Preparation method of tert-butyl peroxyneodecanoate

Abstract

The invention discloses a preparation method of tert-butyl peroxyneodecanoate, which is characterized in that zinc oxide is uniformly dispersed on a graphene oxide / attapulgite composite carrier interface in a nano-particle form through a hydrothermal method to form a supported catalyst with a high specific surface area, active sites are fully exposed, the catalytic efficiency is obviously improved, and the catalytic activity is improved. Zinc oxide and a carrier form strong interaction, in the reaction process, an adaptive alkaline system is optimized, the composite catalyst shows high selectivity in a sodium hydroxide / tert-butyl hydroperoxide system, the residual quantity of byproducts is smaller than or equal to 0.01%, reaction conditions are mild, high-temperature and high-pressure equipment is not needed, the catalyst can be recycled, and the content of metal ions in waste liquid is smaller than or equal to 0.1 ppm; the purity of the obtained product tert-butyl peroxyneodecanoate is more than or equal to 99.5%, the active oxygen content reaches 7.2-7.5%, the decomposition temperature is more than or equal to 120 DEG C, the 10h half-life period temperature is 75-80 DEG C, the initiation efficiency is more than or equal to 95% when the tert-butyl peroxyneodecanoate is used as an initiator, the light transmittance is more than or equal to 92%, the molecular weight distribution index is less than or equal to 2.5, no implosion phenomenon exists in the polymerization process, and the advantages of high efficiency, low consumption

Description

Technical Field

[0001] The present invention relates to the field of polymer materials, and in particular to a method for preparing tert-butyl peroxyneodecanoate. Background Art

[0002] Tert-butyl peroxyneodecanoate, as a highly efficient organic peroxide, is widely used as a polymerization initiator for photovoltaic-grade EVA resins. Its performance directly affects the resin's light transmittance, molecular weight distribution, and polymerization stability. Traditional preparation methods have the following significant drawbacks:

[0003] 1. Insufficient metal oxide loading. Traditional metal oxide catalysts (such as zinc oxide) have low specific surface area and poor dispersion of the support, resulting in insufficient exposure of active sites and limited catalytic efficiency (yield is usually less than 85%).

[0004] 2. Stability issues: zinc oxide tends to agglomerate and fall off at high temperatures or during multiple cycles, and its activity decreases significantly after regeneration (e.g., activity loss ≥ 20% after three cycles);

[0005] 3. Environmental protection and cost: homogeneous catalysts (such as sulfuric acid) are not recyclable and produce a large amount of metal-containing wastewater, which has high treatment costs;

[0006] To address the above problems, there is an urgent need to develop a catalyst with a high specific surface area carrier composite zinc oxide, improve the dispersibility and stability by optimizing the loading process, and adapt it to the alkaline reaction system (such as tert-butyl hydroperoxide) to achieve efficient, low-consumption, and environmentally friendly preparation of tert-butyl peroxyneodecanoate. Summary of the Invention

[0007] Therefore, in order to solve the above-mentioned shortcomings, the present invention provides a preparation method of tert-butyl peroxyneodecanoate.

[0008] The present invention is achieved by constructing a method for preparing tert-butyl peroxyneodecanoate, which method comprises the following steps:

[0009] Step S1, preparation of catalyst:

[0010] Step S11, acidification and purification of attapulgite:

[0011] The raw attapulgite and sodium hexametaphosphate are mixed in a mass ratio of 50:0.5-4, distilled water is added, stirred for 10-30 minutes, and then allowed to stand for 2-4 hours. The white paste is obtained by centrifugation, which is mixed with 0.5-3 mol / L hydrochloric acid in a mass ratio of 1:5, stirred at 300-500 rpm for 1-2 hours, and then centrifuged at 9000-10000 rpm for 3-5 times. After each centrifugation, the paste is washed with distilled water until neutral, vacuum dried at 60-80°C for 12-24 hours, and ground to a particle size of ≤50 μm.

[0012] Step S12: preparing graphene oxide:

[0013] Concentrated sulfuric acid, graphite powder and sodium nitrate in a mass ratio of 1:0.8-1.5:0.5-1.2 are mixed, the temperature is controlled at 0-5°C in an ice bath, potassium permanganate in a mass ratio of 1:0.3-0.6 is slowly added, and the mixture is reacted in an ice bath for 0.5-4h, then transferred to a 20-40°C water bath, stirred at 200-400rpm for 0.5-4h, and hydrogen peroxide with a mass fraction of 30%-50% is added to terminate the reaction, followed by alternating washing with 5%-10% dilute hydrochloric acid and distilled water until the pH is ≥5, and freeze-dried to obtain graphene oxide;

[0014] Step S13, preparing a composite catalyst:

[0015] The graphene oxide obtained in step 12 is dispersed in deionized water to form a 0.5-2 mg / mL dispersion, ascorbic acid is added at a volume ratio of 1:1-2.5, and after ultrasonic treatment for 20-40 min, the acidified attapulgite obtained in step S1 is added at a mass ratio of 1:1, and ultrasonic dispersion is continued for 30-60 min. Then, a zinc oxide precursor solution is added, and the mass ratio of graphene oxide to zinc oxide is 1:0.2-0.6. The mixture is transferred to a polytetrafluoroethylene reactor and hydrothermally reacted at 80-160° C. for 3-14 h. After the reaction is completed, it is washed alternately with ethanol and distilled water for 3-5 times, and vacuum dried at 60-100° C. for 6-12 h to obtain a supported composite catalyst;

[0016] Step S2, esterification reaction:

[0017] In a reaction vessel equipped with a stirrer, add a 20% to 30% sodium hydroxide solution and tert-butyl hydroperoxide in a molar ratio of 1:1.05 to 1.2, stir for 10 to 30 minutes to form a homogeneous salt system, add the composite catalyst obtained in step S1 in an amount of 0.5% to 4% of the mass of neodecanoyl chloride, control the temperature at 15 to 30°C, and add 90% to 98% neodecanoyl chloride dropwise at a rate of 0.5 to 2 mL / min for 20 to 60 minutes. After the addition is complete, continue stirring to react for 0. The method comprises the following steps: washing the crude product with a 5% to 10% sodium hydroxide solution at 0 to 15° C. for 2 to 3 times, each washing for 10 to 30 minutes, and then adjusting the pH value to 6.5 to 7.5 with 30 to 50 mL of a 5% sodium bicarbonate solution. The crude product is dried over a molecular sieve or magnesium sulfate for 6 to 12 hours to obtain tert-butyl peroxyneodecanoate with a purity of ≥99.5% and a yield of ≥94%, and the residual amounts of tert-butyl hydroperoxide and di-tert-butyl peroxide are both ≤0.01%.

[0018] In step S13, the zinc oxide precursor is zinc nitrate, the hydrothermal reaction temperature is 100-140° C., the reaction time is 8-12 h, the zinc oxide loading is 20%-30% of the mass of graphene oxide, the ultrasonic dispersion power is 200-400 W, and the frequency is 40-60 kHz.

[0019] The zinc oxide in the composite catalyst is uniformly dispersed in the graphene oxide / attapulgite interface in the form of nanoparticles, and the specific surface area of ​​the catalyst is ≥180m 2 / g, and the activity retention rate is ≥90% after recycling 3 to 5 times.

[0020] In step S2, the reaction temperature is 20-25° C., the dropwise addition time is 30-40 min, the mass ratio of neodecanoyl chloride to catalyst is 100 mL:1-2 g; the concentration of the sodium hydroxide solution is 25%-28%, and the molar excess ratio of tert-butyl hydroperoxide is 1:1.1-1.15.

[0021] The composite catalyst can be recycled 3 to 5 times, and after each cycle, it is regenerated by vacuum drying at 100 to 120° C. for 2 to 3 hours. After regeneration, the specific surface area loss rate is ≤5%, and the zinc oxide particles do not agglomerate or fall off.

[0022] The present invention has the following advantages: The present invention provides a method for preparing tert-butyl peroxyneodecanoate by improvement, which has the following improvements compared with the prior art:

[0023] The preparation method of tert-butyl peroxyneodecanoate of the present invention has the advantages of high catalyst performance, wherein zinc oxide is uniformly dispersed in the form of nanoparticles (10-20 nm) on the interface of graphene oxide / attapulgite composite carrier by hydrothermal method, forming a high specific surface area (≥180m 2 / g) of supported catalyst, the active sites are fully exposed, the catalytic efficiency is significantly improved, the reaction yield is ≥94%, and at the same time, a strong interaction is formed between zinc oxide and the support, giving the catalyst excellent cyclic stability. After 5 cycles of use, the activity retention rate is ≥90%, and the specific surface area loss after regeneration is ≤5% (SEM characterization verifies that there is no particle agglomeration or shedding). The reaction process is optimized and adapted to the alkaline system. The composite catalyst shows high selectivity (≥98%) in the sodium hydroxide / tert-butyl hydroperoxide system, and the residual amounts of by-products (tert-butyl hydroperoxide, di-tert-butyl peroxide) are ≤0.01%, and the reaction conditions are mild (15-30°C normal temperature). The process is environmentally friendly and economical, with the catalyst being recyclable and the metal ion content in the waste liquid being ≤0.1ppm (ICP test), meeting green chemical standards. The resulting product, tert-butyl peroxyneodecanoate, has a purity ≥99.5%, an active oxygen content of 7.2-7.5%, a decomposition temperature ≥120°C, and a 10-hour half-life temperature of 75-80°C, fully meeting the requirements of the high-temperature polymerization process for photovoltaic-grade EVA resins. When used as an initiator, the initiation efficiency is ≥95%, the transmittance is ≥92%, the molecular weight distribution index is ≤2.5, and there is no implosion during the polymerization process, combining the advantages of high efficiency, low consumption, and environmental protection. BRIEF DESCRIPTION OF THE DRAWINGS

[0024] Figure 1 It is a flow chart of the preparation process of the present invention. DETAILED DESCRIPTION

[0025] The following will be combined with the Figure 1 The present invention is described in detail, and the technical solutions in the embodiments of the present invention are clearly and completely described. Obviously, the embodiments described are only some embodiments of the present invention, not all embodiments. All other embodiments obtained by ordinary technicians in this field based on the embodiments of the present invention without making any creative efforts shall fall within the scope of protection of the present invention.

[0026] Example 1

[0027] See also Figure 1 , a preparation method of tert-butyl peroxyneodecanoate, the method specifically comprising the following steps:

[0028] Step S1, preparation of catalyst:

[0029] Step S11, acidification and purification of attapulgite:

[0030] The raw attapulgite and sodium hexametaphosphate are mixed in a mass ratio of 50:0.5-4, distilled water is added, stirred for 10-30 minutes, and then allowed to stand for 2-4 hours. The white paste is obtained by centrifugation, which is mixed with 0.5-3 mol / L hydrochloric acid in a mass ratio of 1:5, stirred at 300-500 rpm for 1-2 hours, and then centrifuged at 9000-10000 rpm for 3-5 times. After each centrifugation, the paste is washed with distilled water until neutral, vacuum dried at 60-80°C for 12-24 hours, and ground to a particle size of ≤50 μm.

[0031] The specific operations are:

[0032] 1. Take 50g of raw attapulgite, add 1g of sodium hexametaphosphate, mix well, add 500mL of distilled water, stir at 300rpm for 20min, and let it stand for 3h;

[0033] 2. Take the supernatant suspension, centrifuge at 9000 rpm for 10 minutes, and collect the white paste;

[0034] 3. Mix the white paste with 1 mol / L hydrochloric acid in a mass ratio of 1:5, stir at 400 rpm for 1.5 h, and then centrifuge and wash 4 times at 9000 rpm, washing each time with distilled water until neutral (pH ≈ 7);

[0035] 4. The washed solid was placed in a vacuum drying oven at 75°C and dried for 18 hours, and then ground to a particle size of ≤50 μm to obtain acidified attapulgite with a specific surface area of ​​230 m 2 / g, metal impurity content <0.1%.

[0036] Step S12: preparing graphene oxide:

[0037] Concentrated sulfuric acid, graphite powder and sodium nitrate in a mass ratio of 1:0.8-1.5:0.5-1.2 are mixed, the temperature is controlled at 0-5°C in an ice bath, potassium permanganate in a mass ratio of 1:0.3-0.6 is slowly added, and the mixture is reacted in an ice bath for 0.5-4h, then transferred to a 20-40°C water bath, stirred at 200-400rpm for 0.5-4h, and hydrogen peroxide with a mass fraction of 30%-50% is added to terminate the reaction, followed by alternating washing with 5%-10% dilute hydrochloric acid and distilled water until the pH is ≥5, and freeze-dried to obtain graphene oxide;

[0038] The specific operations are:

[0039] 1. In an ice bath, mix 60 mL of concentrated sulfuric acid, 1.3 g of graphite powder, and 1 g of sodium nitrate, slowly add 7 g of potassium permanganate (addition rate 0.8 g / min), control the temperature ≤ 4 ° C, and react for 2.5 hours;

[0040] 2. Transfer to a 30°C water bath and stir at 300 rpm for 2 h until the system turns brown;

[0041] 3. Slowly add 20 mL of 30% hydrogen peroxide (the amount added accounts for 12% of the total volume of the system) and stir until the solution turns bright yellow;

[0042] 4. Alternately wash with 5% dilute hydrochloric acid and distilled water until pH = 6, and freeze-dry to obtain graphene oxide with an oxygen content of 28% and an interlayer spacing of 1.0 nm.

[0043] Step S13, preparing a composite catalyst:

[0044] The graphene oxide obtained in step 12 is dispersed in deionized water to form a 0.5-2 mg / mL dispersion, ascorbic acid is added at a volume ratio of 1:1-2.5, and after ultrasonic treatment for 20-40 min, the acidified attapulgite obtained in step S1 is added at a mass ratio of 1:1, and ultrasonic dispersion is continued for 30-60 min. Then, a zinc oxide precursor solution is added, and the mass ratio of graphene oxide to zinc oxide is 1:0.2-0.6. The mixture is transferred to a polytetrafluoroethylene reactor and hydrothermally reacted at 80-160° C. for 3-14 h. After the reaction is completed, it is washed alternately with ethanol and distilled water for 3-5 times, and vacuum dried at 60-100° C. for 6-12 h to obtain a supported composite catalyst;

[0045] The zinc oxide precursor is zinc nitrate, the hydrothermal reaction temperature is 100-140° C., the reaction time is 8-12 hours, the zinc oxide loading is 20%-30% of the mass of the graphene oxide, the ultrasonic dispersion power is 200-400W, and the frequency is 40-60kHz;

[0046] The specific operations are:

[0047] 1. Disperse graphene oxide in 80 mL of deionized water and ultrasonicate (power 350 W, frequency 50 kHz) to form a 1 mg / mL dispersion;

[0048] 2. Add 120 mg of ascorbic acid (mass ratio 1:1.8) and disperse by ultrasonic for 30 minutes;

[0049] 3. Add 80 mg of acidified attapulgite and continue ultrasonication for 40 minutes;

[0050] 4. Add 1.2 g of zinc nitrate solution (25% of the mass of graphene oxide, calculated as ZnO), transfer to a polytetrafluoroethylene reactor, and hydrothermally react at 120°C for 10 h;

[0051] 5. After the reaction, the catalyst was washed alternately with ethanol and distilled water for 3 times and dried in vacuum at 80℃ for 8h to obtain a composite catalyst. The particle size of zinc oxide nanoparticles was 10-20nm and they were evenly dispersed. The specific surface area of ​​the catalyst was 190m 2 / g.

[0052] Step S2, esterification reaction:

[0053] In a reaction vessel equipped with a stirrer, add a 20% to 30% sodium hydroxide solution and tert-butyl hydroperoxide in a molar ratio of 1:1.05 to 1.2, stir for 10 to 30 minutes to form a homogeneous salt system, add the composite catalyst obtained in step S1 in an amount of 0.5% to 4% of the mass of neodecanoyl chloride, control the temperature at 15 to 30°C, and add 90% to 98% neodecanoyl chloride dropwise at a rate of 0.5 to 2 mL / min for 20 to 60 minutes. After the addition is complete, continue stirring to react for 0. The crude product was washed with a 5% to 10% sodium hydroxide solution at 0 to 15° C. for 2 to 3 times, each washing lasting 10 to 30 minutes, and then the pH value was adjusted to 6.5 to 7.5 with 30 to 50 mL of a 5% sodium bicarbonate solution. The product was dried over molecular sieves or magnesium sulfate for 6 to 12 hours to obtain tert-butyl peroxyneodecanoate with a purity of ≥99.5% and a yield of ≥94%, with the residual amounts of tert-butyl hydroperoxide and di-tert-butyl peroxide both being ≤0.01%.

[0054] The reaction temperature is 20-25°C, the addition time is 30-40 minutes, the mass ratio of neodecanoyl chloride to catalyst is 100 mL:1-2 g; the concentration of sodium hydroxide solution is 25%-28%, and the molar excess ratio of tert-butyl hydroperoxide is 1:1.1-1.15;

[0055] The zinc oxide in the composite catalyst is uniformly dispersed in the form of nanoparticles at the graphene oxide / attapulgite interface, and the specific surface area of ​​the catalyst is ≥180m 2 / g, the activity retention rate is ≥90% after 3-5 cycles;

[0056] The composite catalyst can be recycled 3 to 5 times, and after each cycle, it is regenerated by vacuum drying at 100 to 120° C. for 2 to 3 hours. After regeneration, the specific surface area loss rate is ≤5%, and the zinc oxide particles do not agglomerate or fall off.

[0057] The specific operations are:

[0058] 1. Add 240 g of 25% sodium hydroxide solution (w / w) and 172.5 g of tert-butyl hydroperoxide (molar ratio 1:1.1) to a 1000 mL three-necked flask and stir at 400 rpm for 20 min.

[0059] 2. Add 1.5g composite catalyst (1.2% of the mass of neodecanoyl chloride) and control the temperature to 22°C;

[0060] 3. Add 208 g of 95% neodecanoyl chloride dropwise at a rate of 1 mL / min for 35 min.

[0061] 4. After the addition is complete, continue stirring the reaction for 2 hours, let it stand for 20 minutes to separate the layers, and separate the lower layer of waste liquid;

[0062] 5. Wash the crude product twice with 8% sodium hydroxide solution at 0-5°C (liquid-to-solid ratio 7:1), each time for 15 minutes;

[0063] 6. Add 30 mL of 5% sodium bicarbonate solution to adjust the pH to 7.0, and dry over 3A molecular sieves for 10 h to obtain a white solid product.

[0064] Test results:

[0065] Purity of tert-butyl peroxyneodecanoate: 99.6% (HPLC determination);

[0066] Yield: 94.2%

[0067] The activity retention rate of the catalyst after 3 cycles: 91%;

[0068] Zinc oxide loading: 24.8% (determined by ICP-OES);

[0069] Specific surface area loss rate after regeneration: 4.3%.

[0070] Example 2: Comparative experiment on optimizing reaction conditions

[0071] Step 1, preparation of the composite catalyst, same as steps 1 to 3 of Example 1;

[0072] Step 2: Optimization of esterification reaction conditions:

[0073] In the same reaction system, the reaction temperature was adjusted to 28°C, the addition rate was 2 mL / min, and the addition time was 20 min.

[0074] Other conditions are the same as in Example 1.

[0075] Test results:

[0076] Product purity: 98.9%;

[0077] Residual tert-butyl hydroperoxide: 0.03%;

[0078] Yield: 89.2%

[0079] The by-product generation rate increased by 15%.

[0080] The conclusion is that the increase in reaction temperature and the excessively fast addition rate lead to an increase in side reactions, which verifies the necessity of controlling the temperature at 20-25°C and the addition time at 30-40 min.

[0081] Example 3: Catalyst cycle performance verification

[0082] Step 1: Catalyst regeneration:

[0083] The used composite catalyst of Example 1 was washed with ethanol three times and regenerated in a vacuum drying oven at 110° C. for 2.5 h;

[0084] Step 2: Recycle experiment:

[0085] The regenerated catalyst was used to repeat the esterification reaction steps, and the catalyst performance was tested after being recycled 5 times.

[0086] Test results:

[0087] Catalyst specific surface area after the 5th cycle: 182m 2 / g (loss rate ≤ 5%);

[0088] There is no agglomeration or shedding of zinc oxide particles;

[0089] Product yield: 92.8%.

[0090] The conclusion is that the catalyst still maintains high efficiency and activity after 5 cycles, which meets the requirement of "catalyst is recycled 3 to 5 times and activity retention rate ≥ 90%".

[0091] Example 4: Product application performance test

[0092] Step 1, EVA resin polymerization experiment:

[0093] The tert-butyl peroxyneodecanoate (purity 99.6%) prepared in Example 1 was used as an initiator and added to the EVA resin prepolymer in an amount of 0.5%. The polymerization reaction was carried out at 140° C., and the induction period and the polymerization process were monitored.

[0094] Test results:

[0095] Initiation efficiency: 95%;

[0096] Polymerization induction period: 4.8 min;

[0097] EVA resin transmittance: 92.5%;

[0098] Molecular weight distribution index (PDI): 2.4;

[0099] No implosion phenomenon.

[0100] It is concluded that the product meets the requirements of high efficiency and stability as a photovoltaic-grade EVA resin initiator.

[0101] The above description of the disclosed embodiments is intended to enable one skilled in the art to implement or use the present invention. Various modifications to these embodiments will be readily apparent to one skilled in the art, and the general principles defined herein may be implemented in other embodiments without departing from the spirit or scope of the present invention. Therefore, the present invention is not limited to the embodiments shown herein but is intended to conform to the widest scope consistent with the principles and novel features disclosed herein.

Claims

1. A method for preparing tert-butyl peroxyneodecanoate, characterized in that: The following steps are involved: Step S1, preparation of catalyst: Step S11, acidification and purification of attapulgite: The raw attapulgite and sodium hexametaphosphate are mixed in a mass ratio of 50:0.5-4, distilled water is added, stirred for 10-30 minutes, and then allowed to stand for 2-4 hours. The white paste is obtained by centrifugation, which is mixed with 0.5-3 mol / L hydrochloric acid in a mass ratio of 1:5, stirred at 300-500 rpm for 1-2 hours, and then centrifuged at 9000-10000 rpm for 3-5 times. After each centrifugation, the paste is washed with distilled water until neutral, vacuum dried at 60-80°C for 12-24 hours, and ground to a particle size of ≤50 μm. Step S12: preparing graphene oxide: Concentrated sulfuric acid, graphite powder and sodium nitrate in a mass ratio of 1:0.8-1.5:0.5-1.2 are mixed, the temperature is controlled at 0-5°C in an ice bath, potassium permanganate in a mass ratio of 1:0.3-0.6 is slowly added, and the mixture is reacted in an ice bath for 0.5-4h, then transferred to a 20-40°C water bath, stirred at 200-400rpm for 0.5-4h, and hydrogen peroxide with a mass fraction of 30%-50% is added to terminate the reaction, followed by alternating washing with 5%-10% dilute hydrochloric acid and distilled water until the pH is ≥5, and freeze-dried to obtain graphene oxide; Step S13, preparing a composite catalyst: The graphene oxide obtained in step 12 is dispersed in deionized water to form a 0.5-2 mg / mL dispersion, ascorbic acid is added at a volume ratio of 1:1-2.5, and after ultrasonic treatment for 20-40 min, the acidified attapulgite obtained in step S1 is added at a mass ratio of 1:1, and ultrasonic dispersion is continued for 30-60 min. Then, a zinc oxide precursor solution is added, and the mass ratio of graphene oxide to zinc oxide is 1:0.2-0.

6. The mixture is transferred to a polytetrafluoroethylene reactor and hydrothermally reacted at 80-160° C. for 3-14 h. After the reaction is completed, it is washed alternately with ethanol and distilled water for 3-5 times, and vacuum dried at 60-100° C. for 6-12 h to obtain a supported composite catalyst; Step S2, esterification reaction: In a reaction vessel equipped with a stirrer, add a 20% to 30% sodium hydroxide solution and tert-butyl hydroperoxide in a molar ratio of 1:1.05 to 1.2, stir for 10 to 30 minutes to form a homogeneous salt system, add the composite catalyst obtained in step S1 in an amount of 0.5% to 4% of the mass of neodecanoyl chloride, control the temperature at 15 to 30°C, and add 90% to 98% neodecanoyl chloride dropwise at a rate of 0.5 to 2 mL / min for 20 to 60 minutes. After the addition is complete, continue stirring to react for 0. The method comprises the following steps: washing the crude product with a 5% to 10% sodium hydroxide solution at 0 to 15° C. for 2 to 3 times, each washing for 10 to 30 minutes, and then adjusting the pH value to 6.5 to 7.5 with 30 to 50 mL of a 5% sodium bicarbonate solution. The crude product is dried over a molecular sieve or magnesium sulfate for 6 to 12 hours to obtain tert-butyl peroxyneodecanoate with a purity of ≥99.5% and a yield of ≥94%, and the residual amounts of tert-butyl hydroperoxide and di-tert-butyl peroxide are both ≤0.01%.

2. The method for preparing tert-butyl peroxyneodecanoate according to claim 1, wherein: In step S13, the zinc oxide precursor is zinc nitrate, the hydrothermal reaction temperature is 100-140° C., the reaction time is 8-12 h, the zinc oxide loading is 20%-30% of the mass of graphene oxide, the ultrasonic dispersion power is 200-400 W, and the frequency is 40-60 kHz.

3. The preparation method of tert-butyl peroxyneodecanoate according to claim 1, wherein: The zinc oxide in the composite catalyst is uniformly dispersed in the graphene oxide / attapulgite interface in the form of nanoparticles, and the specific surface area of ​​the catalyst is ≥180m 2 / g, and the activity retention rate is ≥90% after recycling 3 to 5 times.

4. The method for preparing tert-butyl peroxyneodecanoate according to claim 1, wherein: In step S2, the reaction temperature is 20-25° C., the dropwise addition time is 30-40 min, the mass ratio of neodecanoyl chloride to catalyst is 100 mL:1-2 g; the concentration of the sodium hydroxide solution is 25%-28%, and the molar excess ratio of tert-butyl hydroperoxide is 1:1.1-1.

15.

5. The method for preparing tert-butyl peroxyneodecanoate according to claim 1, wherein: The composite catalyst can be recycled for 3 to 5 times, and after each cycle, it is regenerated by vacuum drying at 100 to 120° C. for 2 to 3 hours.

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