A method for preparing dibenzoyl peroxide by TS-1 catalysis
By using potassium peroxide monosulfate and TS-1 catalyst to react with benzoyl chloride at room temperature, the hazards and high temperature requirements in the traditional dibenzoyl peroxide production process are solved, and high efficiency, safe and high yields are achieved and high purity preparation, suitable for food and feed processing.
Patent Information
- Application Number
- CN202410595531.3
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2024-05-14
- Publication Date
- 2024-12-10
- Estimated Expiration
- 2044-05-14
AI Technical Summary
The traditional dibenzoyl peroxide production process has problems such as hazards, high temperature demand, low yield, product odor and high toxicity, and cannot be used in food and feed processing.
Potassium peroxide monosulfate (PMS) is used as an oxidant, and the TS-1 catalyst is used to react with benzoyl chloride at room temperature to prepare dibenzoyl peroxide. Through the combination of deionized aqueous solution and surfactant, efficient and safe production is achieved. process.
The use of hydrogen peroxide is avoided, the risk of explosion is reduced, and the preparation of dibenzoyl peroxide with high yield and high purity is achieved. It is suitable for food and feed processing.
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Figure CN118530152B_ABST
Abstract
Description
Technical Field
[0001] The invention belongs to the technical field of chemical industry and relates to a method for preparing dibenzoyl peroxide by catalysis of TS-1. Background Art
[0002] Dibenzoyl peroxide, also known as benzoyl peroxide, commonly known as BPO, is an organic compound with a chemical formula of C 14 H 10 O4 is a white crystalline powder at room temperature with a slight smell of bitter almonds. It is soluble in benzene, chloroform, ether, slightly soluble in ethanol and water. It is a common organic peroxide compound and is widely used in medicine, food, chemical industry and other fields. It can be used to treat acne, bleach, polymerization initiator, disinfectant and hardener.
[0003] Traditional benzoyl peroxide production generally adopts the hydrogen peroxide method. The process is divided into two steps. The first step is to react 30% liquid alkali with hydrogen peroxide to generate sodium peroxide solution; the second step is to react with benzoyl chloride at about 0°C, filter, wash and dry the benzoyl peroxide precipitated in the product to obtain the finished product. The disadvantages of this method are: (a) the production and transportation of hydrogen peroxide are dangerous; (b) low temperature reaction is required, the operating cost is high, and the yield is not high; (c) the product has a strong odor and high toxicity. At the same time, to obtain a powdered product, it is often necessary to add organic solvents such as dimethyl sulfoxide, ethylene oxide derivatives, etc. for reaction and crystallization. The obtained product cannot be used in food and feed processing due to the toxicity and odor of the organic solvent, and cannot become a high-grade product.
[0004] Potassium peroxymonosulfate salt is an inorganic peroxide, also known as potassium monopersulfate (PMS). The molecular formula of PMS is KHSO6, and the molecular weight is 168.2. It is a white powdery solid that is easily soluble in water. It is usually relatively stable in the solid state, decomposes slowly, and does not produce harmful substances. After dissolving in water, it releases active oxygen through a chain reaction and then forms hydroxyl free radicals, hydrogen peroxide free radicals and other active ingredients, thus becoming a highly effective disinfectant. Compared with hydrogen peroxide, the composite powder is easy to store and transport and has high stability; it is non-flammable and non-explosive, and overcomes the safety hazards of other disinfectants such as leakage, overturning, explosion, and corrosion in multiple links such as production, transportation, storage and use;
[0005] However, PMS has strong oxidation ability and is often used for environmentally friendly indiscriminate degradation of organic matter. It has certain uses in organic synthesis. For example, PMS can oxidize alcohols to aldehydes or ketones, imines to iminealdehydes, and disulfides to dithioketones. Removal of degreasing groups in alcohol, ether or thioether molecules, such as the deprotection reaction of tosyl or benzyl. Activation reagent: In some cases, PMS can also be used as an activation reagent to promote specific reactions by combining with other reagents (such as triethylamine). For example, CN200810200293.2 reported that acetanilide, sodium bromide, and potassium peroxymonosulfate salt Oxone were dissolved in a mixed solvent of dioxane and water to achieve coupling through oxidation, and finally achieved the synthesis of 4'-methoxy-2-amino-5-acetylbiphenyl. CN202111238098.0 reports that Chuanxiong oil is extracted with an aqueous solvent, and the extract is added with potassium peroxymonosulfate to react to obtain chuanxiong lactone; CN201310328226.X reports a method for 2-substituted benzoxazinone, which uses 2-arylindole as a raw material and PMS as an oxidant to oxidize it. CN201410235515.X dissolves 1,3-dipyridyl bromopropane in water, then adds potassium bromide, and then adds potassium peroxymonosulfate aqueous solution to prepare a clear solution, and then stirs the reaction at -10°C to 0°C until a solid precipitates, and separates the solid to obtain bistribromo 1,3-dipyridinium salt propane. Summary of the invention
[0006] In view of the shortcomings of the existing hydrogen peroxide process technology, potassium peroxymonosulfate (PMS) is used as an oxidant, and TS-1 is used to catalyze PMS to oxidize benzoyl chloride to obtain dibenzoyl peroxide chloride. The process of the invention is simple, a large amount of water is used as a solvent, the reaction is carried out at room temperature, the temperature is stable and easy to control, the yield is high, and it has a strong industrial prospect.
[0007] The technical solution of the present invention is:
[0008] A method for preparing dibenzoyl peroxide by TS-1 catalysis comprises the following steps:
[0009] S1: Weigh the pH regulator and surfactant and place them in a beaker, add deionized water and stir until the pH regulator is completely dissolved, and add catalyst TS-1 to the solution;
[0010] S2: Weigh potassium peroxymonosulfate salt and dissolve it in deionized water, transfer benzoyl chloride, and add it dropwise to the solution in step (1) through a separatory funnel, and stir to react to obtain a crude product;
[0011] S3: After the reaction is completed, the obtained mixture is filtered, and the filter residue is washed several times with a large amount of deionized water to remove the soluble pH regulator and surfactant, and then vacuum dried;
[0012] S4: adding the product obtained in step S3 to a good solvent, standing to completely dissolve, filtering the obtained solution to remove insoluble impurities, heating the obtained solution to remove the good solvent, and obtaining a dibenzoyl peroxide product.
[0013] Preferably, the catalyst is titanium silicalite TS-1 or a combination comprising TS-1.
[0014] Preferably, the mass ratio of pH regulator, surfactant, catalyst TS-1, potassium peroxymonosulfate and benzoyl chloride in S1, S2, S3 and S4 is 0.2-70:0.5-2:0.1:1.2-4.8:15.25-61.
[0015] Preferably, the pH regulator in S1 is one or more of sodium bicarbonate, sodium carbonate, sodium hydroxide and acetic acid; more preferably sodium bicarbonate.
[0016] Preferably, the surfactant in S1 is one or more of sodium dodecyl sulfate, sodium dodecyl sulfonate, sodium dodecylbenzene sulfonate, potassium sorbate and hexadecyltrimethylammonium salt; more preferably, it is sodium dodecyl sulfate.
[0017] Preferably, S2 is added dropwise for 30 minutes, and the reaction is stirred at 20-30°C for 2-3 hours; more preferably, the reaction is stirred at 25°C for 2.5 hours.
[0018] Preferably, S3 is vacuum dried at 25° C. for 48 hours.
[0019] Preferably, the good solvent added in S4 is one or more of chloroform, dichloromethane, acetone, tetrachloromethane, tetrahydrofuran, methanol, and ethanol; preferably chloroform.
[0020] Preferably, the heating temperature in S4 is 25°C.
[0021] The beneficial effects of the present invention are:
[0022] 1. Compared with the existing technology, this reaction avoids the use of hydrogen peroxide, PMS is highly safe, has no explosion risk, and is safe and reliable.
[0023] 2. This reaction does not require strong alkali and low temperature, and is carried out at room temperature and neutral solution. It has few process steps, high yield and high product purity.
[0024] 3. The catalyst prepared by the present invention can achieve a benzoyl chloride conversion rate of >96%. BRIEF DESCRIPTION OF THE DRAWINGS
[0025] In order to more clearly illustrate the specific implementation methods of the present invention or the technical solutions in the prior art, the drawings required for use in the specific implementation methods or the description of the prior art will be briefly introduced below. Obviously, the drawings described below are some implementation methods of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying any creative work.
[0026] Figure 1 : Flow chart of preparation of dibenzoyl peroxide.
[0027] Figure 2 : Actual picture of dibenzoyl peroxide.
[0028] Figure 3 : Infrared spectrum of dibenzoyl peroxide.
[0029] Figure 4 : UV spectrum of dibenzoyl peroxide.
[0030] Figure 5 : Dibenzoyl peroxide 1 H NMR spectra. DETAILED DESCRIPTION
[0031] Hereinafter, the present invention will be described in detail. Before describing, it should be understood that the terms used in this specification and the appended claims should not be interpreted as being limited to the general meaning and dictionary meaning, but should be interpreted according to the meaning and concept corresponding to the technical aspects of the present invention on the basis of the principle that the inventor is allowed to appropriately define the terms for the best interpretation. Therefore, the descriptions presented here are only preferred examples for illustrative purposes and are not intended to limit the scope of the present invention, so that it should be understood that other equivalents or improvements can be obtained therefrom without departing from the spirit and scope of the present invention.
[0032] The following examples are only listed as examples of embodiments of the present invention and do not constitute any limitation to the present invention. It can be understood by those skilled in the art that modifications within the scope of the essence and concept of the present invention fall within the scope of protection of the present invention. Unless otherwise specified, the reagents and instruments used in the following examples are all commercially available products.
[0033] Hereinafter, the preferred embodiments of the present disclosure will be described in detail with reference to the accompanying drawings. Before the description, it should be understood that the terms used in the specification and the appended claims should not be interpreted as limited to the general and dictionary meanings, but should be interpreted based on the principle of allowing the inventor to appropriately define the terms for the best interpretation, based on the meaning and concept corresponding to the technical level of the present invention. Therefore, the description herein is only a preferred example for illustrative purposes, and is not intended to limit the scope of the present invention, so it should be understood that other equivalent implementations and modifications can be made without departing from the spirit and scope of the present invention.
[0034] As used herein, the terms "include", "comprising", "having", "containing" or any other similar terms are open-ended transitional phrases, which are intended to cover non-exclusive inclusions. For example, a composition or article containing multiple elements is not limited to the elements listed herein, but may also include other elements that are not explicitly listed but are generally inherent to the composition or article. In addition, unless otherwise expressly stated, the term "or" refers to an inclusive "or" rather than an exclusive "or". For example, any of the following situations satisfies the condition "A or B": A is true (or exists) and B is false (or does not exist), A is false (or does not exist) and B is true (or exists), and both A and B are true (or exist). In addition, as used herein, the terms "include", "comprising", "having", and "containing" should be interpreted as being specifically disclosed and simultaneously covering closed or semi-closed transitional phrases such as "consisting of" and "consisting essentially of".
[0035] In this article, all features or conditions defined in the form of numerical ranges or percentage ranges are only for brevity and convenience. Accordingly, the description of numerical ranges or percentage ranges should be deemed to have covered and specifically disclosed all possible secondary ranges and individual values within the range, especially integer values. For example, the range description of "1 to 8" should be deemed to have specifically disclosed all secondary ranges such as 1 to 7, 2 to 8, 2 to 6, 3 to 6, 4 to 8, 3 to 8, etc., especially secondary ranges defined by all integer values, and should be deemed to have specifically disclosed individual values such as 1, 2, 3, 4, 5, 6, 7, 8, etc. within the range. Unless otherwise specified, the above interpretation method applies to all contents of the entire present invention, regardless of whether the range is broad or not.
[0036] If the quantity or other numerical value or parameter is expressed as a range, a preferred range or a series of upper and lower limits, it should be understood that all ranges consisting of any upper limit or preferred value of the range and the lower limit or preferred value of the range have been specifically disclosed herein, regardless of whether these ranges are disclosed separately. In addition, if a numerical range is mentioned herein, unless otherwise specified, the range should include its endpoints and all integers and fractions within the range.
[0037] In this document, under the premise of achieving the purpose of the invention, numerical values should be understood to have the accuracy of the number of significant digits of the numerical value. For example, the number 40.0 should be understood to cover the range from 39.50 to 40.49.
[0038] In addition, unless otherwise specified, the sources of materials involved in the examples of the present invention are: sodium bicarbonate and sodium dodecyl sulfate (purchased from TCI (Shanghai) Chemical Industry Development Co., Ltd.), TS-1 (purchased from Shanghai Aladdin Biochemical Technology Co., Ltd.), potassium peroxymonosulfate (purchased from Anage Chemical), benzoyl chloride (purchased from Shanghai McLean Biochemical Technology Co., Ltd.), deionized water (resistivity: 18.22 MΩ·cm)
[0039] Example 1: 0.417 mol (35 g) of sodium bicarbonate was dissolved in 50 mL of deionized water, 3.5 mmol (1 g) of sodium dodecyl sulfate was added, and 0.1 g of TS-1 was added to the solution. 3.9 mmol (2.4 g) of potassium peroxymonosulfate and 35 mL of benzoyl chloride 0.217 mol (30.5 g) were slowly (30 minutes) added dropwise to the solution, stirred at 25°C for 2.5 hours, and the precipitate was separated by suction filtration, washed several times with a large amount of deionized water to remove the soluble sodium bicarbonate and sodium dodecyl sulfate, and dried under vacuum at 25°C for 48 hours.
[0040] The crude dibenzoyl peroxide product obtained by vacuum drying was added with 50 mL of chloroform and allowed to stand for 5 hours until the dibenzoyl peroxide in the crude product was completely dissolved.
[0041] The chloroform solution was heated at 25°C overnight, and the chloroform solvent was removed to obtain the final dibenzoyl peroxide product, with a mass of 26.02 g and a yield of 99%. The reaction process conditions and results are shown in Table 1.
[0042] Example 2: 0.01 mol (0.4 g) of sodium hydroxide was dissolved in 50 mL of deionized water, 3.5 mmol (1 g) of sodium dodecyl sulfate was added, and 0.1 g of TS-1 was added to the solution. 3.9 mmol (2.4 g) of potassium peroxymonosulfate and 0.217 mol (30.5 g) of benzoyl chloride (35 mL) were slowly added dropwise (30 minutes) to the solution, and the reaction was stirred at 25°C for 2.5 hours, and the precipitate was separated by suction filtration, and washed several times with a large amount of deionized water to remove the soluble sodium bicarbonate and sodium dodecyl sulfate, and then dried under vacuum at 25°C for 48 hours.
[0043] The crude dibenzoyl peroxide product obtained by vacuum drying was added with 50 mL of chloroform and allowed to stand for 5 hours until the dibenzoyl peroxide in the crude product was completely dissolved.
[0044] The chloroform solution was heated at 25°C overnight, and the chloroform solvent was removed to obtain the final dibenzoyl peroxide product, with a mass of 24.18 g and a yield of 92%. The reaction process conditions and results are shown in Table 1.
[0045] Example 3: 0.417 mol (35 g) of sodium bicarbonate was dissolved in 50 mL of deionized water, 3.5 mmol (0.525 g) of potassium sorbate was added, and 0.1 g of TS-1 was added to the solution. 3.9 mmol (2.4 g) of potassium peroxymonosulfate and 35 mL of benzoyl chloride 0.217 mol (30.5 g) were slowly (30 minutes) added dropwise to the solution, and after stirring at 25° C. for 2.5 hours, the precipitate was separated by suction filtration, and washed several times with a large amount of deionized water to remove the soluble sodium bicarbonate and sodium dodecyl sulfate, and then dried under vacuum at 25° C. for 48 hours.
[0046] The crude dibenzoyl peroxide product obtained by vacuum drying was added with 50 mL of chloroform and allowed to stand for 5 hours until the dibenzoyl peroxide in the crude product was completely dissolved.
[0047] The chloroform solution was heated at 25°C overnight, and the chloroform solvent was removed to obtain the final dibenzoyl peroxide product, with a mass of 23.79 g and a yield of 90.5%. The reaction process conditions and results are shown in Table 1.
[0048] Example 4: 0.417 mol (35 g) of sodium bicarbonate was dissolved in 50 mL of deionized water, 3.5 mmol (1 g) of sodium dodecyl sulfate was added, and 0.1 g of TS-1 was added to the solution. 3.9 mmol (2.4 g) of potassium peroxymonosulfate and 0.217 mol (30.5 g) of benzoyl chloride (35 mL) were slowly (30 minutes) added dropwise to the solution, and stirred at 25°C for 2.5 hours, and the precipitate was separated by suction filtration, and washed several times with a large amount of deionized water to remove the soluble sodium bicarbonate and sodium dodecyl sulfate, and then dried under vacuum at 25°C for 48 hours.
[0049] The crude dibenzoyl peroxide product obtained by vacuum drying was added with 50 mL of acetone and allowed to stand for 5 hours until the dibenzoyl peroxide in the crude product was completely dissolved.
[0050] The acetone solution was heated at 25°C overnight, and the acetone solvent was removed to obtain the final dibenzoyl peroxide product, with a mass of 24.63 g and a yield of 93.7%. The reaction process conditions and results are shown in Table 1.
[0051] Example 5: 0.417 mol (35 g) of sodium bicarbonate was dissolved in 50 mL of deionized water, 3.5 mmol (1 g) of sodium dodecyl sulfate was added, and 0.05 g of TS-1 was added to the solution. 3.9 mmol (2.4 g) of potassium peroxymonosulfate and 35 mL of benzoyl chloride 0.217 mol (30.5 g) were slowly added dropwise (30 minutes) to the solution, and stirred at 25°C for 2.5 hours, and the precipitate was separated by suction filtration, and washed several times with a large amount of deionized water to remove the soluble sodium bicarbonate and sodium dodecyl sulfate, and then dried under vacuum at 25°C for 48 hours.
[0052] The crude dibenzoyl peroxide product obtained by vacuum drying was added with 50 mL of chloroform and allowed to stand for 5 hours until the dibenzoyl peroxide in the crude product was completely dissolved.
[0053] The chloroform solution was heated at 25°C overnight, and the chloroform solvent was removed to obtain the final dibenzoyl peroxide product, with a mass of 25.47 g and a yield of 96.9%. The reaction process conditions and results are shown in Table 1.
[0054] Example 6: 0.417 mol (35 g) of sodium bicarbonate was dissolved in 50 mL of deionized water, 3.5 mmol (1 g) of sodium dodecyl sulfate was added, and 0.2 g of TS-1 was added to the solution. 3.9 mmol (2.4 g) of potassium peroxymonosulfate and 35 mL of benzoyl chloride 0.217 mol (30.5 g) were slowly added dropwise (30 minutes) to the solution, and stirred at 25°C for 2.5 hours, and the precipitate was separated by suction filtration, and washed several times with a large amount of deionized water to remove the soluble sodium bicarbonate and sodium dodecyl sulfate, and then dried under vacuum at 25°C for 48 hours.
[0055] The crude dibenzoyl peroxide product obtained by vacuum drying was added with 50 mL of chloroform and allowed to stand for 5 hours until the dibenzoyl peroxide in the crude product was completely dissolved.
[0056] The chloroform solution was heated at 25°C overnight, and the chloroform solvent was removed to obtain the final dibenzoyl peroxide product, with a mass of 25.7 g and a yield of 97.8%. The reaction process conditions and results are shown in Table 1.
[0057] Example 7: 0.417 mol (35 g) of sodium bicarbonate was dissolved in 50 mL of deionized water, 3.5 mmol (1 g) of sodium dodecyl sulfate was added, and 0.1 g of TS-1 was added to the solution. 3.9 mmol (2.4 g) of potassium peroxymonosulfate and 0.217 mol (30.5 g) of benzoyl chloride (35 mL) were slowly added dropwise (30 minutes) to the solution, and stirred at 20°C for 2.5 hours, and the precipitate was separated by suction filtration, and washed several times with a large amount of deionized water to remove the soluble sodium bicarbonate and sodium dodecyl sulfate, and then dried under vacuum at 25°C for 48 hours.
[0058] The crude dibenzoyl peroxide product obtained by vacuum drying was added with 50 mL of chloroform and allowed to stand for 5 hours until the dibenzoyl peroxide in the crude product was completely dissolved.
[0059] The chloroform solution was heated at 25° C. overnight, and the chloroform solvent was removed to obtain the final dibenzoyl peroxide product with a mass of 25.31 g and a yield of 96.3%. The conditions and results are shown in Table 1.
[0060] Example 8: 0.417 mol (35 g) of sodium bicarbonate was dissolved in 50 mL of deionized water, 3.5 mmol (1 g) of sodium dodecyl sulfate was added, and 0.1 g of TS-1 was added to the solution. 1.95 mmol (1.2 g) of potassium peroxymonosulfate and 35 mL of benzoyl chloride 0.217 mol (30.5 g) were slowly (30 minutes) added dropwise to the solution, stirred at 30°C for 2.5 hours, and the precipitate was separated by suction filtration, washed several times with a large amount of deionized water to remove the soluble sodium bicarbonate and sodium dodecyl sulfate, and dried under vacuum at 25°C for 48 hours.
[0061] The crude dibenzoyl peroxide product obtained by vacuum drying was added with 50 mL of chloroform and allowed to stand for 5 hours until the dibenzoyl peroxide in the crude product was completely dissolved.
[0062] The above chloroform solution was heated at 25° C. overnight, and the chloroform solvent was removed to obtain the final dibenzoyl peroxide product with a mass of 25.02 g and a yield of 95.2. The process conditions and results are shown in Table 1.
[0063] Example 9: 0.417 mol (35 g) of sodium bicarbonate was dissolved in 50 mL of deionized water, 3.5 mmol (1 g) of sodium dodecyl sulfate was added, and 0.1 g of TS-1 was added to the solution. 3.9 mmol (2.4 g) of potassium peroxymonosulfate and 35 mL of benzoyl chloride 0.217 mol (30.5 g) were slowly (30 minutes) added dropwise to the solution, stirred at 30°C for 2 hours, and the precipitate was separated by suction filtration, washed several times with a large amount of deionized water to remove the soluble sodium bicarbonate and sodium dodecyl sulfate, and dried under vacuum at 25°C for 48 hours.
[0064] The crude dibenzoyl peroxide product obtained by vacuum drying was added with 50 mL of chloroform and allowed to stand for 5 hours until the dibenzoyl peroxide in the crude product was completely dissolved.
[0065] The chloroform solution was heated at 25° C. overnight, and the chloroform solvent was removed to obtain the final dibenzoyl peroxide product with a mass of 25.89 g and a yield of 98.5%. The process conditions and results are shown in Table 1.
[0066] Example 10: 0.417 mol (35 g) of sodium bicarbonate was dissolved in 50 mL of deionized water, 3.5 mmol (1 g) of sodium dodecyl sulfate was added, and 0.1 g of TS-1 was added to the solution. 3.9 mmol (2.4 g) of potassium peroxymonosulfate and 0.217 mol (30.5 g) of benzoyl chloride (35 mL) were slowly added dropwise (30 minutes) to the solution, and stirred at 25°C for 3 hours, and the precipitate was separated by suction filtration, and washed several times with a large amount of deionized water to remove the soluble sodium bicarbonate and sodium dodecyl sulfate, and then dried under vacuum at 25°C for 48 hours.
[0067] The crude dibenzoyl peroxide product obtained by vacuum drying was added with 50 mL of chloroform and allowed to stand for 5 hours until the dibenzoyl peroxide in the crude product was completely dissolved.
[0068] The chloroform solution was heated at 25° C. overnight, and the chloroform solvent was removed to obtain the final dibenzoyl peroxide product with a mass of 25.65 g and a yield of 97.6%. The process conditions and results are shown in Table 1.
[0069] Table 1. Reaction process conditions and results
[0070]
[0071] Examples 1-5 were subjected to a series of tests. Figure 1 Flow chart of the preparation of dibenzoyl peroxide. Figure 2 This is a physical picture of the final product of dibenzoyl peroxide. Dibenzoyl peroxide is a white crystalline solid. Figure 3 The infrared spectrum of dibenzoyl peroxide shows good overlap in peak position compared with the standard sample in the literature, indicating that dibenzoyl peroxide was successfully synthesized. Figure 4 : The UV spectrum of dibenzoyl peroxide shows good overlap with that of the standard sample, indicating that dibenzoyl peroxide was successfully synthesized. Figure 5 : Dibenzoyl peroxide 1 The H NMR spectrum was consistent with the simulated peak position, indicating that dibenzoyl peroxide was successfully synthesized.
[0072] The above is only a specific embodiment of the present invention, but the protection scope of the present invention is not limited thereto. Any person skilled in the art can easily think of changes or substitutions within the technical scope disclosed by the present invention, which should be included in the protection scope of the present invention. Therefore, the protection scope of the present invention should be based on the protection scope of the claims.
Claims
1. A method for preparing dibenzoyl peroxide by TS-1 catalysis, characterized in that: The steps include: S1: Weigh the pH regulator and surfactant and place them in a beaker, add deionized water and stir until the pH regulator is completely dissolved, and add catalyst TS-1 to the solution; S2: Weigh potassium peroxymonosulfate salt and dissolve it in deionized water, transfer benzoyl chloride, and add it dropwise to the solution in step (1) through a separatory funnel, and stir to react to obtain a crude product; S3: After the reaction is completed, the obtained mixture is filtered, and the filter residue is washed several times with a large amount of deionized water to remove the soluble pH regulator and surfactant, and then vacuum dried; S4: adding the product obtained in step S3 to a good solvent, standing to completely dissolve, filtering the obtained solution to remove insoluble impurities, heating the obtained solution to remove the good solvent, and obtaining a dibenzoyl peroxide product.
2. The method according to claim 1, characterized in that: The mass ratios of pH regulator, surfactant, catalyst TS-1, potassium peroxymonosulfate and benzoyl chloride in S1, S2, S3 and S4 are 0.2-70:0.5-2:0.1:1.2-4.8:15.25-61.
3. The method according to claim 1, characterized in that The pH regulator in S1 is one or more of sodium bicarbonate, sodium carbonate, sodium hydroxide and acetic acid.
4. The method according to claim 3, characterized in that The pH regulator in S1 is sodium bicarbonate.
5. The method according to claim 1, characterized in that The surfactant in S1 is one or more of sodium dodecyl sulfate, sodium dodecyl sulfonate, sodium dodecylbenzene sulfonate, potassium sorbate and hexadecyltrimethylammonium salt.
6. The method according to claim 5, characterized in that The surfactant in S1 is sodium dodecyl sulfate.
7. The method according to claim 1, characterized in that The S2 was added dropwise for 30 minutes and the reaction was stirred at 20-30°C for 2-3 hours.
8. The method according to claim 7, characterized in that The reaction was stirred in S2 at 25°C for 2.5 hours.
9. The method according to claim 1, characterized in that: S3 was dried in vacuum at 25°C for 48 hours.
10. The method according to claim 1, characterized in that The good solvent added to S4 is one or more of chloroform, dichloromethane, acetone, tetrachloromethane, tetrahydrofuran, methanol, and ethanol.
11. The method according to claim 10, characterized in that The good solvent added to S4 is chloroform.
12. The method according to claim 1, characterized in that The heating temperature in S4 is 25°C.
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