CN108250120A - A kind of preparation method of poly-putty base cyclohexanone peroxide - Google Patents
A kind of preparation method of poly-putty base cyclohexanone peroxide Download PDFInfo
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- CN108250120A CN108250120A CN201810114038.XA CN201810114038A CN108250120A CN 108250120 A CN108250120 A CN 108250120A CN 201810114038 A CN201810114038 A CN 201810114038A CN 108250120 A CN108250120 A CN 108250120A
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- cyclohexanone
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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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Abstract
The invention belongs to technical field of organic synthesis, and in particular to cyclohexanone and phthalic acid ester are mixed into solution A, hydrogen peroxide and inorganic acid are mixed into solution B by a kind of preparation method of poly-putty base cyclohexanone peroxide；Solution A is added dropwise in solution B, occur White Flocculus after stirring and is layered；It removes layer to be washed with water to neutrality, then adds in phthalic acid ester and stabilizer is uniformly mixed and obtains poly-putty base cyclohexanone peroxide.The method and step that the present invention prepares cyclohexanone peroxide paste is relatively simple, and reaction condition is mild and easily controllable, and the cyclohexanone peroxide yield of preparation is higher, and yield can reach more than 98%.
Description
Technical field
The invention belongs to technical field of organic synthesis, and in particular to a kind of preparation side of poly-putty base cyclohexanone peroxide
Method.
Background technology
Poly-putty base is commonly called as putty, also known as unsaturated polyester resin putty, is to develop a kind of faster novel pointing material, energy
Body surface is perfectly adhered to, and is not cracked in the drying process.Poly-putty base is a kind of high molecular material, by main putty
(base ash) and curing agent two parts composition, wherein, cyclohexanone peroxide is one of common curing agent of unsaturated polyester resin.It crosses
Peroxyester white in appearance or pale yellow needles crystalline powder since its property is unstable, usually use phthalic acid
Ester is diluted to paste, and as cyclohexanone peroxide is pasted.
At present, the preparation method of cyclohexanone peroxide is mainly the following：
(1) ketone method is dripped：Hydrogen peroxide and dibutyl phthalate are mixed into solution A, then by cyclohexanone and O-phthalic
Dibutyl phthalate is mixed into solution B, and solution B is added drop-wise in solution A, and reaction temperature is controlled at 20 DEG C or so, instills 4/5 material
When, nitric acid is added in, then proceedes to that remaining 1/5 material is added dropwise, maintains 1h to the reaction was complete.It is neutralized to a little powdered sodium carbonate
Neutrality, then stratification, separates lower floor's product, adds in ethylene glycol as stabilizer, stirring can be prepared by cyclohexanone peroxide.
(2) less than 10 DEG C of hydrogen peroxide is will be cooled to, is added in less than 10 DEG C of equimolar cyclohexanone, is warming up to 40
DEG C or so, 15 DEG C then are dropped to again, is added with stirring hydrochloric acid or nitric acid as catalyst, temperature rises immediately, controls temperature
No more than 30 DEG C, temperature declines after about 1h, and object gradually cures in cup, keeps stirring and adds in distilled water, 1h is placed after stirring evenly, and inhales
Filter is washed with distillation.Then paste is tuned into water, adding in 10% sodium hydroxide makes pH value be 8, filters, washing is filtered dry rear room temperature
It dries, obtains white crystals finished product, yield 81%.
(3) it is 0-180 DEG C in temperature using the gaseous mixture of ozone or ozone and diluent gas as oxidant, pressure 0.1-
Under the conditions of 3MPa, the molar ratio according to cyclohexanone, ozone and solvent is 1:0.1-10:The ratio reaction of 1-150, was prepared
Peroxyester.
In the preparation method of more than cyclohexanone peroxide, ozone is larger as oxidant toxicity, and not environmentally, reaction condition is not
Mildly.Other two is with hydrogen peroxide as the preparation method of oxidant, and obtained cyclohexanone peroxide yield is not high and step is numerous
It is trivial.
Invention content
The object of the present invention is to provide a kind of preparation methods of poly-putty base cyclohexanone peroxide, solve traditional preparation methods
The technical issues of middle reaction is not mild, complex steps and larger reaction raw materials toxicity.
The technical scheme is that：
A kind of preparation method of poly-putty base cyclohexanone peroxide, includes the following steps：
(1) cyclohexanone and phthalic acid ester are mixed into solution A, hydrogen peroxide and inorganic acid is mixed into solution B；
(2) solution A is added dropwise in solution B, occurs White Flocculus after being stirred to react and be layered；
(3) it removes layer to be washed with water to neutrality, then adds in phthalic acid ester and stabilizer is uniformly mixed and obtains atom
Ash cyclohexanone peroxide.
Preferably, the mass ratio of cyclohexanone and phthalic acid ester is 1 in step (1):1.5-2 wherein phthalic acid
Ester is phthalic acid ester methyl ester or butyl phthalate.
Preferably, the mass ratio of hydrogen peroxide and inorganic acid is 15-20 in step (1):1, wherein inorganic acid is sulfuric acid, salt
One kind in acid, nitric acid, hydrogen peroxide refer to 30wt.% aqueous hydrogen peroxide solutions.
Preferably, the molar ratio of cyclohexanone and hydrogen peroxide is 1 in step (2):1-1.5.
Preferably, reaction temperature is 20 DEG C -40 DEG C in step (2).
Preferably, in step (3) phthalic acid ester be phthalic acid ester methyl ester or butyl phthalate, stabilizer
For ethylene glycol or cyclohexanediol.
Preferably, the mass ratio that phthalic acid ester and stabilizer are added in step (3) is 8-10:1.
Beneficial effects of the present invention are as follows：
The method and step that the present invention prepares cyclohexanone peroxide is relatively simple, and reaction condition is mild and easily controllable, prepares
Cyclohexanone peroxide yield it is higher, yield can reach more than 98%.
Specific embodiment
With reference to embodiment, technical scheme of the present invention is described in further detail, but do not formed pair
Any restrictions of the present invention.
Embodiment 1
(1) 500 grams of cyclohexanone and 800 grams of repefrals is taken to be mixedly configured into cyclohexanone solution, take 250 grams pairs
Oxygen water (30wt.% aqueous hydrogen peroxide solutions) is mixedly configured into hydrogenperoxide steam generator with 15 grams of 68wt.% aqueous solution of nitric acid；
(2) and then under stirring and cooling cyclohexanone solution is slowly dropped in hydrogenperoxide steam generator, speed is added dropwise in control
Degree so that temperature of reaction system is maintained at 20 DEG C -40 DEG C, gradually appears White Flocculus；
(3) after cyclohexanone solution is added dropwise to complete, continue stirring 1.5 hours, then stratification, upper solution separation is removed
It goes, lower floor adds deionized water to be rinsed repeatedly to neutrality, filters out residual moisture, then adds in 750 grams of repefrals
With 80 grams of ethylene glycol, cyclohexanone peroxide paste is obtained after stirring evenly, the yield of cyclohexanone peroxide is 98.4%.
Embodiment 2
(1) 306 grams of cyclohexanone and 510 grams of dibutyl phthalates is taken to be mixedly configured into cyclohexanone solution, take 196 grams pairs
Oxygen water (30wt.% aqueous hydrogen peroxide solutions) is configured to hydrogenperoxide steam generator with 11 grams of 38wt.% combineds；
(2) and then under stirring and cooling cyclohexanone solution is slowly dropped in hydrogenperoxide steam generator, speed is added dropwise in control
Degree so that temperature of reaction system is maintained at 20 DEG C -40 DEG C, gradually appears White Flocculus；
(3) after cyclohexanone solution is added dropwise to complete, continue stirring 1.5 hours, then stratification, upper solution separation is removed
It goes, lower floor adds deionized water to be rinsed repeatedly to neutrality, filters out residual moisture, then adds in 485 grams of repefrals
With 50 grams of ethylene glycol, cyclohexanone peroxide paste is obtained after stirring evenly, the yield of cyclohexanone peroxide is 99.1%.
Embodiment 3
(1) 750 grams of cyclohexanone and 1200 grams of repefrals is taken to be mixedly configured into cyclohexanone solution, take 410 grams
Hydrogen peroxide (30wt.% aqueous hydrogen peroxide solutions) is mixedly configured into hydrogenperoxide steam generator with 23 grams of 98wt.% aqueous sulfuric acids；
(2) and then under stirring and cooling cyclohexanone solution is slowly dropped in hydrogenperoxide steam generator, speed is added dropwise in control
Degree so that temperature of reaction system is maintained at 20 DEG C -40 DEG C, gradually appears White Flocculus；
(3) after cyclohexanone solution is added dropwise to complete, continue stirring 1.5 hours, then stratification, upper solution separation is removed
It goes, lower floor adds deionized water to be rinsed repeatedly to neutrality, filters out residual moisture, then adds in 1040 grams of repefrals
With 120 grams of ethylene glycol, cyclohexanone peroxide paste is obtained after stirring evenly, the yield of cyclohexanone peroxide is 98.9%.
Above-described embodiment is the preferable embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any Spirit Essences without departing from the present invention with made under principle change, modification, replacement, combine, simplification,
Equivalent substitute mode is should be, is included within protection scope of the present invention.
Claims (7)
1. a kind of preparation method of poly-putty base cyclohexanone peroxide, which is characterized in that include the following steps：
(1) cyclohexanone and phthalic acid ester are mixed into solution A, hydrogen peroxide and inorganic acid is mixed into solution B；
(2) solution A is added dropwise in solution B, occurs White Flocculus after being stirred to react and be layered；
(3) it removes layer to be washed with water to neutrality, then adds in phthalic acid ester and stabilizer is uniformly mixed and obtains poly-putty base use
Cyclohexanone peroxide.
A kind of 2. preparation method of poly-putty base cyclohexanone peroxide according to claim 1, which is characterized in that step
(1) mass ratio of cyclohexanone and phthalic acid ester is 1 in:1.5-2, wherein phthalic acid ester are phthalic acid ester methyl ester
Or butyl phthalate.
A kind of 3. preparation method of poly-putty base cyclohexanone peroxide according to claim 1, which is characterized in that step
(1) mass ratio of hydrogen peroxide and inorganic acid is 15-20 in:1, wherein inorganic acid be sulfuric acid, hydrochloric acid, one kind in nitric acid, dioxygen
Water refers to 30wt.% aqueous hydrogen peroxide solutions.
A kind of 4. preparation method of poly-putty base cyclohexanone peroxide according to claim 1, which is characterized in that step
(2) molar ratio of cyclohexanone and hydrogen peroxide is 1 in:1-1.5.
A kind of 5. preparation method of poly-putty base cyclohexanone peroxide according to claim 1, which is characterized in that step
(2) reaction temperature is 20 DEG C -40 DEG C in.
A kind of 6. preparation method of poly-putty base cyclohexanone peroxide according to claim 1, which is characterized in that step
(3) phthalic acid ester is phthalic acid ester methyl ester or butyl phthalate in, and stabilizer is ethylene glycol or cyclohexanediol.
A kind of 7. preparation method of poly-putty base cyclohexanone peroxide according to claim 1, which is characterized in that step
(3) mass ratio that phthalic acid ester and stabilizer are added in is 8-10:1.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810114038.XA CN108250120A (en) | 2018-02-05 | 2018-02-05 | A kind of preparation method of poly-putty base cyclohexanone peroxide |
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| CN201810114038.XA CN108250120A (en) | 2018-02-05 | 2018-02-05 | A kind of preparation method of poly-putty base cyclohexanone peroxide |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111909072A (en) * | 2020-08-26 | 2020-11-10 | 英德市城泰化工有限公司 | Preparation process of cyclohexanone peroxide ointment |
| CN116640472A (en) * | 2023-04-27 | 2023-08-25 | 英德市城泰化工有限公司 | Production process of cyclohexanone peroxide transparent liquid with stable 50% content |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2046793C1 (en) * | 1993-08-13 | 1995-10-27 | Липес Владислав Вениаминович | Stable cyclohexanone solution and method for its production |
-
2018
- 2018-02-05 CN CN201810114038.XA patent/CN108250120A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2046793C1 (en) * | 1993-08-13 | 1995-10-27 | Липес Владислав Вениаминович | Stable cyclohexanone solution and method for its production |
Non-Patent Citations (2)
| Title |
|---|
| 况水根等: "液态过氧化环己酮的研制", 《热固性树脂》 * |
| 宁炳全等: "生产不饱和聚酯树脂I号引发剂的新工艺", 《合成树脂及塑料》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111909072A (en) * | 2020-08-26 | 2020-11-10 | 英德市城泰化工有限公司 | Preparation process of cyclohexanone peroxide ointment |
| CN116640472A (en) * | 2023-04-27 | 2023-08-25 | 英德市城泰化工有限公司 | Production process of cyclohexanone peroxide transparent liquid with stable 50% content |
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