CN104909990B - The method efficiently producing cumyl peroxide DCP intermediate products - Google Patents
The method efficiently producing cumyl peroxide DCP intermediate products Download PDFInfo
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- CN104909990B CN104909990B CN201510229823.6A CN201510229823A CN104909990B CN 104909990 B CN104909990 B CN 104909990B CN 201510229823 A CN201510229823 A CN 201510229823A CN 104909990 B CN104909990 B CN 104909990B
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- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/132—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by reduction of an oxygen containing functional group
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Abstract
A kind of method that the present invention relates to efficient production cumyl peroxide DCP intermediate products, mainly solves intermittently operated in prior art, reaction rate is slow, the problem that expends time length.The present invention is by a kind of method using efficient production cumyl peroxide DCP intermediate products, by 2～8 stirred autoclave series connection, the bottom outlet of each reactor is respectively provided with oil water separator, in addition to last oil water separator, the isolated oil phase material of other oil water separator enters next stirred autoclave from top；CHP raw material enters from the top of first stirred autoclave, reducing solution enters from the top of last stirred autoclave, first isolated aqueous phase of oil water separator is discharged as reducing waste water, the isolated oil phase of last oil water separator is intermediate products dimethyl benzyl alcohol, the technical scheme at the top that isolated aqueous phase returns a upper stirred autoclave preferably solves the problems referred to above, can be used in the production of cumyl peroxide DCP intermediate products.
Description
Technical field
A kind of method that the present invention relates to efficient production cumyl peroxide DCP intermediate products.
Background technology
Cumyl peroxide, also known as DCP, is a kind of common Non-symmetrical dialkyl organic peroxide, and purposes is quite varied.
Industrial production DCP is with isopropylbenzene as raw material, by air, cumene oxidation is become cumyl hydroperoxide CHP, and
A part of CHP reduction generates dimethyl benzyl alcohol CA, and then CA and another part CHP carry out condensation reaction and generated
Oxidation diisopropylbenzene (DIPB) DCP.CHP reduction reaction is a very important course of reaction during DCP produces, the product to DCP
Quality, safety in production affect huge.
Number of patent application CN93104129.5 relates to the manufacture method of 2-phenyl-2-propanol, discloses with water-soluble sulfide also
Former isopropyl benzene hydroperoxide CHP manufactures the method for 2-phenyl-2-propanol.Use Na2S reducing agent replaces Na2SO3Reducing agent,
And describe employing Na2S prepares the technological process of 2-phenyl-2-propanol as reducing agent.The usage amount detailing MxS is:
From determined by itself and CHP reaction equation, theoretical amount is to the 200% of theoretical amount, and reaction temperature is 0～150 DEG C, instead
It is 0.5～8h between Ying Shi.Having reacted rear stratification, point sub-cloud aqueous phase, upper organic phase is washed with water to the pH of aqueous phase
When value is 6～8, organic facies is CA intermediate products.
Number of patent application CN201310208646.4 relates to produce the production equipment of the reduction reaction of cumyl peroxide
And method, disclose production equipment and include aoxidizing liquid bath, reductant solution make-up tank, reduction kettle and controller, controller
The temperature sensor of with reduction kettle agitator motor, measuring reduction reaction temperature, detection reduction kettle circulating cooling water pressure
Pressure transducer and reduction kettle recirculated cooling water cut valve electrical connection soon.When reducing agent reacts in reduction kettle with oxidation solution,
Controller judges that motor stops operating or reduction kettle reduction reaction temperature is more than reduction kettle reduction reaction temperature setting value
Or reduction kettle circulating cooling water pressure is less than reduction kettle recirculated cooling water pressure set points and extends the setting time, the most automatically cuts
Disconnected motor power, it is automatically switched off oxidation solution inlet valve and automatically opens up reduction kettle recirculated cooling water and cut valve soon.Controller
This chain control, the safety that cumyl peroxide reduction reaction has been effectively ensured is carried out.This patent of invention uses intermittently operated
Reduction reaction process, after in liquid to be restored, the content of CHP is 0.2wt%≤CHP≤2wt%, stop reduction reaction still
Interior stirring, quiescent settling separates about 1h, and stratification oil phase is the intermediate products CA reducing solution obtained.
Prior art is during producing cumyl peroxide intermediate products dimethyl benzyl alcohol, and reduction reaction uses interval anti-
Answer still operational approach, by CHP oxidation solution and Na2S reducing solution puts in reactor in the lump and reacts, reaction mass along with
Constantly carrying out of reaction, concentration from high to low, is gradually reduced in time, there is unstable, the reduction reaction concentration of operation and more comes
The problems such as the lowest, reaction rate slow, consuming time length.
The present invention solves this problem targetedly.
Summary of the invention
The technical problem to be solved is intermittently operated in prior art, reaction rate is slow, expend the problem of time length,
A kind of new method efficiently producing cumyl peroxide DCP intermediate products is provided.The method is used for peroxidating diisopropyl
In the production of benzene DCP intermediate products, there is continuous operation, reaction rate is fast, the consuming time is short advantage.
For solving the problems referred to above, the technical solution used in the present invention is as follows: a kind of efficiently production cumyl peroxide DCP
The method of intermediate products, by 2～8 stirred autoclave series connection, the bottom outlet of each stirred autoclave is respectively provided with profit
Separator, in addition to last oil water separator, the isolated oil phase material of other oil water separator enters the next one from top
Stirred autoclave；Oxidation solution CHP raw material enters from the top of first stirred autoclave, and reducing solution sodium sulfide is from last
The top of individual stirred autoclave enters, and first isolated aqueous phase of oil water separator is discharged as reducing waste water, last
The isolated oil phase of oil water separator is intermediate products dimethyl benzyl alcohol, and the isolated aqueous phase of last oil water separator returns
The top of a upper stirred autoclave.
In technique scheme, it is preferable that CHP and Na2S molar ratio is 4:1.0～1.2.
In technique scheme, it is preferable that entering CHP concentration range in the oxidation solution of the 1st stirred autoclave is
45～50wt%, reduction reaction temperature is 65～70 DEG C, and reduction reaction pressure is normal pressure, and the time of staying is 2.0～3.8h, works as oxygen
After change liquid CHP reduction reaction terminates, last 1 reduction reaction bottom CHP lowering of concentration is between 0.10～0.60wt%.
The present invention uses the mode of 2～8 order reaction still series connection continuous flow upstreams to carry out reduction reaction, due to counter-current operation, makes every grade
Reaction motive force in reactor is the highest, causes reaction rate the highest, thus reduces the time of reaction, makes behaviour
Making more steady, reaction is more abundant, and reaction end CHP lowering of concentration to 0.10～0.60wt% achieves preferable technology
Effect.
Accompanying drawing explanation
Fig. 1 is the schematic flow sheet of the method for the invention.
In Fig. 1, as a example by 4 cascade reaction stills: fresh oxidation solution cumyl hydroperoxide (1) and fresh reduction molten sulfur
Change sodium (14) and enter reduction reaction still (15) and reduction reaction still (21) participation reaction respectively from two contrary directions.
Fresh oxidation solution cumyl hydroperoxide (1) sends into reactor (15) with follow-up return aqueous portion (12) reducing solution sodium sulfide
In carry out reduction reaction；Reacted reactant liquor (2) enters oil water separator (16) and carries out oil-water separation, after separation
Aqueous portion (13) is discharged as reducing waste water.Oil phase part (3) and follow-up return aqueous portion (11) reduction molten sulfur
Change in sodium feeding reactor (17) and carry out reduction reaction；Reacted reactant liquor (4) enters oil water separator (18) and enters
Row oil-water separation, the aqueous portion (12) after separation backs into reactor (15).Oil phase part (5) is returned with follow-up
Return aqueous portion (10) reducing solution sodium sulfide feeding reactor (19) and carry out reduction reaction；Reacted reactant liquor (6)
Entering oil water separator (20) and carry out oil-water separation, the aqueous portion (11) after separation backs into reactor (17).
Oil phase part (7) and fresh reducing solution sodium sulfide (14) are sent into reactor (21) and are carried out reduction reaction；Reacted instead
Answering liquid (8) to enter oil water separator (22) and carry out oil-water separation, the aqueous portion (10) after separation backs into reaction
Still (19)；Oil phase part (9) is intermediate products dimethyl benzyl alcohol.
Below by embodiment, the invention will be further elaborated, but is not limited only to the present embodiment.
Detailed description of the invention
[comparative example 1]
Prior art use intermittently operated, cumyl peroxide device when in reducing solution the content of CHP be 0.2wt%≤
During CHP≤2wt%, stopping the stirring in reduction reaction still, therefore reduction reaction is the most abundant.Additionally the reduction reaction time is
0.5～8h, quiescent settling disengaging time is 1h, and after reaction required time and reaction, needed for quiescent settling, the intermittent time is longer, behaviour
Make the most steady.
[embodiment 1]
As a example by 200 tons/year of cumyl peroxide DCP commercial plants of production scale, the present invention is used efficiently to produce CA
Method, 4 reduction reaction stills of series arrangement, adverse current put into material mol ratio be CHP:Na2S=4:1.1, enters
The CHP concentration of each reduction reaction still is 48wt%, 32wt%, 18wt%, 8wt%, each reduction reaction still operation temperature
Degree is 68 DEG C, 68 DEG C, 67 DEG C, 67 DEG C, and operation pressure is normal pressure, each reduction reaction still time of staying is 2.2h, 2.3h,
2.3h、2.2h.Hereby it is achieved that efficient, continuous, the quiet run of reduction reaction, and by last 1 reduction reaction still
The concentration of end CHP is reduced to below 0.50wt%.
[embodiment 2]
According to the condition described in embodiment 1, only the production scale of DCP commercial plant changes 1000 tons/year into, uses this
The method of bright continuous production CA, it is achieved that efficient, continuous, the quiet run of reduction reaction, and by anti-for last 1 reduction
The concentration answering bottom CHP is reduced to below 0.45wt%.
[embodiment 3]
According to the condition described in embodiment 1, only the production scale of DCP commercial plant changes 20,000 tons/year into, uses this
The method of bright continuous production CA, it is achieved that efficient, continuous, the quiet run of reduction reaction, and by anti-for last 1 reduction
The concentration answering bottom CHP is reduced to below 0.25wt%.
[embodiment 4]
According to the condition described in embodiment 1, only the production scale of DCP commercial plant changes 60,000 tons/year into, uses this
The method of bright continuous production CA, it is achieved that efficient, continuous, the quiet run of reduction reaction, and by anti-for last 1 reduction
The concentration answering bottom CHP is reduced to below 0.25wt%.
[embodiment 5]
According to the condition described in embodiment 3, the production scale of DCP commercial plant is still 20,000 tons/year, only equipment number of units
Reducing, operating condition changes.2 reduction reaction stills of series arrangement, it is CHP:Na that adverse current puts into the mol ratio of material2S=4:
1.2, the CHP concentration entering each reduction reaction still is 45wt%, 17wt%, each reduction reaction still operation temperature is 70 DEG C,
69 DEG C, operation pressure is normal pressure, and each reduction reaction still time of staying is 3.8h, 3.8h.Thus, the present invention is used to give birth to continuously
The method producing CA, it is achieved that efficient, continuous, the quiet run of reduction reaction, and by last 1 reduction reaction bottom CHP
Concentration be reduced to below 0.60wt%.
[embodiment 6]
According to the condition described in embodiment 3, the production scale of DCP commercial plant is still 20,000 tons/year, and only equipment number of units increases
Adding, operating condition changes.8 reduction reaction stills of series arrangement, it is CHP:Na that adverse current puts into the mol ratio of material2S=4:
1.0, the CHP concentration entering each reduction reaction still is 50wt%, 39wt%, 31wt%, 24wt%, 18wt%,
12wt%, 7wt%, 3wt%, each reduction reaction still operation temperature is 66 DEG C, 66 DEG C, 66 DEG C, 66 DEG C, 65 DEG C, 65 DEG C,
65 DEG C, 65 DEG C, operation pressure is normal pressure, each reduction reaction still time of staying is 2.0h, 2.0h, 2.1h, 2.1h, 2.1h,
2.1h、2.0h、2.0h.Thus, the method that the present invention produces CA continuously is used, it is achieved that efficient, the company of reduction reaction
Continuous, quiet run, and the concentration of last 1 reduction reaction bottom CHP is reduced to below 0.10wt%.
Claims (2)
1. the method producing cumyl peroxide DCP intermediate products, by 2～8 stirred autoclave series connection,
The bottom outlet of each stirred autoclave is respectively provided with oil water separator, in addition to last oil water separator,
The isolated oil phase material of other oil water separator enters next stirred autoclave from top；Oxidation solution peroxidating
Hydrogen isopropylbenzene raw material enters from the top of first stirred autoclave, and reducing solution sodium sulfide stirs from last
The top of reactor enters, and first isolated aqueous phase of oil water separator is discharged as reducing waste water, last
The isolated oil phase of individual oil water separator is intermediate products dimethyl benzyl alcohol, and last oil water separator is isolated
Aqueous phase return a upper stirred autoclave top, wherein, enter the 1st stirred autoclave oxidation solution
Middle cumyl hydroperoxide concentration range is 45～50wt%, and reduction reaction temperature is 65～70 DEG C, and reduction is anti-
Answering pressure is normal pressure, and the time of staying is 2.0～3.8h, when oxidation solution cumyl hydroperoxide reduction reaction terminates
After, last 1 reduction reaction bottom cumyl hydroperoxide lowering of concentration is between 0.10～0.60wt%.
The most according to claim 1, the method producing cumyl peroxide DCP intermediate products, its feature exists
In cumyl hydroperoxide and Na2S molar ratio is 4:1.0～1.2.
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| CN107382663A (en) * | 2017-07-26 | 2017-11-24 | 江苏道明化学有限公司 | A kind of improved method of the production technology automatic control equipment of Bian alcohol |
| CN107382664A (en) * | 2017-07-26 | 2017-11-24 | 江苏道明化学有限公司 | A kind of improved method of reduction reaction |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1093352A (en) * | 1993-03-31 | 1994-10-12 | 兰州大学 | The manufacture method of 2-phenyl-2-propyl alcohol |
| CN102911014A (en) * | 2011-08-04 | 2013-02-06 | 中国石油化工股份有限公司 | Di-(2-hydroxyl isopropyl) benzene production method |
| CN103772141A (en) * | 2012-10-19 | 2014-05-07 | 中国石油化工集团公司 | Hydroperoxide reduction reaction technology |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7557252B2 (en) * | 2006-02-17 | 2009-07-07 | Sumitomo Chemical Company, Limited | Process for producing dihydroxybenzene and diisopropylbenzendicarbinol |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1093352A (en) * | 1993-03-31 | 1994-10-12 | 兰州大学 | The manufacture method of 2-phenyl-2-propyl alcohol |
| CN102911014A (en) * | 2011-08-04 | 2013-02-06 | 中国石油化工股份有限公司 | Di-(2-hydroxyl isopropyl) benzene production method |
| CN103772141A (en) * | 2012-10-19 | 2014-05-07 | 中国石油化工集团公司 | Hydroperoxide reduction reaction technology |
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