Process for the synthesis of tert-butyl peroxyacetate

Abstract

This invention belongs to the field of acyclic compound technology, specifically relating to a method for preparing tert-butyl peroxide. An alkaline solution is added to acetic anhydride, and the mixture is stirred to obtain a reaction solution. A composite catalyst is added to a purified tert-butyl hydrogen peroxide solution, and the mixture is stirred to obtain a mixture. The reaction solution is added to the mixture, and the mixture is stirred to obtain an organic phase. The organic phase is acid-washed to obtain an oil phase. The oil phase is then alkali-washed, salt-washed, and freeze-dried to obtain tert-butyl peroxide. This invention purifies the tert-butyl hydrogen peroxide solution, effectively removing di-tert-butyl peroxide impurities. A composite catalyst composed of p-toluenesulfonic acid, perfluorosulfonic acid resin, and sulfonated carbon is used as the catalyst, reducing the destructive effect on the product tert-butyl peroxide and significantly improving the yield of tert-butyl peroxide, thus possessing industrial production significance.

Description

Technical Field

[0001] This invention belongs to the field of acyclic compound technology, specifically relating to a synthesis process of tert-butyl peroxide. Background Technology

[0002] tert-butyl peroxide (TBPA) is a D-type liquid organic peroxide, belonging to class 5.2. Its self-accelerating decomposition temperature is 70°C, and its 10-hour half-life corresponds to a temperature of 100°C. It possesses advantages such as high reactive oxygen content and high reactivity, but it is prone to decomposition and can cause safety accidents. TBPA can be used as a low-temperature polymerization initiator for high-pressure polyethylene and can form composite initiation systems with other initiators, making the polyethylene polymerization process more stable and safe. In addition, TBPA can also be used as a high-temperature curing agent for unsaturated resins. The traditional synthesis method for TBPA is to first synthesize tert-butyl hydroperoxide from tert-butanol and hydrogen peroxide under strong acid conditions, and then react the tert-butyl hydroperoxide with acetic anhydride to produce tert-butyl peroxide. However, when using this synthesis method to prepare tert-butyl peroxide, the intermediate tert-butyl hydroperoxide contains a large amount of di-tert-butyl peroxide impurities, which adversely affects the quality and yield of tert-butyl peroxide.

[0003] Chinese patent CN119219538A discloses a method for preparing tert-butyl peroxide. The method involves pumping liquid alkali and water into a reaction vessel, adding tert-butyl hydrogen peroxide to the vessel for a salt-forming reaction, and then adding benzoyl chloride and a catalyst for a condensation reaction to obtain crude tert-butyl peroxide. The crude tert-butyl peroxide is then washed with alkali and water, and a stabilizer and co-solvent are added to obtain the final product. However, the catalyst preparation process in this patent is cumbersome and costly, making it unsuitable for industrial application. Furthermore, the tert-butyl hydrogen peroxide raw material contains many impurities, resulting in low purity of the final product, which fails to meet the requirements for commercial applications. Summary of the Invention

[0004] The purpose of this invention is to provide a synthesis process for tert-butyl peroxide, which can effectively improve the purity and yield of tert-butyl peroxide.

[0005] The synthesis process of tert-butyl peroxide ester according to the present invention includes the following steps:

[0006] (1) Add alkaline solution to acetic anhydride, stir to react, and obtain reaction solution;

[0007] (2) Add the composite catalyst to the purified tert-butyl hydrogen peroxide solution and stir to obtain a mixture;

[0008] (3) Add the reaction solution to the mixture, stir to react, let stand, separate, and obtain the organic phase;

[0009] (4) The organic phase is acid-washed to obtain the oil phase;

[0010] (5) The oil phase was washed with alkali and salt, and then freeze-dried to obtain tert-butyl peroxide.

[0011] In step (1), the molar ratio of alkali to acetic anhydride in the alkaline solution is 1.8 to 1.9:1. The alkaline solution is a potassium hydroxide solution or a sodium hydroxide solution with a concentration of 35 to 37 wt.%. The addition temperature is 50 to 53°C. The stirring reaction time is 45 to 50 min and the stirring reaction temperature is 50 to 53°C.

[0012] In step (2), the concentration of the purified tert-butyl hydrogen peroxide solution is 79.3-80 wt.%, the composite catalyst is a mixture of p-toluenesulfonic acid, perfluorosulfonic acid resin and sulfonated carbon, wherein the mass ratio of p-toluenesulfonic acid, perfluorosulfonic acid resin and sulfonated carbon is 1.06-1.1:1.04-1.1:1; the mass ratio of the composite catalyst to the purified tert-butyl hydrogen peroxide solution is 1:8-10, the addition temperature is 10-15℃, the stirring time is 5-15 min, the stirring temperature is 10-15℃, and the mass ratio of the purified tert-butyl hydrogen peroxide solution to the acetic anhydride in step (1) is 2-2.2:1.

[0013] In step (3), the temperature is 15-20℃, the stirring reaction temperature is 15-20℃, the stirring reaction time is 55-59min, the standing time is 15-30min, and the standing temperature is 15-20℃.

[0014] In step (4), the acid washing process involves adding sodium metabisulfite solution, stirring, allowing it to stand, and then separating. The concentration of the sodium metabisulfite solution is 2-10 wt.%, the volume ratio of sodium metabisulfite solution to organic phase is 1:1.30-1.40, the stirring temperature is 3-5℃, the stirring time is 5-10 minutes, the standing temperature is 5-15℃, and the standing time is 22-28 minutes.

[0015] In step (5), the alkaline washing involves washing with an alkaline solution and allowing it to stand to separate the aqueous phase. The alkaline solution is a sodium bicarbonate solution with a concentration of 3 wt.% to saturation. The washing is performed 2 to 3 times, and the standing time is 15 to 30 minutes at a temperature of 5 to 15°C. The salt washing involves washing with a salt solution until neutral. The salt solution is a sodium chloride solution with a concentration of 3 to 10 wt.%. The freeze-drying time is 10 to 12 hours, and the freeze-drying temperature is -10 to -5°C.

[0016] The preparation method of purified tert-butyl hydrogen peroxide solution in step (2) includes the following steps:

[0017] (a) Add alkali to tert-butyl hydrogen peroxide solution, react, let stand, separate, and obtain aqueous phase;

[0018] (b) Add sulfuric acid to the aqueous phase to react and obtain a reaction solution. Let the reaction solution stand and separate to obtain a purified tert-butyl hydrogen peroxide solution.

[0019] In step (a), the tert-butyl hydrogen peroxide solution contains 65–75 wt.% tert-butyl hydrogen peroxide, 10–15 wt.% di-tert-butyl peroxide, and the remainder is water; the addition temperature is 15–25°C, the reaction temperature is 15–25°C, the reaction time is 20–30 min, the alkali solution is potassium hydroxide solution or sodium hydroxide solution, the concentration of the alkali solution is 10–20 wt.%, the molar ratio of alkali in the alkali solution to tert-butyl hydrogen peroxide in the tert-butyl hydrogen peroxide solution is 1–1.3:1, the standing time is 15–30 min, and the standing temperature is 20–25°C.

[0020] In step (b), the temperature is 15-25°C, the reaction temperature is 15-25°C, and the concentration of sulfuric acid is 20-25 wt.%.

[0021] In step (b), the pH of the reaction solution is 4-6, the standing time is 15-30 min, and the standing temperature is 20-25℃.

[0022] This invention first hydrolyzes acetic anhydride under alkaline conditions to obtain sodium acetate / potassium acetate, then protonates the sodium acetate / potassium acetate under the action of a composite catalyst, and then reacts it directly with purified tert-butyl hydroperoxide to generate crude tert-butyl peroxide. Finally, after subsequent processing, the target product tert-butyl peroxide is obtained.

[0023] The reaction principle of this invention is as follows: an alkaline solution is added to acetic anhydride, which is first hydrolyzed to acetic acid. Then, the acetic acid reacts with the alkaline solution to generate sodium / potassium acetate. Since acetic anhydride is in excess during this process, the resulting reaction solution is weakly acidic. Purified tert-butyl hydroperoxide is premixed with a composite catalyst to obtain a mixture. The reaction solution is added to the mixture, and under the action of the composite catalyst, the sodium / potassium acetate is first protonated, and then undergoes a nucleophilic esterification reaction with tert-butyl hydroperoxide to generate the target product, tert-butyl peroxide.

[0024] The beneficial effects of this invention are as follows:

[0025] 1. The tert-butyl hydrogen peroxide solution used in the preparation of tert-butyl peroxide mostly contains the impurity di-tert-butyl peroxide. The presence of this impurity leads to a high impurity content in the product tert-butyl peroxide, significantly reducing the product purity. Therefore, this invention purifies the tert-butyl hydrogen peroxide solution to effectively remove the di-tert-butyl peroxide impurity: First, an alkaline solution is added to the tert-butyl hydrogen peroxide solution. The tert-butyl hydrogen peroxide reacts with the alkaline solution to generate tert-butyl peroxide salt, which is transferred to the aqueous phase. The impurity di-tert-butyl peroxide does not react with the alkaline solution and remains in the organic phase. Sulfuric acid is added to the aqueous phase containing tert-butyl peroxide salt, causing the tert-butyl peroxide salt to react with the sulfuric acid to generate tert-butyl hydrogen peroxide and sulfate. The sulfate remains soluble in the aqueous phase, while the tert-butyl hydrogen peroxide is an organic phase that separates from the aqueous phase. After separation, high-purity purified tert-butyl hydrogen peroxide can be obtained.

[0026] 2. Tert-butyl peroxide is a small-molecule organic peroxide. In high-concentration strong acids in solution, it will dissociate to release a large amount of free H+. + The free H + The presence of harmful substances can catalyze the breaking of the peroxy bond in tert-butyl peroxide, leading to its decomposition. Therefore, this invention employs a composite catalyst that exhibits low destructiveness to tert-butyl peroxide while maintaining high catalytic efficiency, balancing reaction efficiency and product stability. This composite catalyst is an acidic catalyst composed of p-toluenesulfonic acid, perfluorosulfonic acid resin, and sulfonated carbon, and it does not generate large amounts of free H₂ during use. + This catalyst possesses characteristics such as high catalytic efficiency, good thermal stability, and strong chemical stability. Sulfonated carbon itself provides acidic sites, enabling a synergistic catalytic effect with the sulfonic acid groups in p-toluenesulfonic acid and perfluorosulfonic acid resins, thus improving the selectivity and catalytic efficiency of the entire reaction and contributing to increased product yield. Using a composite catalyst composed of p-toluenesulfonic acid, perfluorosulfonic acid resin, and sulfonated carbon reduces the destructive effect on the product tert-butyl peroxide. The synergistic catalytic action of p-toluenesulfonic acid, perfluorosulfonic acid resin, and sulfonated carbon significantly improves the yield of tert-butyl peroxide, making it suitable for industrial production.

[0027] Perfluorosulfonic acid resin is a solid strong acid with high strength and extreme stability. It can serve as a long-lasting protonation center to maintain catalytic sustainability. Its perfluorohydrophobic framework and surface sulfonic acid groups can anchor liquid p-toluenesulfonic acid firmly to the surface of the perfluorosulfonic acid resin through hydrophobic association and intermolecular hydrogen bonds, achieving solid-phase dispersion of the liquid acid and ensuring that p-toluenesulfonic acid always exists in molecular form on the surface of the perfluorosulfonic acid resin. The strong hydrophobicity of the perfluorosulfonic acid resin can inhibit the dissociation of p-toluenesulfonic acid in the presence of trace amounts of water, thereby reducing free H+. + Generate, avoid free H +The non-specific attack on the peroxy bond in the product tert-butyl peroxide enhances the product's stability. Sulfonated carbon is a porous carbon-based solid acid that can directionally adsorb and enrich polar reactants through its pore structure, forming a localized high-concentration reactant microenvironment, providing an efficient reaction interface for the protonation of p-toluenesulfonic acid. P-Toluenesulfonic acid can diffuse into the pores of sulfonated carbon in molecular form, supplementing the protonation active sites within the pores and compensating for the slow protonation rate of sulfonated carbon. The presence of van der Waals forces between the hydrophobic groups of the perfluorosulfonic acid resin and sulfonated carbon allows for the formation of a stable composite phase, preventing catalyst delamination or loss and ensuring a uniform distribution of catalytic sites. Furthermore, the perfluoroalkyl framework of the perfluorosulfonic acid resin and the carbon-based support of the sulfonated carbon can jointly form hydrophobic microdomains. This hydrophobic microenvironment can enrich organic reactants such as tert-butyl hydroperoxide, significantly increasing the local concentration of organic reactants around the catalytic sites. Acetate is enriched through the polar adsorption of sulfonic acid groups on the catalyst surface. This dual enrichment effect accelerates the reaction rate and improves the reaction conversion rate.

[0028] Perfluorosulfonic acid resin achieves solid-phase dispersion and inhibits the dissociation of p-toluenesulfonic acid through hydrophobic association and hydrogen bonding. The two then form a stable composite phase with sulfonated carbon through van der Waals forces. The reactants are enriched by the porous structure of sulfonated carbon, ultimately achieving a synergistic effect of complementary protonation sites, directional aggregation of reactants, and stability of the catalytic system, thereby efficiently improving the reaction rate and selectivity. Detailed Implementation

[0029] The present invention will be further described below with reference to embodiments.

[0030] Example 1

[0031] Preparation of purified tert-butyl hydrogen peroxide solution:

[0032] (a) 126g of tert-butyl hydrogen peroxide solution (tert-butyl hydrogen peroxide content is 69wt.%, di-tert-butyl peroxide content is 12.1wt.%, and the remainder is water) was placed in a reactor, and a 20wt.% sodium hydroxide solution was added dropwise at 15°C. The molar ratio of sodium hydroxide in the sodium hydroxide solution to tert-butyl hydrogen peroxide in the tert-butyl hydrogen peroxide solution was controlled to be 1:1. The reaction was carried out at 20°C for 20min. After the reaction was completed, the mixture was allowed to stand at 20°C for 30min. The upper layer was the organic phase and the lower layer was the aqueous phase. The mixture was separated to obtain the lower aqueous phase.

[0033] (b) Add sulfuric acid with a concentration of 20 wt.% to the aqueous phase obtained in step (a) at 25°C and react to obtain a reaction solution. When the pH of the reaction solution is 4, the reaction ends and the addition of sulfuric acid is stopped. The reaction solution is allowed to stand at 25°C for 15 min to separate into layers. The upper layer is the organic phase and the lower layer is the aqueous phase. The lower aqueous phase is separated and removed to obtain a purified tert-butyl hydrogen peroxide solution with a concentration of 80 wt.%.

[0034] Preparation of tert-butyl peroxide:

[0035] (1) Add 49g of acetic anhydride to the reaction vessel and slowly heat it to 52℃. Add 101g of sodium hydroxide solution (concentration of 35wt.%) to the reaction vessel and stir at 52℃ for 45min to obtain the reaction solution.

[0036] (2) Add 10g of composite catalyst to 100g of purified tert-butyl hydrogen peroxide solution with a concentration of 80wt.% at 10℃, stir at 10℃ for 10min to obtain a mixture, wherein the composite catalyst is composed of 3.4g of p-toluenesulfonic acid, 3.4g of perfluorosulfonic acid resin and 3.2g of sulfonated carbon.

[0037] (3) At 15°C, add the reaction solution obtained in step (1) to the mixture obtained in step (2). After the addition is complete, stir the reaction at 15°C for 55 min and let it stand for 30 min. The upper layer is the organic phase and the lower layer is the reaction mother liquor. Separate and remove the lower reaction mother liquor to obtain the organic phase.

[0038] (4) Add 100 mL of 5 wt.% sodium metabisulfite solution to 133 mL of organic phase, stir at 5 °C for 5 minutes, and let stand at 15 °C for 22 minutes. The upper layer is the oil phase and the lower layer is the aqueous phase. Separate and remove the lower aqueous phase to obtain the oil phase.

[0039] (5) The oil phase obtained in step (4) was washed twice with a sodium bicarbonate solution with a concentration of 6 wt.%, stood at 5°C for 30 min and the aqueous phase was separated, and then washed with a sodium chloride solution with a concentration of 6 wt.% until neutral. It was freeze-dried at -10°C for 10 h to remove trace amounts of water, and 116.49 g of tert-butyl peroxide was obtained. The active oxygen content was 11.66% and the reaction yield was 95.59%.

[0040] Example 2

[0041] Preparation of purified tert-butyl hydrogen peroxide solution:

[0042] (a) 165g of tert-butyl hydrogen peroxide solution (tert-butyl hydrogen peroxide content is 71.5wt.%, di-tert-butyl peroxide content is 10.5wt.%, and the remainder is water) was placed in a reactor, and a 10wt.% potassium hydroxide solution was added dropwise at 25°C. The molar ratio of potassium hydroxide in the potassium hydroxide solution to tert-butyl hydrogen peroxide in the tert-butyl hydrogen peroxide solution was controlled to be 1.3:1. The reaction was carried out at 25°C for 25min. After the reaction was completed, the mixture was allowed to stand at 25°C for 20min. The upper layer was the organic phase and the lower layer was the aqueous phase. The mixture was separated to obtain the lower aqueous phase.

[0043] (b) Add sulfuric acid with a concentration of 25 wt.% to the aqueous phase obtained in step (a) at 15 °C and react to obtain a reaction solution. When the pH of the reaction solution is 6, the reaction ends and the addition of sulfuric acid is stopped. The reaction solution is allowed to stand at 15 °C for 30 min to separate into layers. The upper layer is the organic phase and the lower layer is the aqueous phase. Separate and remove the lower aqueous phase to obtain a purified tert-butyl hydrogen peroxide solution with a concentration of 79.5 wt.%.

[0044] Preparation of tert-butyl peroxide:

[0045] (1) Add 63g of acetic anhydride to the reaction vessel and slowly heat it to 53℃. Add 123g of sodium hydroxide solution (concentration of 37wt.%) to the reaction vessel and stir the reaction at 53℃ for 48min to obtain the reaction solution.

[0046] (2) Add 14g of composite catalyst to 129g of purified tert-butyl hydrogen peroxide solution with a concentration of 79.5wt.% at 15℃, stir at 15℃ for 5min to obtain a mixture, wherein the composite catalyst is composed of 4.8g of p-toluenesulfonic acid, 4.7g of perfluorosulfonic acid resin and 4.5g of sulfonated carbon.

[0047] (3) At 20°C, add the reaction solution obtained in step (1) to the mixture obtained in step (2). After the addition is complete, stir the reaction at 20°C for 59 min and let it stand for 15 min. The upper layer is the organic phase and the lower layer is the reaction mother liquor. Separate and remove the lower reaction mother liquor to obtain the organic phase.

[0048] (4) Add 127 mL of 2 wt.% sodium metabisulfite solution to 171 mL of organic phase, stir at 3 °C for 10 minutes, and let stand at 5 °C for 25 minutes. The upper layer is the oil phase and the lower layer is the aqueous phase. Separate and remove the lower aqueous phase to obtain the oil phase.

[0049] (5) The oil phase obtained in step (4) was washed three times with a sodium bicarbonate solution with a concentration of 3 wt.%, stood at 15°C for 15 min and the aqueous phase was separated. Then it was washed with a sodium chloride solution with a concentration of 10 wt.% until neutral. It was freeze-dried at -5°C for 12 h to remove trace amounts of water and 149.31 g of tert-butyl peroxide was obtained. The active oxygen content was 11.65% and the reaction yield was 95.49%.

[0050] Example 3

[0051] Preparation of purified tert-butyl hydrogen peroxide solution:

[0052] (a) 190g of tert-butyl hydrogen peroxide solution (tert-butyl hydrogen peroxide content is 70.5wt.%, di-tert-butyl peroxide content is 11.3wt.%, and the remainder is water) was placed in a reactor, and a 15wt.% sodium hydroxide solution was added dropwise at 20°C. The molar ratio of sodium hydroxide in the sodium hydroxide solution to tert-butyl hydrogen peroxide in the tert-butyl hydrogen peroxide solution was controlled to be 1.2:1. The reaction was carried out at 15°C for 30min. After the reaction was completed, the mixture was allowed to stand at 22°C for 15min. The upper layer was the organic phase and the lower layer was the aqueous phase. The mixture was separated to obtain the lower aqueous phase.

[0053] (b) Add sulfuric acid with a concentration of 23 wt.% to the aqueous phase obtained in step (a) at 20°C and react to obtain a reaction solution. When the pH of the reaction solution is 5, the reaction ends and the addition of sulfuric acid is stopped. The reaction solution is allowed to stand at 20°C for 20 min to separate into layers. The upper layer is the organic phase and the lower layer is the aqueous phase. Separate and remove the lower aqueous phase to obtain a purified tert-butyl hydrogen peroxide solution with a concentration of 79.3 wt.%.

[0054] Preparation of tert-butyl peroxide:

[0055] (1) Add 72g of acetic anhydride to the reaction vessel and slowly heat it to 50℃. Add 204.5g of potassium hydroxide solution (concentration of 36wt.%) to the reaction vessel and stir at 50℃ for 50min to obtain the reaction solution.

[0056] (2) 17.5g of composite catalyst was added to 149.5g of purified tert-butyl hydrogen peroxide solution with a concentration of 79.3wt.% at 13℃, and stirred at 13℃ for 15min to obtain a mixture, wherein the composite catalyst was composed of 6g of p-toluenesulfonic acid, 6g of perfluorosulfonic acid resin and 5.5g of sulfonated carbon.

[0057] (3) At 18°C, add the reaction solution obtained in step (1) dropwise to the mixture obtained in step (2). After the dropwise addition is complete, stir the reaction at 18°C ​​for 58 min and let it stand at 18°C ​​for 25 min. The upper layer is the organic phase and the lower layer is the reaction mother liquor. Separate and remove the lower reaction mother liquor to obtain the organic phase.

[0058] (4) Add 145 mL of 10 wt.% sodium metabisulfite solution to 199 mL of organic phase, stir at 4 °C for 8 minutes, and let stand at 12 °C for 28 minutes. The upper layer is the oil phase and the lower layer is the aqueous phase. Separate and remove the lower aqueous phase to obtain the oil phase.

[0059] (5) The oil phase obtained in step (4) was washed three times with a sodium bicarbonate solution of saturated concentration, allowed to stand at 10°C for 25 min and the aqueous phase was separated, and then washed with a sodium chloride solution of 3 wt.% until neutral. It was freeze-dried at -8°C for 11 h to remove trace amounts of water, and 173 g of tert-butyl peroxide was obtained. The active oxygen content was 11.62% and the reaction yield was 95.47%.

[0060] Comparative Example 1

[0061] Without adding p-toluenesulfonic acid, the other operations were the same as in Example 1, yielding 117.9 g of tert-butyl peroxide; the active oxygen content was measured to be 11.15%, and the reaction yield was 92.52%.

[0062] Comparative Example 2

[0063] Without adding perfluorosulfonic acid resin, the other operations were the same as in Example 1, yielding 117.7 g of tert-butyl peroxide; the active oxygen content was 10.97%, and the reaction yield was 90.87%.

[0064] Comparative Example 3

[0065] Without adding sulfonated carbon, the other operations were the same as in Example 1, yielding 116.5 g of tert-butyl peroxide; the active oxygen content was measured to be 11.10%, and the reaction yield was 91.01%.

[0066] Comparative Example 4

[0067] The composite catalyst in step (2) was replaced with sulfuric acid, and the other operations were the same as in Example 1, to obtain 114.9 g of tert-butyl peroxide; the active oxygen content was 11.00%, and the reaction yield was 88.95%.

Claims

1. A process for synthesizing tert-butyl peroxide, characterized in that... Includes the following steps: (1) Add alkaline solution to acetic anhydride, stir to react, and obtain reaction solution; (2) Add the composite catalyst to the purified tert-butyl hydrogen peroxide solution and stir to obtain a mixture; (3) Add the reaction solution to the mixture, stir to react, let stand, separate, and obtain the organic phase; (4) The organic phase is acid-washed to obtain the oil phase; (5) The oil phase was washed with alkali and salt, and then freeze-dried to obtain tert-butyl peroxide; In step (2), the concentration of the purified tert-butyl hydrogen peroxide solution is 79.3-80 wt.%, the composite catalyst is a mixture of p-toluenesulfonic acid, perfluorosulfonic acid resin and sulfonated carbon, wherein the mass ratio of p-toluenesulfonic acid, perfluorosulfonic acid resin and sulfonated carbon is 1.06-1.1:1.04-1.1:1; the mass ratio of the composite catalyst to the purified tert-butyl hydrogen peroxide solution is 1:8-10, the addition temperature is 10-15℃, the stirring time is 5-15 min, the stirring temperature is 10-15℃, and the mass ratio of the purified tert-butyl hydrogen peroxide solution to the acetic anhydride in step (1) is 2-2.2:

1.

2. The synthesis process of tert-butyl peroxide according to claim 1, characterized in that... In step (1), the molar ratio of alkali to acetic anhydride in the alkaline solution is 1.8 to 1.9:

1. The alkaline solution is a potassium hydroxide solution or a sodium hydroxide solution with a concentration of 35 to 37 wt.%. The addition temperature is 50 to 53°C. The stirring reaction time is 45 to 50 min and the stirring reaction temperature is 50 to 53°C.

3. The synthesis process of tert-butyl peroxide according to claim 1, characterized in that... In step (3), the temperature is 15-20℃, the stirring reaction temperature is 15-20℃, the stirring reaction time is 55-59min, the standing time is 15-30min, and the standing temperature is 15-20℃.

4. The synthesis process of tert-butyl peroxide according to claim 1, characterized in that... In step (4), the acid washing process involves adding sodium metabisulfite solution, stirring, allowing it to stand, and then separating. The concentration of the sodium metabisulfite solution is 2-10 wt.%, the volume ratio of sodium metabisulfite solution to organic phase is 1:1.30-1.40, the stirring temperature is 3-5℃, the stirring time is 5-10 minutes, the standing temperature is 5-15℃, and the standing time is 22-28 minutes.

5. The synthesis process of tert-butyl peroxide according to claim 1, characterized in that... In step (5), the alkaline washing involves washing with an alkaline solution and allowing it to stand to separate the aqueous phase. The alkaline solution is a sodium bicarbonate solution with a concentration of 3 wt.% to saturation. The washing is performed 2 to 3 times, and the standing time is 15 to 30 minutes at a temperature of 5 to 15°C. The salt washing involves washing with a salt solution until neutral. The salt solution is a sodium chloride solution with a concentration of 3 to 10 wt.%. The freeze-drying time is 10 to 12 hours, and the freeze-drying temperature is -10 to -5°C.

6. The synthesis process of tert-butyl peroxide according to claim 1, characterized in that... The preparation method of purified tert-butyl hydrogen peroxide solution in step (2) includes the following steps: (a) Add alkali to tert-butyl hydrogen peroxide solution, react, let stand, separate, and obtain aqueous phase; (b) Add sulfuric acid to the aqueous phase to react and obtain a reaction solution. Let the reaction solution stand and separate to obtain a purified tert-butyl hydrogen peroxide solution.

7. The synthesis process of tert-butyl peroxide according to claim 6, characterized in that... In step (a), the tert-butyl hydrogen peroxide solution contains 65–75 wt.% tert-butyl hydrogen peroxide, 10–15 wt.% di-tert-butyl peroxide, and the remainder is water; the addition temperature is 15–25°C, the reaction temperature is 15–25°C, the reaction time is 20–30 min, the alkali solution is potassium hydroxide solution or sodium hydroxide solution, the concentration of the alkali solution is 10–20 wt.%, the molar ratio of alkali in the alkali solution to tert-butyl hydrogen peroxide in the tert-butyl hydrogen peroxide solution is 1–1.3:1, the standing time is 15–30 min, and the standing temperature is 20–25°C.

8. The synthesis process of tert-butyl peroxide according to claim 6, characterized in that... In step (b), the temperature is 15-25°C, the reaction temperature is 15-25°C, and the concentration of sulfuric acid is 20-25 wt.%.

9. The synthesis process of tert-butyl peroxide according to claim 6, characterized in that... In step (b), the pH of the reaction solution is 4-6, the standing time is 15-30 min, and the standing temperature is 20-25℃.