Preparation method of 1,1,3,3-tetramethylbutyl peroxide

Abstract

This invention belongs to the field of organic compound production technology, specifically relating to a method for preparing 1,1,3,3-tetramethylbutyl peroxide, comprising the following steps: S1, adding 2,4,4-trimethyl-2-pentanol to cooled sulfuric acid, then adding an aqueous solution of hydrogen peroxide and stirring to initiate a preliminary reaction, followed by adding a modified resin catalyst to continue the reaction, separating the organic phase after the reaction, washing and drying the organic phase to obtain 1,1,3,3-tetramethylbutyl hydrogen peroxide; S2, under stirring conditions, adding an alkaline solution dropwise to the 1,1,3,3-tetramethylbutyl hydrogen peroxide to initiate a reaction, followed by adding trimethylacetyl chloride to initiate an acylation reaction, continuing the acylation reaction after the addition is complete, separating the organic phase after the reaction, washing the organic phase to obtain 1,1,3,3-tetramethylbutyl peroxide. This invention employs a one-pot method for preparation and uses a modified resin catalyst, thereby improving the conversion rate.

Description

Technical Field

[0001] This invention belongs to the field of organic compound production technology, specifically relating to a method for preparing 1,1,3,3-tetramethylbutyl peroxide. Background Technology

[0002] Organic peroxides are common polymerization initiators, and can be classified into hydrocarbon peroxides, peroxycarboxylic acids, acyl peroxides, ester peroxides, ketone peroxides, etc., based on the different substituent functional groups. 1,1,3,3-Tetramethylbutyl peroxide (TMP) is a commonly used organic peroxide polymerization initiator, characterized by its non-toxicity and low-temperature activity. It is widely used as an oxidant or polymerization initiator, primarily for the polymerization of vinyl chloride, ethylene, and various other olefins, offering advantages such as shortened polymerization reaction time and a narrow molecular weight distribution. As a highly efficient initiator for polymer synthesis, TPP has a wide range of applications. It is used in small quantities during polymerization, disperses easily in the polymerization system, exhibits uniform exothermic activity, is easy to control, and produces PVC products that are less prone to discoloration and have a mild odor. Its low solubility in water and low volatility make it a safe, efficient, and stable initiator for polymer synthesis. Excessive peroxide raw materials eventually enter the wastewater, leading to an increase in the COD value of the wastewater and increasing the cost of wastewater treatment. If the COD value of the wastewater is not reduced to the discharge standard before being discharged, it will cause environmental pollution.

[0003] In current organic peroxide synthesis, most methods revolve around alcohols as raw materials, which are readily available. However, further research is needed on using other substances as raw materials to prepare 1,1,3,3-tetramethylbutyl peroxide.

[0004] Chinese patent CN104557652A discloses a method for preparing tert-butyl peroxide using a heterogeneous catalyst. The method involves using tert-butanol and hydrogen peroxide as raw materials, an acidic ion exchange resin as a catalyst, reflux reaction, cooling, and separation by settling to obtain an oil phase and an aqueous phase. The oil phase is then washed with alkali and water to obtain a di-tert-butyl peroxide solution (DTBP). The oil phase washing liquid and the aqueous phase constitute a tert-butyl hydrogen peroxide aqueous solution (TBHP). The resin used in this patented technology has a small specific surface area and few active sites, failing to provide chemical anchoring and adsorption networks for the reactants on the catalyst surface. Summary of the Invention

[0005] In view of the shortcomings of the prior art, the technical problem to be solved by the present invention is to provide a method for preparing 1,1,3,3-tetramethylbutyl peroxide, establish a complete catalytic reaction system, and improve the yield of 1,1,3,3-tetramethylbutyl hydroperoxide and 1,1,3,3-tetramethylbutyl peroxide.

[0006] The technical solution adopted by this invention to solve its technical problem is:

[0007] The preparation method of 1,1,3,3-tetramethylbutyl peroxide (TMP) according to the present invention includes the following steps:

[0008] S1. Add 2,4,4-trimethyl-2-pentanol to cooled sulfuric acid, then add hydrogen peroxide aqueous solution and stir to carry out a preliminary reaction. Subsequently, add modified resin catalyst to continue the reaction. After the reaction, separate the organic phase, wash and dry the organic phase to obtain 1,1,3,3-tetramethylbutyl hydrogen peroxide.

[0009] S2. Under stirring conditions, an alkaline solution was added dropwise to 1,1,3,3-tetramethylbutyl hydroperoxide to carry out the reaction. Then, trimethylacetyl chloride was added dropwise to carry out the acylation reaction. After the addition was completed, the acylation reaction was continued. After the reaction, the organic phase was separated and washed to obtain trimethylacetic acid peroxide-1,1,3,3-tetramethylbutyl ester.

[0010] in:

[0011] The modified resin catalyst in step S1 is a fatty alcohol polyoxyethylene ether modified D113 resin catalyst, and the structural formula of the fatty alcohol polyoxyethylene ether modified D113 resin catalyst is as follows:

[0012]

[0013] In the formula: R is a C1-C8 alkyl group.

[0014] The modified resin catalyst is prepared as follows:

[0015] a1. D113 resin is obtained by soaking, washing and drying the D113 resin to be treated;

[0016] a2: Add the modifier and D113 resin to the solvent and stir evenly. Then add the catalyst and polymerization inhibitor to react. After the reaction is completed, cool, filter, wash and dry to obtain the modified resin catalyst.

[0017] D113 resin is a weakly acidic cation exchange resin based on a macroporous acrylic copolymer crosslinked polymer matrix.

[0018] In step a1, the soaking is carried out using deionized water and anhydrous ethanol for 13-15 hours. The washing is carried out using anhydrous ethanol for 2-3 times. The drying is carried out under vacuum at a temperature of 55-65℃ for 8-12 hours.

[0019] In step a2, the modifier is fatty alcohol polyoxyethylene ether, which is one of diethylene glycol propyl ether, diethylene glycol butyl ether, diethylene glycol monohexyl ether, or diethylene glycol monophenyl ether. The mass ratio of the modifier to D113 resin is 2-5:1. The solvent is toluene, and the mass ratio of the solvent to D113 resin is 12-15:1. The catalyst is p-toluenesulfonic acid, and the amount of catalyst is 0.5-0.6% of the mass of D113 resin. The polymerization inhibitor is hydroquinone, and the amount of polymerization inhibitor is 0.05-0.08% of the mass of D113 resin. The reaction temperature is 80-110℃, the reaction time is 3-6h, and the reaction is cooled to room temperature. The washing is performed sequentially with toluene, ethanol, an aqueous ethanol solution, and deionized water. The drying is performed under vacuum at a temperature of 40-60℃ for 8-12h.

[0020] In step S1, the cooling temperature is 0-2℃, the sulfuric acid concentration is 58-63wt%, the hydrogen peroxide aqueous solution concentration is 45-55wt%, the molar ratio of 2,4,4-trimethyl-2-pentanol, sulfuric acid, and hydrogen peroxide in the hydrogen peroxide aqueous solution is 1:1-1.5:1-2.5, and the mass ratio of the modified resin catalyst to 2,4,4-trimethyl-2-pentanol is 0.018-0.034:1.

[0021] In step S1, the initial reaction time is 1.5-2.5 h, the initial reaction temperature is 20-30 °C, the stirring speed is 200-300 rpm, the continued reaction time is 6.5-14 h, and the continued reaction temperature is 20-30 °C.

[0022] In step S2, the alkaline solution is a NaOH solution with a concentration of 25-35 wt%, the trimethylacetyl chloride has a purity of 95-99%, and the molar ratio of trimethylacetyl chloride, NaOH in the NaOH solution, and 2,4,4-trimethyl-2-pentanol in step S1 is 1-1.5:1-1.5:1.

[0023] In step S2, the stirring temperature is 0-10℃, the stirring speed is 200-300rpm, and the reaction time is 0.5-1h.

[0024] In step S2, the dropping temperature is 0-10℃ and the dropping time is 1.5-3h. The acyl chlorination reaction continues at a temperature of 0-10℃ for 0.5-2.5h. The washing is performed 2-3 times with distilled water.

[0025] The reaction equation of this invention is as follows:

[0026]

[0027]

[0028] This invention uses 2,4,4-trimethyl-2-pentanol and hydrogen peroxide as raw materials to prepare 1,1,3,3-tetramethylbutyl hydrogen peroxide under the catalysis of a modified resin catalyst, thus improving the yield of 1,1,3,3-tetramethylbutyl hydrogen peroxide. Subsequently, this 1,1,3,3-tetramethylbutyl hydrogen peroxide can also be used to prepare trimethylacetic acid peroxide-1,1,3,3-tetramethylbutyl ester. The preparation of 1,1,3,3-tetramethylbutyl hydrogen peroxide adopts a one-pot synthesis method, which differs from the traditional stepwise addition of alcohol and hydrogen peroxide. The one-time addition reaction method can control and reduce the changes in reaction conditions during the synthesis process. Furthermore, the reaction between sulfuric acid and hydrogen peroxide in the preparation of 1,1,3,3-tetramethylbutyl hydrogen peroxide is a reversible reaction. The addition of a modified resin catalyst can provide a certain acidic environment for the reaction system, which can improve the reaction efficiency when subsequently introducing ether oxygen bonds and ester groups. Because D113 resin itself has a macroporous structure and carboxyl acidic sites, it is suitable for the D113 reaction. The modification of D113 resin can further introduce ether oxygen bonds and ester groups, thus providing an anchoring effect for the reactions of hydrogen peroxide, 2,4,4-trimethyl-2-pentanol, and sulfuric acid through hydrogen bonds. This provides more reaction sites for the reactions, promotes the forward direction of the reversible reactions, and increases the yield of 1,1,3,3-tetramethylbutyl hydrogen peroxide. In addition, the introduction of ether oxygen bonds and ester groups into D113 resin can form hydrogen bonds with the carboxyl groups and water molecules in the D113 resin in water, which can build more porous structures and increase the specific surface area of ​​the modified resin catalyst.

[0029] The modified resin catalyst exhibits increased surface wrinkle density and specific surface area. Ether-oxygen bonds and ester groups jointly construct a catalytic system. In aqueous solution, these bonds synergistically interact, forming a branched network structure through hydrogen bonding, resulting in a three-dimensional network morphology. Compared to a single ester group structure, the network structure formed by the synergistic interaction of ether-oxygen bonds and ester groups is more dense, adaptable, and controllable. Simultaneously, in aqueous solution, the ether-oxygen bonds and ester groups synergistically interact with the carboxyl groups in the catalyst through hydrogen bonding, further enhancing the network density and robustness of the catalyst in aqueous solution. This provides more reaction sites, promotes reaction progress, and improves reaction conversion. From a structural perspective, the ester group is a strong electron-withdrawing group, while the ether oxygen bond has lone pairs of electrons, exhibiting an electron-donating effect. Introducing both the ester group and the ether oxygen bond into the D113 resin structure can create a novel "push-pull" electron effect. During the reaction, the ester group and the ether oxygen bond form adsorption active centers with the reactants through hydrogen bonding. The ether oxygen bond "pushes" electrons towards the active center, while the ester group "pushes" electrons from it. This synergistic effect can significantly polarize the reactive sites, giving them both electrophilic and nucleophilic properties. This effectively enhances the anchoring and activation of the reactants, lowers the reaction energy barrier, and increases the reaction rate. Furthermore, the introduction of ether oxygen bonds and ester groups into the D113 resin, besides forming hydrogen bonds with the carboxyl groups and increasing the catalyst's catalytic surface area and pore structure, can also enhance the "Lewis acidity" of the modified resin catalyst during the reaction, improving reaction efficiency and conversion rate. The purity and yield of 1,1,3,3-tetramethylbutyl hydroperoxide are significantly improved. Choosing highly reactive trimethylacetyl chloride can improve the yield of subsequent products. When it reacts with 1,1,3,3-tetramethylbutyl hydroperoxide to prepare trimethylacetic acid peroxide-1,1,3,3-tetramethylbutyl ester, the yield of trimethylacetic acid peroxide-1,1,3,3-tetramethylbutyl ester is further improved.

[0030] The beneficial effects of this invention are:

[0031] In this invention, 1,1,3,3-tetramethylbutyl hydroperoxide is prepared using a one-pot method, which improves the conversion rate of raw materials and significantly increases the product yield. A modified resin catalyst is used in the synthesis of 1,1,3,3-tetramethylbutyl hydroperoxide, which improves the degree of reaction conversion. Using 1,1,3,3-tetramethylbutyl hydroperoxide and trimethylacetyl chloride as raw materials, 1,1,3,3-tetramethylbutyl peroxide is synthesized. It has a low activation energy and high activity, making it easier to initiate polymerization reactions.

[0032] The 1,1,3,3-tetramethylbutyl hydrogen peroxide produced by the modified resin catalyst can be used as a raw material for the next reaction, and the yield of 1,1,3,3-tetramethylbutyl hydrogen peroxide is increased to over 90%. Using the obtained 1,1,3,3-tetramethylbutyl hydrogen peroxide as a reactant, it reacts with NaOH and trimethylacetyl chloride at 0-10℃ to obtain trimethylacetic acid peroxide-1,1,3,3-tetramethylbutyl ester in a yield of over 92%. Attached Figure Description

[0033] Figure 1 This is a SEM image of D113 resin;

[0034] Figure 2 This is a SEM image of the modified resin catalyst prepared in Example 1 of this invention;

[0035] Figure 3 This is the 1H NMR spectrum of 1,1,3,3-tetramethylbutyl hydroperoxide prepared in Example 1 of this invention;

[0036] Figure 4 This is the carbon NMR spectrum of 1,1,3,3-tetramethylbutyl hydroperoxide prepared in Example 1 of this invention;

[0037] Figure 5 This is the 1H NMR spectrum of 1,1,3,3-tetramethylbutyl hydroperoxide prepared in Comparative Example 1 of this invention.

[0038] Figure 6 This is the 1H NMR spectrum of 1,1,3,3-tetramethylbutylhydrogen peroxide prepared in Comparative Example 2 of this invention. Detailed Implementation

[0039] The technical solution of the present invention will be further described below with reference to the embodiments.

[0040] Example 1

[0041] Preparation of modified resin catalysts:

[0042] a1. The D113 resin to be treated was soaked in deionized water for 1 hour, then soaked in anhydrous ethanol for 12 hours, washed three times with ethanol, and then vacuum dried at 60℃ for 10 hours to obtain D113 resin. SEM images of the D113 resin are shown below. Figure 1 ;

[0043] a2. 3g of diethylene glycol butyl ether and 1.5g of D113 resin were added to 18g of toluene and stirred until homogeneous. Then, 0.0075g of p-toluenesulfonic acid and 0.00075g of hydroquinone were added, and the mixture was reacted at 80℃ for 6 hours. After the reaction was complete, the mixture was cooled to room temperature and filtered. The catalyst was washed twice with toluene, once with ethanol, once with an ethanol-water solution (ethanol to water volume ratio 1:1), and finally rinsed once with deionized water. The catalyst was then vacuum dried at 50℃ for 10 hours to obtain the modified resin catalyst. Its SEM image is shown below. Figure 2 .

[0044] Depend on Figure 1 and Figure 2 It can be seen that the surface wrinkle structure density of the modified resin catalyst increases, and the specific surface area increases.

[0045] A method for preparing 1,1,3,3-tetramethylbutyl peroxide includes the following steps:

[0046] S1. 13g of 2,4,4-trimethyl-2-pentanol was added to 21.23g of 60wt% sulfuric acid at 0℃, followed by 10.2g of 50wt% hydrogen peroxide aqueous solution. The mixture was initially reacted at 20℃ and 300rpm for 2 hours with stirring. Then, 0.3g of modified resin catalyst was added, and the reaction was continued at 20℃ for 10 hours. After the reaction, the mixture was allowed to stand and separate into layers. The upper organic phase was collected and washed twice with distilled water. The liquid-liquid chromatography yielded 1,1,3,3-tetramethylbutyl hydrogen peroxide, with a yield of 91.05%. The 1H and 1C NMR spectra are shown below. Figure 3 , 4 As shown, 1,1,3,3-tetramethylbutyl hydroperoxide is stored at -10°C.

[0047] S2. Under stirring conditions of 2℃ and 300 rpm, 17.33 g of 30 wt% sodium hydroxide solution was added dropwise to the 1,1,3,3-tetramethylbutyl hydroperoxide prepared in S1 and reacted for 0.75 h. Subsequently, 15.68 g of 98% pure trimethylacetyl chloride was added dropwise over 2 h at 2℃ to carry out an acylation reaction. After the addition was completed, the acylation reaction was continued at 2℃ for 1.5 h. After the reaction, the organic phase was separated by standing and allowed to separate into layers. The organic phase was washed three times with distilled water and separated to obtain trimethylacetic acid peroxide-1,1,3,3-tetramethylbutyl ester with a yield of 94.63%. Trimethylacetic acid peroxide-1,1,3,3-tetramethylbutyl ester was diluted with xylene and stored at -20℃ in the dark.

[0048] Example 2

[0049] Preparation of modified resin catalysts:

[0050] a1. The D113 resin to be treated was soaked in deionized water for 1.5 h, then soaked in anhydrous ethanol for 13.5 h, washed twice with ethanol, and then vacuum dried at 55 °C for 12 h to obtain D113 resin.

[0051] a2. 7.5g of diethylene glycol monophenyl ether and 1.5g of D113 resin were added to 22.5g of toluene and stirred evenly. Then, 0.009g of p-toluenesulfonic acid and 0.0012g of hydroquinone were added and reacted at 100℃ for 5h. After the reaction was completed, the mixture was cooled to room temperature and filtered. The solution was washed 3 times with toluene, 2 times with ethanol, and 1 time with an ethanol-water solution (ethanol and water volume ratio of 1:1). Finally, it was rinsed 2 times with deionized water and then vacuum dried at 40℃ for 12h to obtain the modified resin catalyst.

[0052] A method for preparing 1,1,3,3-tetramethylbutyl peroxide includes the following steps:

[0053] S1. Add 15g of 2,4,4-trimethyl-2-pentanol to 26g of 63wt% sulfuric acid at 0℃, then add 8.9g of 45wt% hydrogen peroxide aqueous solution. React initially at 30℃ and 200rpm for 2.5h with stirring. Then add 0.5g of modified resin catalyst and continue the reaction at 30℃ for 6.5h. After the reaction, allow the mixture to stand and separate into layers. Take the upper organic phase and wash it twice with distilled water. Separate the liquid to obtain 1,1,3,3-tetramethylbutyl hydrogen peroxide with a yield of 91.54%. Store 1,1,3,3-tetramethylbutyl hydrogen peroxide at -10℃.

[0054] S2. Under stirring conditions of 5℃ and 200 rpm, 18.5 g of 25 wt% sodium hydroxide solution was added dropwise to the 1,1,3,3-tetramethylbutyl hydroperoxide prepared in S1 and reacted for 1 h. Then, 21.5 g of 95% pure trimethylacetyl chloride was added dropwise over 3 h at 5℃ to carry out an acylation reaction. After the addition was completed, the acylation reaction was carried out again at 5℃ for 0.5 h. After the reaction, the organic phase was separated by standing and layering. The organic phase was washed three times with distilled water and then separated to obtain trimethylacetic acid peroxide-1,1,3,3-tetramethylbutyl ester with a yield of 92.72%.

[0055] Example 3

[0056] Preparation of modified resin catalysts:

[0057] a1. The D113 resin to be treated was soaked in deionized water for 2 hours, then soaked in anhydrous ethanol for 11 hours, washed with ethanol 3 times, and then vacuum dried at 65°C for 8 hours to obtain D113 resin.

[0058] a2. Add 5g of diethylene glycol propyl ether and 1.5g of D113 resin to 20g of toluene and stir until homogeneous. Then add 0.008g of p-toluenesulfonic acid and 0.001g of hydroquinone and react at 110℃ for 3h. After the reaction is complete, cool to room temperature and filter. Wash once with toluene, twice with ethanol, twice with an ethanol-water solution (ethanol and water volume ratio of 1:1), and finally rinse twice with deionized water. Then vacuum dry at 60℃ for 8h to obtain the modified resin catalyst.

[0059] A method for preparing 1,1,3,3-tetramethylbutyl peroxide includes the following steps:

[0060] S1. Add 16g of 2,4,4-trimethyl-2-pentanol to 22.1g of 55wt% sulfuric acid at 2℃, then add 11.4g of 55wt% hydrogen peroxide aqueous solution. React initially at 25℃ and 250rpm for 1.5h with stirring. Then add 0.29g of modified resin catalyst and continue the reaction at 25℃ for 14h. After the reaction, allow the mixture to stand and separate into layers. Take the upper organic phase and wash it three times with distilled water. Separate the liquid to obtain 1,1,3,3-tetramethylbutyl hydrogen peroxide with a yield of 90.86%. Store 1,1,3,3-tetramethylbutyl hydrogen peroxide at -10℃.

[0061] S2. Under stirring conditions of 10℃ and 250 rpm, 21 g of 35 wt% sodium hydroxide solution was added dropwise to the 1,1,3,3-tetramethylbutyl hydroperoxide prepared in S1 and reacted for 0.5 h. Subsequently, 15.5 g of 99% pure trimethylacetyl chloride was added dropwise over 1.5 h at 10℃ to carry out an acylation reaction. After the addition was completed, the acylation reaction was carried out again at 10℃ for 2.5 h. After the reaction, the organic phase was allowed to stand and separated into layers. The organic phase was washed three times with distilled water and then separated to obtain trimethylacetic acid peroxide-1,1,3,3-tetramethylbutyl ester with a yield of 94.37%.

[0062] Comparative Example 1

[0063] In step a2, diethylene glycol butyl ether was not added, and the remaining steps were the same as in Example 1; the yield of 1,1,3,3-tetramethylbutyl hydroperoxide was 75.84%, and the yield of trimethylacetic acid peroxide-1,1,3,3-tetramethylbutyl ester was 80.35%; the 1H NMR spectrum of 1,1,3,3-tetramethylbutyl hydroperoxide is shown below. Figure 5 As shown.

[0064] Comparative Example 2

[0065] In step a2, diethylene glycol butyl ether was replaced with diethylene glycol, and the remaining steps were the same as in Example 1; the yield of 1,1,3,3-tetramethylbutyl hydroperoxide was 83.72%, and the yield of trimethylacetic acid peroxide-1,1,3,3-tetramethylbutyl ester was 87.65%; the 1H NMR spectrum of 1,1,3,3-tetramethylbutyl hydroperoxide is shown below. Figure 6 As shown.

Claims

1. A method for preparing 1,1,3,3-tetramethylbutyl peroxide, characterized in that, Includes the following steps: S1. 2,4,4-Trimethyl-2-pentanol is added to cooled sulfuric acid, followed by the addition of hydrogen peroxide aqueous solution and stirring to initiate a preliminary reaction. Then, a modified resin catalyst is added to continue the reaction. After the reaction, the organic phase is separated, washed, and dried to obtain 1,1,3,3-tetramethylbutyl hydrogen peroxide. The modified resin catalyst is a fatty alcohol polyoxyethylene ether modified D113 resin catalyst, and the fatty alcohol polyoxyethylene ether is one of diethylene glycol propyl ether, diethylene glycol butyl ether, diethylene glycol monohexyl ether, or diethylene glycol monophenyl ether. S2. Under stirring conditions, alkaline solution was added dropwise to 1,1,3,3-tetramethylbutyl hydroperoxide to carry out the reaction, followed by the addition of trimethylacetyl chloride to carry out the acyl chloride reaction. After the addition was completed, the acyl chloride reaction was continued. After the reaction, the organic phase was separated and washed to obtain trimethylacetic acid peroxide-1,1,3,3-tetramethylbutyl ester. The preparation method of the modified resin catalyst is as follows: a1. D113 resin is obtained by soaking, washing and drying the D113 resin to be treated; a2: Add the modifier and D113 resin to the solvent and stir evenly. Then add the catalyst and polymerization inhibitor to react. After the reaction is completed, cool, filter, wash and dry to obtain the modified resin catalyst. In step a2, the modifier is fatty alcohol polyoxyethylene ether, and the mass ratio of the modifier to D113 resin is 2-5:

1. The solvent is toluene, and the mass ratio of the solvent to D113 resin is 12-15:

1. The catalyst is p-toluenesulfonic acid, and the amount of catalyst is 0.5-0.6% of the mass of D113 resin. The polymerization inhibitor is hydroquinone, and the amount of polymerization inhibitor is 0.05-0.08% of the mass of D113 resin. The reaction temperature is 80-110℃, and the reaction time is 3-6h.

2. The method for preparing 1,1,3,3-tetramethylbutyl peroxide according to claim 1, characterized in that, In step a1, the soaking is carried out using deionized water and anhydrous ethanol for 13-15 hours. The washing is done with anhydrous ethanol 2-3 times. The drying is done under vacuum at a temperature of 55-65℃ for 8-12 hours.

3. The method for preparing 1,1,3,3-tetramethylbutyl peroxide according to claim 1, characterized in that, In step a2, the mixture is cooled to room temperature, washed sequentially with toluene, ethanol, an aqueous ethanol solution, and deionized water, and dried under vacuum at a temperature of 40-60°C for 8-12 hours.

4. The method for preparing 1,1,3,3-tetramethylbutyl peroxide according to claim 1, characterized in that, In step S1, the cooling temperature is 0-2℃, the sulfuric acid concentration is 58-63wt%, the hydrogen peroxide aqueous solution concentration is 45-55wt%, the molar ratio of 2,4,4-trimethyl-2-pentanol, sulfuric acid, and hydrogen peroxide in the hydrogen peroxide aqueous solution is 1:1-1.5:1-2.5, and the mass ratio of the modified resin catalyst to 2,4,4-trimethyl-2-pentanol is 0.018-0.034:

1.

5. The method for preparing 1,1,3,3-tetramethylbutyl peroxide according to claim 1, characterized in that, In step S1, the initial reaction time is 1.5-2.5 h, the initial reaction temperature is 20-30 °C, the stirring speed is 200-300 rpm, the continued reaction time is 6.5-14 h, and the continued reaction temperature is 20-30 °C.

6. The method for preparing 1,1,3,3-tetramethylbutyl peroxide according to claim 1, characterized in that, In step S2, the alkaline solution is a NaOH solution with a concentration of 25-35 wt%, and the trimethylacetyl chloride has a purity of 95-99%. The molar ratio of trimethylacetyl chloride, NaOH in the NaOH solution, and 2,4,4-trimethyl-2-pentanol in step S1 is 1-1.5:1-1.5:

1.

7. The method for preparing 1,1,3,3-tetramethylbutyl peroxide according to claim 1, characterized in that, In step S2, the stirring temperature is 0-10℃, the stirring speed is 200-300rpm, and the reaction time is 0.5-1h.

8. The method for preparing 1,1,3,3-tetramethylbutyl peroxide according to claim 1, characterized in that, In step S2, the dropping temperature is 0-10℃ and the dropping time is 1.5-3h. The acyl chlorination reaction continues at a temperature of 0-10℃ and a reaction time of 0.5-2.5h. The washing is performed 2-3 times with distilled water.

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