CN107382806A - A kind of production method of cumyl peroxide - Google Patents
A kind of production method of cumyl peroxide Download PDFInfo
- Publication number
- CN107382806A CN107382806A CN201710615569.2A CN201710615569A CN107382806A CN 107382806 A CN107382806 A CN 107382806A CN 201710615569 A CN201710615569 A CN 201710615569A CN 107382806 A CN107382806 A CN 107382806A
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- oxidation solution
- isopropylbenzene
- cumyl
- water
- reaction
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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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- 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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- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a kind of production method of cumyl peroxide, concrete operations are as follows：(1) pretreatment of raw material；(2) cumyl hydroperoxide is generated；(3) cumyl hydroperoxide purifies；(4) intermediate product Bian alcohol is generated；(5) Bian alcohol refines；(6) condensation reaction.The present invention solves the weak point that DCP is produced in traditional handicraft, shortens production procedure, saves production cost, reduces environmental pollution.
Description
Technical field
The invention belongs to chemical field, and in particular to a kind of production method of cumyl peroxide.
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.
In DCP production technologies, conventional process techniques exist DCP is selectively low, yield is low, technological parameter fluctuation is huge,
The problem of being difficult to heavy industrialization application.
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 of cumyl peroxide
Method.
Technical scheme：A kind of production method of cumyl peroxide, concrete operations are as follows：
(1) pretreatment of raw material：It is 1 by weight by the raw material containing isopropylbenzene and alkali lye:0.9-1.1 ratio is mixing
Mixed in device, carry out alkali cleaning, the temperature of the alkali cleaning is 20 DEG C -28 DEG C, and material is entered in time 1-3h, the oxidation obtained after reaction
The pH value of middle isopropylbenzene is controlled 6~7；
(2) cumyl hydroperoxide is generated：Isopropylbenzene after processing and air are transported to oxidizing tower together, generate peroxide
Change hydrogen isopropylbenzene CHP；
(3) cumyl hydroperoxide purifies：Hydrogen oxide isopropylbenzene CHP is first delivered in special water scrubber with pump, with
Water is as cleaning agent, and oxidation solution is that cleansing medium is washed, and the oxidation solution is by weight 1.8-2.2 with water:1 ratio
Mixed, to remove the water-solubility impurity being entrained in oxidation solution, the wash temperature is 22 DEG C -28 DEG C, and wash time is
2-4h, finally give cumyl hydroperoxide oxidation solution；
(4) intermediate product Bian alcohol is generated：Cumyl hydroperoxide oxidation solution and sodium sulfide solution are pressed into 3.5-4.5:1 rubs
You are reacted than directly, and reaction temperature is 55-65 DEG C, and normal pressure, the reaction time is adjusted to 1.5-2.5 hours, obtains Bian alcohol；
(5) Bian alcohol refines：Bian alcohol is refined into smart Bian alcohol by rectifying column；
(6) condensation reaction：Smart Bian alcohol carries out being condensed instead with the CHP after another part concentrate under the catalytic action of perchloric acid
Should, generate cumyl peroxide.
As optimization：In the pretreatment of raw material：It is 1 by weight by the raw material containing isopropylbenzene and alkali lye:1.0 ratio
Example mixes in a mixer, carries out alkali cleaning, and the temperature of the alkali cleaning is 26 DEG C, time 2h, the oxidation charging obtained after reaction
The pH value of isopropylbenzene is controlled 6 in thing.
As optimization：The cumyl hydroperoxide purification：Hydrogen oxide isopropylbenzene CHP is first delivered to special water with pump
Wash in tower, using water as cleaning agent, oxidation solution is that cleansing medium is washed, and the oxidation solution is 2.1 by weight with water:1
Ratio mixed, be entrained in water-solubility impurity in oxidation solution to remove, the wash temperature is 24 DEG C, and wash time is
3h, finally give cumyl hydroperoxide oxidation solution.
As optimization：In the generation intermediate product Bian alcohol：Cumyl hydroperoxide oxidation solution is pressed with sodium sulfide solution
3.8:1 mol ratio is directly reacted, and reaction temperature is 62 DEG C, and normal pressure, the reaction time is adjusted to 2.2 hours, obtains Bian alcohol.
Beneficial effect：The present invention solves the weak point that DCP is produced in traditional handicraft, shortens production procedure, saves life
Cost is produced, is reduced environmental pollution.
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.
Specific embodiment 1
A kind of production method of cumyl peroxide, concrete operations are as follows：
(1) pretreatment of raw material：It is 1 by weight by the raw material containing isopropylbenzene and alkali lye:0.9 ratio is in a mixer
Mixing, alkali cleaning is carried out, the temperature of the alkali cleaning is 20 DEG C, time 1h, isopropylbenzene during what is obtained after reaction aoxidize into material
PH value is controlled 6；
(2) cumyl hydroperoxide is generated：Isopropylbenzene after processing and air are transported to oxidizing tower together, generate peroxide
Change hydrogen isopropylbenzene CHP；
(3) cumyl hydroperoxide purifies：Hydrogen oxide isopropylbenzene CHP is first delivered in special water scrubber with pump, with
For water as cleaning agent, oxidation solution is that cleansing medium is washed, and the oxidation solution is 1.8 by weight with water:1 ratio is carried out
Mixing, water-solubility impurity in oxidation solution being entrained in remove, the wash temperature is 22 DEG C, wash time 2h, final
To cumyl hydroperoxide oxidation solution；
(4) intermediate product Bian alcohol is generated：Cumyl hydroperoxide oxidation solution and sodium sulfide solution are pressed 3.5:1 mol ratio
Directly reacted, reaction temperature is 55 DEG C, and normal pressure, the reaction time is adjusted to 1.5 hours, obtains Bian alcohol；
(5) Bian alcohol refines：Bian alcohol is refined into smart Bian alcohol by rectifying column；
(6) condensation reaction：Smart Bian alcohol carries out being condensed instead with the CHP after another part concentrate under the catalytic action of perchloric acid
Should, generate cumyl peroxide.
Specific embodiment 2
A kind of production method of cumyl peroxide, concrete operations are as follows：
(1) pretreatment of raw material：It is 1 by weight by the raw material containing isopropylbenzene and alkali lye:1.1 ratio is in a mixer
Mixing, alkali cleaning is carried out, the temperature of the alkali cleaning is 28 DEG C, time 3h, isopropylbenzene during what is obtained after reaction aoxidize into material
PH value is controlled 7；
(2) cumyl hydroperoxide is generated：Isopropylbenzene after processing and air are transported to oxidizing tower together, generate peroxide
Change hydrogen isopropylbenzene CHP；
(3) cumyl hydroperoxide purifies：Hydrogen oxide isopropylbenzene CHP is first delivered in special water scrubber with pump, with
For water as cleaning agent, oxidation solution is that cleansing medium is washed, and the oxidation solution is 2.2 by weight with water:1 ratio is carried out
Mixing, water-solubility impurity in oxidation solution being entrained in remove, the wash temperature is 28 DEG C, wash time 4h, final
To cumyl hydroperoxide oxidation solution；
(4) intermediate product Bian alcohol is generated：Cumyl hydroperoxide oxidation solution and sodium sulfide solution are pressed 4.5:1 mol ratio
Directly reacted, reaction temperature is 65 DEG C, and normal pressure, the reaction time is adjusted to 2.5 hours, obtains Bian alcohol；
(5) Bian alcohol refines：Bian alcohol is refined into smart Bian alcohol by rectifying column；
(6) condensation reaction：Smart Bian alcohol carries out being condensed instead with the CHP after another part concentrate under the catalytic action of perchloric acid
Should, generate cumyl peroxide.
Specific embodiment 3
A kind of production method of cumyl peroxide, concrete operations are as follows：
(1) pretreatment of raw material：It is 1 by weight by the raw material containing isopropylbenzene and alkali lye:1.0 ratio is in a mixer
Mixing, alkali cleaning is carried out, the temperature of the alkali cleaning is 26 DEG C, time 2h, isopropylbenzene during what is obtained after reaction aoxidize into material
PH value is controlled 6；
(2) cumyl hydroperoxide is generated：Isopropylbenzene after processing and air are transported to oxidizing tower together, generate peroxide
Change hydrogen isopropylbenzene CHP；
(3) cumyl hydroperoxide purifies：Hydrogen oxide isopropylbenzene CHP is first delivered in special water scrubber with pump, with
For water as cleaning agent, oxidation solution is that cleansing medium is washed, and the oxidation solution is 2.1 by weight with water:1 ratio is carried out
Mixing, water-solubility impurity in oxidation solution being entrained in remove, the wash temperature is 24 DEG C, wash time 3h, final
To cumyl hydroperoxide oxidation solution；
(4) intermediate product Bian alcohol is generated：Cumyl hydroperoxide oxidation solution and sodium sulfide solution are pressed 3.8:1 mol ratio
Directly reacted, reaction temperature is 62 DEG C, and normal pressure, the reaction time is adjusted to 2.2 hours, obtains Bian alcohol；
(5) Bian alcohol refines：Bian alcohol is refined into smart Bian alcohol by rectifying column；
(6) condensation reaction：Smart Bian alcohol carries out being condensed instead with the CHP after another part concentrate under the catalytic action of perchloric acid
Should, generate cumyl peroxide.
The present invention solves the weak point that DCP is produced in traditional handicraft, shortens production procedure, saves production cost, subtracts
Few environmental pollution.
Claims (4)
- A kind of 1. production method of cumyl peroxide, it is characterised in that：Concrete operations are as follows：(1) pretreatment of raw material：It is 1 by weight by the raw material containing isopropylbenzene and alkali lye:0.9-1.1 ratio is in a mixer Mixing, alkali cleaning is carried out, the temperature of the alkali cleaning is 20 DEG C -28 DEG C, and time 1-3h, the oxidation obtained after reaction is entered different in material The pH value of propyl benzene is controlled 6~7；(2) cumyl hydroperoxide is generated：Isopropylbenzene after processing and air are transported to oxidizing tower together, generate hydrogen peroxide Isopropylbenzene CHP；(3) cumyl hydroperoxide purifies：Hydrogen oxide isopropylbenzene CHP is first delivered in special water scrubber with pump, made with water For cleaning agent, oxidation solution is that cleansing medium is washed, and the oxidation solution is by weight 1.8-2.2 with water:1 ratio is carried out Mixing, to remove the water-solubility impurity being entrained in oxidation solution, the wash temperature is 22 DEG C -28 DEG C, wash time 2-4h, Finally give cumyl hydroperoxide oxidation solution；(4) intermediate product Bian alcohol is generated：Cumyl hydroperoxide oxidation solution and sodium sulfide solution are pressed into 3.5-4.5:1 mol ratio Directly reacted, reaction temperature is 55-65 DEG C, and normal pressure, the reaction time is adjusted to 1.5-2.5 hours, obtains Bian alcohol；(5) Bian alcohol refines：Bian alcohol is refined into smart Bian alcohol by rectifying column；(6) condensation reaction：Smart Bian alcohol carries out condensation reaction with the CHP after another part concentrate under the catalytic action of perchloric acid, Generate cumyl peroxide.
- 2. the production method of cumyl peroxide according to claim 1, it is characterised in that：The pretreatment of raw material In：It is 1 by weight by the raw material containing isopropylbenzene and alkali lye:1.0 ratio mixes in a mixer, carries out alkali cleaning, described The temperature of alkali cleaning is 26 DEG C, time 2h, and the pH value of isopropylbenzene is controlled 6 during what is obtained after reaction aoxidize into material.
- 3. the production method of cumyl peroxide according to claim 1, it is characterised in that：The hydrogen peroxide isopropyl Benzene purifies：Hydrogen oxide isopropylbenzene CHP is first delivered in special water scrubber with pump, using water as cleaning agent, oxidation solution is clear Wash medium to be washed, the oxidation solution is 2.1 by weight with water:1 ratio is mixed, and oxidation solution is entrained in remove In water-solubility impurity, the wash temperature be 24 DEG C, wash time 3h, finally give cumyl hydroperoxide oxidation solution.
- 4. the production method of cumyl peroxide according to claim 1, it is characterised in that：The generation intermediate product In Bian alcohol：Cumyl hydroperoxide oxidation solution and sodium sulfide solution are pressed 3.8:1 mol ratio is directly reacted, reaction temperature For 62 DEG C, normal pressure, the reaction time is adjusted to 2.2 hours, obtains Bian alcohol.
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| CN201710615569.2A CN107382806A (en) | 2017-07-26 | 2017-07-26 | A kind of production method of cumyl peroxide |
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| CN201710615569.2A CN107382806A (en) | 2017-07-26 | 2017-07-26 | A kind of production method of cumyl peroxide |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108276320A (en) * | 2018-01-23 | 2018-07-13 | 庞志兰 | A kind of process units and its production method of cumyl peroxide |
| CN109534952A (en) * | 2018-12-17 | 2019-03-29 | 实友化工（扬州）有限公司 | A kind of phenol preparation method can reduce by-product tar yield |
| CN109824564A (en) * | 2019-03-07 | 2019-05-31 | 江苏道明化学有限公司 | A kind of finished product production technology of cumyl peroxide |
| CN109912480A (en) * | 2019-04-01 | 2019-06-21 | 江苏道明化学有限公司 | A kind of DCP rectification working process process |
| CN109942472A (en) * | 2019-04-01 | 2019-06-28 | 江苏道明化学有限公司 | A kind of condensation liquid concentrate crystallization processes |
| CN110066234A (en) * | 2019-04-01 | 2019-07-30 | 江苏道明化学有限公司 | A kind of DCP reduction reaction process |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102827051A (en) * | 2012-09-24 | 2012-12-19 | 金魏 | Method for synthesizing dicumyl peroxide |
| CN104230856A (en) * | 2013-06-17 | 2014-12-24 | 中国石油化工股份有限公司 | Production method of epoxybutane |
| CN104860861A (en) * | 2015-04-01 | 2015-08-26 | 中石化上海工程有限公司 | Production method for dicumyl peroxide (DCP) |
-
2017
- 2017-07-26 CN CN201710615569.2A patent/CN107382806A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102827051A (en) * | 2012-09-24 | 2012-12-19 | 金魏 | Method for synthesizing dicumyl peroxide |
| CN104230856A (en) * | 2013-06-17 | 2014-12-24 | 中国石油化工股份有限公司 | Production method of epoxybutane |
| CN104860861A (en) * | 2015-04-01 | 2015-08-26 | 中石化上海工程有限公司 | Production method for dicumyl peroxide (DCP) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108276320A (en) * | 2018-01-23 | 2018-07-13 | 庞志兰 | A kind of process units and its production method of cumyl peroxide |
| CN109534952A (en) * | 2018-12-17 | 2019-03-29 | 实友化工（扬州）有限公司 | A kind of phenol preparation method can reduce by-product tar yield |
| CN109824564A (en) * | 2019-03-07 | 2019-05-31 | 江苏道明化学有限公司 | A kind of finished product production technology of cumyl peroxide |
| CN109912480A (en) * | 2019-04-01 | 2019-06-21 | 江苏道明化学有限公司 | A kind of DCP rectification working process process |
| CN109942472A (en) * | 2019-04-01 | 2019-06-28 | 江苏道明化学有限公司 | A kind of condensation liquid concentrate crystallization processes |
| CN110066234A (en) * | 2019-04-01 | 2019-07-30 | 江苏道明化学有限公司 | A kind of DCP reduction reaction process |
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Application publication date: 20171124 |