High-stability cross-linking agent BIPB and preparation method thereof

Abstract

The invention belongs to the technical field of cross-linking agents, and particularly relates to a high-stability cross-linking agent BIPB and a preparation method thereof. The high-stability cross-linking agent BIPB is prepared from the following raw materials in parts by weight: 20-30 parts of tert-butyl hydroperoxide, 5-10 parts of a BaSO4 / 4A zeolite composite material, 0.1-2 parts of polypropylene, 0.1-2 parts of alpha, beta, beta, beta, beta, beta, beta, beta, beta, beta, beta, beta, beta, beta, beta, beta, a BaSO4 / 4A zeolite composite material is introduced in the process of preparing the cross-linking agent BIPB, the strong stability of the cross-linking agent BIPB is improved, the activity of the cross-linking agent is further improved by influencing the specific surface area and pore size distribution of 4A zeolite in the presence of BaSO4, the cross-linking reaction is accelerated, and the cross-linking effect of the cross-linking agent BIPB is improved. The compounding of BaSO4 and 4A zeolite can improve the dispersibility of BaSO4 and promote the uniform distribution of the cross-linking agent BIPB.

Description

Technical Field

[0001] The present invention belongs to the technical field of crosslinking agents, and particularly relates to a crosslinking agent BIPB with strong stability and a preparation method thereof. Background Art

[0002] Bis(tert-butylperoxyisopropyl)benzene (abbreviated as BIPB) is a new type of dialkyl organic peroxide crosslinking agent, an upgraded product of dicumyl peroxide (DCP), commonly known as "odorless DCP". BIPB can be used as a good crosslinking agent for plastics and rubbers such as chlorinated polyethylene, ethylene-propylene-diene monomer rubber, and ethylene-vinyl acetate copolymer. During the crosslinking process, BIPB thermally decomposes to generate free radicals, enabling the crosslinking of plastics to improve the toughness and strength of the rubber compound. At the same time, BIPB does not produce irritating odors during the crosslinking process, has high crosslinking efficiency, and less dosage under the same crosslinking effect. With the enhancement of our environmental awareness, BIPB has replaced most of the DCP products that can produce odors and is widely used.

[0003] However, in the synthesis of traditional crosslinking agent BIPB, sodium carbonate and sodium sulfate or toluene are mostly used as dehydrating agents for tert-butyl hydroperoxide solution, and sodium perchlorate and sulfuric acid with a mass fraction of 70% or sodium perchlorate solution are used as catalysts. The traditional synthesis method not only has a relatively complex synthesis process, cumbersome steps, and high raw material costs, but also toluene is toxic and can cause harm to the environment and human health. Sulfuric acid has strong corrosiveness to stainless steel equipment, with many by-products, generating a large amount of dark red waste sulfuric acid, and the wastewater is not easy to treat. Moreover, sodium perchlorate and perchloric acid aqueous solution are extremely unstable, decomposing at room temperature and exploding when heated, which are not conducive to large-scale safe production. In addition, the prepared crosslinking agent BIPB has insufficient stability and cannot improve the mechanical properties of polymer materials. Therefore, it is urgent to develop a crosslinking agent BIPB with low toxicity, high activity, and high stability. Summary of the Invention

[0004] In view of the deficiencies of the prior art, the present invention provides a crosslinking agent BIPB with strong stability and a preparation method thereof. In the process of preparing the highly stable crosslinking agent BIPB, a BaSO 4 / 4A zeolite composite material is added to increase the stability of the crosslinking agent BIPB. The combination of 4A zeolite and BaSO 4 helps to accelerate the crosslinking reaction of the crosslinking agent BIPB. The presence of BaSO 4 affects the performance of 4A zeolite, thereby improving the activity of the crosslinking agent and accelerating the crosslinking reaction. The combination of BaSO 4 and 4A zeolite improves the dispersion of BaSO 4 , enhances the compatibility of the two in the crosslinking agent, and promotes the uniform distribution of the crosslinking agent. The BaSO 4The addition of the BaSO4 / 4A zeolite composite material can improve the barrier property of the material, thereby enhancing the stability. Crosslinking reactions usually involve volume shrinkage, and the addition of BaSO 4 acts as a volume filler to reduce the volume shrinkage during crosslinking, thus reducing internal stress. The combination of 4A zeolite and BaSO 4 can affect the rheological properties of the crosslinking agent, thereby improving its fluidity and processability during processing. The combination of 4A zeolite and BaSO 4 helps to reduce the migration of the crosslinking agent in the rubber or plastic matrix, thereby enhancing the long-term stability of the product. The crosslinking agent BIPB prepared by the present invention can increase the mechanical properties of rubber and plastics and improve the crosslinking efficiency, having potential application prospects.

[0005] To achieve the above technical objectives, the technical solutions adopted by the present invention are as follows: The present invention provides a highly stable crosslinking agent BIPB, which is prepared from the following raw materials in parts by weight: 20-30 parts of tert-butyl hydroperoxide, 5-10 parts of BaSO 4 / 4A zeolite composite material, 0.1-2 parts of polypropylene, 10-20 parts of a,a'-dihydroxy-1,3-diisopropylbenzene, 40-70 parts of acetic anhydride, and 0.1-2 parts of poly-4-methyl-1-pentene; The preparation raw materials of the BaSO 4 / 4A zeolite composite material are sodium sulfate, barium chloride, and 4A zeolite; The preparation method of the BaSO 4 / 4A zeolite composite material specifically includes the following steps: (1) Dissolve sodium sulfate in deionized water to form solution A, add barium chloride to solution A, stir, and stir at 400 rpm for 30 min to form a mixture; (2) Rinse 4A zeolite repeatedly with deionized water, place it in an oven for drying, and then place it in a muffle furnace for calcination. At room temperature, heat it to 500 °C at a rate of 5 °C / min and keep it at 500 °C for 2 h to obtain activated 4A zeolite; (3) Slowly add the activated 4A zeolite obtained in step (2) to the mixture obtained in step (1), then transfer it to a 100 mL autoclave with a polytetrafluoroethylene liner, react at 160-200 °C for 24 h, wash, and dry to obtain a powder material; (4) Calcinate the powder material obtained in step (3), heat it to 300 °C at a rate of 3 °C / min at room temperature, and keep it at 300 °C for 1-3 h, and then cool it to room temperature to obtain the BaSO 4 / 4A zeolite composite material.

[0006] Further, the mass ratio of the sodium sulfate, barium chloride and deionized water is 1:1:20.

[0007] Further, the mass ratio of the activated 4A zeolite to the mixture is 1-4:20.

[0008] The present invention also provides a method for preparing a highly stable crosslinking agent BIPB, which specifically comprises the following steps: S1, Weigh tert-butyl hydroperoxide by weight parts and add it to a reaction kettle. Then add acetic anhydride thereto by weight parts for dehydration reaction. Stir well to mix and disperse evenly. The temperature is 30-50 °C and the time is 5-30 min to obtain a mixed solution. S2, Add a,a'-dihydroxy-1,3-diisopropylbenzene to the mixed solution obtained in step S1 by weight parts, stir and mix well. Then add BaSO 4 / 4A zeolite composite material, and carry out a condensation reaction at 50-60 °C for 10-30 min to obtain a reaction solution. S3, Weigh polypropylene and poly-4-methyl-1-pentene by weight parts, mix the two, put them into a ball mill for grinding, pass through a 70-mesh sieve after grinding, and add them to the reaction solution obtained in step S2, stir and mix well to obtain a reaction mixture. S4, Wash the reaction mixture, then carry out liquid separation with a separating funnel to obtain an organic layer solution. Then wash the organic layer solution with a 15% sodium hydroxide aqueous solution by mass concentration, and then carry out liquid separation to obtain an organic phase. S5, Carry out vacuum flash drying on the organic phase obtained in step S4 for 1-2 h. The temperature of the vacuum flash is 50 °C and the pressure is -0.095-0 MPa. Then cool and solidify at room temperature to obtain a highly stable crosslinking agent BIPB.

[0009] Compared with the prior art, the beneficial effects obtained by the present invention are as follows: In the process of preparing the highly stable crosslinking agent BIPB of the present invention, a BaSO 4 / 4A zeolite composite material is introduced, which increases the stability of the crosslinking agent BIPB. 4A zeolite has a high specific surface area and a unique pore structure. When used as a filler, its performance is affected due to too high water content. After combining 4A zeolite with BaSO 4 part of it will fill the pores of the zeolite, changing the pore size distribution and specific surface area of 4A zeolite, thereby reducing the water content and further increasing the stability of the BaSO 4 / 4A zeolite composite material. The large specific surface area and good adsorption performance of 4A zeolite enable it to be used as a filler to help BaSO 4 / 4A zeolite composite material. The large specific surface area and good adsorption performance of 4A zeolite enable it to be used as a filler to help BaSO 4Disperse better in the crosslinking agent BIPB, thereby improving the uniformity of the crosslinking agent BIPB, BaSO 4 As a filler, it can enhance the hardness and wear resistance of the composite material. The addition of 4A zeolite further optimizes its hardness and wear resistance, BaSO 4 is a high-temperature resistant compound. Its addition will improve the thermal stability of the crosslinking agent, making BIPB more stable at high temperatures, which is necessary for rubber or plastic products used in high-temperature environments; The combination of 4A zeolite and BaSO 4 helps to accelerate the crosslinking reaction of the crosslinking agent BIPB. The presence of BaSO 4 affects the pore structure of 4A zeolite, thereby increasing the activity of the crosslinking agent and accelerating the crosslinking reaction, BaSO 4 tends to agglomerate alone in the crosslinking agent BIPB. The combination with 4A zeolite will improve the dispersion of BaSO 4 and enhance the compatibility of the two in the crosslinking agent. BaSO 4 has excellent barrier properties and helps to prevent the penetration of gases and liquids. In the crosslinking agent BIPB, the addition of the BaSO 4 / 4A zeolite composite material will improve the barrier properties of the crosslinked material, thereby enhancing stability. The crosslinking reaction is usually accompanied by volume shrinkage, while the addition of BaSO 4 as a volume filler reduces the volume shrinkage during the crosslinking process, thereby reducing internal stress and enhancing stability. The combination of 4A zeolite and BaSO 4 will affect the rheological properties of the crosslinking agent BIPB, thereby improving its fluidity and processing performance during processing. The combination of 4A zeolite and BaSO 4 helps to reduce the migration of the crosslinking agent in the rubber or plastic matrix, thereby improving the long-term stability and performance of the product. BaSO 4 and 4A zeolite are inexpensive, and their use can reduce the cost of the crosslinking agent BIPB, thereby reducing the cost of the final product. During the preparation process of the crosslinking agent BIPB of the present invention, polypropylene and poly(4-methyl-1-pentene) are also added, which helps to combine BaSO 4The 4A zeolite composite material improves the stability of the crosslinking agent BIPB, thereby enhancing the crosslinking efficiency during the crosslinking process. The preparation method of the crosslinking agent BIPB adopted in the present invention has mild reaction conditions, little corrosion to the reaction equipment, high safety, excellent quality of the obtained crosslinking agent BIPB, and low toxicity. The present invention uses acetic anhydride as a dehydrating agent, which shortens the reaction cycle and makes the operation easier. The acetic acid obtained from acetic anhydride and water is directly used as the catalyst for the next dehydration condensation reaction, saving raw material costs. Moreover, the excessive acetic anhydride will further react with the water generated in the dehydration condensation reaction, promoting the forward reaction, accelerating the reaction rate, making the dehydration condensation reaction more complete, and contributing to improving the product yield. The strongly stable crosslinking agent BIPB prepared in the present invention can increase the mechanical properties of rubber and plastics and improve the crosslinking efficiency, having potential application prospects. BRIEF DESCRIPTION OF THE DRAWINGS

[0010] Figure 1 It is a schematic diagram of the purity of the strongly stable crosslinking agent BIPB prepared in the present invention; Figure 2 It is a schematic diagram of the yield of the strongly stable crosslinking agent BIPB prepared in the present invention; Figure 3 It is a schematic diagram of the stability of the strongly stable crosslinking agent BIPB prepared in the present invention. DETAILED DESCRIPTION OF THE EMBODIMENTS

[0011] In order to enable those skilled in the art to better understand the technical solutions of the present invention and make the above features, objectives, and advantages of the present invention clearer and easier to understand, the present invention will be further described below with reference to the embodiments. The embodiments are only used to illustrate the present invention and are not used to limit the scope of the present invention.

[0012] It should be noted that unless otherwise specified, the chemical reagents involved in the present invention are all purchased through commercial channels.

[0013] Example 1: This example provides a strongly stable crosslinking agent BIPB, which is prepared from the following raw materials in parts by weight: 20 parts of tert-butyl hydroperoxide, 10 parts of BaSO 4 / 4A zeolite composite material, 0.1 part of polypropylene, 10 parts of a,a'-dihydroxy-1,3-diisopropylbenzene, 40 parts of acetic anhydride, 0.1 part of poly-4-methyl-1-pentene; The preparation method of the BaSO 4 / 4A zeolite composite material specifically includes the following steps: (1) Take 5 parts of sodium sulfate and dissolve it in deionized water to form solution A. Add barium chloride to solution A, and the mass ratio of sodium sulfate, barium chloride, and deionized water is 1:1:20. Stir at 400 rpm for 30 min to form a mixture; (2) The 4A zeolite was repeatedly rinsed with deionized water, dried in an oven at 70 °C for 24 h, and then calcined in a muffle furnace. At room temperature, it was heated to 500 °C at a rate of 5 °C / min and maintained at 500 °C for 2 h to obtain activated 4A zeolite; (3) The activated 4A zeolite obtained in step (2) was slowly added to the mixture obtained in step (1). The mass ratio of the activated 4A zeolite to the mixture was 1:20. Then it was transferred to a 100 mL autoclave with a polytetrafluoroethylene liner. At 160 °C, a hydrothermal reaction was carried out for 24 h, washed alternately with deionized water and absolute ethanol 3 times, and dried in an oven at 70 °C for 12 h to obtain a powder material; (4) The powder material obtained in step (3) was calcined. At room temperature, it was heated to 300 °C at a rate of 3 °C / min and maintained at 300 °C for 1 h, and then cooled to room temperature to obtain BaSO 4 / 4A zeolite composite material.

[0014] This example also provides a preparation method of a highly stable crosslinking agent BIPB, which specifically includes the following steps: S1, Weigh 20 parts of tert-butyl hydroperoxide and add it to a glass reaction kettle. Then add 40 parts of acetic anhydride to the glass reaction kettle for dehydration reaction. Stir well and mix evenly. The temperature is 50 °C and the time is 30 min. Carry out the reaction at a stirring speed of 300 rpm to obtain a mixed solution; S2, Add 10 parts of a,a’-dihydroxy-1,3-diisopropylbenzene to the mixed solution obtained in step S1, stir and mix evenly at a speed of 200 rpm, and then add 10 parts of BaSO 4 / 4A zeolite composite material, carry out a condensation reaction at 50 °C, and the reaction time is 10 min to obtain a reaction solution; S3, Take 0.1 part of polypropylene and 0.1 part of poly(4-methyl-1-pentene), mix the two, put them into a ball mill for grinding, sieve through a 70-mesh sieve after grinding, and add them to the reaction solution obtained in step S2, stir and mix evenly to obtain a reaction mixture; S4, Wash the reaction mixture with water at 45 °C, then carry out liquid separation with a separating funnel to obtain an organic layer solution. Then wash the organic layer solution with a 15% sodium hydroxide aqueous solution at a temperature of 45 °C, and then carry out liquid separation to obtain an organic phase; S4, Carry out vacuum flash drying on the organic phase obtained in step S4 for 1 h. The temperature of vacuum flash drying is 50 °C and the pressure is -0.095 MPa, and then cool and solidify at room temperature to obtain a highly stable crosslinking agent BIPB.

[0015] Example 2: This example provides a crosslinking agent BIPB with strong stability. The crosslinking agent BIPB is prepared from the following raw materials in parts by weight: 25 parts of tert-butyl hydroperoxide, 4 8 parts of BaSO / 4A zeolite composite material, 1 part of polypropylene, 15 parts of a,a'-dihydroxy-1,3-diisopropylbenzene, 60 parts of acetic anhydride, and 1 part of poly-4-methyl-1-pentene; 4 The preparation method of the BaSO / 4A zeolite composite material specifically includes the following steps: (1) Dissolve 5 parts of sodium sulfate in deionized water to form solution A. Add barium chloride to solution A. The mass ratio of sodium sulfate, barium chloride, and deionized water is 1:1:20. Stir at 400 rpm for 30 min to form a mixture; (2) Rinse 4A zeolite repeatedly with deionized water, place it in an oven at 70 °C for drying for 24 h, then place it in a muffle furnace for calcination. Heat it from room temperature to 500 °C at a rate of 5 °C / min and keep it at 500 °C for 2 h to obtain activated 4A zeolite; (3) Slowly add the activated 4A zeolite obtained in step (2) to the mixture obtained in step (1). The mass ratio of the activated 4A zeolite to the mixture is 3:20. Then transfer it to a 100 mL autoclave with a polytetrafluoroethylene inner liner. Carry out a hydrothermal reaction at 180 °C for 24 h, wash it 3 times alternately with deionized water and absolute ethanol, and place it in an oven at 70 °C for drying for 12 h to obtain a powder material; 4 (4) Calcinate the powder material obtained in step (3). Heat it from room temperature to 300 °C at a rate of 3 °C / min and keep it at 300 °C for 2 h, then cool it to room temperature to obtain the BaSO

[0016] This example also provides a preparation method of a crosslinking agent BIPB with strong stability, which specifically includes the following steps: S1. Weigh 25 parts of tert-butyl hydroperoxide and add it to a glass reaction kettle. Then add 60 parts of acetic anhydride to the glass reaction kettle for dehydration reaction. Stir well and mix evenly. The temperature is 40 °C and the time is 20 min. Carry out the reaction at a stirring speed of 300 rpm to obtain a mixed solution; S2. Add 15 parts of a,a'-dihydroxy-1,3-diisopropylbenzene to the mixed solution obtained in step S1, stir and mix evenly at a speed of 200 rpm, then add 8 parts of BaSO 4 / 4A zeolite composite material, carry out a condensation reaction at 55 °C for 20 min to obtain a reaction solution; S3. Take 1 part of polypropylene and 1 part of poly(4-methyl-1-pentene), mix the two, put them into a ball mill for grinding, sieve through a 70-mesh sieve after grinding, add them to the reaction solution obtained in step S2, stir and mix evenly to obtain a reaction mixture; S4. Wash the reaction mixture with water at 45 °C, then separate the layers with a separatory funnel to obtain an organic layer solution. Then wash the organic layer solution with an aqueous sodium hydroxide solution with a mass concentration of 15% at a temperature of 45 °C, and then separate the layers to obtain an organic phase; S5. Vacuum flash dry the organic phase obtained in step S4 for 1.5 - 2 h. The temperature of the vacuum flash is 50 °C and the pressure is -0.082 MPa, and then cool and solidify at room temperature to obtain the crosslinking agent BIPB with strong stability.

[0017] Example 3: This example provides a crosslinking agent BIPB with strong stability. The crosslinking agent BIPB is prepared from the following raw materials in parts by weight: 30 parts of tert-butyl hydroperoxide, 5 parts of BaSO 4 / 4A zeolite composite material, 2 parts of polypropylene, 20 parts of a,a'-dihydroxy-1,3-diisopropylbenzene, 70 parts of acetic anhydride, and 1 part of poly(4-methyl-1-pentene); The preparation method of the BaSO 4 / 4A zeolite composite material specifically includes the following steps: (1) Take 5 parts of sodium sulfate and dissolve it in deionized water to form solution A. Add barium chloride to solution A. The mass ratio of sodium sulfate, barium chloride to deionized water is 1:1:20, and stir at 400 rpm for 30 min to form a mixture; (2) Rinse the 4A zeolite repeatedly with deionized water, dry it in an oven at 70 °C for 24 h, then put it into a muffle furnace for calcination. At room temperature, heat it to 500 °C at a rate of 5 °C / min and keep it at 500 °C for 2 h to obtain activated 4A zeolite; (3) Slowly add the activated 4A zeolite obtained in step (2) to the mixture obtained in step (1). The mass ratio of the activated 4A zeolite to the mixture is 1:5, then transfer it to a 100 mL autoclave with a polytetrafluoroethylene inner liner. Carry out a hydrothermal reaction at 200 °C for 24 h, wash it alternately with deionized water and absolute ethanol 3 times, and dry it in an oven at 70 °C for 12 h to obtain a powder material; (4) Calcinate the powder material obtained in step (3). At room temperature, heat it to 300 °C at a rate of 3 °C / min and keep it at 300 °C for 3 h, and then cool it to room temperature to obtain the BaSO 4 / 4A zeolite composite material.

[0018] This embodiment also provides a method for preparing a crosslinking agent BIPB with strong stability, which specifically includes the following steps: S1, Weigh 30 parts of tert-butyl hydroperoxide and add it to a glass reaction kettle. Then add 70 parts of acetic anhydride to the glass reaction kettle for dehydration reaction. Stir well to mix and disperse evenly. The temperature is 30 °C and the time is 5 min. Carry out the reaction at a stirring speed of 300 rpm to obtain a mixed solution; S2, Add 20 parts of a,a’-dihydroxy-1,3-diisopropylbenzene to the mixed solution obtained in step S1, stir and mix evenly at a speed of 200 rpm, and then add 10 parts of BaSO 4 / 4A composite material, carry out a condensation reaction at 60 °C for 30 min to obtain a reaction solution; S3, Take 2 parts of polypropylene and 2 parts of poly(4-methyl-1-pentene), mix the two, put them into a ball mill for grinding, sieve through a 70-mesh sieve after grinding, and add them to the reaction solution obtained in step S2, stir and mix evenly to obtain a reaction mixture; S4, Wash the reaction mixture with water at 45 °C, then carry out liquid separation with a separatory funnel to obtain an organic layer solution. Then wash the organic layer solution with a 15% sodium hydroxide aqueous solution at a temperature of 45 °C, and then carry out liquid separation to obtain an organic phase; S5, Carry out vacuum flash drying on the organic phase obtained in step S4 for 2 h. The temperature of vacuum flash drying is 50 °C and the pressure is 0 MPa. Then cool and solidify at room temperature to obtain a crosslinking agent BIPB with strong stability.

[0019] The difference between Comparative Example 1 and Example 1 is that the addition of BaSO 4 / 4A zeolite composite material is cancelled, and the rest is the same as Example 1.

[0020] The difference between Comparative Example 2 and Example 1 is that acetic anhydride is replaced with toluene, and the rest is the same as Example 1.

[0021] The difference between Comparative Example 3 and Example 1 is that the preparation method of the crosslinking agent BIPB is as follows: Weigh tert-butyl hydroperoxide by weight parts and add it to a reaction kettle, add diisopropylbenzene by weight parts to it for dehydration reaction, stir well to mix and disperse evenly, the temperature is 30 - 50 °C, and the time is 5 - 30 min to obtain a mixed solution; Add nickel bromide powder by weight parts to the obtained mixed solution, stir and mix evenly to obtain a reaction solution; Wash the reaction solution, and then carry out liquid separation with a separatory funnel to obtain an organic layer solution, and dry the organic layer solution to obtain a crosslinking agent BIPB.

[0022] The strong stability crosslinking agent BIPB prepared by using Examples 1-3 and Comparative Examples 1-3 of the present invention was used to prepare a rubber-plastic synthetic crosslinked body. The required raw materials were: 80 parts of natural rubber, 12 parts of polyethylene, 3 parts of crosslinking agent BIPB, and 2 parts of antioxidant. The preparation method of the rubber-plastic synthetic crosslinked body was as follows: The natural rubber and polyethylene were respectively plasticized. The natural rubber was heated to 80 °C and kept warm for baking for 15 h for standby, and the polyethylene was heated to 140 °C. The plasticized natural rubber, polyethylene, initiator, and antioxidant were added to an internal mixer and kneaded for 10 min. After adding the crosslinking agent and mixing for 5 min, the temperature of the internal mixer was 95-100 °C. Then, after open milling and extrusion granulation, rubber synthetic crosslinked body particles were obtained.

[0023] The control group did not add the strong stability crosslinking agent BIPB prepared by the present invention, and the rest was the same as the preparation method of the rubber-plastic synthetic crosslinked body.

[0024] Then, the performance test was carried out on the prepared rubber-plastic synthetic crosslinked body, which was divided into Examples 1-3, Comparative Examples 1-3, and the control group.

[0025] Experimental Example 1: According to GB / T528-2009, the tensile properties of the rubber-plastic synthetic crosslinked body were tested. A TCS-2000 type computer system tensile testing machine of China High-Speed Rail Testing Instruments Co., Ltd. was used, and the test was carried out at a tensile speed of 5 mm / min. Examples 1-3, Comparative Examples 1-3, and the control group were tested. The initial specimen was cut from the middle and then prepared into a test specimen through natural splicing. After repairing at 30 °C for 20 min, a tensile test was carried out, and the tensile test was carried out 3 times, and the average value of the tensile strength was calculated. The calculation results were recorded in Table 1.

[0026] Experimental Example 2: The tear strength is tested according to GB-T 529-2008 "Determination of tear strength of vulcanized rubber or thermoplastic rubber". The sample is cut from the test piece by a punching machine using a cutter. For trouser-shaped samples, the cut is located at the center of the sample width and the depth is (40±5) mm. For right-angled samples, the cut depth is (1.0±0.2) mm. For crescent-shaped samples, the cut depth is (1.0±0.2) mm and is located at the center of the concave inner edge of the sample. The sample cutting, measurement and testing are carried out continuously. The sample is installed on a tensile testing machine and stretched at the following gripper movement speeds: (500±50) mm / min for right-angled and crescent-shaped samples and (100±10) mm / min for trouser-shaped samples until the sample breaks. The maximum force value of the right-angled and crescent-shaped samples is recorded. When using trouser-shaped samples, the force value of the entire tearing process should be automatically recorded. The tear strength is calculated according to the formula Ta=F / d, where Ta is the tear strength in kilonewtons per meter (KN / m), F is the force required to tear the sample in Newtons (N), and d is the median thickness of the sample in millimeters (mm). The results are recorded in Table 1.

[0027] Experimental Example 3: According to GB / T2411-2008, the Shore A hardness test was carried out. The sample was placed on a hard, solid horizontal plane. The hardness tester was held in a vertical position, and the tip of the pressure needle was 10 mm away from any edge of the sample. The pressure seat was immediately added to the sample without impact, and the pressure seat was parallel to the sample and sufficient pressure was applied. The pressure seat was in close contact with the sample. After 15 s, the indication of the indicating device was read. Five hardness values ​​were measured on the same sample at an interval of 6 mm, and the average value was calculated. The calculated hardness average value was recorded in Table 1.

[0028] Table 1

[0029] The results in Table 1 show that the tensile strength, tear strength and Shore hardness of Examples 1-3 are all higher than those of the control group and Comparative Examples 1-3, indicating that the rubber-plastic synthetic crosslinked body added with the highly stable crosslinking agent BIPB prepared by the present invention has increased mechanical properties and mechanical properties, indicating that the crosslinking agent BIPB prepared by the present invention can significantly improve the properties of rubber. Figure 1 The purity of the crosslinking agent BIPB prepared by the present invention reached 99.28%, indicating that the BaSO added by the present invention 4 / 4A zeolite composite material, the purity of the crosslinking agent BIPB is improved, indicating that during the preparation process, the target product has fewer impurities, resulting in a higher purity. Figure 2The yield of the crosslinking agent BIPB prepared by the present invention reaches 93.26%, indicating that the by-products generated by the crosslinking agent BIPB prepared by the present invention are less, so that the yield of the crosslinking agent BIPB remains at a high level. Figure 3 The aging resistance performance of the crosslinking agent BIPB prepared by the present invention over time is shown. It can be clearly seen that the crosslinking agent BIPB prepared by the present invention still has an aging resistance performance of more than 90% after being placed for one week, indicating that the added BaSO 4 / 4A zeolite composite material can enhance the stability of the crosslinking agent BIPB, making it have good practicability in various situations.

[0030] In summary, by introducing the BaSO 4 / 4A zeolite composite material into the crosslinking agent BIPB, the stability of the crosslinking agent is significantly improved, the crosslinking efficiency is increased, so that the same crosslinking effect can be achieved with less addition amount. Moreover, the mechanical properties of the rubber-plastic crosslinked composite synthesized by using the crosslinking agent BIPB prepared by the present invention are significantly increased, and the stability at high temperature is enhanced. By adding the BaSO 4 / 4A zeolite composite material, the performance of the crosslinking agent BIPB is significantly improved, so that the crosslinking agent BIPB prepared by the present invention can be widely applied to more fields such as rubber, plastic, wire and cable.

[0031] The above are only the preferred embodiments of the present invention, and are not limitations on the present invention in other forms. Any person skilled in the art may use the technical content disclosed above to make changes or modifications into equivalent embodiments with equivalent changes and apply them to other fields. However, as long as it does not depart from the technical solution content of the present invention, any simple modification, equivalent change and modification made to the above embodiments according to the technical essence of the present invention still belong to the protection scope of the technical solution of the present invention.

Claims

1. A highly stable crosslinking agent BIPB, characterized in that: The highly stable crosslinking agent BIPB is prepared from the following raw materials in parts by weight: 20-30 parts of tert-butyl hydroperoxide, 5-10 parts of BaSO4 / 4A zeolite composite material, 0.1-2 parts of polypropylene, 10-20 parts of a,a'-dihydroxy-1,3-diisopropylbenzene, 40-70 parts of acetic anhydride, and 0.1-2 parts of poly-4-methyl-1-pentene; The raw materials for preparing the BaSO4 / 4A zeolite composite material are: sodium sulfate, barium chloride and 4A zeolite; The preparation method of the BaSO4 / 4A zeolite composite material specifically comprises the following steps: (1) dissolving sodium sulfate in deionized water to form solution A, adding barium chloride to solution A and stirring to form a mixture; (2) repeatedly washing the 4A zeolite with deionized water, drying, and then calcining to obtain activated 4A zeolite; (3) slowly adding the activated 4A zeolite obtained in step (2) to the mixture obtained in step (1), and then subjecting the mixture to a hydrothermal reaction, washing, and drying to obtain a powder material; (4) The powder material obtained in step (3) is calcined and then cooled to room temperature to obtain a BaSO4 / 4A zeolite composite material.

2. A highly stable crosslinking agent BIPB according to claim 1, characterized in that: In step (1), the mass ratio of the sodium sulfate to the barium chloride to the deionized water is 1:1:

20.

3. A highly stable crosslinking agent BIPB according to claim 1, characterized in that: In step (3), the mass ratio of the activated 4A zeolite to the mixture is 1-4:

20.

4. A highly stable crosslinking agent BIPB according to claim 1, characterized in that: In step (3), the temperature of the hydrothermal reaction is set to 160-200 °C, and the time is set to 24 h.

5. A method for preparing the highly stable crosslinking agent BIPB according to any one of claims 1 to 4, characterized in that: The specific steps include: S1, weighing tert-butyl hydroperoxide and acetic anhydride in parts by weight, adding tert-butyl hydroperoxide to acetic anhydride to carry out a dehydration reaction, and stirring and mixing to be uniformly dispersed to obtain a mixed solution; S2, adding a,a'-dihydroxy-1,3-diisopropylbenzene by weight to the mixed solution obtained in step S1, stirring and mixing, and then adding BaSO4 / 4A zeolite composite material by weight to carry out condensation reaction to obtain a reaction solution; S3, taking polypropylene and poly-4-methyl-1-pentene in parts by weight, mixing and grinding the two, adding the two to the reaction solution obtained in step S2, stirring and mixing, and obtaining a reaction mixture; S4, washing the reaction mixture, and then separating the liquids to obtain an organic layer solution, and further washing the organic layer solution, and then separating the liquids to obtain an organic phase; S5, vacuum flash drying the organic phase obtained in step S4, and then cooling and solidifying at room temperature to obtain a highly stable cross-linking agent BIPB.

6. The method for preparing the highly stable cross-linking agent BIPB according to claim 5, characterized in that: In step S2, the condensation reaction temperature is 50-60°C, and the reaction time is 10-30 min.

7. The method for preparing the highly stable cross-linking agent BIPB according to claim 5, characterized in that: In step S5, the vacuum flash evaporation conditions are as follows: the temperature is set to 50°C, the pressure is set to 0.095-0 MPa, and the time is set to 1-2 h.

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