintenance cost is high, and current consumption is big, reaches 110KW/H.
Summary of the invention
The object of the invention is: for overcoming above-mentioned deficiency, provide a kind of side reaction less, influence the compound method of a kind of Di Cumyl Peroxide 99 of device unit consumption, energy consumption minimum.
The object of the invention realizes through following technical proposals: a kind of compound method of Di Cumyl Peroxide 99 is a raw material with oxidation liquid and smart benzylalcohol, is that building-up reactions is carried out in 1:1.0～1.2 in reaction kettle by smart benzylalcohol and oxidation liquid mol ratio, comprises the steps:
1) metering of smart benzylalcohol: with pump delivery to smart benzylalcohol scale tank, liquid level is presented between 3000Kg～3200Kg the qualified smart benzylalcohol of benzylalcohol tower production;
2) metering of oxidation liquid: with pump delivery to oxidation liquid scale tank, liquid level is presented between 7000 Kg～oxidation liquid and the smart benzylalcohol 7500Kg oxidation liquid, above-mentioned 1) and 2) liquid level shows and can adopt the accurate measurement weighing system;
3) feeding sequence of reaction kettle: drive reaction kettle and stir; Utilize the vacuum system on the reaction kettle to throw the smart benzylalcohol that measures to reaction kettle, when smart benzylalcohol is dosed to 1/3, add promotor; After extremely smart benzylalcohol has been thrown; Drop into the oxidation liquid that measures in the reaction kettle with the vacuum pump on the reaction kettle, wherein, described promotor percentage composition by weight is 47% perchloric acid, 20% DMSO 99.8MIN. and 33% water; The add-on of described perchloric acid is by weight: perchloric acid: oxidation liquid=0.076:100;
4) condition of building-up reactions control: feed intake finish after; Open Polycondensation Reactor and Esterification Reactor bubbling valve, regulate the still bottom pressure, pass through reacting kettle jacketing heating and reaction kettle coil pipe cooling water control synthesis reaction temperature then at 43～45 ℃ at-0.04 ± 0.001 MPa; The water that reaction generates is with the condensate collector of gas phase to condensing surface; The lowering speed of oxidation liquid hold-up is 3～6%wt/h in the control still, when reacting oxidation liquid hold-up to still≤0.8% wt, in reaction kettle, adds the water termination reaction;
5) processing of impurity in the reaction process: in synthetic reaction process, can decomposite phenol, acetone under the tart condition again owing to oxidation liquid; So reacted reaction solution is that 1:0.1 mixes at the cleaning still with alkali lye by mass ratio; Purpose is removed residual phenol, acetone in the reaction process; Through the reaction solution that alkali lye cleaned, the content of its impurity can be controlled in 1%.Obviously improved the quality of product, dropped to 3～4% by original 20%.
On the such scheme basis, described smart benzylalcohol content >=90% wt.
On the such scheme basis, described oxidation liquid hold-up is 46～48%wt.
On the such scheme basis, described vacuum pump is a water-ring vacuum pump, and the reaction vacuum system is to have replaced W type reciprocating vacuum pump by water-ring vacuum pump; Water-ring vacuum pump is stable, and fault is few, has reduced maintenance cost; And the power of motor of water-ring vacuum pump is less, the same rate of air sucked in required that satisfies reaction usefulness, and as long as its power of motor is 55KW/H; Only be the half the of W type reciprocating vacuum pump, practiced thrift power consumption greatly.
On the such scheme basis, the hot water that adds thermal recovery≤60 ℃ of described reacting kettle jacketing, adopt≤60 ℃ hot water to replace original LP steam after, temperature of reaction reduces.
On the such scheme basis, described reaction kettle coil pipe water coolant adopts≤33 ℃ recirculated water, replaces direct river, and the water of finished product per ton consumes and can reduce more than 90%, is cleaner production, and the conserve water resource has been made huge contribution.
On the such scheme basis, the concentration of described alkali lye is the aqueous sodium hydroxide solution about 10% wt, in cleaning still, fully mixes with 1:0.1 by mass ratio.
Meliority of the present invention is:
Reacting kettle jacketing heating can be controlled between 43～45 ℃ basically, if temperature is low again then reaction efficiency is too poor.Temperature of reaction between 43～45 ℃, the by product that reaction produces descends significantly, drops to 3～4% by original 20%.Achievement is more obvious.
The practical implementation method
Embodiment 1
A kind of compound method of Di Cumyl Peroxide 99, it comprises the steps:
Drive reaction kettle and stir, utilize the vacuum system on the reaction kettle to throw the smart benzylalcohol that measures to reaction kettle, when smart benzylalcohol is dosed to 1/3, add promotor., all drops into the oxidation liquid that measures in the reaction kettle smart benzylalcohol after all having thrown with the vacuum system on the reaction kettle.Feed intake finish after, open Polycondensation Reactor and Esterification Reactor bubbling valve, regulate the still bottom pressure about-0.04MPa.Then through 44 ~ 45 ℃ of reacting kettle jacketing hot water (≤60 ℃) variable valve, reaction kettle coil pipe recirculated water variable valve control synthesis reaction temperatures.The MV of the lowering speed of its oxidation liquid hold-up is controlled at 6.2 %wt/h.Reaction times is 5.2 hours/still.Content of by-products such as the by-product phenol of reaction post analysis reaction, acetone are up to about 4.2%.Reacted reaction solution and alkali lye (aqueous sodium hydroxide solution about 10% wt) fully mix in cleaning still with 1:0.1 by mass ratio, and content of by-products such as its impurity phenol, acetone can be about 0.8%.
Embodiment 2
A kind of compound method of Di Cumyl Peroxide 99, it comprises the steps:
Drive reaction kettle and stir, utilize the vacuum system on the reaction kettle to throw the smart benzylalcohol that measures to reaction kettle, when smart benzylalcohol is dosed to 1/3, add promotor., all drops into the oxidation liquid that measures in the reaction kettle smart benzylalcohol after all having thrown with the vacuum system on the reaction kettle.Feed intake finish after, open Polycondensation Reactor and Esterification Reactor bubbling valve, regulate the still bottom pressure about-0.04MPa.Then through 43 ~ 44 ℃ of reacting kettle jacketing hot water (≤60 ℃) variable valve, reaction kettle coil pipe recirculated water variable valve control synthesis reaction temperatures.The MV of the lowering speed of its oxidation liquid hold-up is controlled at 5.3 %wt/h.Reaction times is 6 hours/still.Content of by-products such as the by-product phenol of reaction post analysis reaction, acetone are up to about 3.5%.Reacted reaction solution and alkali lye (aqueous sodium hydroxide solution about 10% wt) fully mix in cleaning still with 1:0.1 by mass ratio, and content of by-products such as its impurity phenol, acetone can be about 0.64%.
Embodiment 3
A kind of compound method of Di Cumyl Peroxide 99, it comprises the steps:
Drive reaction kettle and stir, utilize the vacuum system on the reaction kettle to throw the smart benzylalcohol that measures to reaction kettle, when smart benzylalcohol is dosed to 1/3, add promotor., all drops into the oxidation liquid that measures in the reaction kettle smart benzylalcohol after all having thrown with the vacuum system on the reaction kettle.Feed intake finish after, open Polycondensation Reactor and Esterification Reactor bubbling valve, regulate the still bottom pressure about-0.04MPa.Then through 43 ~ 45 ℃ of reacting kettle jacketing hot water (≤50 ℃) variable valve, reaction kettle coil pipe recirculated water variable valve control synthesis reaction temperatures.The MV of the lowering speed of its oxidation liquid hold-up is controlled at 5.5%wt/h.Reaction times is 5.8 hours/still.Content of by-products such as the by-product phenol of reaction post analysis reaction, acetone are up to about 3.7%.Reacted reaction solution and alkali lye (aqueous sodium hydroxide solution about 10% wt) fully mix in cleaning still with 1:0.1 by mass ratio, and content of by-products such as its impurity phenol, acetone can be about 0.67%.
Need to prove that above embodiment only is used to explain technical scheme of the present invention and is unrestricted.Although with reference to preferred embodiment the present invention has been carried out detailed explanation, those of ordinary skill in the art should be appreciated that and can make amendment or be equal to replacement the technical scheme of invention.And not breaking away from the scope of technical scheme of the present invention, it all is encompassed in the claim scope of the present invention.
Claims (7)
1. the compound method of a Di Cumyl Peroxide 99 is a raw material with oxidation liquid and smart benzylalcohol, is that building-up reactions is carried out in 1:1.0～1.2 in reaction kettle by smart benzylalcohol and oxidation liquid mol ratio, it is characterized in that it comprises the steps:
1) metering of smart benzylalcohol: with pump delivery to smart benzylalcohol scale tank, liquid level is presented between 3000Kg～3200Kg the qualified smart benzylalcohol of benzylalcohol tower production;
2) metering of oxidation liquid: with pump delivery to oxidation liquid scale tank, liquid level is presented between 7000 Kg～oxidation liquid and the smart benzylalcohol 7500Kg oxidation liquid;
3) feeding sequence of reaction kettle: drive reaction kettle and stir; Utilize the vacuum system on the reaction kettle to throw the smart benzylalcohol that measures to reaction kettle, when smart benzylalcohol is dosed to 1/3, add promotor; After extremely smart benzylalcohol has been thrown; Drop into the oxidation liquid that measures in the reaction kettle with the vacuum pump on the reaction kettle, wherein, described promotor percentage composition by weight is 47% perchloric acid, 20% DMSO 99.8MIN. and 33% water; The add-on of described perchloric acid is by weight: perchloric acid: oxidation liquid=0.076:100;
4) condition of building-up reactions control: feed intake finish after; Open Polycondensation Reactor and Esterification Reactor bubbling valve, regulate the still bottom pressure, pass through 43～45 ℃ of reacting kettle jacketing heating and reaction kettle coil pipe cooling water control synthesis reaction temperatures then at-0.04 ± 0.001 MPa; The water that reaction generates is with gas phase to condenser condenses collection; The lowering speed of oxidation liquid hold-up is 3～6%wt/h in the control still, when reacting oxidation liquid hold-up to still≤0.8% wt, in reaction kettle, adds the water termination reaction;
5) processing of impurity in the reaction process: reacted reaction solution is that 1:0.1 mixes at the cleaning still with alkali lye by mass ratio.
2. the compound method of Di Cumyl Peroxide 99 according to claim 1 is characterized in that, described smart benzylalcohol content >=90% wt.
3. the compound method of Di Cumyl Peroxide 99 according to claim 1 is characterized in that, described oxidation liquid hold-up: 46～48%wt.
4. the compound method of Di Cumyl Peroxide 99 according to claim 1 is characterized in that, described vacuum pump is a water-ring vacuum pump.
5. the compound method of Di Cumyl Peroxide 99 according to claim 1 is characterized in that, the hot water that adds thermal recovery≤60 ℃ of described reacting kettle jacketing.
6. the compound method of Di Cumyl Peroxide 99 according to claim 1 is characterized in that, described reaction kettle coil pipe water coolant adopts≤33 ℃ recirculated water.
7. the compound method of Di Cumyl Peroxide 99 according to claim 1 is characterized in that, the concentration of described alkali lye is the aqueous sodium hydroxide solution of 10% wt.
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| CN2012103567306A CN102827051A (en) | 2012-09-24 | 2012-09-24 | Method for synthesizing dicumyl peroxide |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103145597A (en) * | 2013-03-13 | 2013-06-12 | 中国石油化工集团公司 | Method for producing dicumyl peroxide |
| CN105175301A (en) * | 2015-10-12 | 2015-12-23 | 中石化上海工程有限公司 | Safe type condensation reaction method of DCP (dicumyl peroxide) device |
| CN105294529A (en) * | 2015-10-12 | 2016-02-03 | 中石化上海工程有限公司 | Energy-saving type dicumyl peroxide (DCP) device condensation reaction method |
| CN107382806A (en) * | 2017-07-26 | 2017-11-24 | 江苏道明化学有限公司 | A kind of production method of cumyl peroxide |
| CN108623877A (en) * | 2018-04-17 | 2018-10-09 | 全球能源互联网研究院有限公司 | A kind of high voltage direct current cable insulating materials and preparation method thereof |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103145597A (en) * | 2013-03-13 | 2013-06-12 | 中国石油化工集团公司 | Method for producing dicumyl peroxide |
| CN103145597B (en) * | 2013-03-13 | 2015-05-20 | 中国石油化工集团公司 | Method for producing dicumyl peroxide |
| CN105175301A (en) * | 2015-10-12 | 2015-12-23 | 中石化上海工程有限公司 | Safe type condensation reaction method of DCP (dicumyl peroxide) device |
| CN105294529A (en) * | 2015-10-12 | 2016-02-03 | 中石化上海工程有限公司 | Energy-saving type dicumyl peroxide (DCP) device condensation reaction method |
| CN105175301B (en) * | 2015-10-12 | 2017-04-05 | 中石化上海工程有限公司 | The method of safety-type cumyl peroxide DCP device condensation reactions |
| CN105294529B (en) * | 2015-10-12 | 2017-05-24 | 中石化上海工程有限公司 | Energy-saving type dicumyl peroxide (DCP) device condensation reaction method |
| CN107382806A (en) * | 2017-07-26 | 2017-11-24 | 江苏道明化学有限公司 | A kind of production method of cumyl peroxide |
| CN108623877A (en) * | 2018-04-17 | 2018-10-09 | 全球能源互联网研究院有限公司 | A kind of high voltage direct current cable insulating materials and preparation method thereof |
| WO2019201153A1 (en) * | 2018-04-17 | 2019-10-24 | 全球能源互联网研究院有限公司 | Insulation material for high-voltage direct current cable and preparation method therefor |
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Application publication date: 20121219 |