A catalyst for preparing perfluoro-2,3-epoxy-2-methylpentane from hexafluoropropylene dimer

Abstract

The present invention provides a catalyst for preparing perfluoro-2,3-epoxy-2-methylpentane from hexafluoropropylene dimer, belonging to the technical field of perfluoro-2,3-epoxy-2-methylpentane synthesis. A fluorocarbon cyclic ether compound is added as a reaction medium to a polymerization vessel with an agitator, the reaction vessel is started and stirred, and then the hexafluoropropylene dimer and an oxidation catalyst are added. The polymerization vessel is heated to perform a molecular oxygen oxidation reaction to obtain perfluoro-2,3-epoxy-2-methylpentane. This method effectively improves the efficiency of the molecular oxygen oxidation reaction and the molar yield of perfluoro-2,3-epoxy-2-methylpentane. Both the reaction medium and the oxidation catalyst can be recycled, generating less three wastes, and being environmentally friendly.

Description

Technical Field

[0001] The invention relates to the technical field of perfluoro-2,3-epoxy-2-methylpentane synthesis, in particular to a catalyst for preparing perfluoro-2,3-epoxy-2-methylpentane from a hexafluoropropylene dimer. Background Art

[0002] Perfluoro-2,3-epoxy-2-methylpentane is an important organic synthesis intermediate used in the synthesis of fluorinated alcohols. It can also react with other electrophiles to incorporate fluorine atoms into its molecular structure. Fluorinated compounds have attracted significant attention due to their biological activity and molecular mimicry in the human body, making perfluoro-2,3-epoxy-2-methylpentane a promising candidate for application.

[0003] Chinese invention patent CN115385873B discloses a continuous synthesis method for perfluoro-2,3-epoxy-2-methylpentane. The method comprises the following steps: 1) mixing a transition metal salt, a polypyridine-like amino compound, and an aprotic solvent to form a uniform catalytic solution; 2) introducing perfluoro-2-methyl-2-pentene, the catalytic solution obtained in step 1), and oxygen into a microreactor for a continuous reaction to produce perfluoro-2,3-epoxy-2-methylpentane. This method replaces traditional batch reaction methods based on chemical oxidation, enabling the recycling of the catalytic solution, achieving environmental friendliness, and enhancing reaction safety.

[0004] For example, Chinese invention patent CN103508983B discloses a method for preparing perfluoro-2,3-epoxy-2-methylpentane, in which perfluoro-2-methyl-2-pentene is used as a raw material and reacted with sodium hypochlorite to prepare perfluoro-2,3-epoxy-2-methylpentane. The prepared perfluoro-2,3-epoxy-2-methylpentane can be used to synthesize fluorine-containing alcohol compounds.

[0005] In view of the above-mentioned patent disclosure and prior art, the applicant believes that there is room for further improvement in the oxidation efficiency and reaction yield of the existing method for preparing perfluoro-2,3-epoxy-2-methylpentane.

[0006] Based on this, the present invention proposes a catalyst for preparing perfluoro-2,3-epoxy-2-methylpentane from hexafluoropropylene dimer. Summary of the Invention

[0007] The present invention provides a catalyst for preparing perfluoro-2,3-epoxy-2-methylpentane from hexafluoropropylene dimer, so as to solve at least one technical problem raised in the above background technology, and belongs to the technical field of perfluoro-2,3-epoxy-2-methylpentane synthesis.

[0008] In order to achieve the above-mentioned object of the invention, the present invention adopts the following technical solutions:

[0009] A catalyst for preparing perfluoro-2,3-epoxy-2-methylpentane from hexafluoropropylene dimer, characterized by comprising the following steps:

[0010] 100-300 parts by weight of a fluorocarbon cyclic ether compound as a reaction medium are added to a polymerization container equipped with a stirrer. The reaction container is stirred, and then 100-300 parts of hexafluoropropylene dimer and 1-5 parts of an oxidation catalyst are added. The polymerization container is heated to carry out a molecular oxygen oxidation reaction to obtain perfluoro-2,3-epoxy-2-methylpentane.

[0011] As a preferred embodiment, the fluorocarbon cyclic ether compound is at least one selected from perfluoro-2-n-propyl-cyclopentyl ether, perfluoro-2-n-butyl-cyclopentyl ether, perfluoromethylcyclohexane, and perfluoro-2-n-propyl-cyclohexyl ether.

[0012] As a preferred embodiment, the hexafluoropropylene dimer structure is selected from D2, namely perfluoro-2-methyl-2-pentene.

[0013] Furthermore, the preparation method of the oxidation catalyst in the above technical solution is:

[0014] S1: Add 20-30 parts of 4,4'-divinyl-2,2'-bipyridine, 200-300 parts of DMF, 2-4 parts of 20-30% by weight hydrochloric acid, 1-4 parts of cobalt dichloride, 1-4 parts of chromium dichloride, and 1-4 parts of lanthanum trichloride to a stirred tank, and stir at 70-80°C for 50-100 minutes;

[0015] S2: Add 0.3-2.5 parts of dimethyldiallylammonium chloride, 30-48 parts of 2,5-dimercaptothiadiazole zinc salt, and 2-6 parts of potassium tert-butoxide, and stir at 70-80° C. for 60-150 minutes to obtain an active component of the organometallic impregnation solution;

[0016] S3: Under a nitrogen atmosphere, add 50-100 parts of tourmaline ceramic balls treated with acrylsilane, stir at 70-80°C for 200-300 minutes, filter, stand and dry at 70-80°C for 50-70 hours, and then calcine at 250-380°C in air atmosphere for 3-5 hours to obtain an oxidation catalyst.

[0017] As a preferred embodiment, the active component loading amount of the organic metal impregnation solution accounts for 0.5-15.0 wt% of the entire oxidation catalyst.

[0018] Furthermore, the preparation method of the tourmaline ceramic balls treated with acrylsilane in the above technical solution is:

[0019] Add 3-5 parts of acrylsiloxane, 300-500 parts of tourmaline ceramic balls, and 1000-2000 parts of water according to mass parts, stir at 30-50° C. for 60-100 minutes, filter, and dry to obtain acrylsilane-treated tourmaline ceramic balls.

[0020] As a preferred embodiment, the acryloxysilane is at least one of 3-(methacryloyloxy)propyltrimethoxysilane (CAS No.: 2530-85-0), 3-(diethoxymethylsilyl)propyl 2-acrylate (CAS No.: 13732-00-8), and acryloxymethyltrimethoxysilane (CAS No.: 21134-38-3).

[0021] As a preferred embodiment, the reaction temperature is 30-150°C.

[0022] As a preferred solution, the reaction environment is an oxygen environment, and high-purity oxygen with a purity of not less than 99 wt % is introduced into the reaction container during the reaction.

[0023] As a preferred solution, the pressure inside the reaction container is maintained at 0.5 to 1.6 MPa by injecting pure oxygen into the reaction container.

[0024] Reaction mechanism:

[0025] In the present invention, tourmaline ceramic balls treated with acrylsilane undergo a mercapto-propylene addition reaction with an organic metal complex of 4,4'-divinyl-2,2'-bipyridine / cobalt dichloride / chromium dichloride / lanthanum trichloride, and excess 4,4'-divinyl-2,2'-bipyridine undergoes an amino-propylene addition reaction with dimethyldiallylammonium chloride and 2,5-dimercaptothiadiazole zinc salt. Cobalt, chromium, lanthanum, and zinc are chemically bonded to the surface and micropores of the tourmaline ceramic balls, resulting in uniform distribution of the components and tight bonding of the metal ions to the tourmaline ceramic balls. After calcination, a uniform and dense tourmaline ceramic ball / cobalt oxide / chromium oxide / lanthanum oxide / zinc oxide composite material is obtained. The composite material is used as an oxidation catalyst and has good catalytic effect and long service life.

[0026] Beneficial effects:

[0027] 1) This method can improve the efficiency of molecular oxygen oxidation reaction and increase the molar yield of perfluoro-2,3-epoxy-2-methylpentane;

[0028] 2) The reaction medium and oxidation catalyst used in this method can be recycled, generating less "three wastes", which is green and environmentally friendly.

[0029] 3) The oxidation catalyst prepared by this method combines metal ions with the surface and micropores of the tourmaline ceramic ball through chemical bonds, thereby obtaining a uniform and dense tourmaline ceramic ball / cobalt oxide / chromium oxide / lanthanum oxide / zinc oxide composite material with good catalytic effect and long service life.

[0030] The weight parts mentioned in the present invention are weight units such as μg, mg, g, kg, etc. known in the art, or multiples thereof, such as 1 / 10, 1 / 100, 10 times, 100 times, etc.

[0031] On the basis of conforming to the common sense in this field, the above-mentioned preferred conditions can be combined with each other to obtain the preferred embodiments of the present invention. DETAILED DESCRIPTION

[0032] The present invention will be further described below with reference to specific embodiments, but the present invention is not limited to these specific embodiments. Those skilled in the art should recognize that the present invention covers all possible alternatives, improvements and equivalents within the scope of the claims.

[0033] <Example 1>

[0034] A catalyst for preparing perfluoro-2,3-epoxy-2-methylpentane from hexafluoropropylene dimer, characterized by comprising the following steps:

[0035] 100 g of a fluorocarbon cyclic ether compound was added as a reaction medium to a polymerization container equipped with a stirrer. The reaction container was stirred, and then 100 g of a hexafluoropropylene dimer and 1 g of an oxidation catalyst were added. The polymerization container was heated to carry out a molecular oxygen oxidation reaction to obtain perfluoro-2,3-epoxy-2-methylpentane.

[0036] The fluorocarbon cyclic ether compound is selected from at least one of perfluoro-2-n-propyl-cyclopentyl ether, perfluoro-2-n-butyl-cyclopentyl ether, perfluoromethylcyclohexane, and perfluoro-2-n-propyl-cyclohexyl ether.

[0037] The hexafluoropropylene dimer structure is selected from D2, namely perfluoro-2-methyl-2-pentene.

[0038] The preparation method of the oxidation catalyst is:

[0039] S1: Add 20 g of 4,4'-divinyl-2,2'-bipyridine, 200 g of DMF, 2 g of 30% by mass hydrochloric acid, 1 g of cobalt dichloride, 1 g of chromium dichloride, and 1 g of lanthanum trichloride into a stirred tank and stir at 70°C for 50 min;

[0040] S2: Add 0.3 g of dimethyldiallylammonium chloride, 30 g of 2,5-dimercaptothiadiazole zinc salt, and 2 g of potassium tert-butoxide, and stir at 70°C for 60 min to obtain the active component of the organometallic impregnation solution;

[0041] S3: Under nitrogen atmosphere, add 50 g of tourmaline ceramic balls treated with acrylsilane, stir at 70°C for 200 min, filter, stand and dry at 70°C for 50 h, and then calcine at 250°C in air atmosphere for 3 h to obtain an oxidation catalyst.

[0042] The active component loading amount of the organic metal impregnation solution accounts for 2 wt % of the entire oxidation catalyst.

[0043] The preparation method of the tourmaline ceramic balls treated with acrylsilane described in the above technical solution is:

[0044] 3 g of acrylsiloxane, 300 g of tourmaline ceramic balls, and 1000 g of water were added, stirred at 30° C. for 60 min, filtered, and dried to obtain acrylsilane-treated tourmaline ceramic balls.

[0045] The acryloxysilane is 3-(methacryloyloxy)propyltrimethoxysilane (CAS No.: 2530-85-0).

[0046] The reaction temperature was 45°C.

[0047] The reaction environment is an oxygen environment, and high-purity oxygen is introduced into the reaction container during the reaction process, with a purity of not less than 99 wt%.

[0048] The pressure in the reaction vessel was maintained at 0.5 MPa by injecting pure oxygen.

[0049] In this embodiment, after separation and purification, the conversion rate based on perfluoro-2-methyl-2-pentene was 98.1%, and the product yield was 94.4%.

[0050] <Example 2>

[0051] A catalyst for preparing perfluoro-2,3-epoxy-2-methylpentane from hexafluoropropylene dimer, characterized by comprising the following steps:

[0052] 150 g of a fluorocarbon cyclic ether compound was added as a reaction medium to a polymerization container equipped with a stirrer. The reaction container was stirred, and then 150 g of a hexafluoropropylene dimer and 2 g of an oxidation catalyst were added. The polymerization container was heated to carry out a molecular oxygen oxidation reaction to obtain perfluoro-2,3-epoxy-2-methylpentane.

[0053] The fluorocarbon cyclic ether compound is selected from at least one of perfluoro-2-n-propyl-cyclopentyl ether, perfluoro-2-n-butyl-cyclopentyl ether, perfluoromethylcyclohexane, and perfluoro-2-n-propyl-cyclohexyl ether.

[0054] The hexafluoropropylene dimer structure is selected from D2, namely perfluoro-2-methyl-2-pentene.

[0055] The preparation method of the oxidation catalyst is:

[0056] S1: Add 25 g of 4,4'-divinyl-2,2'-bipyridine, 245 g of DMF, 3 g of 20% by mass hydrochloric acid, 2 g of cobalt dichloride, 2 g of chromium dichloride, and 2 g of lanthanum trichloride into a stirred tank and stir at 70°C for 80 min;

[0057] S2: Add 1.2 g of dimethyldiallylammonium chloride, 35 g of 2,5-dimercaptothiadiazole zinc salt, and 3 g of potassium tert-butoxide, and stir at 70°C for 100 min to obtain the active component of the organometallic impregnation solution;

[0058] S3: Under nitrogen atmosphere, add 70g of tourmaline ceramic balls treated with acrylsilane, stir at 70°C for 250min, filter, stand and dry at 70°C for 60h, and then calcine at 275°C in air atmosphere for 3h to obtain an oxidation catalyst.

[0059] The active component loading amount of the organic metal impregnation solution accounts for 8 wt % of the entire oxidation catalyst.

[0060] The preparation method of the tourmaline ceramic balls treated with acrylsilane described in the above technical solution is:

[0061] 4 g of acrylsiloxane, 300 g of tourmaline ceramic balls, and 1200 g of water were added, stirred at 35° C. for 70 min, filtered, and dried to obtain acrylsilane-treated tourmaline ceramic balls.

[0062] The acryloxysilane is 3-(diethoxymethylsilyl)propyl 2-acrylate (CAS No.: 13732-00-8).

[0063] The reaction temperature was 65°C.

[0064] The reaction environment is an oxygen environment, and high-purity oxygen is introduced into the reaction container during the reaction process, with a purity of not less than 99 wt%.

[0065] The pressure in the reaction vessel was maintained at 0.8 MPa by injecting pure oxygen.

[0066] In this embodiment, after separation and purification, the conversion rate based on perfluoro-2-methyl-2-pentene was 98.4%, and the product yield was 94.9%.

[0067] <Example 3>

[0068] A catalyst for preparing perfluoro-2,3-epoxy-2-methylpentane from hexafluoropropylene dimer, characterized by comprising the following steps:

[0069] 200 g of a fluorocarbon cyclic ether compound was added as a reaction medium to a polymerization container equipped with a stirrer. The reaction container was stirred, and then 200 g of a hexafluoropropylene dimer and 3.5 g of an oxidation catalyst were added. The polymerization container was heated to carry out a molecular oxygen oxidation reaction to obtain perfluoro-2,3-epoxy-2-methylpentane.

[0070] The fluorocarbon cyclic ether compound is selected from at least one of perfluoro-2-n-propyl-cyclopentyl ether, perfluoro-2-n-butyl-cyclopentyl ether, perfluoromethylcyclohexane, and perfluoro-2-n-propyl-cyclohexyl ether.

[0071] The hexafluoropropylene dimer structure is selected from D2, namely perfluoro-2-methyl-2-pentene.

[0072] The preparation method of the oxidation catalyst is:

[0073] S1: Add 25 g of 4,4'-divinyl-2,2'-bipyridine, 265 g of DMF, 3 g of 25% by mass hydrochloric acid, 3 g of cobalt dichloride, 3 g of chromium dichloride, and 3 g of lanthanum trichloride into a stirred tank and stir at 75°C for 80 min;

[0074] S2: Add 1.9 g of dimethyldiallylammonium chloride, 40 g of 2,5-dimercaptothiadiazole zinc salt, and 4.5 g of potassium tert-butoxide, and stir at 75°C for 120 min to obtain the active component of the organometallic impregnation solution;

[0075] S3: Under nitrogen atmosphere, add 80g of tourmaline ceramic balls treated with acrylsilane, stir at 75°C for 250min, filter, stand and dry at 75°C for 60h, and then calcine at 340°C in air atmosphere for 4h to obtain an oxidation catalyst.

[0076] The active component loading of the organometallic impregnation solution accounts for 13 wt % of the entire oxidation catalyst.

[0077] The preparation method of the tourmaline ceramic balls treated with acrylsilane described in the above technical solution is:

[0078] Add 4.5 g of acrylsiloxane, 450 g of tourmaline ceramic balls, and 1750 g of water, stir at 45° C. for 80 min, filter, and dry to obtain acrylsilane-treated tourmaline ceramic balls.

[0079] The acryloxysilane is acryloxymethyltrimethoxysilane (CAS No.: 21134-38-3).

[0080] The reaction temperature was 95°C.

[0081] The reaction environment is an oxygen environment, and high-purity oxygen is introduced into the reaction container during the reaction process, with a purity of not less than 99 wt%.

[0082] The pressure in the reaction vessel was maintained at 1.3 MPa by injecting pure oxygen.

[0083] In this embodiment, after separation and purification, the conversion rate based on perfluoro-2-methyl-2-pentene was 99.3%, and the product yield was 95.2%.

[0084] <Example 4>

[0085] A catalyst for preparing perfluoro-2,3-epoxy-2-methylpentane from hexafluoropropylene dimer, characterized by comprising the following steps:

[0086] 300 g of a fluorocarbon cyclic ether compound was added as a reaction medium to a polymerization container equipped with a stirrer. The reaction container was stirred, and then 300 g of a hexafluoropropylene dimer and 5 g of an oxidation catalyst were added. The polymerization container was heated to carry out a molecular oxygen oxidation reaction to obtain perfluoro-2,3-epoxy-2-methylpentane.

[0087] The fluorocarbon cyclic ether compound is selected from at least one of perfluoro-2-n-propyl-cyclopentyl ether, perfluoro-2-n-butyl-cyclopentyl ether, perfluoromethylcyclohexane, and perfluoro-2-n-propyl-cyclohexyl ether.

[0088] The hexafluoropropylene dimer structure is selected from D2, namely perfluoro-2-methyl-2-pentene.

[0089] The preparation method of the oxidation catalyst is:

[0090] S1: 30 g of 4,4'-divinyl-2,2'-bipyridine, 300 g of DMF, 4 g of 30% by mass hydrochloric acid, 4 g of cobalt dichloride, 4 g of chromium dichloride, and 4 g of lanthanum trichloride were added to a stirred tank and stirred at 80°C for 100 min;

[0091] S2: Add 2.5 g of dimethyldiallylammonium chloride, 48 g of 2,5-dimercaptothiadiazole zinc salt, and 6 g of potassium tert-butoxide, and stir at 80°C for 150 min to obtain the active component of the organometallic impregnation solution;

[0092] S3: Under nitrogen atmosphere, add 100 g of tourmaline ceramic balls treated with acrylsilane, stir at 80°C for 300 min, filter, stand and dry at 80°C for 70 h, and then calcine at 380°C in air atmosphere for 5 h to obtain an oxidation catalyst.

[0093] The active component loading amount of the organometallic impregnation solution accounts for 15.0 wt % of the entire oxidation catalyst.

[0094] The preparation method of the tourmaline ceramic balls treated with acrylsilane described in the above technical solution is:

[0095] Add 5 g of acrylsiloxane, 500 g of tourmaline ceramic balls, and 2000 g of water, stir at 50° C. for 100 min, filter, and dry to obtain acrylsilane-treated tourmaline ceramic balls.

[0096] The acryloxysilane is 3-(methacryloyloxy)propyltrimethoxysilane (CAS No.: 2530-85-0).

[0097] The reaction temperature was 115°C.

[0098] The reaction environment is an oxygen environment, and high-purity oxygen is introduced into the reaction container during the reaction process, with a purity of not less than 99 wt%.

[0099] The pressure in the reaction vessel was maintained at 1.6 MPa by injecting pure oxygen.

[0100] In this embodiment, after separation and purification, the conversion rate based on perfluoro-2-methyl-2-pentene was 99.6%, and the product yield was 95.7%.

[0101] <Comparative Example 1>

[0102] A catalyst for preparing perfluoro-2,3-epoxy-2-methylpentane from hexafluoropropylene dimer, characterized by comprising the following steps:

[0103] 100 g of a fluorocarbon cyclic ether compound was added as a reaction medium to a polymerization container equipped with a stirrer. The reaction container was stirred, and then 100 g of a hexafluoropropylene dimer and 1 g of an oxidation catalyst were added. The polymerization container was heated to carry out a molecular oxygen oxidation reaction to obtain perfluoro-2,3-epoxy-2-methylpentane.

[0104] The fluorocarbon cyclic ether compound is selected from at least one of perfluoro-2-n-propyl-cyclopentyl ether, perfluoro-2-n-butyl-cyclopentyl ether, perfluoromethylcyclohexane, and perfluoro-2-n-propyl-cyclohexyl ether.

[0105] The hexafluoropropylene dimer structure is selected from D2, namely perfluoro-2-methyl-2-pentene.

[0106] The preparation method of the oxidation catalyst is:

[0107] S1: Add 20 g of 4,4'-divinyl-2,2'-bipyridine, 200 g of DMF, 2 g of 30% by mass hydrochloric acid, 1 g of cobalt dichloride, 1 g of chromium dichloride, and 1 g of lanthanum trichloride into a stirred tank and stir at 70°C for 50 min;

[0108] S2: Add 30 g of 2,5-dimercaptothiadiazole zinc salt and 2 g of potassium tert-butoxide, and stir at 70°C for 60 min to obtain the active component of the organometallic impregnation solution;

[0109] S3: Under nitrogen atmosphere, add 50 g of tourmaline ceramic balls treated with acrylsilane, stir at 70°C for 200 min, filter, stand and dry at 70°C for 50 h, and then calcine at 250°C in air atmosphere for 3 h to obtain an oxidation catalyst.

[0110] The active component loading amount of the organic metal impregnation solution accounts for 2 wt % of the entire oxidation catalyst.

[0111] The preparation method of the tourmaline ceramic balls treated with acrylsilane described in the above technical solution is:

[0112] 3 g of acrylsiloxane, 300 g of tourmaline ceramic balls, and 1000 g of water were added, stirred at 30° C. for 60 min, filtered, and dried to obtain acrylsilane-treated tourmaline ceramic balls.

[0113] The acryloxysilane is 3-(methacryloyloxy)propyltrimethoxysilane (CAS No.: 2530-85-0).

[0114] The reaction temperature was 45°C.

[0115] The reaction environment is an oxygen environment, and high-purity oxygen is introduced into the reaction container during the reaction process, with a purity of not less than 99 wt%.

[0116] The pressure in the reaction vessel was maintained at 0.5 MPa by injecting pure oxygen.

[0117] In this comparative example, after separation and purification, the conversion rate based on perfluoro-2-methyl-2-pentene was 85.7%, and the product yield was 91.3%.

[0118] <Comparative Example 2>

[0119] A catalyst for preparing perfluoro-2,3-epoxy-2-methylpentane from hexafluoropropylene dimer, characterized by comprising the following steps:

[0120] 100 g of a fluorocarbon cyclic ether compound was added as a reaction medium to a polymerization container equipped with a stirrer. The reaction container was stirred, and then 100 g of a hexafluoropropylene dimer and 1 g of an oxidation catalyst were added. The polymerization container was heated to carry out a molecular oxygen oxidation reaction to obtain perfluoro-2,3-epoxy-2-methylpentane.

[0121] The fluorocarbon cyclic ether compound is selected from at least one of perfluoro-2-n-propyl-cyclopentyl ether, perfluoro-2-n-butyl-cyclopentyl ether, perfluoromethylcyclohexane, and perfluoro-2-n-propyl-cyclohexyl ether.

[0122] The hexafluoropropylene dimer structure is selected from D2, namely perfluoro-2-methyl-2-pentene.

[0123] The preparation method of the oxidation catalyst is:

[0124] S1: Add 20 g of 4,4'-divinyl-2,2'-bipyridine, 200 g of DMF, 2 g of 30% by mass hydrochloric acid, 1 g of cobalt dichloride, 1 g of chromium dichloride, and 1 g of lanthanum trichloride into a stirred tank and stir at 70°C for 50 min;

[0125] S2: Add 0.3 g of dimethyldiallylammonium chloride and 2 g of potassium tert-butoxide, and stir at 70°C for 60 min to obtain the active component of the organometallic impregnation solution;

[0126] S3: Under nitrogen atmosphere, add 50 g of tourmaline ceramic balls treated with acrylsilane, stir at 70°C for 200 min, filter, stand and dry at 70°C for 50 h, and then calcine at 250°C in air atmosphere for 3 h to obtain an oxidation catalyst.

[0127] The active component loading amount of the organic metal impregnation solution accounts for 2 wt % of the entire oxidation catalyst.

[0128] The preparation method of the tourmaline ceramic balls treated with acrylsilane described in the above technical solution is:

[0129] 3 g of acrylsiloxane, 300 g of tourmaline ceramic balls, and 1000 g of water were added, stirred at 30° C. for 60 min, filtered, and dried to obtain acrylsilane-treated tourmaline ceramic balls.

[0130] The acryloxysilane is 3-(methacryloyloxy)propyltrimethoxysilane (CAS No.: 2530-85-0).

[0131] The reaction temperature was 45°C.

[0132] The reaction environment is an oxygen environment, and high-purity oxygen is introduced into the reaction container during the reaction process, with a purity of not less than 99 wt%.

[0133] The pressure in the reaction vessel was maintained at 0.5 MPa by injecting pure oxygen.

[0134] In this comparative example, after separation and purification, the conversion rate based on perfluoro-2-methyl-2-pentene was 87.1%, and the product yield was 93.5%.

[0135] <Comparative Example 3>

[0136] A catalyst for preparing perfluoro-2,3-epoxy-2-methylpentane from hexafluoropropylene dimer, characterized by comprising the following steps:

[0137] 100 g of a fluorocarbon cyclic ether compound was added as a reaction medium to a polymerization container equipped with a stirrer. The reaction container was stirred, and then 100 g of a hexafluoropropylene dimer and 1 g of an oxidation catalyst were added. The polymerization container was heated to carry out a molecular oxygen oxidation reaction to obtain perfluoro-2,3-epoxy-2-methylpentane.

[0138] The fluorocarbon cyclic ether compound is selected from at least one of perfluoro-2-n-propyl-cyclopentyl ether, perfluoro-2-n-butyl-cyclopentyl ether, perfluoromethylcyclohexane, and perfluoro-2-n-propyl-cyclohexyl ether.

[0139] The hexafluoropropylene dimer structure is selected from D2, namely perfluoro-2-methyl-2-pentene.

[0140] The preparation method of the oxidation catalyst is:

[0141] S1: Add 20 g of 4,4'-divinyl-2,2'-bipyridine, 200 g of DMF, 2 g of 30% by mass hydrochloric acid, 1 g of cobalt dichloride, 1 g of chromium dichloride, and 1 g of lanthanum trichloride into a stirred tank and stir at 70°C for 50 min;

[0142] S2: Add 0.3 g of dimethyldiallylammonium chloride, 30 g of 2,5-dimercaptothiadiazole zinc salt, and 2 g of potassium tert-butoxide, and stir at 70°C for 60 min to obtain the active component of the organometallic impregnation solution;

[0143] S3: Under nitrogen atmosphere, tourmaline ceramic balls were added, stirred at 70°C for 200 min, filtered, allowed to stand and dry at 70°C for 50 h, and then calcined at 250°C in air atmosphere for 3 h to obtain an oxidation catalyst.

[0144] The active component loading amount of the organic metal impregnation solution accounts for 2 wt % of the entire oxidation catalyst.

[0145] The reaction temperature was 45°C.

[0146] The reaction environment is an oxygen environment, and high-purity oxygen is introduced into the reaction container during the reaction process, with a purity of not less than 99 wt%.

[0147] The pressure in the reaction vessel was maintained at 0.5 MPa by injecting pure oxygen.

[0148] In this comparative example, after separation and purification, the conversion rate based on perfluoro-2-methyl-2-pentene was 86.6%, and the product yield was 92.0%.

[0149] Although the present invention has been described in detail above using general explanations, specific embodiments, and experiments, it will be apparent to those skilled in the art that modifications and improvements may be made based on the present invention. Therefore, such modifications and improvements, which do not depart from the spirit of the present invention, are intended to be within the scope of protection claimed herein.

Claims

1. A catalyst for preparing perfluoro-2,3-epoxy-2-methylpentane from hexafluoropropylene dimer, characterized in that: The preparation method of the catalyst is: S1: Add 20-30 parts of 4,4'-divinyl-2,2'-bipyridine, 200-300 parts of DMF, 2-4 parts of 20-30% by weight hydrochloric acid, 1-4 parts of cobalt dichloride, 1-4 parts of chromium dichloride, and 1-4 parts of lanthanum trichloride to a stirred tank, and stir at 70-80°C for 50-100 minutes; S2: Add 0.3-2.5 parts of dimethyldiallylammonium chloride, 30-48 parts of 2,5-dimercaptothiadiazole zinc salt, and 2-6 parts of potassium tert-butoxide, and stir at 70-80° C. for 60-150 minutes to obtain an active component of the organometallic impregnation solution; S3: Under a nitrogen atmosphere, add 50-100 parts of tourmaline ceramic balls treated with acryloxysilane, stir at 70-80°C for 200-300 minutes, filter, stand and dry at 70-80°C for 50-70 hours, and then calcine at 250-380°C in air for 3-5 hours to obtain an oxidation catalyst; The acryloxysilane is at least one of 3-(methacryloyloxy)propyltrimethoxysilane, 2-acrylate 3-(diethoxymethylsilyl)propyl ester, and acryloxymethyltrimethoxysilane.

2. The catalyst for preparing perfluoro-2,3-epoxy-2-methylpentane from hexafluoropropylene dimer according to claim 1, characterized in that: The active component loading amount of the organic metal impregnation solution accounts for 0.5-15.0 wt% of the entire oxidation catalyst.

3. The catalyst for preparing perfluoro-2,3-epoxy-2-methylpentane from hexafluoropropylene dimer according to claim 1, characterized in that: The preparation method of the acryloxysilane-treated tourmaline ceramic ball is as follows: Add 3-5 parts of acryloxysilane, 300-500 parts of tourmaline ceramic balls, and 1000-2000 parts of water according to mass parts, stir at 30-50° C. for 60-100 minutes, filter, and dry to obtain acryloxysilane-treated tourmaline ceramic balls.

4. A method for preparing perfluoro-2,3-epoxy-2-methylpentane from hexafluoropropylene dimer, characterized in that: The following steps are included: 100-300 parts by weight of a fluorocarbon cyclic ether compound as a reaction medium is added to a polymerization container equipped with a stirrer. The reaction container is stirred, and then 100-300 parts of hexafluoropropylene dimer and 1-5 parts of an oxidation catalyst are added. The polymerization container is heated to carry out a molecular oxygen oxidation reaction to obtain perfluoro-2,3-epoxy-2-methylpentane; The hexafluoropropylene dimer structure is selected from D2, i.e. perfluoro-2-methyl-2-pentene; The oxidation catalyst is the catalyst according to any one of claims 1 to 3.

5. The catalyst for preparing perfluoro-2,3-epoxy-2-methylpentane from hexafluoropropylene dimer according to claim 4, characterized in that: The fluorocarbon cyclic ether compound is selected from at least one of perfluoro-2-n-propyl-cyclopentyl ether, perfluoro-2-n-butyl-cyclopentyl ether, perfluoromethylcyclohexane, and perfluoro-2-n-propyl-cyclohexyl ether.

6. The catalyst for preparing perfluoro-2,3-epoxy-2-methylpentane from hexafluoropropylene dimer according to claim 4, characterized in that: The reaction temperature is 30-150°C.

7. The catalyst for preparing perfluoro-2,3-epoxy-2-methylpentane from hexafluoropropylene dimer according to claim 4, characterized in that: The reaction environment is an oxygen environment, and high-purity oxygen is introduced into the reaction container during the reaction process, and the purity of the oxygen is not less than 99 wt%.

8. The catalyst for preparing perfluoro-2,3-epoxy-2-methylpentane from hexafluoropropylene dimer according to claim 4, characterized in that: The pressure in the reaction container is maintained at 0.5-1.6 MPa by injecting pure oxygen.