CN109336802B - Synthesis method of diacyl peroxide - Google Patents
Synthesis method of diacyl peroxide Download PDFInfo
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- CN109336802B CN109336802B CN201811384655.8A CN201811384655A CN109336802B CN 109336802 B CN109336802 B CN 109336802B CN 201811384655 A CN201811384655 A CN 201811384655A CN 109336802 B CN109336802 B CN 109336802B
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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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- 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
Abstract
The invention belongs to the technical field of chemical synthesis, and particularly relates to a synthesis method of diacyl peroxide. Adding an acyl compound, hydrogen peroxide and a polyvinyl alcohol compound amino acid catalyst into an organic solvent, and stirring and dehydrating to synthesize diacyl peroxide; the polyvinyl alcohol composite amino acid catalyst is obtained by polymerizing a spherical polyvinyl alcohol matrix and composite amino acid. In the peroxide production process, the invention avoids using expensive chemical raw material acyl chloride, optimizes the synthesis process of the peroxide and reduces the discharge of chloride-containing waste water/waste solids in the industrial production process.
Description
Technical Field
The invention belongs to the technical field of chemical synthesis, and particularly relates to a synthesis method of diacyl peroxide.
Background
Diacyl peroxide is an important industrial polymer polymerization initiator, and is especially suitable for polyacrylate, polyethylene, polyvinyl chloride and polystyrene products. Diacyl peroxides are commercially produced from hydrogen peroxide and the corresponding acid chloride. For example, lauroyl peroxide is synthesized from lauroyl chloride and sodium peroxide, tert-hexyl peroxypivalate is synthesized from tert-hexanol hydroperoxide, 20% NaOH solution and pivaloyl chloride, and tert-amyl peroxypivalate and tert-heptyl peroxypivalate can be synthesized by similar methods. The synthesis method of dicumyl peroxide comprises the following steps: firstly, cumene hydroperoxide is generated by the reaction of cumene and air, then the cumene hydroperoxide is reacted with sodium sulfite to generate benzyl alcohol, and the benzyl alcohol is reacted with the cumene hydroperoxide to generate dicumyl peroxide under the catalysis of perchloric acid.
CN107311906A discloses a production process of di-tert-butyl peroxide, hydrogen peroxide and tert-butyl alcohol react under the catalysis of sulfuric acid to obtain the di-tert-butyl peroxide in one step, so that the production period is shortened, the energy consumption is reduced, and the generation of waste sulfuric acid is reduced.
CN104557652A discloses a preparation method of tert-butyl peroxide, which comprises the steps of taking tert-butyl alcohol and hydrogen peroxide as raw materials, taking acidic ion exchange resin as a catalyst, carrying out reflux reaction, cooling, standing and separating to obtain separated oil phase and water phase; and (3) carrying out alkali washing and water washing on the oil phase to obtain a di-tert-butyl peroxide solution.
CN101298429A discloses a method for preparing tert-butyl hydroperoxide and di-tert-butyl peroxide, which comprises mixing sulfuric acid, hydrogen peroxide and phosphotungstic acid at certain concentration, and adding tert-butyl alcohol into the mixed solution, or adding the mixed solution into tert-butyl alcohol; reacting for 0.5-5 h at 20-60 ℃, and separating the crude reaction product to obtain an oil phase; the oil phase is rectified under reduced pressure to obtain tert-butyl hydroperoxide and di-tert-butyl peroxide products.
CN107056670A discloses a preparation method of di-tert-butyl peroxide, which is to return tert-butyl alcohol, hydrogen peroxide and a catalyst to a micro-reaction device in a continuous manner, so that the tert-butyl alcohol and the hydrogen peroxide are subjected to peroxidation to prepare a material flow containing di-tert-butyl peroxide, then the material flow containing the di-tert-butyl peroxide is led out from the micro-reaction device, and the di-tert-butyl peroxide is obtained through separation, water washing and drying.
CN105523982A discloses a preparation method of tert-butyl hydroperoxide, which comprises peroxidation and condensation reaction, concentrated sulfuric acid is used as a catalyst, hydrogen peroxide and tert-butyl alcohol are used for reaction for 0.5-4 h at 10-50 ℃, an organic phase of a reaction crude product is an intermediate product of tert-butyl hydroperoxide and a byproduct of di-tert-butyl peroxide, and the byproduct of di-tert-butyl peroxide is removed by a salt formation technology; adding 2-ethylhexyl chloroformate and sodium hydroxide solution as a catalyst into the inorganic phase, and reacting at 10-50 ℃ for 1.0-6 h to obtain tert-butyl peroxy-2-ethylhexyl carbonate.
CN105237453A discloses a method for preparing methyl ethyl ketone peroxide by using acidic ion exchange resin as a catalyst, which is to use butanone and hydrogen peroxide as raw materials, use acidic ion exchange resin as a catalyst, use dibutyl phthalate as a diluent, stir at a constant temperature for reaction, stand for separation, and obtain an oil phase, namely methyl ethyl ketone peroxide.
CN1871358A discloses a process for the production of hydrocarbons and oxygenates from biomass for the fermentation of plant-derived carbohydrate substrates to produce C1～C5Alcohols and synthesis of higher alcohols and other oxygenates. The synthetic raw materials are prepared biogas and C2～C5Alcohols, whichWherein optionally leucine, isoleucine and valine or mixtures thereof obtained from yeast autolysis are used as biocatalysts during the fermentation stage.
It can be seen that a disadvantage of the above-mentioned synthetic methods is that acid chlorides are themselves expensive chemical starting materials; in addition, the use of acid chlorides can lead to the formation of hydrogen chloride as a by-product, which is a corrosive substance; moreover, the use of acyl chloride as a raw material also presents environmental problems in the form of chloride waste water/waste solids.
Disclosure of Invention
The invention aims to provide a method for synthesizing diacyl peroxide, which is scientific, reasonable, simple and feasible, avoids using expensive chemical raw material acyl chloride and has good environmental protection effect.
The synthesis method of the diacyl peroxide comprises the following steps:
adding an acyl compound, hydrogen peroxide and a polyvinyl alcohol compound amino acid catalyst into an organic solvent, and stirring and dehydrating to synthesize diacyl peroxide;
the polyvinyl alcohol composite amino acid catalyst is obtained by polymerizing a spherical polyvinyl alcohol matrix and composite amino acid.
The spherical polyvinyl alcohol matrix is obtained by crosslinking polyvinyl alcohol and a crosslinking agent.
The polyvinyl alcohol is available in many grades, products such as 0588, 0599, 1788, 1799, 2088, 2099, 2488 and 2499 are generally selected, products such as 1788, 1799, 2088 and 2099 are preferably used, and 1788 polyvinyl alcohol is more preferably used.
The cross-linking agent is one or more of glutaraldehyde, terephthaldehyde or formaldehyde. As glutaraldehyde as the cross-linking agent has the advantages of high cross-linking speed, large cross-linking network, low toxicity and the like, glutaraldehyde is preferably used as the cross-linking agent in the invention.
The compound amino acid is two or more of cysteine, phenylalanine, alanine, methionine, glycine, glutamic acid, glutamine, arginine, lysine, tyrosine, leucine, aspartic acid, asparagine, proline, tryptophan, serine, threonine, valine, isoleucine or histidine; the preferable compound amino acid is two or more of cysteine, glutamic acid, arginine, aspartic acid, proline, glycine, tyrosine, histidine or serine.
More preferred complex amino acids of the invention are mixtures of cysteine, glutamic acid, arginine, aspartic acid and proline.
More preferred complex amino acids of the invention are mixtures of cysteine, glycine, tyrosine, proline and histidine.
More preferred complex amino acids of the invention are a mixture of cysteine, glutamic acid, arginine, serine and histidine.
The addition amount of the polyvinyl alcohol composite amino acid catalyst is 1-100% of the mass of the hydrogen peroxide.
The amount of polyvinyl alcohol complex amino acid catalyst added depends on several factors known to those skilled in the art of peroxide reactions, including the reactivity between hydrogen peroxide and acyl compounds; reaction conditions such as temperature and reaction time, and stirring speed, etc. In the present invention, the polyvinyl alcohol complex amino acid catalyst is added in an amount of preferably 5 to 50% by mass, more preferably 15 to 25% by mass, based on the mass of the hydrogen peroxide added.
The specific preparation steps of the polyvinyl alcohol compound amino acid catalyst are as follows:
(1) dissolving polyvinyl alcohol in distilled water, stirring for 5 hours in a water bath at 100 ℃, cooling to room temperature, adding a cross-linking agent, and stirring to obtain a raw material A;
(2) adding a surfactant span80 into cyclohexane, and uniformly stirring to obtain a raw material B;
(3) adding the raw material A into a three-necked bottle, adding a hydrochloric acid solution, uniformly stirring, adding the raw material B, controlling the stirring speed at 400-600 r/min, reacting at room temperature for 4h, slowly heating to 70 ℃ for reacting for 4h, cooling, filtering, and washing to obtain a spherical polyvinyl alcohol matrix for later use.
(4) Adding dimethyl sulfoxide and a spherical polyvinyl alcohol matrix into a three-necked bottle, adding a compound amino acid, uniformly mixing, stirring and reacting for 8 hours at a constant temperature of 90-110 ℃, cooling, performing suction filtration, washing twice with ethanol, and drying to obtain the spherical polyvinyl alcohol compound amino acid catalyst with a catalytic active group.
The polyvinyl alcohol composite amino acid catalyst is prepared by taking polyvinyl alcohol as a raw material, utilizing a cross-linking agent to obtain spherical polyvinyl alcohol through inverse polymerization, and reacting the spherical polyvinyl alcohol with composite amino acid.
The organic solvent is petroleum ether or pentane.
The acyl compound has a structural formula of R-C (═ O) OH, wherein R is a straight chain or branched chain or C with an aromatic ring1～C16A group. The R group can be, but is not limited to, methyl, ethyl, propyl, butyl, isobutyl, t-butyl, pentyl, isopentyl, t-pentyl, cyclopentyl, cyclohexyl, phenyl, benzyl, phenethyl, phenylpropyl, isooctyl, undecyl, dodecyl, tridecyl, tetradecyl, pentadecyl, hexadecyl, and the like.
The molar ratio of the hydrogen peroxide to the acyl compound is 1: 10-5: 1.
Generally, the hydrogen peroxide and acyl compound may be reacted in a wide range of molar ratios in order to increase the yield of the reaction product. In the process of the present invention, the reaction is preferably carried out with a molar ratio of hydrogen peroxide to acyl compound of 1: 2.
The reaction temperature is-20-120 ℃, and the reaction time is 1-24 h.
According to the process of the present invention, the peroxide reaction can be carried out over a wide temperature range. The reaction temperature is usually controlled to be between-20 ℃ and 120 ℃, preferably between 0 ℃ and 60 ℃, more preferably between 20 ℃ and 40 ℃. The reaction temperature is usually varied according to the physicochemical properties of the product itself. The preferable reaction time is 4-8 h.
The dehydration is carried out by azeotropic distillation, molecular distillation, stripping with dry air or stripping with inert gas.
In the chemical reaction process of reacting hydrogen peroxide with an acyl compound to produce diacyl peroxide, reaction water is generated. The reaction water is removed from the reaction mixture in time, for example by azeotropic distillation, molecular distillation, stripping with dry air or inert gas such as nitrogen for dehydration; azeotropic distillation, dry air or inert gas stripping such as nitrogen is preferred in the present invention; more preferably, the water of reaction is removed by azeotropic distillation.
The solvent for removing the reaction water by azeotropic distillation is benzene, toluene, xylene, ethylbenzene, butane, pentane, hexane, heptane, isoheptane, octane, isooctane, cyclopentane, cyclohexane, methylcyclopentane, methylcyclohexane, petroleum ether or light gasoline; preferably the solvents toluene, xylene, pentane, hexane, cyclopentane, cyclohexane, petroleum ether or light petrol; more preferably the solvent is pentane or petroleum ether.
The invention relates to a method for preparing diacyl peroxide by using acyl compound and hydrogen peroxide under the action of polyvinyl alcohol composite amino acid catalyst. Diacyl peroxides such as bis- (3,5, 5-trimethylhexanoyl) peroxide, dibenzoyl peroxide, and the like.
The invention adopts polyvinyl alcohol composite amino acid catalyst to catalyze and synthesize diacyl peroxide, in particular to a diacyl peroxide initiator applied to the fields of polyacrylic acid, polyethylene, polyvinyl chloride and polystyrene. The invention overcomes the defects of the prior art and adopts the polyvinyl alcohol composite amino acid catalyst to catalyze and synthesize the diacyl peroxide.
The document "synthesis, structure and heavy metal chelating function of amino acid-containing epoxidized crosslinked polyvinyl alcohol" (Zhejiang university school report, 2009, 37(5): 515-. The invention firstly applies the polyvinyl alcohol compound amino acid catalyst in the field of catalytic synthesis of peroxide, and has innovation.
In the present invention, the amino acid-containing polyvinyl alcohols are all the same as the amino acid-containing polyvinyl alcohols of the prior art documents, but the chemical structures of the amino acid-containing polyvinyl alcohols are completely different from those of the prior art documents. The polyvinyl alcohol high-molecular chelating agent disclosed in the document 'synthesis, structure and heavy metal chelating function of amino acid-containing epoxidized crosslinked polyvinyl alcohol' is formed by connecting polyvinyl alcohol and amino acid together through epichlorohydrin.
The invention discloses a novel method for synthesizing a peroxide by using polyethylene spheres containing a specific combination of amino acids. Compared with amino acid or amino acid mixture, the combination of the combined amino acid and polyvinyl alcohol is the key of the catalysis of the polyethylene ball containing the specific combined amino acid, and the preferable combination of several amino acids has the synergistic catalysis effect of amino, carboxyl, hydroxyl and sulfydryl contained in the catalyst ball in a special space to catalyze the synthesis of peroxide.
The invention has the following beneficial effects:
in the peroxide production process, the invention avoids using expensive chemical raw material acyl chloride, optimizes the synthesis process of the peroxide and reduces the discharge of chloride-containing waste water/waste solids in the industrial production process.
Detailed Description
The present invention is further described below with reference to examples.
And 5, mixing one part of each of five amino acids including cysteine, glutamic acid, arginine, aspartic acid and proline to obtain the compound amino acid A.
And (3) mixing one part of each of five amino acids of cysteine, glycine, tyrosine, proline and histidine to obtain the compound amino acid B.
And mixing one part of each of five amino acids including cysteine, glutamic acid, arginine, serine and histidine to obtain the compound amino acid C.
The polyvinyl alcohol compound amino acid catalyst is synthesized by the following method:
(1) dissolving 10g of polyvinyl alcohol (1788) in 200ml of distilled water, stirring for 5 hours in a water bath at 100 ℃, cooling to room temperature, adding 2.1ml of glutaraldehyde solution (50 percent), and stirring to obtain a raw material A;
(2) adding 4g of surfactant span80 into 600ml of cyclohexane, and uniformly stirring to obtain a raw material B;
(3) adding the raw material A into a 2000ml three-necked bottle, adding 14ml hydrochloric acid solution (0.1mol/L), uniformly stirring, adding the raw material B, controlling the stirring speed at 400-600 r/min, reacting at room temperature for 4h, slowly heating to 70 ℃ for reacting for 4h, cooling, filtering, and washing to obtain spherical polyvinyl alcohol for later use.
(4) Adding 200mL of dimethyl sulfoxide and 10g of spherical polyvinyl alcohol into a 500mL three-necked bottle, adding 5.1g of compound amino acid A, uniformly mixing, stirring and reacting for 8 hours at a constant temperature of 90-110 ℃, cooling, performing suction filtration, washing twice with ethanol, and drying to obtain the spherical polyvinyl alcohol compound amino acid catalyst A with a catalytic active group.
(5) Adding 200mL of dimethyl sulfoxide and 10g of spherical polyvinyl alcohol into a 500mL three-necked bottle, adding 4.8g of compound amino acid B, uniformly mixing, stirring and reacting at a constant temperature of 90-110 ℃ for 8h, cooling, performing suction filtration, washing with ethanol twice, and drying to obtain the spherical polyvinyl alcohol compound amino acid catalyst B with a catalytic active group.
(6) Adding 100mL of dimethyl sulfoxide and 10g of spherical polyvinyl alcohol into a 500mL three-necked bottle, adding 5.2g of compound amino acid C, uniformly mixing, stirring at a constant temperature of 90-110 ℃ for reacting for 8 hours, cooling, performing suction filtration, washing with ethanol twice, and drying to obtain the spherical polyvinyl alcohol compound amino acid catalyst C with a catalytic active group.
Example 1
200ml of petroleum ether (60-90 ℃) is added into a 500ml three-neck bottle, 28g of hydrogen peroxide with the purity of 27.5 percent is added, 72g of 3,5, 5-trimethylhexanoic acid is added, and 6g of spherical polyvinyl alcohol compound amino acid A is added. Stirring the reaction mixture and heating to reflux temperature of 70-80 ℃. After azeotropic distillation, the distillate was cooled and the water of reaction was removed in a water separator. The petroleum ether is separated off and returned to the reaction vessel. After 4h of reaction, the yield of bis- (3,5, 5-trimethylhexanoyl) peroxide product was 86.9% as shown by gas chromatography.
Example 2
200ml of petroleum ether (60-90 ℃) is added into a 500ml three-neck bottle, 28g of hydrogen peroxide with the purity of 27.5 percent is added, 72g of 3,5, 5-trimethylhexanoic acid is added, and 4g of spherical polyvinyl alcohol compound amino acid B is added. Stirring the reaction mixture and heating to reflux temperature of 70-80 ℃. After azeotropic distillation, the distillate was cooled and the water of reaction was removed in a water separator. The petroleum ether is separated off and returned to the reaction vessel. After 4h of reaction, the yield of bis- (3,5, 5-trimethylhexanoyl) peroxide product was 65.6% as shown by gas chromatography.
Example 3
200ml of petroleum ether (60-90 ℃) is added into a 500ml three-neck bottle, 28g of hydrogen peroxide with the purity of 27.5 percent is added, 72g of 3,5, 5-trimethylhexanoic acid is added, and 2g of spherical polyvinyl alcohol compound amino acid C is added. Stirring the reaction mixture and heating to reflux temperature of 70-80 ℃. After azeotropic distillation, the distillate was cooled and the water of reaction was removed in a water separator. The petroleum ether is separated off and returned to the reaction vessel. After 4h of reaction, the yield of bis- (3,5, 5-trimethylhexanoyl) peroxide product was 60.7% as shown by gas chromatography.
Example 4
200ml of pentane is added into a 500ml three-necked bottle, 28g of hydrogen peroxide with the purity of 27.5 percent is added, 72g of 3,5, 5-trimethylhexanoic acid is added, and 1g of spherical polyvinyl alcohol compound amino acid A is added. Stirring the reaction mixture and heating to reflux temperature of 70-80 ℃. After azeotropic distillation, the distillate was cooled and the water of reaction was removed in a water separator. The pentane is separated off and returned back to the reaction vessel. After 8h of reaction, the yield of bis- (3,5, 5-trimethylhexanoyl) peroxide product was 61.3% as shown by gas chromatography.
Example 5
200ml of pentane is added into a 500ml three-necked bottle, 28g of hydrogen peroxide with the purity of 27.5 percent is added, 72g of 3,5, 5-trimethylhexanoic acid is added, and 3g of spherical polyvinyl alcohol compound amino acid B is added. Stirring the reaction mixture and heating to reflux temperature of 70-80 ℃. After azeotropic distillation, the distillate was cooled and the water of reaction was removed in a water separator. The pentane is separated off and returned back to the reaction vessel. After 8h of reaction, the yield of bis- (3,5, 5-trimethylhexanoyl) peroxide product was 94.0% as shown by gas chromatography.
Example 6
200ml of petroleum ether (60-90 ℃) is added into a 500ml three-neck bottle, 28g of hydrogen peroxide with the purity of 27.5 percent is added, 72g of 3,5, 5-trimethylhexanoic acid is added, and 5g of spherical polyvinyl alcohol compound amino acid C is added. Stirring the reaction mixture and heating to reflux temperature of 70-80 ℃. After azeotropic distillation, the distillate was cooled and the water of reaction was removed in a water separator. The petroleum ether is separated off and returned to the reaction vessel. After 4h of reaction, the yield of bis- (3,5, 5-trimethylhexanoyl) peroxide product was 72.8% as shown by gas chromatography.
Example 7
Adding 200ml of petroleum ether (60-90 ℃) into a 500ml three-neck bottle, adding 36g of hydrogen peroxide with the purity of 27.5%, adding 71g of benzoic acid, and adding 6g of spherical polyvinyl alcohol compound amino acid A. Stirring the reaction mixture and heating to reflux temperature of 70-80 ℃. After azeotropic distillation, the distillate was cooled and the water of reaction was removed in a water separator. The petroleum ether is separated off and returned to the reaction vessel. After 4h of reaction, the dibenzoyl peroxide yield was 80.4% by gas chromatography analysis.
Example 8
200ml of pentane is added into a 500ml three-necked bottle, 36g of hydrogen peroxide with the purity of 27.5 percent is added, 71g of benzoic acid is added, and 3g of spherical polyvinyl alcohol compound amino acid B is added. Stirring the reaction mixture and heating to reflux temperature of 70-80 ℃. After azeotropic distillation, the distillate was cooled and the water of reaction was removed in a water separator. The pentane is separated off and returned back to the reaction vessel. After 4h of reaction, the dibenzoyl peroxide yield was 76.2% as shown by gas chromatography.
Example 9
200ml of pentane is added into a 500ml three-necked bottle, 36g of hydrogen peroxide with the purity of 27.5 percent is added, 71g of benzoic acid is added, and 1g of spherical polyvinyl alcohol compound amino acid C is added. Stirring the reaction mixture and heating to reflux temperature of 70-80 ℃. After azeotropic distillation, the distillate was cooled and the water of reaction was removed in a water separator. The pentane is separated off and returned back to the reaction vessel. After 4h of reaction, the dibenzoyl peroxide yield was 61.5% by gas chromatography analysis.
Comparative example 1
Adding 110g of 25% sodium hydroxide solution into a 500ml flask, and stirring and cooling to 0 ℃; dropwise adding 40g of hydrogen peroxide with the purity of 27.5% into the solution, reacting for 30min, and controlling the temperature to be 10-30 ℃; after the mixture is stirred uniformly, 100g of mixed solution of 80 percent isononanoyl chloride and solvent oil is slowly dripped into a flask, the reaction temperature is controlled to be 10-30 ℃, the reaction takes 30min to finish, and the isononanoyl chloride solution is stirred and reacted for 100min after the addition; stopping stirring after the reaction is finished, standing for 30min, separating out reaction mother liquor, and washing a reaction product until the pH value is 5-7; the content of the obtained product is 77.3 percent of di- (3,5, 5-trimethyl hexanoyl) peroxide.
Claims (9)
1. A method for synthesizing diacyl peroxide is characterized by comprising the following steps:
adding an acyl compound, hydrogen peroxide and a polyvinyl alcohol compound amino acid catalyst into an organic solvent, and stirring and dehydrating to synthesize diacyl peroxide;
the polyvinyl alcohol composite amino acid catalyst is obtained by polymerizing a spherical polyvinyl alcohol matrix and composite amino acid;
the structural formula of the acyl compound is R-C (= O) OH, wherein R group is C with straight chain or branched chain or aromatic ring1～C16A group.
2. The method of synthesizing diacyl peroxide as claimed in claim 1, wherein the spherical polyvinyl alcohol precursor is obtained by crosslinking polyvinyl alcohol and a crosslinking agent.
3. The method of claim 2, wherein the crosslinking agent is one or more of glutaraldehyde, terephthaldehyde, or formaldehyde.
4. The method of synthesizing a diacyl peroxide as claimed in claim 1, wherein the complex amino acid is two or more of cysteine, phenylalanine, alanine, methionine, glycine, glutamic acid, glutamine, arginine, lysine, tyrosine, leucine, aspartic acid, asparagine, proline, tryptophan, serine, threonine, valine, isoleucine, or histidine.
5. The method for synthesizing diacyl peroxide according to claim 1, wherein the amount of the polyvinyl alcohol/amino acid composite catalyst added is 1 to 100% by mass of the hydrogen peroxide.
6. The method of synthesizing diacyl peroxides as in claim 1, wherein the organic solvent is petroleum ether or pentane.
7. The method for synthesizing diacyl peroxide according to claim 1, wherein the molar ratio of the hydrogen peroxide to the acyl compound is 1:10 to 5: 1.
8. The method for synthesizing diacyl peroxide according to claim 1, wherein the reaction temperature is-20 to 120 ℃ and the reaction time is 1 to 24 hours.
9. The process for the synthesis of diacyl peroxides as claimed in claim 1, wherein said dehydration is carried out by azeotropic distillation, molecular distillation, stripping with dry air or stripping with inert gas.
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Denomination of invention: Synthesis of diacyl peroxide Effective date of registration: 20211119 Granted publication date: 20200407 Pledgee: Shandong Ruihuang Chemical Co.,Ltd. Pledgor: ZIBO ZHENGHUA AUXILIARY Co.,Ltd. Registration number: Y2021980012831 |