CN107652164A - A kind of production method of diisopropylbenzene (DIPB) alcohol - Google Patents
A kind of production method of diisopropylbenzene (DIPB) alcohol Download PDFInfo
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- CN107652164A CN107652164A CN201710945963.2A CN201710945963A CN107652164A CN 107652164 A CN107652164 A CN 107652164A CN 201710945963 A CN201710945963 A CN 201710945963A CN 107652164 A CN107652164 A CN 107652164A
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- dipb
- diisopropylbenzene
- oxidation
- alcohol
- oxidizing tower
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- 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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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C407/00—Preparation of peroxy compounds
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- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a kind of production method of diisopropylbenzene (DIPB) alcohol,After diisopropylbenzene (DIPB) and the diisopropylbenzene (DIPB) of recovery are mixed,Oxidizing tower is conveyed into by pump,Add liquid caustic soda solution,Open one at the top of oxidizing tower,The cooling water of secondary condenser,Open oxidizing tower circulating pump,Open the steam valve of oxidizing tower bottom heater,Material in oxidizing tower is heated by aoxidizing external circulation heater,Open compressed air valve simultaneously,Oxidation external circulation heat exchanging device heated condition is switched into the state of cooling afterwards,Progressively establish one tower of oxidation and aoxidize the continuous feed of two towers,Continuous oxidation,Continuous discharge,The oxidation solution of generation carries out heterogeneous reduction reaction with reducing agent sodium sulfite,Reducing solution is through deionised water,Cooling,Solid-liquid is carried out using centrifuge,Solid is crude product diisopropylbenzene (DIPB) alcohol,It is transported to again in recrystallization kettle,Add diisopropylbenzene (DIPB) stirring at low speed,Recrystallized,Centrifugation is again passed by afterwards obtains fine work diisopropylbenzene (DIPB) alcohol.
Description
Technical field
The invention belongs to chemical assistant preparation field, and in particular to a kind of production method of diisopropylbenzene (DIPB) alcohol.
Background technology
Commercial scale DCP is using isopropylbenzene as raw material, and hydrogen peroxide isopropyl is changed into by cumene oxidation reaction
Benzene CHP, and part CHP is generated into dimethyl benzyl alcohol DMCA by reduction reaction, then DMCA and another part CHP is condensed
Reaction generation DCP, crystal refining processing is finally carried out to DCP products and obtains final products.
The content of the invention
Goal of the invention：In order to solve the deficiencies in the prior art, the invention provides a kind of production method of diisopropylbenzene (DIPB) alcohol,
Reaction principle：
Technical scheme：A kind of production method of diisopropylbenzene (DIPB) alcohol, comprises the following steps：It is the two different of 92-98% by content
After propyl benzene and the diisopropylbenzene (DIPB) mixing that the content of recovery is 70-80%, oxidizing tower is conveyed into by pump, adds 2-3% liquid
Aqueous slkali, the cooling water of I and II condenser at the top of oxidizing tower is opened, open oxidizing tower circulating pump, open the heating of oxidizing tower bottom
The steam valve of device, material in oxidizing tower is heated by aoxidizing external circulation heater, while opens compressed air valve,
Oxidation external circulation heat exchanging device heated condition is switched into the state of cooling after temperature to be heated to 85-95 DEG C, progressively establishes oxidation
One tower and the oxidation continuous feed of two towers, continuous oxidation, continuous discharge, oxidation solution discharge concentration are about 20-24%, oxidation reaction
During control oxidation tower pressure interior force be about 2.8-3.1 kilograms, between temperature is about 90-100 DEG C, compressed air is continuous bubbling
Add, oxidation solution and temperature of the reducing agent sodium sulfite at 75-85 DEG C of generation carry out heterogeneous reduction reaction, and reducing solution is through departing from
Sub- water washing, is cooled to 25-35 DEG C, carries out solid-liquid using centrifuge, solid is crude product diisopropylbenzene (DIPB) alcohol；Crude product diisopropylbenzene (DIPB)
Alcohol is transported in recrystallization kettle again, is added appropriate 92-98% diisopropylbenzene (DIPB) stirring at low speed, is recrystallized, passed through again afterwards
Cross centrifugation and obtain fine work diisopropylbenzene (DIPB) alcohol.
As optimization：The diisopropylbenzene (DIPB) that content is more than 95% and the diisopropylbenzene (DIPB) that the content of recovery is 75% are mixed.
As optimization：Oxidation solution discharge concentration is about 22%, and control oxidation tower pressure interior force is about 2.9 in oxidation reaction process
Kilogram, temperature is about 95 DEG C.
Beneficial effect：In the present invention, diisopropylbenzene (DIPB) alcohol is the main life of crosslinking agent two (t-butylperoxyisopropyl) benzene
Raw material is produced, obtained product performance is as follows：Outward appearance：White powder, fusing point：114~138 DEG C, boiling point：270 DEG C, smell：Nothing, heap
Product density：500kg/m3, content：80~95%.
Embodiment
The technical scheme in the embodiment of the present invention will be clearly and completely described below, so that the technology of this area
Personnel can be better understood from advantages and features of the invention, so as to make apparent boundary to protection scope of the present invention
It is fixed.Embodiment described in the invention is only part of the embodiment of the present invention, rather than whole embodiments, based on the present invention
In embodiment, the every other implementation that those of ordinary skill in the art are obtained on the premise of creative work is not made
Example, belongs to the scope of protection of the invention.
Embodiment 1
A kind of production method of diisopropylbenzene (DIPB) alcohol, comprises the following steps：By diisopropylbenzene (DIPB) of the content for 92% and recovery
After the diisopropylbenzene (DIPB) mixing that content is 70%, oxidizing tower is conveyed into by pump, adds 2% liquid caustic soda solution, opens oxidizing tower
The cooling water of top I and II condenser, oxidizing tower circulating pump is opened, open the steam valve of oxidizing tower bottom heater, pass through
Oxidation external circulation heater heats to material in oxidizing tower, while opens compressed air valve, to be heated to 85 DEG C of temperature
Oxidation external circulation heat exchanging device heated condition is switched into the state of cooling after degree, one tower of oxidation is progressively established and aoxidizes the continuous of two towers
Charging, continuous oxidation, continuous discharge, oxidation solution discharge concentration are about 20%, control oxidation tower pressure interior force in oxidation reaction process
About 2.8 kilograms, temperature is about 90 DEG C, and compressed air adds for continuous bubbling, oxidation solution and the reducing agent sodium sulfite of generation
Heterogeneous reduction reaction is carried out in 75 DEG C of temperature, reducing solution is cooled to 25 DEG C, consolidated using centrifuge through deionised water
Liquid, solid are crude product diisopropylbenzene (DIPB) alcohol；Crude product diisopropylbenzene (DIPB) alcohol is transported in recrystallization kettle again, and the two of addition appropriate 92% are different
Propyl benzene stirring at low speed, is recrystallized, and is again passed by centrifugation afterwards and is obtained fine work diisopropylbenzene (DIPB) alcohol.
Embodiment 2
A kind of production method of diisopropylbenzene (DIPB) alcohol, comprises the following steps：By diisopropylbenzene (DIPB) of the content for 98% and recovery
After the diisopropylbenzene (DIPB) mixing that content is 80%, oxidizing tower is conveyed into by pump, adds 3% liquid caustic soda solution, opens oxidizing tower
The cooling water of top I and II condenser, oxidizing tower circulating pump is opened, open the steam valve of oxidizing tower bottom heater, pass through
Oxidation external circulation heater heats to material in oxidizing tower, while opens compressed air valve, to be heated to 95 DEG C of temperature
Oxidation external circulation heat exchanging device heated condition is switched into the state of cooling after degree, one tower of oxidation is progressively established and aoxidizes the continuous of two towers
Charging, continuous oxidation, continuous discharge, oxidation solution discharge concentration are about 24%, control oxidation tower pressure interior force in oxidation reaction process
About 3.1 kilograms, between temperature is about 100 DEG C, compressed air adds for continuous bubbling, oxidation solution and the reducing agent sulfurous of generation
Sour sodium carries out heterogeneous reduction reaction in 85 DEG C of temperature, and reducing solution is cooled to 35 DEG C, entered using centrifuge through deionised water
Row solid-liquid, solid are crude product diisopropylbenzene (DIPB) alcohol；Crude product diisopropylbenzene (DIPB) alcohol is transported in recrystallization kettle again, adds appropriate 98%
Diisopropylbenzene (DIPB) stirring at low speed, is recrystallized, and is again passed by centrifugation afterwards and is obtained fine work diisopropylbenzene (DIPB) alcohol.
Embodiment 3
A kind of production method of diisopropylbenzene (DIPB) alcohol, comprises the following steps：By diisopropylbenzene (DIPB) of the content for 95% and recovery
After the diisopropylbenzene (DIPB) mixing that content is 75%, oxidizing tower is conveyed into by pump, adds 2.5% liquid caustic soda solution, opens oxidation
The cooling water of top of tower I and II condenser, oxidizing tower circulating pump is opened, open the steam valve of oxidizing tower bottom heater, led to
Peroxidating external circulation heater heats to material in oxidizing tower, while opens compressed air valve, to be heated to 90 DEG C
Oxidation external circulation heat exchanging device heated condition is switched into the state of cooling after temperature, progressively one tower of oxidation is established and aoxidizes the company of two towers
Continuous charging, continuous oxidation, continuous discharge, oxidation solution discharge concentration is about 22%, and oxidizing tower internal pressure is controlled in oxidation reaction process
Power is about 2.9 kilograms, and between temperature is about 95 DEG C, compressed air adds for continuous bubbling, and the oxidation solution and reducing agent of generation are sub-
Sodium sulphate carries out heterogeneous reduction reaction in 80 DEG C of temperature, and reducing solution is cooled to 30 DEG C, utilizes centrifuge through deionised water
Solid-liquid is carried out, solid is crude product diisopropylbenzene (DIPB) alcohol；Crude product diisopropylbenzene (DIPB) alcohol is transported in recrystallization kettle again, adds appropriate 95%
Diisopropylbenzene (DIPB) stirring at low speed, recrystallized, again pass by centrifugation afterwards and obtain fine work diisopropylbenzene (DIPB) alcohol.
In the present invention, diisopropylbenzene (DIPB) alcohol is the main production raw material of crosslinking agent two (t-butylperoxyisopropyl) benzene, is obtained
The product performance arrived is as follows：Outward appearance：White powder, fusing point：114~138 DEG C, boiling point：270 DEG C, smell：Nothing, bulk density：
500kg/m3, content：80~95%.
Claims (3)
- A kind of 1. production method of diisopropylbenzene (DIPB) alcohol, it is characterised in that：Comprise the following steps：It is the two different of 92-98% by content After propyl benzene and the diisopropylbenzene (DIPB) mixing that the content of recovery is 70-80%, oxidizing tower is conveyed into by pump, adds 2-3% liquid Aqueous slkali, the cooling water of I and II condenser at the top of oxidizing tower is opened, open oxidizing tower circulating pump, open the heating of oxidizing tower bottom The steam valve of device, material in oxidizing tower is heated by aoxidizing external circulation heater, while opens compressed air valve, Oxidation external circulation heat exchanging device heated condition is switched into the state of cooling after temperature to be heated to 85-95 DEG C, progressively establishes oxidation One tower and the oxidation continuous feed of two towers, continuous oxidation, continuous discharge, oxidation solution discharge concentration are about 20-24%, oxidation reaction During control oxidation tower pressure interior force be about 2.8-3.1 kilograms, between temperature is about 90-100 DEG C, compressed air is continuous bubbling Add, oxidation solution and temperature of the reducing agent sodium sulfite at 75-85 DEG C of generation carry out heterogeneous reduction reaction, and reducing solution is through departing from Sub- water washing, is cooled to 25-35 DEG C, carries out solid-liquid using centrifuge, solid is crude product diisopropylbenzene (DIPB) alcohol；Crude product diisopropylbenzene (DIPB) Alcohol is transported in recrystallization kettle again, is added appropriate 92-98% diisopropylbenzene (DIPB) stirring at low speed, is recrystallized, passed through again afterwards Cross centrifugation and obtain fine work diisopropylbenzene (DIPB) alcohol.
- 2. the production method of diisopropylbenzene (DIPB) alcohol according to claim 1, it is characterised in that：By content be more than 95% two Isopropylbenzene and the diisopropylbenzene (DIPB) that the content of recovery is 75% mix.
- 3. the production method of diisopropylbenzene (DIPB) alcohol according to claim 1, it is characterised in that：Oxidation solution discharge concentration is about 22%, control oxidation tower pressure interior force is about 2.9 kilograms in oxidation reaction process, and temperature is about 95 DEG C.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710945963.2A CN107652164A (en) | 2017-10-12 | 2017-10-12 | A kind of production method of diisopropylbenzene (DIPB) alcohol |
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| CN201710945963.2A CN107652164A (en) | 2017-10-12 | 2017-10-12 | A kind of production method of diisopropylbenzene (DIPB) alcohol |
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| CN107652164A true CN107652164A (en) | 2018-02-02 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115403446A (en) * | 2022-09-01 | 2022-11-29 | 山东阳谷华泰化工股份有限公司 | Synthetic method of alpha, alpha' -dihydroxy-1, 3-diisopropylbenzene |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3911020A (en) * | 1969-07-25 | 1975-10-07 | Goodyear Tire & Rubber | Process for the preparation of dialkylbenzene dihydroperoxide |
| CN103159592A (en) * | 2011-12-09 | 2013-06-19 | 中国石油化工集团公司 | Production method for bis-(2-hydroxyl isopropyl)benzene |
| CN103396292A (en) * | 2013-08-09 | 2013-11-20 | 宁波朝日硅材料有限公司 | Method for industrially producing A,A'-dihydroxy-1,3-diisobutylbenzene |
| CN104418706A (en) * | 2013-09-10 | 2015-03-18 | 中国石油化工集团公司 | Method for refining bi(2-hydroxyl isopropyl) benzene |
-
2017
- 2017-10-12 CN CN201710945963.2A patent/CN107652164A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3911020A (en) * | 1969-07-25 | 1975-10-07 | Goodyear Tire & Rubber | Process for the preparation of dialkylbenzene dihydroperoxide |
| CN103159592A (en) * | 2011-12-09 | 2013-06-19 | 中国石油化工集团公司 | Production method for bis-(2-hydroxyl isopropyl)benzene |
| CN103396292A (en) * | 2013-08-09 | 2013-11-20 | 宁波朝日硅材料有限公司 | Method for industrially producing A,A'-dihydroxy-1,3-diisobutylbenzene |
| CN104418706A (en) * | 2013-09-10 | 2015-03-18 | 中国石油化工集团公司 | Method for refining bi(2-hydroxyl isopropyl) benzene |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115403446A (en) * | 2022-09-01 | 2022-11-29 | 山东阳谷华泰化工股份有限公司 | Synthetic method of alpha, alpha' -dihydroxy-1, 3-diisopropylbenzene |
| CN115403446B (en) * | 2022-09-01 | 2023-12-29 | 山东阳谷华泰化工股份有限公司 | Synthesis method of alpha, alpha' -dihydroxyl-1, 3-diisopropylbenzene |
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Application publication date: 20180202 |