CN115043815A - Novel peroxycycloalkane organic peroxide mixture and preparation method thereof - Google Patents
Novel peroxycycloalkane organic peroxide mixture and preparation method thereof Download PDFInfo
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- 239000000203 mixture Substances 0.000 title claims abstract description 42
- 150000001451 organic peroxides Chemical class 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title abstract description 14
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 40
- 238000006243 chemical reaction Methods 0.000 claims abstract description 38
- 150000002576 ketones Chemical class 0.000 claims abstract description 37
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 33
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 27
- 238000000034 method Methods 0.000 claims abstract description 20
- 239000003085 diluting agent Substances 0.000 claims abstract description 17
- 239000002994 raw material Substances 0.000 claims abstract description 17
- 238000003756 stirring Methods 0.000 claims abstract description 14
- 239000003054 catalyst Substances 0.000 claims abstract description 13
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 12
- 238000001816 cooling Methods 0.000 claims abstract description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 9
- 239000007788 liquid Substances 0.000 claims abstract description 9
- 238000002156 mixing Methods 0.000 claims abstract description 9
- 239000007864 aqueous solution Substances 0.000 claims abstract description 7
- 238000010438 heat treatment Methods 0.000 claims abstract description 7
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims abstract description 6
- 239000005457 ice water Substances 0.000 claims abstract description 6
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 6
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims abstract description 3
- 235000017557 sodium bicarbonate Nutrition 0.000 claims abstract description 3
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 claims description 17
- -1 ketone compounds Chemical class 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 5
- 150000001875 compounds Chemical class 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 4
- 150000001335 aliphatic alkanes Chemical class 0.000 claims description 3
- 229920006395 saturated elastomer Polymers 0.000 claims description 3
- 238000003786 synthesis reaction Methods 0.000 abstract description 3
- 239000000243 solution Substances 0.000 description 15
- 229920000642 polymer Polymers 0.000 description 9
- 239000003921 oil Substances 0.000 description 8
- XNLICIUVMPYHGG-UHFFFAOYSA-N pentan-2-one Chemical compound CCCC(C)=O XNLICIUVMPYHGG-UHFFFAOYSA-N 0.000 description 8
- 238000002425 crystallisation Methods 0.000 description 6
- 230000008025 crystallization Effects 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- ZPVFWPFBNIEHGJ-UHFFFAOYSA-N 2-octanone Chemical compound CCCCCCC(C)=O ZPVFWPFBNIEHGJ-UHFFFAOYSA-N 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 238000009776 industrial production Methods 0.000 description 4
- 231100000053 low toxicity Toxicity 0.000 description 4
- VKCYHJWLYTUGCC-UHFFFAOYSA-N nonan-2-one Chemical compound CCCCCCCC(C)=O VKCYHJWLYTUGCC-UHFFFAOYSA-N 0.000 description 4
- 150000002978 peroxides Chemical class 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 3
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- 238000004811 liquid chromatography Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 230000036632 reaction speed Effects 0.000 description 3
- 238000003860 storage Methods 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 239000003350 kerosene Substances 0.000 description 2
- 238000004949 mass spectrometry Methods 0.000 description 2
- 239000000155 melt Substances 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- CNPVJWYWYZMPDS-UHFFFAOYSA-N 2-methyldecane Chemical compound CCCCCCCCC(C)C CNPVJWYWYZMPDS-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003431 cross linking reagent Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000012933 diacyl peroxide Substances 0.000 description 1
- 238000006471 dimerization reaction Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 239000003205 fragrance Substances 0.000 description 1
- 229920006158 high molecular weight polymer Polymers 0.000 description 1
- 150000002432 hydroperoxides Chemical class 0.000 description 1
- 239000003999 initiator Substances 0.000 description 1
- 239000002480 mineral oil Substances 0.000 description 1
- 235000010446 mineral oil Nutrition 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 150000004978 peroxycarbonates Chemical class 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 229920000098 polyolefin Polymers 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000005829 trimerization reaction Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D323/00—Heterocyclic compounds containing more than two oxygen atoms as the only ring hetero atoms
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Abstract
The invention belongs to the technical field of chemical synthesis, and particularly relates to a novel peroxycycloalkane organic peroxide mixture and a preparation method thereof, wherein the preparation method comprises the following steps: taking mixed ketone and hydrogen peroxide as raw materials, taking sulfuric acid and acetic acid as catalysts, uniformly mixing the raw materials and the catalysts, controlling the temperature to be-20-10 ℃ in the mixing process, dropwise adding the mixed ketone into the mixed ketone while stirring, controlling the temperature to be-20-40 ℃ in the dropwise adding process, and finishing the dropwise adding and continuing the low-temperature reaction; then heating to 30-90 ℃, reacting for 0.2-2 hours, and cooling; the liquid after the reaction is added into the mixture of diluent and ice water, stirred, stood and layered, the oil layer is washed by sodium hydroxide or sodium carbonate or sodium bicarbonate aqueous solution, and the product is obtained after drying.
Description
Technical Field
The invention belongs to the technical field of chemical synthesis, and particularly relates to a novel peroxycycloalkane organic peroxide mixture and a preparation method thereof.
Background
Organic peroxides have been widely used in industrial production as initiators, catalysts, crosslinking agents, curing agents, molecular weight regulators, and the like. Organic peroxides commonly used are hydroperoxides (ROOH), dialkyl peroxides (ROOR '), diacyl peroxides (RCOOCR'), peroxyesters (RCOOOR '), peroxycarbonates (ROOOOOCOR'), and ketone peroxides [ R 2 C(OOH) 2 ]Etc., all of which are linear peroxides.
It has long been found that cyclic peroxides prepared by dimerization or trimerization of acetone have not been industrially applicable due to their poor stability and low safety factor. Once disclosed, 3,6, 9-triethyl-3, 6, 9-trimethyl-1, 4, 7-triperoxonane (trade designation 301), developed by aksunobel, has received much attention and, after industrial application, exhibits excellent properties such as high melt index, low odor, low toxicity, high safety factor, and the like.
In industry, 3,6, 9-triethyl-3, 6, 9-trimethyl-1, 4, 7-triperoxonane is dissolved in mineral oil and prepared into about 41 percent of mixed liquid for application, and when the environmental temperature is lower than 10 ℃, the crystallization phenomenon is easy to occur, thereby not only affecting the safety of products, but also causing the difficulty of industrial application.
At present, the new naphthenic organic peroxide has the advantages of high continuous melt index, small smell, low toxicity and the like, and needs to reduce the crystallization temperature, improve the safety, increase the types of raw materials of the naphthenic organic peroxide and widen the application field.
Disclosure of Invention
Aiming at the technical problems existing at present, the invention provides a novel peroxycycloalkane organic peroxide mixture and a preparation method thereof, and the prepared novel peroxycycloalkane organic peroxide mixture has the advantages of high melt index, small smell, low toxicity, low crystallization temperature and the like, and the safety is improved.
The technical scheme of the invention is as follows:
a novel peroxycycloalkane organic peroxide mixture comprises at least two compounds of formula (I),
wherein R1-R8 are C1-C9 alkyl;
the product has the advantages of high melt index, small smell, low toxicity, low crystallization temperature and the like, improves the use safety, is not easy to crystallize at the storage temperature of-10 ℃, and does not block a feeding pipeline when the environmental temperature is lower than 10 ℃ in actual use.
Compared with the prior art in which 3,6, 9-triethyl-3, 6, 9-trimethyl-1, 4, 7-triperoxonane is a trimolecular polymer, the product provided by the invention is a trimolecular polymer, the product structure is greatly changed, the product structure is changed, the stability is increased, the crystallization temperature is reduced, and the safety in the production and use processes is increased.
A preparation method of a novel peroxycycloalkane organic peroxide mixture comprises the following steps:
1) taking mixed ketone and hydrogen peroxide as raw materials, taking sulfuric acid and acetic acid as catalysts, uniformly mixing the hydrogen peroxide, the sulfuric acid and the acetic acid, controlling the temperature to be-20-10 ℃ in the mixing process, dropwise adding the mixture into the mixed ketone under the stirring condition, controlling the temperature to be-20-40 ℃ in the dropwise adding process, and continuing to react for 1-6 hours at the low temperature of-20-40 ℃ after the dropwise adding is finished; then heating to 30-90 ℃, and reacting for 0.2-2 hours; cooling to below 20 deg.C; the mixed ketone is knotHas a general formula of C n H 2n O，3<n<11, and is a mixture of two or more ketone compounds;
(2) and adding the reacted feed liquid into a mixture of a diluent and ice water, stirring, standing, layering, washing an oil layer with 3-10 wt% of sodium hydroxide or sodium carbonate or sodium bicarbonate aqueous solution until the pH value is 5-6, and drying to obtain the product.
Based on the defects of the prior art of the three-molecule polymer of 3,6, 9-triethyl-3, 6, 9-trimethyl-1, 4, 7-triperoxonane, the inventor finds that new ketone raw materials are added, the type of the catalyst is changed, and organic peroxide with relatively stable property can be synthesized. Because such reactions are highly dangerous, the conventional experimental thinking cannot be used for providing data and parameters, and the searching process is extremely dangerous, and the reactions are not easily obtained through conventional repeated experiments. The inventor creatively provides a preparation method of a novel peroxycycloalkane organic peroxide mixture, determines reaction raw materials, reaction conditions, catalysts and reaction processes, realizes production in a relatively safe range, has relatively mild reaction process and high product stability, obtains a high-molecular-weight polymer product, and has a high melt index meeting the industrial production requirements.
The mixed ketone used in the invention has the structural formula C n H 2n O(3<n<11) The mixture of methyl ketone is a mixture of two or more ketone compounds, the structural regularity of a ring structure broken by more than two ketone raw materials is reduced, and the crystallization temperature of the synthesized four-molecular polymer product is reduced; meanwhile, the selection of the mixed ketone can slow down the reaction speed, expand the safe temperature range, ensure that the reaction process is easy to control, and the reaction can be carried out in a kettle type reaction.
Preferably, the mixed ketone comprises 2-butanone, wherein the mole fraction of the 2-butanone is 40-90%, and further preferably, the mole fraction of the 2-butanone in the mixed ketone is 50-80%.
In the selected ketone raw materials, the 2-butanone has the highest reaction activity, and the increased reaction activity of other ketone raw materials is relatively less than that of the 2-butanone, so that a new proposal and a new thought are provided for catalysts and reaction conditions. Meanwhile, the odor of the selected ketone substance (the ketone substance has special fragrance) is different from that of the 2-butanone, and the odor of the ketone substance contributes to the improvement of the environmental odor. Considering the influence of the reaction activity of the ketone on the synthesis difficulty of the four-molecule polymer, the 2-butanone with a specific proportion is selected, and meanwhile, the addition of other ketones can reduce the reaction activity, control the reaction speed, enlarge the safe temperature range, ensure that the reaction process is easy to control, and avoid accidents such as explosion and the like caused by the difficulty in controlling the reaction speed.
Preferably, the molar ratio of the mixed ketone to the hydrogen peroxide, the sulfuric acid and the acetic acid is 1: (1-3): (0.2-1): (0.01-0.5). More preferably, the molar ratio of the mixed ketone hydrogen peroxide, sulfuric acid and acetic acid is as follows: 1: (1.2-2.2): (0.3-0.8): (0.05-0.3);
preferably, the mass concentration of the hydrogen peroxide used is 40-60%.
Preferably, the mass concentration of the sulfuric acid is 85-98%.
Preferably, the temperature is raised to 35-55 ℃ and the reaction is carried out for 0.5-1 hour.
Preferably, when the preparation method is industrially applicable, the reactor is a microchannel reactor or a tank reactor.
The product obtained by the preparation method of the invention is a mixture of various organic peroxides, and can be directly used as a peroxide degradation agent for polymerization modification of polyolefin or other industrial applications such as mask melt-blown cloth production process and the like.
The prepared product is liquid peroxide, is inflammable and explosive, has extremely high storage risk of a pure product, and must be stored in a diluent, so that the storage safety is improved.
The used diluent is C5-C18 saturated straight chain or branched chain alkane, and the dosage of the diluent is 0.8-2 times of the mass of the mixed ketone;
preferred diluents are saturated straight or branched alkanes of C10 to C16;
the preferable dosage of the diluent is 1-1.5 times of the mass of the mixed ketone.
Preferably, the reactor to which the preparation process is applicable is a tank reactor or a microchannel reactor.
According to the invention, the mixed ketone is selected as a reaction raw material, a special catalyst is used in a matched manner, and a safe reaction process is adopted, so that the four-molecular polymer product prepared in a relatively safe reaction environment is high in content, the melt index meets the industrial production requirement, the danger coefficient is reduced, the raw material types of naphthenic organic peroxide are increased, the reaction activity is effectively reduced, the reaction danger is reduced, and the application field is widened.
Drawings
FIG. 1 is a mass spectrometry ion flow diagram of the product prepared in example 1;
FIG. 2 is a mass spectrometry ion flow diagram of a product prepared in comparative example 1.
Detailed Description
For a further understanding of the invention, preferred embodiments of the invention are described below in conjunction with the examples, but it is to be understood that these descriptions are intended only to further illustrate features and advantages of the invention, and not to limit the claims of the invention.
Example 1
The preparation method of the mixture with the structure shown in the formula (I) by taking 2-butanone, 2-pentanone and 2-nonanone as raw materials comprises the following steps:
adding aqueous hydrogen peroxide (29.92g, 50%) into a four-neck flask, cooling to below-10 ℃, slowly dripping sulfuric acid (11.53g, 85%) firstly, after the dripping of the sulfuric acid is finished, slowly dripping acetic acid (2.42g, 99%) in the flask, controlling the temperature to be not more than 5 ℃ in the process, and continuously stirring the mixed material liquid below 10 ℃ until the temperature is not changed, thereby obtaining solution I;
cooling a mixture of 2-butanone (7.27g, 99%) and 2-pentanone (7.82g, 99%) and 2-nonanone (1.43g, 99%) to 15 ℃ to obtain mixed ketone, dropwise adding the prepared solution I into the mixed ketone, continuously stirring in the dropwise adding process, controlling the reaction temperature to be not more than 20 ℃, after the dropwise adding is completed, controlling the temperature of the reaction solution to be 20 ℃, continuing to react for 2 hours, then heating to 50 ℃, reacting for 0.5 hour, finishing the reaction, cooling to 20 ℃, and obtaining solution II;
weighing 18g of diluent (Exxon Mobil isoparaffin solvent oil Isopar H), mixing with 50g of ice water to obtain a mixture, slowly adding the solution II into the mixture, controlling the temperature to be not more than 10 ℃, stirring for 10min, standing, removing a water layer, adding a 6 wt% sodium carbonate aqueous solution into an oil layer, quickly washing until the pH value is 5-6, removing the water layer again, drying the oil layer with anhydrous magnesium sulfate, filtering to obtain a mixture product containing the structural formula (I), and analyzing the product by an Agilent liquid chromatography flight time continuous instrument to obtain a product shown in a figure 1;
the active oxygen content of the product is 5.3 percent, and the proportion of the diluent is 55 percent by weight; the product is stored for 168 hours at the temperature of minus 18 ℃, and no crystal is separated out; the product of the Aksu degradation agent 301, with the chemical name of 3,6, 9-triethyl-3, 6, 9-trimethyl-1, 4, 7-triperoxonane, is placed for 24 hours at the temperature of 0-10 ℃ to generate crystals.
Example 1 a product mixture containing structural formula (i) was obtained comprising the following compounds:
example 2
The preparation method of the mixture with the structure of the formula (I) by taking 2-butanone and 2-octanone as raw materials comprises the following steps:
adding aqueous hydrogen peroxide (34g, 30%) into a four-neck flask, cooling to below 0 ℃, slowly dropwise adding sulfuric acid (16g, 98%), slowly dropwise adding acetic acid (3.64g, 99%) after dropwise adding sulfuric acid, controlling the temperature to be not more than 5 ℃ in the process, continuously stirring the mixed liquid at low temperature until the temperature is not changed, and heating to 10 ℃. This is called solution I;
cooling mixed ketone of butanone (8.72g, 99%) and 2-octanone (23.27g, 99%) to 0 ℃, dropwise adding the prepared solution I into the mixed ketone, stirring in the dropwise adding process, controlling the reaction temperature to be not more than 20 ℃, controlling the temperature of the reaction solution to be 20 ℃ after the dropwise adding is finished, continuing to react for 4 hours, then heating to 60 ℃, reacting for 1 hour, and calling the solution II after the reaction is finished;
weighing 25g of diluent (aviation kerosene), mixing the diluent with 50g of ice water to obtain a mixture, slowly adding the solution II into the mixture, controlling the temperature to be not more than 10 ℃, stirring for 10min, standing, removing a water layer, adding 10 wt% of sodium carbonate aqueous solution into an oil layer, quickly washing until the pH value is 5-6, removing the water layer again, drying the oil layer with anhydrous magnesium sulfate, and filtering to obtain a mixture product;
the active oxygen content of the product is 4.2 percent, and the proportion of the diluent is 44 percent by weight; the product is stored for more than 148 hours at the temperature of 18 ℃ below zero, and no crystal precipitation is seen.
Comparative example 1
The preparation method of the mixture with the structure shown in the formula (I) by taking 2-butanone and 2-pentanone as raw materials and only using sulfuric acid as a catalyst comprises the following steps:
adding a hydrogen peroxide aqueous solution (34g, 50%) into a four-mouth flask, cooling to below 0 ℃, slowly dropwise adding sulfuric acid (20g, 98%), controlling the temperature not to exceed 5 ℃ in the process, after dropwise adding the sulfuric acid, continuously stirring the mixed material liquid at a low temperature until the temperature is not changed, and storing at the low temperature of 0-5 ℃, wherein the mixed material liquid is called a solution I;
cooling mixed ketone of butanone (14.54g, 99%) and 2-pentanone (4.34g, 99%) to 0 ℃, dropwise adding the prepared solution I into the mixed ketone, stirring in the dropwise adding process, controlling the reaction temperature to be not more than 10 ℃, controlling the temperature of the reaction solution to be 10 ℃ after the dropwise adding is finished, continuing to react for 4 hours, then heating to 30 ℃, reacting for 0.5 hour, and calling the solution II after the reaction is finished;
weighing 28g of diluent (aviation kerosene), mixing with 50g of ice water to obtain a mixture, slowly adding the solution II into the mixture, controlling the temperature to be not more than 10 ℃, stirring for 10min, standing, removing a water layer, adding a 5 wt% sodium carbonate aqueous solution into an oil layer, quickly washing until the pH value is 5-6, removing the water layer again, drying the oil layer with anhydrous magnesium sulfate, filtering to obtain a mixture product, wherein the proportion of the diluent is 60 wt%, and the product is analyzed by an Agilent liquid chromatography flight time continuous instrument to obtain a figure 2;
the product was analyzed by liquid chromatography and found to be only 1.46% of the molecular weight polymer product.
The mixture product of comparative example 1 comprises the following compounds:
as can be seen from the comparison between the above examples and comparative examples, when the catalyst is selected from only sulfuric acid, the content of the quaternary polymer obtained is significantly lower than that obtained when the catalyst is selected from sulfuric acid and acetic acid; according to the invention, the mixed ketone is selected as a reaction raw material, a special catalyst is matched, and a safe reaction process is adopted, so that the high content of the prepared four-molecular polymer product is realized in a relatively safe reaction environment, the melt index meets the industrial production requirement, the danger coefficient is reduced, the raw material variety of the naphthenic organic peroxide is increased, the reaction activity is effectively reduced, the reaction danger is reduced, and the application field is widened.
Claims (8)
1. A novel peroxycycloalkane organic peroxide mixture comprising at least two compounds of formula (I),
wherein R1-R8 are C1-C9 alkyl.
2. The process for preparing a novel peroxycycloalkane organic peroxide mixture according to claim 1, comprising the steps of:
(1) using mixed ketone and hydrogen peroxide as raw material, sulfuric acid and acetic acidAs a catalyst, uniformly mixing hydrogen peroxide, sulfuric acid and acetic acid, controlling the temperature to be-20-10 ℃ in the mixing process, dropwise adding the mixture into mixed ketone under the stirring condition, controlling the temperature to be-20-40 ℃ in the dropwise adding process, and continuing to react for 1-6 hours at the low temperature of-20-40 ℃ after dropwise adding is finished; then heating to 30-90 ℃, reacting for 0.2-2 hours, cooling to below 20 ℃; the mixed ketone has a structural general formula of C n H 2n O，3<n<11, and is a mixture of two or more ketone compounds;
(2) and adding the reacted feed liquid into a mixture of a diluent and ice water, stirring, standing, layering, washing an oil layer with 3-10 wt% of sodium hydroxide or sodium carbonate or sodium bicarbonate aqueous solution until the pH value is 5-6, and drying to obtain the product.
3. The method for preparing the novel peroxycycloalkane organic peroxide mixture according to claim 2, wherein the mixed ketone comprises 2-butanone, wherein the mole fraction of 2-butanone is 40-90%.
4. The method for preparing a novel peroxycycloalkane organic peroxide mixture according to claim 2, wherein the molar ratio of the mixed ketone, hydrogen peroxide, sulfuric acid, and acetic acid is 1: 1-3: 0.2-1: 0.01 to 0.5.
5. The method for preparing a novel peroxycycloalkane organic peroxide mixture according to claim 2, wherein the molar ratio of the mixed ketone, hydrogen peroxide, sulfuric acid, and acetic acid is 1: 1.2-2.2: 0.3-0.8: 0.05 to 0.3.
6. The method for preparing a novel peroxycycloalkane organic peroxide mixture according to claim 3, wherein the temperature is raised to 35 to 55 ℃ and the reaction is carried out for 0.5 to 1 hour.
7. The method for preparing a novel peroxycycloalkane organic peroxide mixture according to claim 3, wherein the mass concentration of hydrogen peroxide is 25 to 75% and the mass concentration of sulfuric acid is 65 to 98%.
8. The method for preparing a novel peroxycycloalkane organic peroxide mixture according to claim 3, wherein the diluent is a C5-C18 saturated straight-chain or branched-chain alkane, and the amount of the diluent is 0.8-2 times of the mass of the mixed ketone.
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