CN102911101B - One-step method for production of di-(hydrogen peroxide isopropyl) benzene - Google Patents
One-step method for production of di-(hydrogen peroxide isopropyl) benzene Download PDFInfo
- Publication number
- CN102911101B CN102911101B CN201110221591.1A CN201110221591A CN102911101B CN 102911101 B CN102911101 B CN 102911101B CN 201110221591 A CN201110221591 A CN 201110221591A CN 102911101 B CN102911101 B CN 102911101B
- Authority
- CN
- China
- Prior art keywords
- benzene
- hydrogen peroxide
- diisopropylbenzene
- reaction
- propyl
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Abstract
The invention relates to a one-step method for production of di-(hydrogen peroxide isopropyl) benzene. The method mainly solves the problems of low product yield, long technical process, excessive equipment and large occupied area in the prior art. The technical scheme for better solving the problems includes that diisopropylbenzene, air and oxygen are used as raw materials and enter a plate type reactor from the lower middle, the lower portion and the upper middle to contact in the plate type reactor to generate the di-(hydrogen peroxide isopropyl) benzene, wherein the reaction temperature is 60-240 DEG C, the reaction pressure is 0.2-1.6MPa, the number of plates is 10-50, and the weight ratio of the diisopropylbenzene, the air to the oxygen is (20-40):(4-9):(4-9). The one-step method can be used for industrial production of di-(hydrogen peroxide isopropyl) benzene.
Description
Technical field
The present invention relates to a kind of One-step production two-method of (hydrogen peroxide sec.-propyl) benzene.
Background technology
The method (DHP) of two-(hydrogen peroxide sec.-propyl) benzene is to produce the intermediates of two-(tert-butyl peroxy sec.-propyl) benzene (BIPB).Document US5981805, JP2007217399 and JP2007039435 disclose take diisopropylbenzene(DIPB) as starting raw material, with atmospheric oxidation, obtain a di-isopropylbenzene hydroperoxide MHP, then with atmospheric oxidation, obtain two-(hydrogen peroxide sec.-propyl) benzene DHP, 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, take diisopropylbenzene(DIPB) as starting raw material, first in a reactor, obtain a di-isopropylbenzene hydroperoxide with atmospheric oxidation; Then in another reactor, a di-isopropylbenzene hydroperoxide continues to obtain two-(hydrogen peroxide sec.-propyl) benzene with atmospheric oxidation again.These two reactors are all bubbling reactors, have the serious problem of liquid phase axial backmixing, cause product yield lower.Meanwhile, owing to adopting dual reactor process route, there is the problem that technical process is long, number of devices is many, floor space is large.
Summary of the invention
Technical problem to be solved by this invention is that prior art exists product yield low, and the problem that technical process is long, number of devices is many, floor space is large provides the method for a kind of new One-step production pair-(hydrogen peroxide sec.-propyl) benzene.It is high that the method has product yield, the simple feature of flow process.
For solving the problems of the technologies described above, the technical solution used in the present invention is as follows: a kind of One-step production is two-and the method for (hydrogen peroxide sec.-propyl) benzene, with diisopropylbenzene(DIPB), air and oxygen are raw material, diisopropylbenzene(DIPB), air and oxygen are respectively from middle and lower part, bottom and middle and upper part enter plate-type reactor, 60～240 ℃ of temperature of reaction, reaction pressure 0.2～1.6MPa, stage number is 10～50, diisopropylbenzene(DIPB), the weight ratio of air and oxygen is (20～40): (4～9): under (4～9) condition, reaction raw materials contacts in plate-type reactor, generate two-(hydrogen peroxide sec.-propyl) benzene.
In technique scheme, temperature of reaction preferable range is 80～200 ℃; Reaction pressure preferable range is 0.8～1.2MPa; Stage number preferable range is 18～40, and more preferably scope is 24～36.The weight ratio of diisopropylbenzene(DIPB), air and oxygen is preferable range (20～30): (5～7): (5～7).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, diisopropylbenzene(DIPB) is sent into board-like oxidation reactor middle and lower part, pH value conditioning agent is sent into board-like oxidation reactor top, air is sent into board-like oxidation reactor bottom, oxygen is sent into board-like oxidation reactor middle and upper part, this is to have consumed oxygen because oxidizing reaction occurs in plate-type reactor middle and lower part for diisopropylbenzene(DIPB) and air, and in gas phase, oxygen concentration declines; In order further to improve product yield, in plate-type reactor middle and upper part, send into oxygen to improve the concentration of reactant oxygen.Diisopropylbenzene(DIPB) carries out oxidizing reaction and generates two-(hydrogen peroxide sec.-propyl) benzene in board-like oxidation reactor, and extracts out from board-like oxidation reactor bottom, and waste gas is discharged from board-like oxidation reactor top, and waste water is discharged from board-like oxidation reactor bottom.
The inventive method in a plate-type reactor by injecting respectively air and dioxygen oxidation diisopropylbenzene(DIPB) generates a di-isopropylbenzene hydroperoxide, the oxidation step of going forward side by side generates two-(hydrogen peroxide sec.-propyl) benzene, thereby make reactor apparatus quantity be reduced to 1 of the present invention by 2 of prior art, floor space declines 50%.By adopting plate-type reactor to replace bubbling reactor, make axial backmixing be reduced to minimum degree; In addition the pH value of preferably controlling reaction mass, has improved speed of response; The product yield that makes two-(hydrogen peroxide sec.-propyl) benzene is increased to of the present invention 13.65% by 12.24% (weight) of prior art
(weight), has improved 11.52%, has obtained good technique effect.
Below by embodiment, the present invention is further elaborated.
Embodiment
[embodiment 1]
Diisopropylbenzene(DIPB), air, oxygen and pH value conditioning agent respectively from middle and lower part, bottom, middle and upper part and top enters plate-type reactor, material contacts in plate-type reactor, generates two-(hydrogen peroxide sec.-propyl) benzene.Temperature of reaction is 200 ℃, and reaction pressure is 1.2MPa, and stage number is 24, and diisopropylbenzene(DIPB) is 10: 3 with Air quality ratio, and diisopropylbenzene(DIPB) is 10: 3 with oxygen quality ratio, and pH value conditioning agent is 5 % by weight hydrochloric acid, and regulating reaction mass pH value is 1.60.
Oxidation reactor quantity is 1, and product yield is 13.65% (weight).
[embodiment 2]
With [embodiment 1], be pH value conditioning agent used be the NaOH of 10 % by weight, pH value is 11.68.
Oxidation reactor quantity is 1, and product yield is 13.52% (weight).
[embodiment 3]
With [embodiment 1], just reaction pressure is 0.9MPa, and temperature of reaction is 180 ℃.
Oxidation reactor quantity is 1, and product yield is 13.51% (weight).
[embodiment 4]
With [embodiment 1], just the plate number of oxidation reactor is 36.
Oxidation reactor quantity is 1, and product yield is 13.68% (weight)
[embodiment 5]
With [embodiment 1], just do not add pH value conditioning agent.
Product yield is 12.72% (weight)
[comparative example 1]
Diisopropylbenzene(DIPB) and air carry out oxidizing reaction and generate two-(hydrogen peroxide sec.-propyl) benzene 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.
Oxidation reactor quantity is 2, and product yield is 12.24% (weight).
Claims (5)
- An One-step production two-method of (hydrogen peroxide sec.-propyl) benzene, take diisopropylbenzene(DIPB), air and oxygen as raw material, diisopropylbenzene(DIPB), air and oxygen respectively from middle and lower part, bottom and middle and upper part enter plate-type reactor, 60～240 ℃ of temperature of reaction, reaction pressure 0.2～1.6MPa, stage number is 10～50, the weight ratio of diisopropylbenzene(DIPB), air and oxygen is (20～40): (4～9): under (4～9) condition, reaction raw materials contacts in plate-type reactor, generates two-(hydrogen peroxide sec.-propyl) benzene; Reaction mass is under 1.0～3.0 conditions in pH value.
- According to claim 1 One-step production two-method of (hydrogen peroxide sec.-propyl) benzene, it is characterized in that temperature of reaction is 80～200 ℃, reaction pressure is 0.8～1.2MPa, stage number is 18～40, and the weight ratio of diisopropylbenzene(DIPB), air and oxygen is (20～30): (5～7): (5～7).
- According to claim 1 One-step production two-method of (hydrogen peroxide sec.-propyl) benzene, it is characterized in that reaction mass is under 1.1～2.8 conditions in pH value.
- According to claim 3 One-step production two-method of (hydrogen peroxide sec.-propyl) benzene, it is characterized in that reaction mass is under 1.2～2.5 conditions in pH value.
- 5. 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.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110221591.1A CN102911101B (en) | 2011-08-04 | 2011-08-04 | One-step method for production of di-(hydrogen peroxide isopropyl) benzene |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110221591.1A CN102911101B (en) | 2011-08-04 | 2011-08-04 | One-step method for production of di-(hydrogen peroxide isopropyl) benzene |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102911101A CN102911101A (en) | 2013-02-06 |
| CN102911101B true CN102911101B (en) | 2014-04-02 |
Family
ID=47609707
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201110221591.1A Active CN102911101B (en) | 2011-08-04 | 2011-08-04 | One-step method for production of di-(hydrogen peroxide isopropyl) benzene |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102911101B (en) |
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 |
-
2011
- 2011-08-04 CN CN201110221591.1A patent/CN102911101B/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-液反应及反应器.《化学反应工程》.化学工业出版社,2001,第262-263页. * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102911101A (en) | 2013-02-06 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106957283B (en) | A kind of mono-acid method alcoholizing propenyl chloride Synthesis of Propylene Oxide | |
| CN103159592B (en) | The production method of two-(2-hydroxyisopropyl) benzene | |
| RU2013130867A (en) | METHOD FOR PRODUCING PROPYLENE OXIDE | |
| CN105541583A (en) | Method for directly synthesizing 2,2,4-trimethyl-1,3-pentanediol diisobutyrate from isobutyraldehyde | |
| CN102911101B (en) | One-step method for production of di-(hydrogen peroxide isopropyl) benzene | |
| CN109134217A (en) | Oxidation unit and oxidation technology improved method during a kind of cyclohexane oxidation process production cyclohexanone | |
| CN102911100B (en) | Di-(hydrogen peroxide isopropyl) benzene preparation method | |
| CN102584640B (en) | The technique that a kind of multi-floating bodies formula produces ADC foaming agent continuously | |
| CN106699695B (en) | A kind of production method of propylene oxide | |
| CN105272808B (en) | The equipment of propylene recovery | |
| CN102911097B (en) | Diisopropylbenzene hydroperoxide production method | |
| CN105693584A (en) | Peroxided neodecanoic acid isopropyl phenyl ester and method for preparing peroxided neodecanoic acid isopropyl phenyl ester through phase transfer catalyst | |
| CN102911014B (en) | Di-(2-hydroxyl isopropyl) benzene production method | |
| CN106699696B (en) | A kind of co-production of propylene oxide and cyclohexanone | |
| CN102911099B (en) | Di-(hydrogen peroxide isopropyl) benzene preparation method | |
| CN107488099A (en) | A kind of method for producing expoxy propane and cyclohexanol | |
| CN104909990B (en) | The method efficiently producing cumyl peroxide DCP intermediate products | |
| CN105272806B (en) | The method of propylene recovery | |
| CN102911098B (en) | Method for producing mono-hydrogen peroxide diisopropylbenzene | |
| CN103819380A (en) | New method for producing p-menthane hydroperoxide with series connection of multiple bubbling-tower reactors | |
| CN108774198A (en) | A kind of method that toluene conjugated oxidation prepares propylene oxide | |
| CN109516966B (en) | Method for oxidizing styrene by molecular oxygen | |
| KR20130017943A (en) | Method for preparing phenol, acetone and alpha methyl styrene | |
| RU2648887C1 (en) | Method for obtaining peroxide of hydrogen | |
| CN102911015B (en) | Di-(2-hydroxyl isopropyl) benzene production method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |