CN109336802A - The synthetic method of diacyl peroxide - Google Patents

The synthetic method of diacyl peroxide Download PDF

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Publication number
CN109336802A
CN109336802A CN201811384655.8A CN201811384655A CN109336802A CN 109336802 A CN109336802 A CN 109336802A CN 201811384655 A CN201811384655 A CN 201811384655A CN 109336802 A CN109336802 A CN 109336802A
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amino acid
synthetic method
diacyl peroxide
peroxide
added
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CN109336802B (en
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陈唐建
翟志强
许淑女
黄燕民
崔黎明
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Zibo Zhenghua Auxiliary Co Ltd
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Zibo Zhenghua Auxiliary Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C407/00—Preparation of peroxy compounds
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
    • B01J31/02—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides
    • B01J31/06—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides containing polymers
    • B01J31/068—Polyalkylene glycols

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The invention belongs to technical field of chemical synthesis, and in particular to a kind of synthetic method of diacyl peroxide.Acyl compounds, hydrogen peroxide and polyvinyl alcohol compounded amino acid catalyst are added into organic solvent and stirs dehydration synthesis of diacyl peroxide；The polyvinyl alcohol compounded amino acid catalyst is polymerize to obtain by spherical polyethylene alcohol parent with compound amino acid.The present invention avoids optimizing the synthesis technology of peroxide using expensive chemical raw material acyl chlorides in peroxide production process, reduces in industrial processes containing chloride waste water/solid discharge of giving up.

Description

The synthetic method of diacyl peroxide
Technical field
The invention belongs to technical field of chemical synthesis, and in particular to a kind of synthetic method of diacyl peroxide.
Background technique
Diacyl peroxide is industrial critically important macromolecular polymerization reaction initiator, especially suitable for polyacrylic acid Ester, polyethylene, polyvinyl chloride and polystyrene products.Industrially, diacyl peroxide is by hydrogen peroxide and corresponding acyl chlorides It is made.As dilauroyl peroxide be using lauroyl chloride, sodium peroxide as Material synthesis, talkyl peropivalate be with uncle oneself Alcohol hydrogen peroxide, 20%NaOH solution and pivaloyl chloride are Material synthesis, can also synthesize peroxidating pivalic acid with similar method Tert-pentyl ester and the tertiary heptyl ester of peroxidating pivalic acid.The synthetic method of cumyl peroxide is: first by isopropylbenzene and air reaction Cumyl hydroperoxide is generated, then cumyl hydroperoxide is reacted with sodium sulfite again generates benzylalcohol, under perchloric acid catalysis Benzylalcohol is reacted with cumyl hydroperoxide again generates cumyl peroxide.
CN107311906A discloses a kind of production technology of di-tert-butyl peroxide, hydrogen peroxide and the tert-butyl alcohol and urges in sulfuric acid The step that reacts under change obtains di-tert-butyl peroxide, shortens the production cycle, reduces energy consumption, reduces Waste Sulfuric Acid It generates.
CN104557652A discloses a kind of preparation method of tert-butyl peroxide, using the tert-butyl alcohol and hydrogen peroxide as raw material, Using acid-exchange resin as catalyst, back flow reaction is cooling, and settle and separate obtains oily phase and water phase liquid separation；Oily phase is through alkali After washing and washing, di-tert-butyl peroxide solution is obtained.
CN101298429A discloses the preparation method of a kind of tert-butyl hydroperoxide and di-tert-butyl peroxide, certain After sulfuric acid, hydrogen peroxide, the phosphotungstic acid of concentration mix, the tert-butyl alcohol is added in mixed solution, or the tert-butyl alcohol is added in mixed solution In；0.5~5h is reacted at 20~60 DEG C, reacting coarse product liquid separation obtains oily phase；Oily phase obtains tert-butyl hydroperoxide through rectification under vacuum With di-tert-butyl peroxide product.
CN107056670A discloses a kind of preparation method of two tertiary base peroxide, is by the tert-butyl alcohol, hydrogen peroxide, catalysis Agent returns in micro-reaction device in a continuous manner, so that peroxidization occurs for the tert-butyl alcohol and hydrogen peroxide, being made includes two Then the logistics of tert-butyl peroxide draws the logistics comprising di-tert-butyl peroxide from micro-reaction device, through dividing From, washing, be dried to obtain di-tert-butyl peroxide.
CN105523982A discloses a kind of preparation method of tert-butyl hydroperoxide, including peroxidization and condensation are instead It answers, is using the concentrated sulfuric acid as catalyst, with hydrogen peroxide and the tert-butyl alcohol in 10~50 DEG C of 0.5~4h of reaction, reacting coarse product has Machine is mutually intermediate product tert-butyl hydroperoxide and by-product di-tert-butyl peroxide, removes by-product two using at salt technology Tert-butyl peroxide；It is above-mentioned it is inorganic be added to carbonochloridic acid -2- ethylhexyl, sodium hydroxide solution is catalyst, 10 ~50 DEG C of 1.0~6h of reaction, obtain the peroxidating -2- ethylhexyl carbonate tert-butyl ester.
CN105237453A discloses a kind of side for making catalyst preparation methyl ethyl ketone peroxide using acid-exchange resin Method is to make catalyst using butanone and hydrogen peroxide as raw material with acid-exchange resin, is dilution with dibutyl phthalate Agent, after constant temperature is stirred to react, settle and separate, gained oil is mutually methyl ethyl ketone peroxide.
CN1871358A discloses a kind of method by biomass production hydro carbons and oxygenatedchemicals, the carbon for plant origin Hydrate fermenting substrate is to produce C1~C5Alcohols and synthesis higher carbon alcohols and other oxygenatedchemicals.Synthesis material is Biogas obtained and C2~C5Alcohols, wherein the leucine optionally acted on from yeast autolysis, isoleucine and valine or The amino acid of its mixture is used as biocatalyst in fermentation stage.
It can be seen that it is expensive chemical raw material that the shortcomings that above-mentioned synthetic method, which is acyl chlorides itself,；In addition, using acyl chlorides meeting Hydrogen chloride by-product is resulted in, this by-product is a kind of corrosive substance；Moreover, the use of acyl chlorides being that raw material can also be with chlorine There is environmental issue in compound waste water/solid form of giving up.
Summary of the invention
It is scientific and reasonable the object of the present invention is to provide a kind of synthetic method of diacyl peroxide, it is simple and easy, it avoids Using expensive chemical raw material acyl chlorides, environment protecting is good.
The synthetic method of diacyl peroxide of the present invention, steps are as follows:
Acyl compounds, hydrogen peroxide and the stirring dehydration of polyvinyl alcohol compounded amino acid catalyst are added into organic solvent React synthesis of diacyl peroxide；
The polyvinyl alcohol compounded amino acid catalyst is polymerize to obtain by spherical polyethylene alcohol parent with compound amino acid.
The spherical polyethylene alcohol parent is by obtaining after polyvinyl alcohol and cross-linking agents.
The polyvinyl alcohol trade mark is more, it is domestic generally have 0588,0599,1788,1799,2088,2099,2488, 2499 equal products, generally select the products such as 0588,0599,1788,1799,2088,2099,2488,2499, it is preferable to use 1788, the products such as 1799,2088,2099, more preferable 1788 polyvinyl alcohol product.
The crosslinking agent is one or more of glutaraldehyde, terephthalic aldehyde or formaldehyde.Since glutaraldehyde is as crosslinking Agent is fast with crosslinking rate, cross-linked network is big, low toxin, so the preferred glutaraldehyde as cross linker of the present invention.
The compound amino acid is cysteine, phenylalanine, alanine, methionine, glycine, glutamic acid, paddy ammonia Amide, arginine, lysine, tyrosine, leucine, L-aminobutanedioic acid, asparagine, proline, tryptophan, serine, Soviet Union's ammonia Two or more in acid, valine, isoleucine or histidine；Preferred compound amino acid is cysteine, paddy ammonia Two or more in acid, arginine, L-aminobutanedioic acid, proline, glycine, tyrosine, histidine or serine.
The preferred compound amino acid of the present invention is the mixed of cysteine, glutamic acid, arginine, L-aminobutanedioic acid and proline Close object.
The preferred compound amino acid of the present invention is the mixing of cysteine, glycine, tyrosine, proline and histidine Object.
The preferred compound amino acid of the present invention is the mixing of cysteine, glutamic acid, arginine, serine and histidine Object.
The additive amount of the polyvinyl alcohol compounded amino acid catalyst is the 1~100% of hydrogen peroxide quality.
The additive amount of polyvinyl alcohol compounded amino acid catalyst depends on known to the technical staff of peroxide reactions field Several factors, including the reactivity between hydrogen peroxide and acyl compounds；Reaction condition such as temperature and reaction time, and Mixing speed etc..In the present invention, using the quality of the hydrogen peroxide of addition as radix, polyvinyl alcohol compounded amino acid catalyst The preferred ratio of additive amount be between 5% to 50% quality, more preferably between 15% to 25%.
Specific preparation process is as follows for the polyvinyl alcohol compounded amino acid catalyst:
(1) polyvinyl alcohol is dissolved in distilled water, in 100 DEG C of stirred in water bath 5h, is cooled to room temperature, crosslinking agent is added, Raw material first is obtained after stirring；
(2) it takes surfactant span80 to be added in hexamethylene, obtains raw material second after mixing evenly；
(3) raw material first is added in there-necked flask, hydrochloric acid solution is added, after mixing evenly, raw material second is added, control is stirred Speed is mixed in 400~600r/min, reacts 4h at room temperature, is then slowly warming up to 70 DEG C of reaction 4h, after cooling, filtering, Washing obtains spherical polyethylene alcohol parent, spare.
(4) dimethyl sulfoxide and spherical polyethylene alcohol parent are added in there-necked flask, adds compound amino acid, mixes Afterwards, 8h is stirred to react under 90~110 DEG C of constant temperature, it is cooling, filter, with ethanol washing twice, obtain that there is catalysis to live after dry The spherical polyethylene alcohol compounded amino acid catalyst of property group.
Polyvinyl alcohol compounded amino acid catalyst of the present invention is, using crosslinking agent, to pass through reverse phase using polyvinyl alcohol as raw material Polymerization obtains spherical polyethylene alcohol, and it is reacted with compound amino acid, and it is poly- to obtain the spherical shape with catalytic action of the invention Vinyl alcohol compounded amino acid catalyst.
The organic solvent is petroleum ether or pentane.
The structural formula of the acyl compounds is R-C (=O) OH, wherein R group is linear chain or branched chain or has fragrant The C of ring1~C16Group.R group can be but not limited to, methyl, ethyl, propyl, butyl, isobutyl group, tert-butyl, and amyl is different Amyl, tertiary pentyl, cyclopenta, cyclohexyl, phenyl, benzyl, phenethyl, phenylpropyl, iso-octyl, undecyl, dodecyl, Tridecyl, myristyl, pentadecyl, cetyl etc..
The molar ratio of the hydrogen peroxide and acyl compounds is 1:10~5:1.
Generally for improving reaction product yield, hydrogen peroxide and acyl compounds can molar ratios in a wider range It is reacted.Preferred hydrogen peroxide is that 1:2 is reacted with the molar ratio of acyl compounds in the method for the present invention.
The reaction temperature be -20~120 DEG C, the reaction time be 1~for 24 hours.
According to the method for the present invention, peroxide reactions can be reacted in wider temperature range.Usual situation Lower reaction temperature control is between -20 DEG C to 120 DEG C, preferably 0 DEG C to 60 DEG C, more preferably 20 DEG C to 40 DEG C.Generally according to The physicochemical properties of product itself, are varied reaction temperature.The preferred reaction time is 4~8h.
The dehydration is to strip by azeotropic distillation, molecular distillation, with dry air or carried out with inert gas stripping Dehydration.
In the chemical reaction process for generating diacyl peroxide by hydrogen peroxide and acyl compounds reaction, have anti- Water is answered to generate.The reaction water will be removed from reaction mixture in time, for example, by azeotropic distillation, molecular distillation, with dry empty Gas or inert gas such as nitrogen stripping are dehydrated；The preferred azeotropic distillation of the present invention, dry air or inert gas such as nitrogen stripping；More It is preferred that azeotropic distillation removes reaction water.
Azeotropic distillation removal reaction water solvent for use have benzene,toluene,xylene, ethylbenzene, butane, pentane, hexane, heptane, Isoheptane, octane, isooctane, pentamethylene, hexamethylene, methyl cyclopentane, hexahydrotoluene, petroleum ether or light petrol；It is preferred that molten Agent toluene, dimethylbenzene, pentane, hexane, pentamethylene, hexamethylene, petroleum ether or light petrol；More preferable solvent is pentane or petroleum Ether.
The present invention is by preparing acyl compounds and hydrogen peroxide under polyvinyl alcohol compound amino acid catalyst action The method of diacyl peroxide.Diacyl peroxide such as peroxidating two-(3,5,5- trimethyl acetyl), diphenyl peroxide first Acyl etc..
The present invention uses polyvinyl alcohol compound amino acid catalyst synthesis of diacyl peroxide, especially applies The diacyl peroxide initiator of polyacrylic acid, polyethylene, polyvinyl chloride and polystyrene type field.The present invention overcomes existing There is the shortcomings that technology, using polyvinyl alcohol compound amino acid catalyst synthesis of diacyl peroxide.
Document " synthesis, structure and the chelating huge sum of money function of dominant of the cross-linking polyvinyl alcohol of epoxidation containing amino acid " (Zhejiang industry College journal, 2009,37 (5): 515-519) a kind of high-molecular polyvinyl alcohol chelating agent containing amino acid is described, as one The chelating agent of hazardous solid waste of the kind processing containing heavy metal uses.The present invention is applied for the first time catalyzing and synthesizing peroxide field Polyvinyl alcohol compounded amino acid catalyst has novelty.
The present invention is compared with the polyvinyl alcohol containing amino acid of existing literature, although being all the poly- second containing amino acid Enol, but the chemical structure of the two is completely different.Document " synthesis of the cross-linking polyvinyl alcohol of epoxidation containing amino acid, Structure and chelating the huge sum of money function of dominant " high-molecular polyvinyl alcohol chelating agent be by epoxychloropropane polyvinyl alcohol and amino acid It links together, the present invention is by esterification, amino acid and the polyethylene between amino acid and the hydroxyl of polyvinyl alcohol Etherified reaction and the hydrogen-oxygen between amino acid and polyvinyl alcohol are keyed together, are completely different in chemical structure Sample.
Use the polyethylene ball for containing specific combination amino acid as the synthetic catalyst of peroxide be the present invention for the first time It was found that, there is novelty.Compared with amino acid or ispol, of the invention combination amino acid and polyvinyl alcohol In conjunction with, it is the key that the polyethylene ball containing specific combination amino acid has catalytic action, the combination of preferred several amino acid, In distinctive space, amino, carboxyl, hydroxyl and the sulfydryl contained in catalyst spheres has played concerted catalysis effect, catalysis Peroxide synthesis.
Beneficial effects of the present invention are as follows:
The present invention avoids optimizing peroxide using expensive chemical raw material acyl chlorides in peroxide production process Synthesis technology, reduce in industrial processes containing chloride waste water/solid discharge of giving up.
Specific embodiment
The present invention is described further with reference to embodiments.
Cysteine, glutamic acid, arginine, L-aminobutanedioic acid and each portion of proline five amino acid, are mixed to get compound Amino acid A.
Cysteine, glycine, tyrosine, proline and each portion of histidine five amino acid, are mixed to get compound ammonia Base acid B.
Cysteine, glutamic acid, arginine, serine and each portion of histidine five amino acid, are mixed to get compound ammonia Base acid C.
Polyvinyl alcohol compounded amino acid catalyst synthesizes by the following method:
(1) 10g polyvinyl alcohol (1788) is dissolved in 200ml distilled water, in 100 DEG C of stirred in water bath 5h, is cooled to room Temperature is added 2.1ml glutaraldehyde solution (50%), raw material first is obtained after stirring；
(2) it takes 4g surfactant span80 to be added in 600ml hexamethylene, obtains raw material second after mixing evenly；
(3) raw material first is added in the there-necked flask of 2000ml, is added 14ml hydrochloric acid solution (0.1mol/L), stirs evenly Afterwards, raw material second is added, controls mixing speed in 400~600r/min, reacts 4h at room temperature, be then slowly warming up to 70 DEG C Reaction 4h is filtered, washed to obtain spherical polyethylene alcohol after cooling, spare.
(4) 200ml dimethyl sulfoxide and 10g spherical polyethylene alcohol are added in 500mL there-necked flask, the compound ammonia of 5.1g is added Base acid A after mixing, is stirred to react 8h under 90~110 DEG C of constant temperature, cooling, filter, with ethanol washing twice, obtained after dry Spherical polyethylene alcohol compounded amino acid catalyst A with catalytic activity group.
(5) 200ml dimethyl sulfoxide and 10g spherical polyethylene alcohol are added in 500mL there-necked flask, the compound ammonia of 4.8g is added Base acid B after mixing, is stirred to react 8h under 90~110 DEG C of constant temperature, cooling, filter, with ethanol washing twice, obtained after dry Spherical polyethylene alcohol compounded amino acid catalyst B with catalytic activity group.
(6) 100ml dimethyl sulfoxide and 10g spherical polyethylene alcohol are added in 500mL there-necked flask, the compound ammonia of 5.2g is added Base acid C after mixing, is stirred to react 8h under 90~110 DEG C of constant temperature, cooling, filter, with ethanol washing twice, obtained after dry Spherical polyethylene alcohol compounded amino acid catalyst C with catalytic activity group.
Embodiment 1
In 500ml there-necked flask, petroleum ether (60~90 DEG C) 200ml is added, the hydrogen peroxide that purity is 27.5% is added 3,5,5- tri-methyl hexanoic acid 72g is added in 28g, and 6g spherical polyethylene alcohol compound amino acid A is added.It is stirred to react mixture and adds Heat is to 70~80 DEG C of reflux temperature.It is after azeotropic distillation, distillate is cooling, reaction water is removed in water segregator.Isolate petroleum Ether is simultaneously returned in reaction vessel.After reacting 4h, shown by gas chromatographic analysis, peroxidating two-(3,5,5- front threes Base hexanoyl) product yield is 86.9%.
Embodiment 2
In 500ml there-necked flask, petroleum ether (60~90 DEG C) 200ml is added, the hydrogen peroxide that purity is 27.5% is added 3,5,5- tri-methyl hexanoic acid 72g is added in 28g, and 4g spherical polyethylene alcohol compound amino acid B is added.It is stirred to react mixture and adds Heat is to 70~80 DEG C of reflux temperature.It is after azeotropic distillation, distillate is cooling, reaction water is removed in water segregator.Isolate petroleum Ether is simultaneously returned in reaction vessel.After reacting 4h, shown by gas chromatographic analysis, peroxidating two-(3,5,5- front threes Base hexanoyl) product yield is 65.6%.
Embodiment 3
In 500ml there-necked flask, petroleum ether (60~90 DEG C) 200ml is added, the hydrogen peroxide that purity is 27.5% is added 3,5,5- tri-methyl hexanoic acid 72g is added in 28g, and 2g spherical polyethylene alcohol compound amino acid C is added.It is stirred to react mixture and adds Heat is to 70~80 DEG C of reflux temperature.It is after azeotropic distillation, distillate is cooling, reaction water is removed in water segregator.Isolate petroleum Ether is simultaneously returned in reaction vessel.After reacting 4h, shown by gas chromatographic analysis, peroxidating two-(3,5,5- front threes Base hexanoyl) product yield is 60.7%.
Embodiment 4
In 500ml there-necked flask, pentane 200ml is added, the hydrogen peroxide 28g that purity is 27.5% is added, is added 3,5,5- 1g spherical polyethylene alcohol compound amino acid A is added in tri-methyl hexanoic acid 72g.It is stirred to react mixture and is heated to reflux temperature 70 ~80 DEG C.It is after azeotropic distillation, distillate is cooling, reaction water is removed in water segregator.It isolates pentane and is returned to In reaction vessel.After reacting 8h, shown by gas chromatographic analysis, peroxidating two-(3,5,5- trimethyl acetyl) product yield It is 61.3%.
Embodiment 5
In 500ml there-necked flask, pentane 200ml is added, the hydrogen peroxide 28g that purity is 27.5% is added, is added 3,5,5- 3g spherical polyethylene alcohol compound amino acid B is added in tri-methyl hexanoic acid 72g.It is stirred to react mixture and is heated to reflux temperature 70 ~80 DEG C.It is after azeotropic distillation, distillate is cooling, reaction water is removed in water segregator.It isolates pentane and is returned to In reaction vessel.After reacting 8h, shown by gas chromatographic analysis, peroxidating two-(3,5,5- trimethyl acetyl) product yield It is 94.0%.
Embodiment 6
In 500ml there-necked flask, petroleum ether (60~90 DEG C) 200ml is added, the hydrogen peroxide that purity is 27.5% is added 3,5,5- tri-methyl hexanoic acid 72g is added in 28g, and 5g spherical polyethylene alcohol compound amino acid C is added.It is stirred to react mixture and adds Heat is to 70~80 DEG C of reflux temperature.It is after azeotropic distillation, distillate is cooling, reaction water is removed in water segregator.Isolate petroleum Ether is simultaneously returned in reaction vessel.After reacting 4h, shown by gas chromatographic analysis, peroxidating two-(3,5,5- front threes Base hexanoyl) product yield is 72.8%.
Embodiment 7
In 500ml there-necked flask, petroleum ether (60~90 DEG C) 200ml is added, the hydrogen peroxide that purity is 27.5% is added Benzoic acid 71g is added in 36g, and 6g spherical polyethylene alcohol compound amino acid A is added.It is stirred to react mixture and is heated to reflux temperature 70~80 DEG C of degree.It is after azeotropic distillation, distillate is cooling, reaction water is removed in water segregator.Isolate petroleum ether and its is heavy It is new to return in reaction vessel.After reacting 4h, shown by gas chromatographic analysis, dibenzoyl peroxide yield is 80.4%.
Embodiment 8
In 500ml there-necked flask, pentane 200ml is added, the hydrogen peroxide 36g that purity is 27.5% is added, benzoic acid is added 3g spherical polyethylene alcohol compound amino acid B is added in 71g.It is stirred to react mixture and is heated to 70~80 DEG C of reflux temperature.Azeotropic It is after distillation, distillate is cooling, reaction water is removed in water segregator.It isolates pentane and is returned in reaction vessel. After reacting 4h, shown by gas chromatographic analysis, dibenzoyl peroxide yield is 76.2%.
Embodiment 9
In 500ml there-necked flask, pentane 200ml is added, the hydrogen peroxide 36g that purity is 27.5% is added, benzoic acid is added 1g spherical polyethylene alcohol compound amino acid C is added in 71g.It is stirred to react mixture and is heated to 70~80 DEG C of reflux temperature.Azeotropic It is after distillation, distillate is cooling, reaction water is removed in water segregator.It isolates pentane and is returned in reaction vessel. After reacting 4h, shown by gas chromatographic analysis, dibenzoyl peroxide yield is 61.5%.
Comparative example 1
In 500ml flask, the sodium hydroxide solution 110g that content is 25% is added, stirring is cooled to 0 DEG C；Into solution The hydrogen peroxide 40g that purity is 27.5% is added dropwise, reacts 30min, temperature is controlled at 10~30 DEG C；After stirring evenly into flask It is 80% isononanoyl chloride and solvent naphtha mixed solution 100g that concentration, which is slowly added dropwise, and reaction temperature control is at 10~30 DEG C, the used time 30min is added, and is stirred to react 100min after adding isononanoyl chloride solution；Stop stirring after reaction, stands 30min, it will be anti- It answers mother liquor to separate, reaction product is washed until pH value is 5~7；Be made content be 77.3% peroxidating two-(3, 5,5- trimethyl acetyl).

Claims (10)

1. a kind of synthetic method of diacyl peroxide, it is characterised in that steps are as follows:
Acyl compounds, hydrogen peroxide and polyvinyl alcohol compounded amino acid catalyst are added into organic solvent and stirs dehydration Synthesis of diacyl peroxide；
The polyvinyl alcohol compounded amino acid catalyst is polymerize to obtain by spherical polyethylene alcohol parent with compound amino acid.
2. the synthetic method of diacyl peroxide according to claim 1, it is characterised in that the spherical polyethylene Alcohol parent is by obtaining after polyvinyl alcohol and cross-linking agents.
3. the synthetic method of diacyl peroxide according to claim 2, it is characterised in that the crosslinking agent is penta One or more of dialdehyde, terephthalic aldehyde or formaldehyde.
4. the synthetic method of diacyl peroxide according to claim 1, it is characterised in that the compound amino acid For cysteine, phenylalanine, alanine, methionine, glycine, glutamic acid, glutamine, arginine, lysine, junket ammonia Acid, leucine, L-aminobutanedioic acid, asparagine, proline, tryptophan, serine, threonine, valine, isoleucine or group ammonia Two or more in acid.
5. the synthetic method of diacyl peroxide according to claim 1, it is characterised in that the polyvinyl alcohol is multiple The additive amount for closing amino acid catalyst is the 1~100% of hydrogen peroxide quality.
6. the synthetic method of diacyl peroxide according to claim 1, it is characterised in that the organic solvent is Petroleum ether or pentane.
7. the synthetic method of diacyl peroxide according to claim 1, it is characterised in that the acyl compounds Structural formula be R-C (=O) OH, wherein R group is linear chain or branched chain or the C with aromatic rings1~C16Group.
8. the synthetic method of diacyl peroxide according to claim 1, it is characterised in that the hydrogen peroxide with The molar ratio of acyl compounds is 1:10~5:1.
9. the synthetic method of diacyl peroxide according to claim 1, it is characterised in that the reaction temperature be- 20~120 DEG C, the reaction time be 1~for 24 hours.
10. the synthetic method of diacyl peroxide according to claim 1, it is characterised in that the dehydration is to pass through Azeotropic distillation, molecular distillation are stripped with dry air or are dehydrated with inert gas stripping.
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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101215251A (en) * 2008-01-10 2008-07-09 江苏强盛化工有限公司 Method for preparing 3,4-dichlorobenzoperoxide
CN102199115A (en) * 2011-04-15 2011-09-28 江苏强盛功能化学股份有限公司 Method for preparing benzoyl peroxide
CN102532352A (en) * 2011-12-26 2012-07-04 淄博正华助剂股份有限公司 Preparation method of emulsion-type 50wt% bis-(3,5,5-trimethyl caproyl) peroxide
CN102558010A (en) * 2011-12-02 2012-07-11 江苏远洋药业股份有限公司 Preparation method of benzoyl peroxide

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101215251A (en) * 2008-01-10 2008-07-09 江苏强盛化工有限公司 Method for preparing 3,4-dichlorobenzoperoxide
CN102199115A (en) * 2011-04-15 2011-09-28 江苏强盛功能化学股份有限公司 Method for preparing benzoyl peroxide
CN102558010A (en) * 2011-12-02 2012-07-11 江苏远洋药业股份有限公司 Preparation method of benzoyl peroxide
CN102532352A (en) * 2011-12-26 2012-07-04 淄博正华助剂股份有限公司 Preparation method of emulsion-type 50wt% bis-(3,5,5-trimethyl caproyl) peroxide

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