CN104909991A - Method for continuously producing dicumyl peroxide (DCP) intermediate product - Google Patents
Method for continuously producing dicumyl peroxide (DCP) intermediate product Download PDFInfo
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- CN104909991A CN104909991A CN201510231086.3A CN201510231086A CN104909991A CN 104909991 A CN104909991 A CN 104909991A CN 201510231086 A CN201510231086 A CN 201510231086A CN 104909991 A CN104909991 A CN 104909991A
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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
The invention relates to a method for continuously producing a DCP intermediate product. The problems of intermittent operation, long reaction and standing layering time and poor production stability in the prior art are mainly solved in the invention. The method for continuously producing the DCP intermediate product comprises the following steps: at least two stirring reaction kettles are serially connected, an oil-water separator is arranged between adjacent serially connected stirring reaction kettles, a CHP raw material and a reducing agent which is an aqueous solution of sodium sulfide enter the first stirring reaction kettle from the top, materials discharged from the bottoms of the stirring reaction kettles enter oil-water separators, oil phases and water phases separated by the oil-water separators sequentially enter a next reaction kettle according to a certain ratio, and a material discharged from the bottom of the last one stirring reaction kettle enters an oil-water collector. The method adopting the above technical scheme well solves the problems, and can be used in the production of the DCP intermediate product.
Description
Technical field
The present invention relates to a kind of method of continuous seepage dicumyl peroxide DCP intermediates.
Background technology
Industrial usual production DCP technique take isopropyl benzene as raw material, hydrogen phosphide cumene CHP is changed into by cumene oxidation reaction, and part CHP is generated intermediates by reduction reaction---DMCA, then DMCA and rest part CHP carries out condensation reaction and generates DCP, then obtains DCP product through crystallizing and drying.Wherein DCP reduction reaction mainly comprises the following steps: will put in reduction reaction still containing CHP oxidation solution and sodium sulfide solution, and carry out reduction reaction and generate DMCA, reaction principle is as follows:
CN 1051541C relates to the manufacture method of 2-phenyl-2-propyl alcohol, disclose the method manufacturing 2-phenyl-2-propyl alcohol with water-soluble sulfide reduction isopropyl benzene hydroperoxide CHP, the usage quantity disclosing MxS is that itself and the determined theoretical amount of CHP reaction equation are to 200% of theoretical amount, temperature of reaction is 0 ~ 150 DEG C, and the reaction times is 0.5 ~ 8h.Reacted rear stratification, point sub-cloud aqueous phase, organic phase washed with water is intermediates when the pH value of aqueous phase is 6 ~ 8.
CN 104211628A relates to production unit for the production of the reduction reaction of dicumyl peroxide and method, disclose production unit and comprise oxidation liquid bath, reductant solution Preparation tank, reduction kettle and controller, controller is cut valve soon with reduction kettle agitator electric motor, the temperature sensor measuring reduction reaction temperature, the pressure transmitter detecting reduction kettle circulating cooling water pressure and reduction kettle recirculated cooling water and is electrically connected.When reductive agent and oxidation solution react in reduction kettle, controller judges that electric motor stops operating or reduction kettle reduction reaction temperature is greater than reduction kettle reduction reaction temperature set(ting)value or reduction kettle circulating cooling water pressure is less than reduction kettle recirculated cooling water pressure set points and extends setting-up time, then automatically cut off motor power, automatically closedown oxidation solution feed valve and automatically open reduction kettle recirculated cooling water and cut valve soon.This chain control of controller, effectively ensure that the safety of dicumyl peroxide reduction reaction is carried out.This patent of invention adopts the reduction reaction process of periodical operation, in liquid to be restored, the content of CHP is after 0.2wt%≤CHP≤2wt%, stop the stirring in reduction reaction still, quiescent settling is separated about 1h, and stratification oil phase is the intermediates DMCA reduced liquid obtained.
CHP oxidation solution in CN 1051541C and CN 104211628A and sodium sulphite reductive agent carry out reduction reaction, all adopt the reactor of periodical operation, there is the intermittent time needed for reaction required time and the rear quiescent settling of reaction longer, operation is steady not, the problems such as continuous seepage ability.
The present invention solves this problem targetedly.
Summary of the invention
Technical problem to be solved by this invention adopts periodical operation, reaction and the stratification time is long, production stability is poor problem in prior art, provides a kind of method of new continuous seepage dicumyl peroxide DCP intermediates.The method is used for, in the production of dicumyl peroxide DCP intermediates, having operate continuously, reaction and the stratification time is short, production stability is good advantage.
For solving the problem, the technical solution used in the present invention is as follows: a kind of method of continuous seepage dicumyl peroxide DCP intermediates, at least two stirred autoclaves are connected, between the stirred autoclave of each series connection, water-and-oil separator is set, oxidation solution CHP raw material and reductive agent sodium sulfide solution enter stirred autoclave from the top of first stirred autoclave, stirred autoclave bottoms material enters water-and-oil separator, water-and-oil separator top oil phase and bottom aqueous phase rate of discharge are controlled by flow director respectively, the oil phase separated and aqueous phase enter next reactor by a certain percentage successively, last stirred autoclave bottoms material enters profit collector, described intermediates DMCA flows out from profit collector top, reducing waste water flows out bottom profit collector.
In technique scheme, preferably, utilize recirculated cooling water or circulating hot water to carry out heating or cool to control reduction reaction temperature by built-in coil pipe in described each stirred autoclave, reduction reaction temperature is 65 ~ 70 DEG C, and reduction reaction pressure is normal pressure.
In technique scheme, preferably, stirred autoclave arranges level gauging instrument, observe level condition in oxidation solution inlet amount accumulated value and reduction kettle.
In technique scheme, preferably, entering CHP concentration range in the oxidation solution of first stirred autoclave described in is 45 ~ 50wt%, CHP and Na
2the mol ratio of S is 4:1.0 ~ 1.2.
In technique scheme, preferably, the residence time of material span of control of each stirred autoclave is 2.0 ~ 4.8h.
In technique scheme, preferably, the CHP concentration span of control bottom last stirred autoclave described is between 0.10 ~ 0.80wt%.
In technique scheme, preferably, the quantity of the stirred autoclave of described series connection is 2 ~ 6.
In technique scheme, preferably, the oil phase separated of water-and-oil separator and aqueous phase are that 1:1.5 ~ 4.0 enter next reactor successively with mass ratio.
The atmospheric agitation reactor of more than 2 and 2 is connected by the present invention, effectively reduces the reaction times needed for reduction reaction operation and reaction quiescent settling oil-water separation time.Reactor is sent into by DCP device oxidation solution CHP raw material and reductive agent sodium sulfide solution also being flowed, achieve efficient, continuous, the quiet run of reduction reaction, effectively shorten the time needed for reduction reaction operation, and CHP concentration at the bottom of last 1 reduction kettle is reduced to 0.10 ~ 0.80wt%, make reduction reaction more abundant, achieve good technique effect.
Below by embodiment, the invention will be further elaborated, but be not limited only to the present embodiment.
Embodiment
[comparative example 1]
Prior art adopts periodical operation, the reduction reaction time of dicumyl peroxide DCP device is 0.5 ~ 8h, in liquid to be restored, the content of CHP is after 0.2 ~ 2wt%, stop the stirring in reduction reaction still, quiescent settling is separated about 1h, after reacting required time and reacting, needed for quiescent settling, the intermittent time is longer, operates steady not.
[embodiment 1]
For industrial scale 200 tons/year of dicumyl peroxide DCP full scale plants, adopt the method for continuous seepage DMCA of the present invention, by raw material flow direction series arrangement 4 reduction reaction stills, atmospheric operation, and stream drops into the mol ratio CHP:Na of material
2s=4:1.1, the CHP concentration entering 4 reduction reaction stills is followed successively by 48wt%, 32wt%, 18wt%, 8wt%, reduction reaction still service temperature controls to be 66 DEG C, 67 DEG C, 68 DEG C, 69 DEG C successively, each reactor residence time controls as 2.8h, 3.0h, 3.4h, 4.2h successively, and the oil phase that a upper water-and-oil separator is separated and aqueous phase are that 1:3.3 enters next reactor successively with mass ratio.Thus, achieve efficient, continuous, the quiet run of reduction reaction, and the concentration of CHP at the bottom of last 1 reduction reaction still is reduced to below 0.55wt%.
[embodiment 2]
According to the condition described in embodiment 1, only the industrial scale of DCP full scale plant changes 20,000 tons/year into, adopt the method for continuous seepage DMCA of the present invention, achieve efficient, continuous, the quiet run of reduction reaction, and the concentration of CHP at the bottom of last 1 reduction reaction still is reduced to below 0.25wt%.
[embodiment 3]
According to the condition described in embodiment 1, only the industrial scale of DCP full scale plant changes 60,000 tons/year into, adopt the method for continuous seepage DMCA of the present invention, achieve efficient, continuous, the quiet run of reduction reaction, and the concentration of CHP at the bottom of last 1 reduction reaction still is reduced to below 0.25wt%t.
[embodiment 4]
According to the condition described in embodiment 2, the industrial scale of DCP full scale plant is still 20,000 tons/year, and only operational condition changes, and adopts the method for continuous seepage DMCA of the present invention, by raw material flow direction series arrangement 4 reduction reaction stills, and stream drops into the mol ratio CHP:Na of material
2s=4:1.0, the CHP concentration entering 4 reduction reaction stills is followed successively by 45wt%, 28wt%, 15wt%, 6wt%, reduction reaction still service temperature controls to be 65 DEG C, 66 DEG C, 67 DEG C, 68 DEG C successively, each reactor residence time controls as 2.0h, 2.6h, 3.0h, 3.8h successively, and the oil phase that a upper water-and-oil separator is separated and aqueous phase are that 1:1.5 enters next reactor successively with mass ratio.Thus, achieve efficient, continuous, the quiet run of reduction reaction, and the concentration of CHP at the bottom of last 1 reduction reaction still is reduced to below 0.80wt%t.
[embodiment 5]
According to the condition described in embodiment 2, the industrial scale of DCP full scale plant is still 20,000 tons/year, only operational condition changes, reactor number of units reduces, adopt the method for continuous seepage DMCA of the present invention, by raw material flow direction series arrangement 2 reduction reaction stills, and stream drops into the mol ratio CHP:Na of material
2s=4:1.2, the CHP concentration entering 2 reduction reaction stills is followed successively by 50wt%, 20wt%, reduction reaction still service temperature controls to be 69 DEG C, 70 DEG C successively, each reactor residence time controls as 4.6h, 4.8h successively, and the oil phase that a upper water-and-oil separator is separated and aqueous phase are that 1:4.0 enters next reactor successively with mass ratio.Thus, achieve efficient, continuous, the quiet run of reduction reaction, and the concentration of CHP at the bottom of last 1 reduction reaction still is reduced to below 0.80wt%t.
[embodiment 6]
According to the condition described in embodiment 2, the industrial scale of DCP full scale plant is still 20,000 tons/year, only reactor number of units increases, the corresponding change of operational condition, adopt the method for continuous seepage DMCA of the present invention, by raw material flow direction series arrangement 5 reduction reaction stills, and stream drops into the mol ratio CHP:Na of material
2s=4:1.1, the CHP concentration entering 5 reduction reaction stills is followed successively by 48wt%, 36wt%, 24wt%, 16wt%, 6wt%, reduction reaction still service temperature controls to be 66,67 DEG C, 67 DEG C, 68 DEG C, 69 DEG C successively, each reactor residence time controls as 2.6h, 2.8h, 3.1h, 3.4h, 3.6h successively, and the oil phase that a upper water-and-oil separator is separated and aqueous phase are that 1:3.3 enters next reactor successively with mass ratio.Thus, achieve efficient, continuous, the quiet run of reduction reaction, and the concentration of CHP at the bottom of last 1 reduction reaction still is reduced to below 0.15wt%.
[embodiment 7]
According to the condition described in embodiment 2, the industrial scale of DCP full scale plant is still 20,000 tons/year, only reactor number of units increases further, operational condition is corresponding change also, adopt the method for continuous seepage DMCA of the present invention, by raw material flow direction series arrangement 6 reduction reaction stills, and stream drops into the mol ratio CHP:Na of material
2s=4:1.1, the CHP concentration entering 6 reduction reaction stills is followed successively by 48wt%, 38wt%, 28wt%, 18wt%, 10wt%, 6wt%, reduction reaction still service temperature controls to be 66 DEG C, 67 DEG C, 67 DEG C, 68 DEG C, 68 DEG C, 69 DEG C successively, each reactor residence time controls as 2.4h, 2.6h, 2.8h, 3.0h, 3.2h, 3.4h successively, and the oil phase that a upper water-and-oil separator is separated and aqueous phase are that 1:3.3 enters next reactor successively with mass ratio.Thus, achieve efficient, continuous, the quiet run of reduction reaction, and the concentration of CHP at the bottom of last 1 reduction reaction still is reduced to below 0.10wt%.
Claims (8)
1. the method for continuous seepage dicumyl peroxide DCP intermediates, at least two stirred autoclaves are connected, between the stirred autoclave of each series connection, water-and-oil separator is set, oxidation solution CHP raw material and reductive agent sodium sulfide solution enter stirred autoclave from the top of first stirred autoclave, stirred autoclave bottoms material enters water-and-oil separator, water-and-oil separator top oil phase and bottom aqueous phase rate of discharge are controlled by flow director respectively, the oil phase separated and aqueous phase enter next reactor by a certain percentage successively, last stirred autoclave bottoms material enters profit collector, described intermediates DMCA flows out from profit collector top, reducing waste water flows out bottom profit collector.
2. the method for continuous seepage dicumyl peroxide DCP intermediates according to claim 1, it is characterized in that utilizing recirculated cooling water or circulating hot water to carry out heating or cool to control reduction reaction temperature by built-in coil pipe in described each stirred autoclave, reduction reaction temperature is 65 ~ 70 DEG C, and reduction reaction pressure is normal pressure.
3. the method for continuous seepage dicumyl peroxide DCP intermediates according to claim 1, is characterized in that on stirred autoclave, arrange level gauging instrument, observes level condition in oxidation solution inlet amount accumulated value and reduction kettle.
4. the method for continuous seepage dicumyl peroxide DCP intermediates according to claim 1, entering CHP concentration range in the oxidation solution of first stirred autoclave described in it is characterized in that is 45 ~ 50wt%, CHP and Na
2the mol ratio of S is 4:1.0 ~ 1.2.
5. the method for continuous seepage dicumyl peroxide DCP intermediates according to claim 1, is characterized in that the residence time of material span of control of each stirred autoclave is 2.0 ~ 4.8h.
6. the method for continuous seepage dicumyl peroxide DCP intermediates according to claim 1, is characterized in that the CHP concentration span of control bottom last stirred autoclave described is between 0.10 ~ 0.80wt%.
7. the method for continuous seepage dicumyl peroxide DCP intermediates according to claim 1, is characterized in that the quantity of the stirred autoclave of described series connection is 2 ~ 6.
8. the method for continuous seepage dicumyl peroxide DCP intermediates according to claim 1, is characterized in that the oil phase that described water-and-oil separator is separated and aqueous phase are that 1:1.5 ~ 4.0 enter next reactor successively with mass ratio.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| 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 |
Citations (5)
| 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 |
| US20070197838A1 (en) * | 2006-02-17 | 2007-08-23 | Sumitomo Chemical Company, Limited | Process for producing dihydroxybenzene and diisopropylbenzendicarbinol |
| 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 |
| CN103771578A (en) * | 2012-10-19 | 2014-05-07 | 中国石油化工集团公司 | Hydroperoxide reduction production technology |
| CN103772141A (en) * | 2012-10-19 | 2014-05-07 | 中国石油化工集团公司 | Hydroperoxide reduction reaction technology |
-
2015
- 2015-05-07 CN CN201510231086.3A patent/CN104909991B/en active Active
Patent Citations (5)
| 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 |
| US20070197838A1 (en) * | 2006-02-17 | 2007-08-23 | Sumitomo Chemical Company, Limited | Process for producing dihydroxybenzene and diisopropylbenzendicarbinol |
| 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 |
| CN103771578A (en) * | 2012-10-19 | 2014-05-07 | 中国石油化工集团公司 | Hydroperoxide reduction production technology |
| CN103772141A (en) * | 2012-10-19 | 2014-05-07 | 中国石油化工集团公司 | Hydroperoxide reduction reaction technology |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| 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 |
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| CN104909991B (en) | 2017-07-21 |
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