Preparation Method of tert-Amyl Peroxy(2-ethylhexyl) Carbonate

By using a composite system of phase transfer catalysts in the synthesis of peroxidized (2-ethylhexyl)carbonate, the problems of many by-products, low yields and difficult catalyst recovery are solved, and efficient and economical production results are achieved.

CN119684190BActive Publication Date: 2025-05-27LINZIZHENGHUA ACCESSORY INGREDIENT ZIBO
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Patent Information

Application Number
CN202510195056.5
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2025-02-21
Publication Date
2025-05-27
Estimated Expiration
2045-02-21

AI Technical Summary

Technical Problem

In the prior art, the synthesis method of tert-amyl peroxidized (2-ethylhexyl)carbonate has problems such as many by-products of dicarbonate, low yields and difficult catalyst recovery.

Method used

Using a composite system of phase transfer catalyst, an intermediate is obtained by adding a phase transfer agent to the salt forming agent and tert-amyl hydrogen peroxide for temperature control reaction; then sodium sulfite, urea and phase transfer catalyst are compounded to form a phase transfer catalyst system, blended with 2-ethylhexyl chloroformate, and undergoing a substitution reaction with the intermediate in parallel, and finally obtaining tert-amyl peroxide peroxidized (2-ethylhexyl)carbonate by detergent.

Benefits of technology

Effectively reduces the production of by-products, improves the yield of peroxidized (2-ethylhexyl)carbonate, and simplifies the recovery and reuse of catalysts, significantly reducing production costs.

✦ Generated by Eureka AI based on patent content.

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Abstract

The present invention belongs to the technical field of organic peroxides, and particularly relates to a preparation method of tert-amyl peroxy (2-ethylhexyl) carbonate. The preparation method comprises the following steps: (1) carrying out a temperature-controlled reaction on a crude product of tert-amyl hydroperoxide and a salifying agent under the action of a phase transfer agent to obtain an intermediate; (2) compounding a phase transfer catalyst system, blending the phase transfer catalyst system with 2-ethylhexyl chloroformate, and adding the blend and the intermediate into a reaction kettle in a co-current manner to carry out a substitution reaction. After the substitution reaction is completed, standing and collecting the upper organic phase to obtain a crude TAEC product; (3) adding a detergent to the crude TAEC product, stirring, standing, collecting the upper oil phase, and washing with water until the oil phase is neutral to obtain TAEC. By compounding the phase transfer catalyst system, the present invention solves the problems of many by-products of dicarbonates, low yield of TAEC and difficult catalyst recovery existing in the current TAEC synthesis method.
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Description

Technical Field

[0001] The invention belongs to the technical field of organic peroxides, and in particular relates to a method for preparing tert-amyl peroxy (2-ethylhexyl) carbonate. Background Art

[0002] Lightweight, high strength, low cost, energy saving and environmental protection are the inevitable trends in the development of materials today. Among them, unsaturated polyester resin has the advantages of low density, good mechanical properties, good formability, low cost, good weather resistance and corrosion resistance, especially the advantages of lightweight and low cost, making it more and more popular in the fields of sports, construction, automobiles and even aerospace. Unsaturated polyester resin is copolymerized between polyester monomers containing unsaturated bonds under the action of initiators. Tert-amyl peroxy (2-ethylhexyl) carbonate (TAEC) is an organic peroxide, which can often be used alone or in combination with other peroxides as an initiator for the copolymerization of various unsaturated polyester monomers.

[0003] At present, tert-amyl peroxidized (2-ethylhexyl) carbonate is mainly prepared by tert-amyl hydroperoxide and 2-ethylhexyl chloroformate as raw materials. For example, Chinese patent CN112300045A discloses a synthesis and purification method of a high-purity tert-amyl peroxidized 2-ethylhexyl carbonate, which first uses tert-amyl alcohol and hydrogen peroxide as raw materials, performs peroxidation under the catalysis of phosphotungstic acid, and then adds an entrainer under reduced pressure distillation to purify, thereby obtaining tert-amyl hydroperoxide; afterwards, an acid binding agent sodium hydroxide, potassium hydroxide or sodium carbonate is added to the tert-amyl hydroperoxide, and under the catalysis of pyridine or a derivative of pyridine, 2-ethylhexyl chloroformate is added, and high-purity tert-amyl peroxidized 2-ethylhexyl carbonate is obtained by reaction and purification.

[0004] In the stage of synthesizing tert-amyl hydroperoxide, the patent uses a catalyst phosphotungstic acid, which is relatively expensive and easily soluble in polar solvents. The phosphotungstic acid is easily lost during the liquid phase reaction of tert-amyl alcohol and hydrogen peroxide, and the patent does not involve measures for recovering the phosphotungstic acid. In addition, in the stage of synthesizing tert-amyl peroxy-2-ethylhexyl carbonate, since pyridine or pyridine derivatives are organic base catalysts, and some 2-ethylhexyl chloroformate will undergo self-condensation under alkaline conditions to produce dicarbonate by-products, the use of pyridine or pyridine derivatives as catalysts in the patent will affect the final yield of TAEC.

[0005] Chinese patent CN115557870A discloses a method for synthesizing tert-amyl peroxide 2-ethylhexanoate, comprising the following steps: (1) preparing a nanometer-scale high-activity catalyst; (2) mixing a tert-amyl hydroperoxide solution with an alkaline solution, stirring the mixture for reaction, and preparing a metal salt solution of tert-amyl hydroperoxide; (3) adding a nanometer-scale high-activity catalyst to the metal salt solution of tert-amyl hydroperoxide, then adding ethylhexanoyl chloride, stirring the mixture for reaction, and finally obtaining tert-amyl peroxide 2-ethylhexanoate. The nanometer-scale high-activity catalyst is prepared by mixing tantalum source, scandium source, aluminum source and silicon source as reactants, and tetrapropylammonium hydroxide as a template agent under an alkaline environment, and then sequentially undergoing low-temperature treatment, high-temperature treatment and sintering treatment, and then crushing and screening to obtain a first reaction solid; and the first reaction solid is sequentially treated with aminopropyltriethoxysilane, alkaline solution and n-octadecylsilane to obtain a nanometer-scale high-activity catalyst.

[0006] The rare metal raw materials such as tantalum and scandium in this patent are expensive, and the ratio of tantalum, scandium, aluminum and silicon needs to be precisely controlled. When preparing the nanocatalyst, measures such as loading the nanocatalyst on a magnetic carrier are not used. It is relatively difficult to simply recover and regenerate the nanocatalyst particles. These will significantly increase the cost of using the catalyst. Summary of the invention

[0007] The invention aims to provide a method for preparing tert-amyl peroxy (2-ethylhexyl) carbonate, and solves the problems of many dicarbonate by-products, low yield of tert-amyl peroxy (2-ethylhexyl) carbonate and difficulty in catalyst recovery in the current method for synthesizing tert-amyl peroxy (2-ethylhexyl) carbonate by using a composite system of a phase transfer catalyst.

[0008] To achieve the above object, the technical solution adopted by the present invention is:

[0009] The preparation method of tert-amyl peroxy (2-ethylhexyl) carbonate of the present invention comprises the following steps:

[0010] (1) adding a phase transfer agent to a salt-forming agent and mixing, and continuing to add a crude product of tert-amyl hydroperoxide to carry out a temperature-controlled reaction, allowing the reaction to stand and collecting the lower aqueous phase to obtain an intermediate; wherein the crude product of tert-amyl hydroperoxide contains tert-amyl hydroperoxide;

[0011] (2) compounding sodium sulfite, urea and a phase transfer catalyst to obtain a phase transfer catalyst system; mixing the phase transfer catalyst system with 2-ethylhexyl chloroformate, and adding the phase transfer catalyst system and the intermediate into a reactor in parallel to carry out a substitution reaction; after the substitution reaction is completed, standing and collecting the upper organic phase to obtain a crude product of tert-amyl peroxy (2-ethylhexyl) carbonate;

[0012] (3) Compounding a detergent, adding the detergent to the crude product of tert-amyl peroxy (2-ethylhexyl) carbonate, stirring, allowing the mixture to stand, collecting the upper oil phase, and washing with water until the oil phase becomes neutral, thereby obtaining tert-amyl peroxy (2-ethylhexyl) carbonate.

[0013] in:

[0014] The salt-forming agent is an aqueous solution of potassium hydroxide, and the molar ratio of potassium hydroxide to tert-amyl hydroperoxide is (1.15-1.21):1.

[0015] The phase transfer agent is tetrabutylammonium chloride, and the ratio of the added amount of tetrabutylammonium chloride to tert-amyl hydroperoxide is (5.6-8.5):1, the tetrabutylammonium chloride is measured in g, and the tert-amyl hydroperoxide is measured in mol.

[0016] The temperature of the temperature control reaction is 10-20°C, the temperature control reaction time is 15-25min, and the standing time is 1-2h.

[0017] The molar ratio of 2-ethylhexyl chloroformate to tert-amyl hydroperoxide is 1:(1.08-1.10).

[0018] The parallel flow addition temperature is 10-25°C, and the parallel flow addition time is 50-60 minutes; the substitution reaction temperature is 8-12°C, and the substitution reaction time is 2-3 hours.

[0019] The phase transfer catalyst is tetrabutylammonium bromide and tetrabutylammonium iodide, the molar ratio of sodium sulfite, urea, tetrabutylammonium bromide and tetrabutylammonium iodide is (0.8-1.5):(0.25-0.5):10:(2-2.5), and the mass ratio of the phase transfer catalyst to tert-amyl hydroperoxide is (0.22-0.37):1.

[0020] The detergent is prepared by compounding trisodium phosphate, sodium linoleate, tetrabutylammonium chloride and water.

[0021] The detergent contains 4-6 wt% of trisodium phosphate, 2-5 wt% of sodium linoleate and 1-5 wt% of tetrabutylammonium chloride, and the balance is water.

[0022] The stirring temperature is 15-20°C, and the stirring time is 15-20min.

[0023] The beneficial effects of the present invention are as follows:

[0024] (1) The phase transfer catalyst (PTC) is a compound of tetrabutylammonium bromide and tetrabutylammonium iodide, preferably with a molar ratio of 10:(2-2.5) between tetrabutylammonium bromide and tetrabutylammonium iodide, which can give full play to their respective advantages and produce a synergistic effect:

[0025] Since tert-amyl hydroperoxide (t-AmOOH) is hydrophilic and is in the aqueous phase, and 2-ethylhexyl chloroformate is hydrophobic and is in the organic phase, the mass transfer efficiency at the interface between the two is poor. At this time, the phase transfer catalyst in the present invention is transferred to the aqueous phase through the hydrophobic tetrabutyl cation ([N(C 4 H 9 ) 4 ] + ) and the active oxygen anion (t-AmOO - ) forms an ion pair ([N(C 4 H 9 ) 4 ] + t-AmOO - ), transfer the nucleophile from the aqueous phase to the organic phase, promoting t-AmOO - The counterion (Br - and I - ) directly affects the lipid solubility and migration efficiency of ion pairs. 4 H 9 ) 4 ] + I - The lipid solubility is much better than [N(C 4 H 9 ) 4 ] + ·Br - , the migration rate at the organic phase and the phase interface is faster, which can improve the diffusion rate of the overall ion pair at the phase interface, thereby improving the reaction rate of the ion pair and 2-ethylhexyl chloroformate; in addition, since tert-amyl peroxide is easy to decompose at high temperature, the low temperature reaction environment (8-12°C) is deliberately selected when 2-ethylhexyl chloroformate and the intermediate are reacted, and the two counterions with different diffusion rates can complement each other, ensuring that [N(C 4 H 9 ) 4 ] + The stability of mass transfer rate, especially at low temperatures, can prevent mass transfer from becoming the rate-limiting step, thereby affecting the reaction efficiency.

[0026] (2) Sodium sulfite, urea and a phase transfer catalyst are compounded to form a phase transfer catalytic system. With the synergistic effect of the three, the generation of by-products is reduced, the mass transfer rate is increased, and the catalytic reaction rate is increased, and the yield of tert-amyl peroxy (2-ethylhexyl) carbonate can be increased:

[0027] Phase transfer catalyst [N(C 4 H 9 ) 4 ] +It will be adsorbed at the phase interface to reduce the interfacial tension; sodium sulfite is a mild reducing agent, and sulfite (SO 3 2- ) can remove the OOH free radicals generated by the hydrolysis of trace intermediates in the reaction system and inhibit the self-decomposition side reaction of peroxides; in addition, SO 3 2- The weak alkalinity produced by the reversible hydrolysis of SO can adjust the pH of the aqueous phase, providing a stable alkaline buffer environment for the reaction and avoiding the addition of strong bases such as sodium hydroxide and sodium carbonate to cause the self-condensation of 2-ethylhexyl chloroformate to produce dicarbonate by-products. 3 2- With the tetrabutyl cation ([N(C 4 H 9 ) 4 ] + ) form a more stable ion pair ([N(C 4 H 9 ) 4 ] + ·SO 3 2- ), indirectly enhancing the effect of t-AmOO - The extraction capacity of urea molecules can improve the catalytic efficiency. 2 ) and carbonyl (C=O) can react with t-AmOO through hydrogen bonding. - or 2-ethylhexyl chloroformate: combined with t-AmOO - When combined, the NH bond of the amino group acts as a hydrogen bond donor to stabilize t-AmOO - The negative charge of urea reduces its nucleophilic activation energy; when combined with 2-ethylhexyl chloroformate, the oxygen atom of the carbonyl group acts as a hydrogen bond receptor and interacts with the C=O polarity of 2-ethylhexyl chloroformate, causing the electron cloud of the C atom to shift, thereby weakening the C-Cl bond and promoting the detachment of the Cl atom; urea slowly releases NH 3 , maintaining a weak alkaline environment to avoid side reactions caused by strong bases. Urea can increase the polarity of the aqueous phase and form a micelle-like structure with the phase transfer catalyst, making t-AmOO - The local concentration of 2-ethylhexyl chloroformate increases, pushing the reaction equilibrium toward the product. BRIEF DESCRIPTION OF THE DRAWINGS

[0028] Figure 1 It is the liquid chromatogram of tert-amyl peroxy (2-ethylhexyl) carbonate in Example 1. DETAILED DESCRIPTION

[0029] The present invention is specifically described and illustrated below in conjunction with embodiments.

[0030] Hereinafter, tert-amyl peroxy (2-ethylhexyl) carbonate is abbreviated as TAEC.

[0031] Example 1

[0032] Prepare 13200g of 15wt% potassium hydroxide aqueous solution, slowly add it to the reactor, start stirring, control the temperature ≤20°C during stirring, add 200g of tetrabutylammonium chloride, control the temperature of the reactor at 15~20°C, then add 3880g of 80wt% tert-amyl hydroperoxide, stir for 15min after adding tert-amyl hydroperoxide, let it stand for 1h, recover the upper impurity oil phase, and the obtained aqueous phase is the intermediate.

[0033] 1150g of phase transfer catalyst system was prepared according to the molar ratio of sodium sulfite, urea, tetrabutylammonium bromide and tetrabutylammonium iodide of 1.1:0.3:10:2.1, added to 5200g of 2-ethylhexyl chloroformate and blended, and added to the reactor in parallel with the intermediate, stirring was turned on, the temperature was controlled at 12°C, the addition was completed in 50min, and then the substitution reaction was carried out at 12°C. After 2h, stirring was stopped, and the layers were allowed to stand for stratification. The lower aqueous phase was the mother liquor, which was passed to the post-treatment process; the upper layer was the crude TAEC product.

[0034] Trisodium phosphate, sodium linoleate, tetrabutylammonium chloride and water were compounded into 7500g of detergent, which contained 5wt% trisodium phosphate, 2wt% sodium linoleate and 1wt% tetrabutylammonium chloride; the detergent was added to the crude TAEC, stirred at 15-20℃ for 15-20min, allowed to stand to remove the lower aqueous phase, the upper oil phase was taken, and the oil phase was washed with clean water several times until the oil phase was neutral. Finally, TAEC was obtained with a purity of 97.0% and a yield of 94.92%. The liquid chromatography test results of TAEC were as follows: Figure 1 shown.

[0035] Example 2

[0036] Prepare 12000g of 20wt% potassium hydroxide aqueous solution, slowly add it to the reactor, start stirring, control the temperature ≤20°C during stirring, add 200g of tetrabutylammonium chloride, control the temperature of the reactor at 10-15°C, then add 4600g of 80wt% tert-amyl hydroperoxide, stir for 20min after adding tert-amyl hydroperoxide, let stand for 1.5h, recover the upper impurity oil phase, and the obtained aqueous phase is the intermediate.

[0037] 1050g of phase transfer catalyst system was prepared according to the molar ratio of sodium sulfite, urea, tetrabutylammonium bromide and tetrabutylammonium iodide of 0.8:0.5:10:2.5, added to 6300g of 2-ethylhexyl chloroformate and mixed, and added to the reactor in parallel with the intermediate, stirring was turned on, the temperature was controlled at 10°C, the addition was completed in 50min, and then the substitution reaction was carried out at 10°C. After 2.5h, stirring was stopped, and the layers were allowed to stand for stratification. The lower aqueous phase was the mother liquor, which was passed to the post-treatment process; the upper layer was the crude TAEC product.

[0038] Trisodium phosphate, sodium linoleate, tetrabutylammonium chloride and water were compounded into 7500g of detergent, which contained 4wt% trisodium phosphate, 2wt% sodium linoleate and 5wt% tetrabutylammonium chloride; the detergent was added to the crude TAEC, stirred at 15-20℃ for 15-20min, allowed to stand to remove the lower aqueous phase, the upper oil phase was taken, and the oil phase was washed with clean water for several times until the oil phase was neutral. Finally, TAEC was obtained with a purity of 96.1% and a yield of 94.76%.

[0039] Example 3

[0040] Prepare 10000g of 25wt% potassium hydroxide aqueous solution, slowly add it to the reactor, start stirring, control the temperature ≤20°C during stirring, add 300g of tetrabutylammonium chloride, control the temperature of the reactor at 12~17°C, then add 4800g of 80wt% tert-amyl hydroperoxide, stir for 25min after adding tert-amyl hydroperoxide, let stand for 2h, recover the upper impurity oil phase, and the obtained aqueous phase is the intermediate.

[0041] 950 g of a phase transfer catalyst system was prepared according to a molar ratio of sodium sulfite, urea, tetrabutylammonium bromide and tetrabutylammonium iodide of 1.4:0.45:10:2, added to 6500 g of 2-ethylhexyl chloroformate and mixed, and added to the reactor in parallel with the intermediate, stirring was turned on, the temperature was controlled at 8°C, the addition was completed within 60 min, and then a substitution reaction was carried out at 8°C. After 3 hours, stirring was stopped, and the mixture was allowed to stand for stratification. The lower aqueous phase was the mother liquor, which was directed to the post-treatment process; the upper layer was the crude TAEC product.

[0042] Trisodium phosphate, sodium linoleate, tetrabutylammonium chloride and water were compounded into 7500g of detergent, which contained 6wt% trisodium phosphate, 5wt% sodium linoleate and 5wt% tetrabutylammonium chloride; the detergent was added to the crude TAEC, stirred at 15-20℃ for 15-20min, allowed to stand to remove the lower aqueous phase, the upper oil phase was taken, and the oil phase was washed with clean water for several times until the oil phase was neutral. Finally, TAEC was obtained with a purity of 96.7% and a yield of 93.65%.

[0043] Example 4

[0044] Prepare 10500g of 23wt% potassium hydroxide aqueous solution, slowly add it to the reactor, start stirring, control the temperature ≤20°C during stirring, add 320g of tetrabutylammonium chloride, control the temperature of the reactor at 14~19°C, then add 4900g of 80wt% tert-amyl hydroperoxide, stir for 20min after adding tert-amyl hydroperoxide, let stand for 2h, recover the upper impurity oil phase, and the obtained aqueous phase is the intermediate.

[0045] 850g of phase transfer catalyst system was prepared according to the molar ratio of sodium sulfite, urea, tetrabutylammonium bromide and tetrabutylammonium iodide of 1.5:0.25:10:2.2, added to 6600g of 2-ethylhexyl chloroformate and blended, and added to the reactor in parallel with the intermediate, stirring was turned on, the temperature was controlled at 8°C, the addition was completed in 55min, and then the substitution reaction was carried out at 8°C. After 3h, stirring was stopped, and the layers were allowed to stand for stratification. The lower aqueous phase was the mother liquor, which was directed to the post-treatment process; the upper layer was the crude TAEC product.

[0046] Trisodium phosphate, sodium linoleate, tetrabutylammonium chloride and water were compounded into 7500g of detergent, which contained 4wt% trisodium phosphate, 4wt% sodium linoleate and 5wt% tetrabutylammonium chloride; the detergent was added to the crude TAEC, stirred at 15-20℃ for 15-20min, allowed to stand to remove the lower aqueous phase, the upper oil phase was taken, and the oil phase was washed with clean water for several times until the oil phase was neutral. Finally, TAEC was obtained with a purity of 96.3% and a yield of 94.02%.

[0047] Comparative Example 1

[0048] When preparing the intermediate, tetrabutylammonium chloride was not added, and the remaining steps were the same as in Example 1, and TAEC was finally obtained with a purity of 95.4% and a yield of 89.21%.

[0049] Comparative Example 2

[0050] The phase transfer catalyst system was replaced with an equal mass of tetrabutylammonium chloride, and the remaining steps were the same as in Example 1, and TAEC was finally obtained with a purity of 92.0% and a yield of 75.12%.

[0051] Comparative Example 3

[0052] When preparing the phase transfer catalyst system, tetrabutylammonium bromide and tetrabutylammonium iodide were replaced with tetrabutylammonium chloride in an equal molar amount, and the remaining steps were the same as in Example 1, and TAEC was finally obtained with a purity of 93.8% and a yield of 82.35%.

[0053] Comparative Example 4

[0054] When preparing the phase transfer catalyst system, sodium sulfite was not added, and the remaining steps were the same as in Example 1, and TAEC was finally obtained with a purity of 91.3% and a yield of 85.60%.

[0055] Comparative Example 5

[0056] When preparing the phase transfer catalyst system, urea was not added, and the remaining steps were the same as in Example 1, and TAEC was finally obtained with a purity of 92.7% and a yield of 84.92%.

[0057] It can be seen from the above that the phase transfer catalyst system of the present invention is crucial to the present invention. Whether the phase transfer catalyst system lacks tetrabutylammonium bromide, tetrabutylammonium iodide, or sodium sulfite and urea, it has a great impact on the purity and yield of the present invention. In addition, the phase transfer catalysts tetrabutylammonium bromide and tetrabutylammonium iodide in the present invention are both easily soluble in the aqueous phase, so it is easy to separate the phase transfer catalyst from the non-polar TAEC in the oil phase, and further, the phase transfer catalyst can be recovered by means of dichloromethane extraction, low-temperature crystallization, etc. for reuse.

[0058] Although the present invention is described in detail by way of the accompanying drawings and in combination with the embodiments, the present invention is not limited thereto. Without departing from the spirit and essence of the present invention, a person of ordinary skill in the art may make various equivalent modifications or substitutions to the embodiments of the present invention, and these modifications or substitutions shall all be within the scope of the present invention.

Claims

1. A method for preparing tert-amyl peroxy (2-ethylhexyl) carbonate, characterized in that: The following steps are involved: (1) Add a phase transfer agent to the salt-forming agent and mix well, continue to add the crude product of tert-amyl hydroperoxide to carry out temperature-controlled reaction, let stand and collect the lower aqueous phase to obtain an intermediate; The crude tert-amyl hydroperoxide product contains tert-amyl hydroperoxide; (2) compounding sodium sulfite, urea and a phase transfer catalyst to obtain a phase transfer catalyst system; mixing the phase transfer catalyst system with 2-ethylhexyl chloroformate, and adding the phase transfer catalyst system and the intermediate into a reaction kettle in parallel to carry out a substitution reaction; after the substitution reaction is completed, standing and collecting the upper organic phase to obtain a crude product of tert-amyl peroxy (2-ethylhexyl) carbonate, wherein the phase transfer catalyst is a mixture of tetrabutylammonium bromide and tetrabutylammonium iodide; (3) Compounding a detergent, adding the detergent to the crude product of tert-amyl peroxy (2-ethylhexyl) carbonate, stirring, allowing the mixture to stand, collecting the upper oil phase, and washing with water until the oil phase becomes neutral, thereby obtaining tert-amyl peroxy (2-ethylhexyl) carbonate.

2. The preparation method of tert-amyl peroxy (2-ethylhexyl) carbonate according to claim 1, characterized in that, The salt-forming agent is an aqueous solution of potassium hydroxide, and the molar ratio of potassium hydroxide to tert-amyl hydroperoxide is (1.15-1.21):

1.

3. The preparation method of tert-amyl peroxy (2-ethylhexyl) carbonate according to claim 1, characterized in that, The phase transfer agent is tetrabutylammonium chloride, and the ratio of the added amount of tetrabutylammonium chloride to tert-amyl hydroperoxide is (5.6~8.5):

1. The tetrabutylammonium chloride is measured in g, and the tert-amyl hydroperoxide is measured in mol.

4. The preparation method of tert-amyl peroxy (2-ethylhexyl) carbonate according to claim 1, characterized in that, The temperature of the reaction is 10~20℃, the reaction time is 15~25min, and the standing time is 1~2h.

5. The preparation method of tert-amyl peroxy (2-ethylhexyl) carbonate according to claim 1, characterized in that, The molar ratio of 2-ethylhexyl chloroformate to tert-amyl hydroperoxide is 1:(1.08~1.10).

6. The preparation method of tert-amyl peroxy (2-ethylhexyl) carbonate according to claim 1, characterized in that, The parallel flow addition temperature is 10~25°C, and the parallel flow addition time is 50~60min; the substitution reaction temperature is 8~12°C, and the substitution reaction time is 2~3h.

7. The preparation method of tert-amyl peroxy (2-ethylhexyl) carbonate according to claim 1, characterized in that, The molar ratio of sodium sulfite, urea, tetrabutylammonium bromide and tetrabutylammonium iodide is (0.8~1.5):(0.25~0.5):10:(2~2.5), and the mass ratio of the phase transfer catalyst to tert-amyl hydroperoxide is (0.22~0.37):

1.

8. The preparation method of tert-amyl peroxy (2-ethylhexyl) carbonate according to claim 1, characterized in that, The detergent is prepared by mixing trisodium phosphate, sodium linoleate, tetrabutylammonium chloride and water.

9. The preparation method of tert-amyl peroxy (2-ethylhexyl) carbonate according to claim 1, characterized in that, The detergent contains 4-6 wt% of trisodium phosphate, 2-5 wt% of sodium linoleate and 1-5 wt% of tetrabutylammonium chloride, and the balance is water.

10. The preparation method of tert-amyl peroxy (2-ethylhexyl) carbonate according to claim 1, characterized in that, The stirring temperature is 15~20℃ and the stirring time is 15~20min.

Citation Information

Patent Citations

  • Synthesis method of tert-amyl peroxy-2-ethylhexanoate

    CN115557870A

  • Synthesis and purification method of high-purity tert-amyl peroxy-2-ethylhexyl carbonate

    CN112300045A

  • Preparation method of solvent type tert-butyl peroxy-2-ethylhexyl carbonate

    CN116178234A