CN102911098B - Method for producing mono-hydrogen peroxide diisopropylbenzene - Google Patents
Method for producing mono-hydrogen peroxide diisopropylbenzene Download PDFInfo
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- CN102911098B CN102911098B CN201110221449.7A CN201110221449A CN102911098B CN 102911098 B CN102911098 B CN 102911098B CN 201110221449 A CN201110221449 A CN 201110221449A CN 102911098 B CN102911098 B CN 102911098B
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- diisopropylbenzene
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Abstract
The invention relates to a method for producing mono-hydrogen peroxide diisopropylbenzene, which solves problems of high additive cost and low product yield in the prior art. According to the invention, the problems are preferably solved through the adoption of the technical scheme as follows: raw materials diisopropylbenzene and air react with each other under conditions that the reaction temperature is 60-240 DEG C, the reaction pressure is 0.2-1.6 MPa, the weight ratio between the diisopropylbenzene and the air is (10-20):3 and the pH value of the reaction materials is 1.0-3.0 or 10.0-13.8, so as to obtain the mono-hydrogen peroxide diisopropylbenzene; and the method for producing the mono-hydrogen peroxide diisopropylbenzene, provided by the invention, can be used for the industrial production of the mono-hydrogen peroxide diisopropylbenzene.
Description
Technical field
The present invention relates to the method for a kind of production one di-isopropylbenzene hydroperoxide.
Background technology
One di-isopropylbenzene hydroperoxide (MHP) is the intermediates of producing two-(tert-butyl peroxy sec.-propyl) benzene (BIPB).Document US5981805, JP2007217399 and JP2007039435 disclose take diisopropylbenzene(DIPB) as starting raw material, with atmospheric oxidation and add water-soluble iron containing compounds and obtain a di-isopropylbenzene hydroperoxide MHP to improve oxidation rate, more further carry out series reaction and obtain two-(tert-butyl peroxy sec.-propyl) benzene BIPB products.
But, in above-mentioned document, prepare a di-isopropylbenzene hydroperoxide MHP and must in diisopropylbenzene(DIPB) raw material, add water-soluble iron containing compounds to improve oxidation rate.And in actual production process, owing to using water-soluble iron containing compounds additive, there is the problem that additive cost is high, product yield is low.
Summary of the invention
Technical problem to be solved by this invention is that prior art exists the problem that additive cost is high, product yield is low, and a kind of method of new production one di-isopropylbenzene hydroperoxide is provided.It is low that the method has production cost, the feature that product yield is high, and further improved oxidizing reaction speed, reduced the residence time.
For solving the problems of the technologies described above, the technical solution used in the present invention is as follows: the method for a kind of production one di-isopropylbenzene hydroperoxide, take diisopropylbenzene(DIPB) and air as raw material, 60～240 ℃ of temperature of reaction, reaction pressure 0.2～1.6MPa, the weight ratio of diisopropylbenzene(DIPB) and air is (10～20): 3, and reaction mass is that under 1.0～3.0 or 10.0～13.8 conditions, reaction obtains a di-isopropylbenzene hydroperoxide in pH value.
In technique scheme, the present pH value of reaction mass, its preferable range is 1.1～2.8 or 10.5～13.4, more preferably scope is 1.2～2.5 or 10.8～12.9.The present invention, by add pH value conditioning agent in diisopropylbenzene(DIPB) raw material, makes reaction mass under described pH value condition, and described pH value conditioning agent preferred version is at least one being selected from hydrochloric acid, sulfuric acid, sodium hydroxide, potassium hydroxide or calcium hydroxide.Temperature of reaction preferable range is 80～200 ℃, and reaction pressure preferable range is 0.8～1.2MPa, and the weight ratio preferable range of diisopropylbenzene(DIPB) and air is (10～15): 3.
In the inventive method, described reaction pressure all refers to gauge pressure.
The present invention replaces water-soluble iron containing compounds additive by add pH adjusting agent in diisopropylbenzene(DIPB) raw material, controlling reaction mass is under 1.0～3.0 or 10.0～13.8 conditions in pH value, improve oxidizing reaction speed, reduced the residence time 10.11%, reduce additive cost 10.08%, improve product yield 32.47%, obtained good technique effect.
Below by embodiment, the present invention is further elaborated.
Embodiment
[embodiment 1]
With 5 % by weight hydrochloric acid, as pH value conditioning agent, regulating reaction mass pH value is 1.60, and in oxidation reactor, reaction pressure is 1.2MPa, and temperature of reaction is 200 ℃, and diisopropylbenzene(DIPB) is 3.33 with Air quality ratio.Diisopropylbenzene(DIPB) and air carry out oxidizing reaction and generate a di-isopropylbenzene hydroperoxide MHP in oxidation reactor.
The residence time is 24.0 hours, and product yield is 20.40 % by weight, and the pH value conditioning agent cost of interpolation is 33.0 yuan of/kilogram of MHP.
[embodiment 2]
With [embodiment 1], be pH value conditioning agent used be the sulfuric acid of 10 % by weight, adjusting reaction mass pH value is 1.40.
The residence time is 24.0 hours, and product yield is 21.25 % by weight, and the pH value conditioning agent cost of interpolation is 33.9 yuan of/kilogram of MHP.
[embodiment 3]
With [embodiment 1], be pH value conditioning agent used be the NaOH of 10 % by weight, adjusting reaction mass pH value is 11.68.
The residence time is 24.0 hours, and product yield is 18.12 % by weight, and the pH value conditioning agent cost of interpolation is 32.1 yuan of/kilogram of MHP.
[embodiment 4]
With [embodiment 1], just reaction pressure is 0.9MPa, and temperature of reaction is 180 ℃, and diisopropylbenzene(DIPB) is 3.33 with Air quality ratio.
The residence time is 24.0 hours, and product yield is 17.66 % by weight, and the pH value conditioning agent cost of interpolation is 33.5 yuan of/kilogram of MHP.
[comparative example 1]
Diisopropylbenzene(DIPB) and air carry out oxidizing reaction and generate a di-isopropylbenzene hydroperoxide MHP in oxidation reactor, use water-soluble iron containing compounds additive iron trichloride FeCl
3.Reaction conditions is: reaction pressure 1.2MPa, and 200 ℃ of temperature of reaction, diisopropylbenzene(DIPB) is 3.33 with Air quality ratio, and the amount ratio of diisopropylbenzene(DIPB) and water-soluble iron containing compounds additive is 10, and the pH value of reaction mass is 7.
The residence time is 26.7 hours, and product yield is 15.40 % by weight, and the water-soluble iron containing compounds additive cost of interpolation is 36.7 yuan of/kilogram of MHP.
Claims (5)
1. a method of producing a di-isopropylbenzene hydroperoxide, take diisopropylbenzene(DIPB) and air as raw material, 60～240 ℃ of temperature of reaction, reaction pressure 0.2～1.6MPa, the weight ratio of diisopropylbenzene(DIPB) and air is (10～20): 3, and reaction mass is that under 1.0～3.0 conditions, reaction obtains a di-isopropylbenzene hydroperoxide in pH value.
2. produce according to claim 1 the method for a di-isopropylbenzene hydroperoxide, it is characterized in that reaction mass is under 1.1～2.8 conditions in pH value.
3. produce according to claim 2 the method for a di-isopropylbenzene hydroperoxide, it is characterized in that reaction mass is under 1.2～2.5 conditions in pH value.
4. produce according to claim 1 the method for a di-isopropylbenzene hydroperoxide, it is characterized in that adding pH value conditioning agent and make reaction mass under described pH value condition, described pH value conditioning agent is selected from least one in hydrochloric acid or sulfuric acid.
5. produce according to claim 1 the method for a di-isopropylbenzene hydroperoxide, it is characterized in that temperature of reaction is 80～200 ℃, reaction pressure is 0.8～1.2MPa, and the weight ratio of diisopropylbenzene(DIPB) and air is (10～15): 3.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201110221449.7A CN102911098B (en) | 2011-08-04 | 2011-08-04 | Method for producing mono-hydrogen peroxide diisopropylbenzene |
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| CN201110221449.7A CN102911098B (en) | 2011-08-04 | 2011-08-04 | Method for producing mono-hydrogen peroxide diisopropylbenzene |
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| CN102911098A CN102911098A (en) | 2013-02-06 |
| CN102911098B true CN102911098B (en) | 2014-04-02 |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB727498A (en) * | 1952-08-23 | 1955-04-06 | Distillers Co Yeast Ltd | The manufacture of organic hydroperoxides |
| CN101003505A (en) * | 2006-01-18 | 2007-07-25 | 住友化学株式会社 | Process for producing alkyl aromatic hydroperoxide |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS4913779B1 (en) * | 1969-09-01 | 1974-04-03 | ||
| JPH0694457B2 (en) * | 1985-02-07 | 1994-11-24 | 三井石油化学工業株式会社 | Method for oxidizing P-diisopropylbenzene |
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- 2011-08-04 CN CN201110221449.7A patent/CN102911098B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB727498A (en) * | 1952-08-23 | 1955-04-06 | Distillers Co Yeast Ltd | The manufacture of organic hydroperoxides |
| CN101003505A (en) * | 2006-01-18 | 2007-07-25 | 住友化学株式会社 | Process for producing alkyl aromatic hydroperoxide |
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