CN102911097B - Diisopropylbenzene hydroperoxide production method - Google Patents
Diisopropylbenzene hydroperoxide production method Download PDFInfo
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- CN102911097B CN102911097B CN201110221431.7A CN201110221431A CN102911097B CN 102911097 B CN102911097 B CN 102911097B CN 201110221431 A CN201110221431 A CN 201110221431A CN 102911097 B CN102911097 B CN 102911097B
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- isopropylbenzene hydroperoxide
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Abstract
The invention relates to a diisopropylbenzene hydroperoxide production method which mainly solves the problems of low product yield caused by serious liquid-phase axial back mixing of bubbling reactors in the prior art. The technical scheme for better solving the problems includes that diisopropylbenzene and air are used as raw materials and enter a plate type reactor from the middle and the lower portion to contact in the plate type reactor to generate the diisopropylbenzene hydroperoxide. The diisopropylbenzene hydroperoxide production method can be used for industrial production of diisopropylbenzene hydroperoxide.
Description
Technical field
The present invention relates to a kind of production method of a 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 while preparing a di-isopropylbenzene hydroperoxide MHP in prior art, the form of its chemical reactor is bubbling reactor, there is the serious problem of liquid phase axial backmixing, cause product yield lower.
Summary of the invention
Technical problem to be solved by this invention is that prior art exists bubbling reactor liquid phase axial backmixing serious, causes the problem that product yield is lower, and a kind of production method of a new di-isopropylbenzene hydroperoxide is provided.The method has the advantages that product yield is high.
For solving the problems of the technologies described above, the technical solution used in the present invention is as follows: a kind of production method of a di-isopropylbenzene hydroperoxide, take diisopropylbenzene(DIPB) and air as raw material, diisopropylbenzene(DIPB) and air enter plate-type reactor from middle part and bottom respectively, and in plate-type reactor, contact generates a di-isopropylbenzene hydroperoxide.
In technique scheme, plate-type reactor operational condition is: 60～240 ℃ of temperature of reaction, and preferable range is 80～200 ℃; Reaction pressure 0.2～1.6MPa, preferable range is 0.8～1.2MPa; Stage number is 4～40, and preferable range is 6～28, and more preferably scope is 8～20.The weight ratio of diisopropylbenzene(DIPB) and air is (10～20): 3, and preferable range is (10～15): 3.Preferred version of the present invention is that reaction mass is under 1.0～3.0 or 10.0～13.8 conditions in pH value, preferable range is that reaction mass is under 1.1～2.8 or 10.5～13.4 conditions in pH value, and more preferably scope is that reaction mass is under 1.2～2.5 or 10.8～12.9 conditions in pH value.For making pH value meet above-mentioned condition, preferred version is for adding pH value conditioning agent, and described pH value conditioning agent is selected from least one in hydrochloric acid, sulfuric acid, sodium hydroxide, potassium hydroxide or calcium hydroxide.
In the inventive method, described reaction pressure all refers to gauge pressure.
When the inventive method is implemented, fresh feed diisopropylbenzene(DIPB) and circulation fluid are sent into feed chute and are mixed and preheating.Raw material after heating is divided into two tunnels and sends into plate-type reactor middle part, and pH value regulator solution is sent into plate-type reactor top, and air is sent into plate-type reactor bottom.Diisopropylbenzene(DIPB) and air carry out oxidizing reaction in plate-type reactor, generate a di-isopropylbenzene hydroperoxide MHP, and extract out from board-like reactor lower part.Waste gas is discharged from board-like reactor head, and waste water is discharged from board-like reactor bottom.
The present invention, by adopting plate-type reactor, makes axial backmixing be reduced to minimum degree; In addition preferably control the pH value of reaction mass; The product yield that makes a di-isopropylbenzene hydroperoxide MHP is increased to 20.40% (weight) of the present invention by 15.40% (weight) of prior art, has improved 32.47%, has 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, pH value is 1.60, and in plate-type reactor, reaction pressure is 1.2MPa, and temperature of reaction is 200 ℃, and diisopropylbenzene(DIPB) is 3.33 with Air quality ratio, and the stage number of reactor is 8.Diisopropylbenzene(DIPB) and air enter plate-type reactor from middle part and bottom respectively, carry out oxidizing reaction and generate a di-isopropylbenzene hydroperoxide MHP in plate-type reactor.
Product yield is 20.40% (weight).
[embodiment 2]
With [embodiment 1], just the stage number of reactor is 12.
Product yield is 20.45% (weight).
[embodiment 3]
With [embodiment 1], just the stage number of reactor is 16.
Product yield is 20.47% (weight).
[embodiment 4]
With [embodiment 1], just the stage number of reactor is 20.
Product yield is 20.48% (weight).
[embodiment 5]
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.
Product yield is 17.66 % by weight.
[embodiment 6]
With [embodiment 1], just do not add pH value conditioning agent.
Product yield is 15.87 % by weight.
[comparative example 1]
Diisopropylbenzene(DIPB) and air carry out oxidizing reaction and generate a di-isopropylbenzene hydroperoxide MHP in bubbling 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.
Product yield is 15.40% (weight).
Claims (8)
1. a production method for a di-isopropylbenzene hydroperoxide, take diisopropylbenzene(DIPB) and air as raw material, and diisopropylbenzene(DIPB) and air enter plate-type reactor from middle part and bottom respectively, and in plate-type reactor, contact generates a di-isopropylbenzene hydroperoxide; Reaction mass is under 1.0～3.0 conditions in pH value.
2. the production method of a di-isopropylbenzene hydroperoxide according to claim 1, is characterized in that plate-type reactor operational condition is: 60～240 ℃ of temperature of reaction, and reaction pressure 0.2～1.6MPa, stage number is 4～40.
3. the production method of a di-isopropylbenzene hydroperoxide according to claim 2, is characterized in that plate-type reactor operational condition is: temperature of reaction is 80～200 ℃, and reaction pressure is 0.8～1.2MPa, and stage number is 6～28.
4. the production method of a di-isopropylbenzene hydroperoxide according to claim 1, the weight ratio that it is characterized in that diisopropylbenzene(DIPB) and air is (10～20): 3.
5. the production method of a di-isopropylbenzene hydroperoxide according to claim 4, the weight ratio that it is characterized in that diisopropylbenzene(DIPB) and air is (10～15): 3.
6. the production method of a di-isopropylbenzene hydroperoxide according to claim 1, is characterized in that reaction mass is under 1.1～2.8 conditions in pH value.
7. the production method of a di-isopropylbenzene hydroperoxide according to claim 6, is characterized in that reaction mass is under 1.2～2.5 conditions in pH value.
8. the production method of a di-isopropylbenzene hydroperoxide according to claim 1, is characterized in that adding pH value conditioning agent and makes reaction mass under described pH value condition, and described pH value conditioning agent is selected from least one in hydrochloric acid or sulfuric acid.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201110221431.7A CN102911097B (en) | 2011-08-04 | 2011-08-04 | Diisopropylbenzene hydroperoxide production method |
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| CN201110221431.7A CN102911097B (en) | 2011-08-04 | 2011-08-04 | Diisopropylbenzene hydroperoxide production method |
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| CN102911097B true CN102911097B (en) | 2014-04-30 |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3953521A (en) * | 1972-08-23 | 1976-04-27 | Sumitomo Chemical Company, Limited | Process for the continuous production of dihydroperoxides |
| 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 (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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
- 2011-08-04 CN CN201110221431.7A patent/CN102911097B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3953521A (en) * | 1972-08-23 | 1976-04-27 | Sumitomo Chemical Company, Limited | Process for the continuous production of dihydroperoxides |
| CN101003505A (en) * | 2006-01-18 | 2007-07-25 | 住友化学株式会社 | Process for producing alkyl aromatic hydroperoxide |
Non-Patent Citations (1)
| Title |
|---|
| 朱炳辰.气液反应器概述.《化学反应工程》.化学工业出版社,2001,第261-263页. * |
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