CN106349139A - Preparation method of high-purity benzoyl peroxide - Google Patents
Preparation method of high-purity benzoyl peroxide Download PDFInfo
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- CN106349139A CN106349139A CN201610736079.3A CN201610736079A CN106349139A CN 106349139 A CN106349139 A CN 106349139A CN 201610736079 A CN201610736079 A CN 201610736079A CN 106349139 A CN106349139 A CN 106349139A
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- benzoyl peroxide
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C407/00—Preparation of peroxy compounds
- C07C407/003—Separation; Purification; Stabilisation; Use of additives
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a preparation method of high-purity benzoyl peroxide. The high-purity benzoyl peroxide is prepared through a synthesis process and a purification process. Alkali selected in the synthesis process is ammonium hydrogen carbonate, so that reaction safety is high, overall reaction is mild and control, and product purity can reach 99.5% and higher. A solvent selected in the purification process is safe and has lower toxicity than chloroform and methanol, operation is easy, and obtained crystal particles are large.
Description
Technical field
The present invention relates to a kind of preparation method of benzoyl peroxide is and in particular to a kind of preparation of high-purity benzoyl peroxide
Method.
Background technology
Benzoyl peroxide is also known as dibenzoyl peroxide, and English name is: dibenzoyl peroxide(is referred to as
Bpo).Its molecular formula is: c14h10o4；Molecular weight is: 242.22；Structural formula is:
Bpo is a kind of broad-spectrum diacyl organic peroxide, white graininess, and micro- have bitter almond odor, belongs to strong
Oxidant.It is mainly used as vinyl monomer polymerization initiator and unsaturated-resin class firming agent, can act also as silicone rubber and fluorine rubber
The cross-linking agent of glue, the anti-oxidation and antisepsis additive of feed industry.Additionally, being alternatively arranged as bleach and oxidant, for oils and fatss
Exquisite, flour brighten, the decolouring of fiber etc..And in medical industry, be commonly used for being configured to various for treating acne
External preparation etc. diseases such as dermatosiss and chronic ulcers.
At present, the existing multiple methods of industrialized production bpo, the method that China produces bpo is mainly Benzenecarbonyl chloride. highly basic oxygen
Change method, the technical process of this method is: is furnished with agitating device and the reactor of temperature measuring equipment to one and puts into the liquid measuring
Alkali and hydrogen peroxide, and control temperature at 5 DEG C about, then press proportioning Deca Benzenecarbonyl chloride. thereto, and need to be by reaction temperature control
At 5 DEG C about, after reaction terminates, to obtain bpo finished product through filtering, washing and separate.
Existing industrialized production does alkali from sodium hydroxide mostly, and alkalescence is stronger, and reaction temperature need to control in -10-0
DEG C, energy consumption is big, and reaction is wayward, easily produces impurity, and product purity is not high；Or do alkali from sodium carbonate, easily
Produce substantial amounts of bubble, have the risk of slug；Add surfactant to be catalyzed, such as dodecyl sodium sulfate, then react meeting
Produce a large amount of foams, have the possibility of spilling, wayward.
Content of the invention
Present invention aims to the deficiencies in the prior art, now provide that a kind of reaction condition is gentle, processing step is simple
The preparation method of the high-purity benzoyl peroxide single, purification rate is high.
For solving above-mentioned technical problem, the technical solution used in the present invention is: a kind of preparation of high-purity benzoyl peroxide
Method, its innovative point is: completes the preparation of high-purity benzoyl peroxide through synthesis technique and purifying process；Described concrete step
Suddenly as follows:
(1) synthesis technique:
A. the hydrogen peroxide of concentration 30% is added in the reactor of 50l, opens stirring, be subsequently adding ammonium hydrogen carbonate, be slowly added dropwise
Benzenecarbonyl chloride., described reactor temperature is 20-30 degree Celsius, and the described response time is 2.5-3.5 hour；
B. reacted reactant liquor is filtered, be filtrated to get filter cake, described washing 20- that filter cake is pulled an oar in mixed solvent
40 minutes, filter；
C. carry out making beating washing 10-20 minute with clear water, repeat making beating washing 3 times；
D. finally carry out drip washing with clear water, be filtered dry, obtain white benzoyl peroxide crude product；
(2) purifying process:
E. white benzoyl peroxide crude product is put in 200l reactor, in reactor, add dichloromethane, control reactor
Interior temperature is 20-30 degree Celsius, stirs to molten clear；
F. by ethanol filter pressing to head tank, Deca ethanol under room temperature condition, open refrigeration, reacting liquid temperature is down to -5-0 Celsius
Degree, crystallize 2.5-3.5 hour of lowering the temperature；
G. filter after the completion of crystallize, after being filtered dry, filter cake taking-up is carried out making beating washing 20-40 minute with clear water, repeat making beating and wash
Wash 3 times, finally give white high-purity benzoyl peroxide.
Further, in described step (1), mixed solvent is the mixed solvent of ethanol and clear water, described ethanol and clear water
Mixing quality is than for 1:1.
Further, the hydrogen peroxide in described step (1), the mass ratio of ammonium hydrogen carbonate, toluene acyl chlorides and mixed solvent are
1-1.5:0.6-0.9:1:1-2.
Further, the usage amount of clear water in described step c and step d and the mass ratio of Benzenecarbonyl chloride. are 2-3:1.
Further, the dichloromethane in described step (2), the mass ratio of ethanol, clear water and Benzenecarbonyl chloride. are 2.5-
3.5:5-7:1.3-1.5:1.
Beneficial effects of the present invention are as follows:
(1) alkali selected in the synthesis technique of the present invention is ammonium hydrogen carbonate, and reaction safety is high, W-response gentle, controlled and
Product purity can reach 99.5% and its more than.
(2) in the purifying process of the present invention select solvent all safer, than chloroform and methanol small toxicity it is easy to behaviour
Make, the crystalline particle obtaining is big.
Specific embodiment
Hereinafter embodiments of the present invention are illustrated by particular specific embodiment, those skilled in the art can be by this explanation
Content disclosed by book understands other advantages and effect of the present invention easily.
Embodiment 1
A kind of preparation method of high-purity benzoyl peroxide, completes high-purity benzoyl peroxide through synthesis technique and purifying process
Preparation；Specifically comprise the following steps that
(1) synthesis technique:
A. the hydrogen peroxide of 15kg concentration 30% is added in the reactor of 50l, opens stirring, be subsequently adding 9.3kg bicarbonate
Ammonium, is slowly added dropwise 15kg Benzenecarbonyl chloride., and reactor temperature is 20 degrees Celsius, and the response time is 2.5 hours；
B. reacted reactant liquor is filtered, is filtrated to get filter cake, by filter cake 15kg ethanol and 15kg clear water mixing
In solvent, making beating washing 20 minutes, filter；
C. carry out making beating washing 10 minutes with 30kg clear water, repeat making beating washing 3 times；
D. finally carry out drip washing with 30kg clear water, be filtered dry, obtain 15.79kg white benzoyl peroxide crude product；
(2) purifying process:
E. white benzoyl peroxide crude product is put in 200l reactor, in reactor, add 37.5kg dichloromethane, control
Reactor temperature is 20 degrees Celsius, stirs to molten clear；
F. by 75kg ethanol filter pressing to head tank, Deca ethanol under room temperature condition, open refrigeration, reacting liquid temperature is down to -5 and takes the photograph
Family name's degree, cooling crystallize 2.5 hours；
G. filter after the completion of crystallize, after being filtered dry, filter cake is taken out and carries out making beating washing 20 minutes with 18kg clear water, repeat making beating and wash
Wash 3 times, finally give 13.5kg white high-purity benzoyl peroxide.
Under the present embodiment, the purity of the benzoyl peroxide of preparation is 99.5%.
Embodiment 2
A kind of preparation method of high-purity benzoyl peroxide, completes high-purity benzoyl peroxide through synthesis technique and purifying process
Preparation；Specifically comprise the following steps that
(1) synthesis technique:
A. the hydrogen peroxide of 22kg concentration 30% is added in the reactor of 50l, opens stirring, be subsequently adding 13.5kg bicarbonate
Ammonium, is slowly added dropwise 15kg Benzenecarbonyl chloride., and reactor temperature is 30 degrees Celsius, and the response time is 3.5 hours；
B. reacted reactant liquor is filtered, is filtrated to get filter cake, by filter cake 30kg ethanol and 30kg clear water mixing
In solvent, making beating washing 40 minutes, filter；
C. carry out making beating washing 20 minutes with 45kg clear water, repeat making beating washing 3 times；
D. finally carry out drip washing with 45kg clear water, be filtered dry, obtain white benzoyl peroxide crude product；
(2) purifying process:
E. white benzoyl peroxide crude product is put in 200l reactor, in reactor, add 52.5kg dichloromethane, control
Reactor temperature is 30 degrees Celsius, stirs to molten clear；
F. by 105kg ethanol filter pressing to head tank, Deca ethanol under room temperature condition, open refrigeration, reacting liquid temperature is down to -5
Degree Celsius, cooling crystallize 2.5 hours；
G. filter after the completion of crystallize, after being filtered dry, filter cake taking-up is carried out making beating washing 20 minutes with clear water, repeat washing 3 of pulling an oar
Secondary, finally give 14.1kg white high-purity benzoyl peroxide.
Under the present embodiment, the purity of the benzoyl peroxide of preparation is 99.5%.
Embodiment 3
A kind of preparation method of high-purity benzoyl peroxide, completes high-purity benzoyl peroxide through synthesis technique and purifying process
Preparation；Specifically comprise the following steps that
(1) synthesis technique:
A. the hydrogen peroxide of 18kg concentration 30% is added in the reactor of 50l, opens stirring, be subsequently adding 10.2kg bicarbonate
Ammonium, is slowly added dropwise 15kg Benzenecarbonyl chloride., and reactor temperature is 25 degrees Celsius, and the response time is 3 hours；
B. reacted reactant liquor is filtered, be filtrated to get filter cake, by filter cake in 22.5kg ethanol and 22.5kg clear water
In mixed solvent, making beating washing 30 minutes, filter；
C. carry out making beating washing 15 minutes with 37.5kg clear water, repeat making beating washing 3 times；
D. finally carry out drip washing with 37.5kg clear water, be filtered dry, obtain 15.82kg white benzoyl peroxide crude product；
(2) purifying process:
E. white benzoyl peroxide crude product is put in 200l reactor, in reactor, add 45kg dichloromethane, control anti-
Answer temperature in the kettle to be 25 degrees Celsius, stir to molten clear；
F. by 90kg ethanol filter pressing to head tank, Deca ethanol under room temperature condition, open refrigeration, reacting liquid temperature is down to -3 and takes the photograph
Family name's degree, cooling crystallize 3 hours；
G. filter after the completion of crystallize, after being filtered dry, filter cake is taken out and carries out making beating washing 30 minutes with 18kg clear water, repeat making beating and wash
Wash 3 times, finally give 13.9kg white high-purity benzoyl peroxide.
Under the present embodiment, the purity of the benzoyl peroxide of preparation is 99.7%.
The alkali selected in the synthesis technique of the present invention is ammonium hydrogen carbonate, and reaction safety is high, W-response gentle, controlled and
Product purity can reach 99.5% and its more than；The solvent selected in the purifying process of the present invention is all safer, than chloroform and first
, it is easy to operate, the crystalline particle obtaining is big for the small toxicity of alcohol.
Above-described embodiment is presently preferred embodiments of the present invention, is not the restriction to technical solution of the present invention, as long as
The technical scheme that can realize on the basis of above-described embodiment without creative work, is regarded as falling into patent of the present invention
Rights protection scope in.
Claims (5)
1. a kind of preparation method of high-purity benzoyl peroxide it is characterised in that: complete height through synthesis technique and purifying process
The preparation of purity benzoyl peroxide；Described specifically comprise the following steps that
Synthesis technique:
The hydrogen peroxide of concentration 30% is added in the reactor of 50l, opens stirring, be subsequently adding ammonium hydrogen carbonate, be slowly added dropwise benzene
Formyl chloride, described reactor temperature is 20-30 degree Celsius, and the described response time is 2.5-3.5 hour；
Reacted reactant liquor is filtered, is filtrated to get filter cake, described washing 20-40 that filter cake is pulled an oar in mixed solvent
Minute, filter；
Carry out making beating washing 10-20 minute with clear water, repeat making beating washing 3 times；
Finally carry out drip washing with clear water, be filtered dry, obtain white benzoyl peroxide crude product；
Purifying process:
E. white benzoyl peroxide crude product is put in 200l reactor, in reactor, add dichloromethane, control reactor
Interior temperature is 20-30 degree Celsius, stirs to molten clear；
F. by ethanol filter pressing to head tank, Deca ethanol under room temperature condition, open refrigeration, reacting liquid temperature is down to -5-0 Celsius
Degree, crystallize 2.5-3.5 hour of lowering the temperature；
G. filter after the completion of crystallize, after being filtered dry, filter cake taking-up is carried out making beating washing 20-40 minute with clear water, repeat making beating and wash
Wash 3 times, finally give white high-purity benzoyl peroxide.
2. a kind of high-purity benzoyl peroxide according to claim 1 preparation method it is characterised in that: described step
(1) in, mixed solvent is the mixed solvent of ethanol and clear water, and the mixing quality of described ethanol and clear water ratio is for 1:1.
3. a kind of high-purity benzoyl peroxide according to claim 1 preparation method it is characterised in that: described step
(1) hydrogen peroxide in, the mass ratio of ammonium hydrogen carbonate, toluene acyl chlorides and mixed solvent are 1-1.5:0.6-0.9:1:1-2.
4. a kind of high-purity benzoyl peroxide according to claim 1 preparation method it is characterised in that: described step c
It is 2-3:1 with the usage amount of the clear water in step d and the mass ratio of Benzenecarbonyl chloride..
5. a kind of high-purity benzoyl peroxide according to claim 1 preparation method it is characterised in that: described step
(2) mass ratio of the dichloromethane in, ethanol, clear water and Benzenecarbonyl chloride. is 2.5-3.5:5-7:1.3-1.5:1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201610736079.3A CN106349139A (en) | 2016-08-29 | 2016-08-29 | Preparation method of high-purity benzoyl peroxide |
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| CN201610736079.3A CN106349139A (en) | 2016-08-29 | 2016-08-29 | Preparation method of high-purity benzoyl peroxide |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107141242A (en) * | 2017-05-04 | 2017-09-08 | 江苏强盛功能化学股份有限公司 | A kind of processing method by introduction of contaminants BPO |
| 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 |
| CN115403498A (en) * | 2022-09-22 | 2022-11-29 | 山东阳谷华泰化工股份有限公司 | Synthesis method of dibenzoyl peroxide |
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| US4155937A (en) * | 1967-04-12 | 1979-05-22 | Polaroid Corporation | Novel polymerization initiators |
| CN1065263A (en) * | 1992-04-15 | 1992-10-14 | 天津大学 | Production of phenylformacyl peroxide |
| KR20010069248A (en) * | 2000-09-25 | 2001-07-25 | 차희태 | Method of purifying benzoylperoxide |
| CN105111122A (en) * | 2015-09-11 | 2015-12-02 | 江苏嘉逸医药有限公司 | Method for synthesizing and purifying benzoyl peroxide |
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2016
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| US4155937A (en) * | 1967-04-12 | 1979-05-22 | Polaroid Corporation | Novel polymerization initiators |
| CN1065263A (en) * | 1992-04-15 | 1992-10-14 | 天津大学 | Production of phenylformacyl peroxide |
| KR20010069248A (en) * | 2000-09-25 | 2001-07-25 | 차희태 | Method of purifying benzoylperoxide |
| CN105111122A (en) * | 2015-09-11 | 2015-12-02 | 江苏嘉逸医药有限公司 | Method for synthesizing and purifying benzoyl peroxide |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107141242A (en) * | 2017-05-04 | 2017-09-08 | 江苏强盛功能化学股份有限公司 | A kind of processing method by introduction of contaminants BPO |
| CN107141242B (en) * | 2017-05-04 | 2019-01-11 | 江苏强盛功能化学股份有限公司 | A kind of processing method by introduction of contaminants BPO |
| 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 |
| CN115403498A (en) * | 2022-09-22 | 2022-11-29 | 山东阳谷华泰化工股份有限公司 | Synthesis method of dibenzoyl peroxide |
| CN115403498B (en) * | 2022-09-22 | 2024-04-30 | 山东阳谷华泰化工股份有限公司 | Synthesis method of dibenzoyl peroxide |
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Application publication date: 20170125 |