CN108239010A - The synthetic method of benzoyl peroxide organic intermediate - Google Patents
The synthetic method of benzoyl peroxide organic intermediate Download PDFInfo
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- CN108239010A CN108239010A CN201710836676.8A CN201710836676A CN108239010A CN 108239010 A CN108239010 A CN 108239010A CN 201710836676 A CN201710836676 A CN 201710836676A CN 108239010 A CN108239010 A CN 108239010A
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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 Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses the synthetic methods of benzoyl peroxide organic intermediate, include the following steps：Benzamide is added in reaction vessel, Klorvess Liquid, control solution temperature is to 20 26 DEG C, aqueous solution is added in, 310 330rpm of mixing speed is controlled, adds in phenetole solution in batches in 30 50min, then N chloro-acetamides, the reaction was continued 80 130min are added in；Then nickel sesquioxide powder is added in, solution temperature is increased in 20 30min to 30 34 DEG C, the reaction was continued 2 3h, addition potassium nitrate solution, solution layering, detach oil-yielding stratum, 20 40min are washed with metabisulfite solution, 10 30min is washed with dimethyl carbonate solution, is recrystallized in acetylacetone,2,4-pentanedione solution, dehydrating agent is dehydrated, and obtains finished product benzoyl peroxide.
Description
Technical field
The present invention relates to a kind of preparation methods of organic intermediate, belong to organic synthesis field more particularly to benzoyl peroxide
The synthetic method of formyl organic intermediate.
Background technology
Benzoyl peroxide is mainly used for initiators for polymerization, as PVC, polyacrylonitrile, acrylate, vinyl acetate
Solvent polymeric, neoprene, SBS polymerize the curing of unsaturated polyester resins, organic glass gluing with methyl methacrylate-grafted
Initiator, the crosslinking agent of agent etc..It is used as vulcanizing agent, the crosslinking agent of silicon rubber and fluorubber in rubber industry.It can also be in chemical industry
Production is used as bleaching agent, oxidant.Existing synthetic method is mostly using in the cooling condition by a concentration of 30% peroxide
Change the sodium hydroxide solution that hydrogen solution adds in 30%, generate sodium peroxide aqueous solution.Then the agitation and dropping benzene first at 0~10 DEG C
Acyl chlorides, the benzoyl peroxide of generation is precipitated, through cooling down, being filtered, washed, and with 2：1 methanol/chloroform solution recrystallization is done
It is dry to obtain product.Since this synthetic method is needed using hydrogenperoxide steam generator, sodium hydroxide solution, methanol solution as reaction
Raw material.Reaction raw materials hydrogen peroxide belongs to explosive strong oxidant, can react releasing amount of heat and oxygen with combustible and
Cause Fire explosion.Hydrogen peroxide has strong corrosivity, and sucking the product steam or mist has respiratory tract intense irritation, and eye is straight
Connecing contact liq can cause irreversible damage even to blind.Therefore, hydrogen peroxide can cause building-up process dangerous as reaction raw materials
Coefficient increases, and larger to production operation personnel health harm, is unfavorable for keeping the safety in production.Reaction raw materials sodium hydroxide has strongly
Stimulation and corrosivity, dust or smog can stimulate eye and respiratory tract, corrode nasal septum, skin and eye and are in direct contact meeting with NaOH
Cause and burn, these factors all can generate harm, and the corrosivity of sodium hydroxide can cause instead to production operation personnel health
Container corrosion degree is answered to increase, equipment damage rate rises, and is unfavorable for plant maintenance and cost control.Reaction raw materials methanol is to maincenter
Nervous system has anesthetic effect；There is special selection index system to optic nerve and retina, cause lesion；It can cause metabolic acidosis.
These can all endanger the health of producers, be unfavorable for keeping the safety in production.These above-mentioned factor analyses show that this synthetic method is deposited
In many shortcomings, it is therefore necessary to propose a kind of new synthetic method.
Invention content
Technical problems based on background technology, the present invention propose the synthesis side of benzoyl peroxide organic intermediate
Method includes the following steps：
A:Benzamide, Klorvess Liquid are added in reaction vessel, control solution temperature adds in water-soluble to 20-26 DEG C
Liquid controls mixing speed 310-330rpm, adds in phenetole solution in batches in 30-50min, then adds in N- chloroacetyls
Amine, the reaction was continued 80-130min；
B:Then nickel sesquioxide powder is added in, solution temperature is increased in 20-30min to 30-34 DEG C, the reaction was continued 2-
3h adds in potassium nitrate solution, and solution layering detaches oil-yielding stratum, 20-40min is washed with metabisulfite solution, molten with dimethyl carbonate
Liquid washs 10-30min, is recrystallized in acetylacetone,2,4-pentanedione solution, and dehydrating agent dehydration obtains finished product benzoyl peroxide.
Preferably, Klorvess Liquid mass fraction is 10-16%.
Preferably, phenetole liquid quality fraction is 15-22%.
Preferably, potassium nitrate solution mass fraction is 10-15%.
Preferably, metabisulfite solution mass fraction is 20-26%.
Preferably, dimethyl carbonate liquid quality fraction is 40-47%.
Preferably, acetylacetone,2,4-pentanedione liquid quality fraction is 60-66%.
Entire building-up process can be used following net reaction to represent：
Compared to synthetic method disclosed in background technology, the synthesis of benzoyl peroxide organic intermediate provided by the invention
Method does not need to avoid explosive strong as reaction raw materials using hydrogenperoxide steam generator, sodium hydroxide solution, methanol solution
Harm of the oxidants hydrogen peroxide to production safety, avoid intense stimulus and corrosive sodium hydroxide to production equipment
Corrosion and the health hazard of production operation personnel, also avoiding reaction raw materials methanol causes to the maincenter of production operation personnel god
Injury through system and optic nerve and retina, these all greatly improve the safety coefficient of production link, are conducive to safety
Production.And reaction intermediate link reduces very much, and the reaction time also shortens much, and reaction yield also improves, while this hair
It is bright to provide a kind of new synthetic route, it lays a good foundation further to promote reaction yield.
Description of the drawings
Fig. 1 is the infrared analysis spectrogram of finished product benzoyl peroxide.
Specific embodiment
Embodiment 1：
The synthetic method of benzoyl peroxide organic intermediate, includes the following steps：
A:3mol benzamides are added in reaction vessel, 1.2L mass fractions are 10% Klorvess Liquid, control solution
Temperature adds in 6mol aqueous solutions to 20 DEG C, controls mixing speed 310rpm, and point 2 addition 6mol mass fractions are in 30min
Then 15% phenetole solution adds in 6mol N- chloro-acetamides, the reaction was continued 80min；
B:Then 3mol nickel sesquioxide powder is added in, solution temperature is increased in 20min to 30 DEG C, the reaction was continued 2h,
It is 10% potassium nitrate solution to add in 800ml mass fractions, and solution layering detaches oil-yielding stratum, is 20% sodium sulphate with mass fraction
Solution washs 20min, and 10min is washed for 40% dimethyl carbonate solution with mass fraction, is 60% levulinic in mass fraction
It is recrystallized in ketone solution, the dehydration of anhydrous magnesium sulfate dehydrating agent obtains finished product benzoyl peroxide 716.562g, yield 98.7%.
Embodiment 2：
The synthetic method of benzoyl peroxide organic intermediate, includes the following steps：
A:3mol benzamides are added in reaction vessel, 1.2L mass fractions are 13% Klorvess Liquid, control solution
Temperature adds in 7mol aqueous solutions to 23 DEG C, controls mixing speed 320rpm, 7mol mass fractions are added three times in 40min is
Then 18% phenetole solution adds in 7mol N- chloro-acetamides, the reaction was continued 100min；
B:Then 4mol nickel sesquioxide powder is added in, solution temperature is increased in 25min to 32 DEG C, the reaction was continued
2.5h, it is 13% potassium nitrate solution to add in 800ml mass fractions, and solution layering detaches oil-yielding stratum, is 23% sulphur with mass fraction
Acid sodium solution washs 30min, and 20min is washed for 44% dimethyl carbonate solution with mass fraction, is 63% second in mass fraction
It is recrystallized in acyl acetone soln, the dehydration of anhydrous magnesium sulfate dehydrating agent obtains finished product benzoyl peroxide 718.041g, yield
98.9%.
Embodiment 3：
The synthetic method of benzoyl peroxide organic intermediate, includes the following steps：
A:3mol benzamides are added in reaction vessel, 1.2L mass fractions are 16% Klorvess Liquid, control solution
Temperature adds in 8mol aqueous solutions to 26 DEG C, controls mixing speed 330rpm, and point 4 addition 8mol mass fractions are in 50min
Then 22% phenetole solution adds in 8mol N- chloro-acetamides, the reaction was continued 130min；
B:Then 5mol nickel sesquioxide powder is added in, solution temperature is increased in 30min to 34 DEG C, the reaction was continued 3h,
It is 15% potassium nitrate solution to add in 800ml mass fractions, and solution layering detaches oil-yielding stratum, is 26% sodium sulphate with mass fraction
Solution washs 40min, and 30min is washed for 47% dimethyl carbonate solution with mass fraction, is 66% levulinic in mass fraction
It is recrystallized in ketone solution, the dehydration of anhydrous magnesium sulfate dehydrating agent obtains finished product benzoyl peroxide 720.192g, yield 99.2%.
Fig. 1 is the infrared analysis spectrogram of finished product benzoyl peroxide.
Table 1 is infrared analysis data.
1 infrared analysis data of table
It described in above example, is merely preferred embodiments of the present invention, but protection scope of the present invention not office
Be limited to this, any one skilled in the art in the technical scope disclosed by the present invention, the technique according to the invention
Scheme and its inventive concept are subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (6)
1. the synthetic method of benzoyl peroxide organic intermediate, which is characterized in that include the following steps：
A:Benzamide, Klorvess Liquid are added in reaction vessel, control solution temperature adds in aqueous solution, control to 20-26 DEG C
Mixing speed 310-330rpm processed, adds in phenetole solution in batches in 30-50min, then adds in N- chloro-acetamides, after
Continuous reaction 80-130min；
B:Then nickel sesquioxide powder is added in, solution temperature is increased in 20-30min to 30-34 DEG C, the reaction was continued 2-3h,
Potassium nitrate solution is added in, solution layering detaches oil-yielding stratum, 20-40min washed with metabisulfite solution, with dimethyl carbonate solution
10-30min is washed, is recrystallized in acetylacetone,2,4-pentanedione solution, dehydrating agent dehydration obtains finished product benzoyl peroxide.
2. the synthetic method of benzoyl peroxide organic intermediate according to claim 1, which is characterized in that the chlorination
Potassium solution mass fraction is 10-16%.
3. the synthetic method of benzoyl peroxide organic intermediate according to claim 1, which is characterized in that the benzene second
Ethereal solution mass fraction is 15-22%.
4. the synthetic method of benzoyl peroxide organic intermediate according to claim 1, which is characterized in that the nitric acid
Potassium solution mass fraction is 10-15%.
5. the synthetic method of benzoyl peroxide organic intermediate according to claim 1, which is characterized in that the sulfuric acid
Sodium solution mass fraction is 20-26%.
6. the synthetic method of benzoyl peroxide organic intermediate according to claim 1, which is characterized in that including walking as follows
Suddenly：
A:3mol benzamides are added in reaction vessel, 1.2L mass fractions are 16% Klorvess Liquid, control solution temperature
To 26 DEG C, 8mol aqueous solutions are added in, control mixing speed 330rpm, point 4 addition 8mol mass fractions are 22% in 50min
Then phenetole solution adds in 8mol N- chloro-acetamides, the reaction was continued 130min；
B:Then 5mol nickel sesquioxide powder is added in, solution temperature is increased in 30min to 34 DEG C, the reaction was continued 3h, addition
800ml mass fractions are 15% potassium nitrate solution, and solution layering detaches oil-yielding stratum, is 26% metabisulfite solution with mass fraction
40min is washed, 30min is washed for 47% dimethyl carbonate solution with mass fraction, it is molten for 66% acetylacetone,2,4-pentanedione in mass fraction
It is recrystallized in liquid, the dehydration of anhydrous magnesium sulfate dehydrating agent obtains finished product benzoyl peroxide.
Priority Applications (4)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710836676.8A CN108239010A (en) | 2017-09-17 | 2017-09-17 | The synthetic method of benzoyl peroxide organic intermediate |
| GBGB1719126.3A GB201719126D0 (en) | 2017-09-17 | 2017-11-20 | Benzoyl peroxide organic intermediates synthesis method |
| AU2018101146A AU2018101146A4 (en) | 2017-09-17 | 2018-08-13 | Benzoyl peroxide organic intermediates synthesis method |
| IE20180281U IE20180281U1 (en) | 2017-09-17 | 2018-08-23 | Benzoyl peroxide organic intermediates synthesis method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710836676.8A CN108239010A (en) | 2017-09-17 | 2017-09-17 | The synthetic method of benzoyl peroxide organic intermediate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108239010A true CN108239010A (en) | 2018-07-03 |
Family
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710836676.8A Withdrawn CN108239010A (en) | 2017-09-17 | 2017-09-17 | The synthetic method of benzoyl peroxide organic intermediate |
Country Status (4)
| Country | Link |
|---|---|
| CN (1) | CN108239010A (en) |
| AU (1) | AU2018101146A4 (en) |
| GB (1) | GB201719126D0 (en) |
| IE (1) | IE20180281U1 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113214128A (en) * | 2021-05-26 | 2021-08-06 | 乳源东阳光药业有限公司 | Preparation method of small-particle-size benzoyl peroxide |
-
2017
- 2017-09-17 CN CN201710836676.8A patent/CN108239010A/en not_active Withdrawn
- 2017-11-20 GB GBGB1719126.3A patent/GB201719126D0/en not_active Ceased
-
2018
- 2018-08-13 AU AU2018101146A patent/AU2018101146A4/en not_active Ceased
- 2018-08-23 IE IE20180281U patent/IE20180281U1/en unknown
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113214128A (en) * | 2021-05-26 | 2021-08-06 | 乳源东阳光药业有限公司 | Preparation method of small-particle-size benzoyl peroxide |
Also Published As
| Publication number | Publication date |
|---|---|
| AU2018101146A4 (en) | 2018-09-13 |
| IE20180281U1 (en) | 2020-10-14 |
| GB201719126D0 (en) | 2018-01-03 |
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Application publication date: 20180703 |