A strong stability cross-linking agent BIPB and a preparation method thereof

Abstract

The application belongs to the technical field of crosslinking agents, and particularly relates to a strong-stability crosslinking agent BIPB and a preparation method thereof. The strong-stability crosslinking agent BIPB is prepared from the following raw materials in parts by weight: 20-30 parts of t-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. In the preparation of the crosslinking agent BIPB, the BaSO4 / 4A zeolite composite material is introduced, so that the strong stability of the crosslinking agent BIPB is increased. The existence of BaSO4 affects the specific surface area and pore size distribution of 4A zeolite, thereby improving the activity of the crosslinking agent, accelerating the crosslinking reaction. The compounding of BaSO4 and 4A zeolite improves the dispersibility of BaSO4 and promotes the uniform distribution of the crosslinking agent BIPB.

Description

TECHNICAL FIELD

[0001] The application 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

[0002] Bis (tert-butyl peroxyisopropyl) benzene (BIPB for short) 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 chlorinated polyethylene, ethylene-propylene-diene rubber, ethylene-vinyl acetate copolymer and other plastics and rubbers. In the crosslinking process, BIPB will decompose to produce free radicals, so as to crosslink the plastics to improve the toughness and strength of the rubber. At the same time, BIPB will not produce irritating odor in the crosslinking process, has the characteristics of high crosslinking efficiency, less dosage under the same crosslinking effect, etc. With the enhancement of our environmental awareness, BIPB has replaced most DCP products that can produce odor and is widely used.

[0003] However, the traditional synthesis of crosslinking agent BIPB mostly uses sodium carbonate and sodium sulfate or toluene as the dehydrating agent of tert-butyl hydroperoxide solution, uses sodium perchlorate and 70% mass fraction sulfuric acid or sodium perchlorate solution as the catalyst. The traditional synthesis method is not only complex in synthesis process, tedious in steps and high in raw material cost, but also toxic toluene will cause harm to the environment and human health, sulfuric acid has strong corrosion to stainless steel equipment, there are many by-products, a large amount of deep black red waste sulfuric acid will be produced, and the wastewater is not easy to treat. Sodium perchlorate and sodium perchlorate aqueous solution are extremely unstable, decompose at room temperature, and explode when heated, which are not conducive to large-scale safe production. Moreover, the prepared crosslinking agent BIPB has insufficient stability and cannot improve the mechanical properties of high polymer materials. Therefore, it is urgent to develop a crosslinking agent BIPB with low toxicity, high activity and high stability. SUMMARY

[0004] In view of the deficiencies of the prior art, the present application provides a crosslinking agent BIPB with strong stability and a preparation method thereof. In the preparation of the crosslinking agent BIPB with strong stability, BaSO4 / 4A zeolite composite material is added to increase the stability of the crosslinking agent BIPB. The composite of 4A zeolite and BaSO4 helps to accelerate the crosslinking reaction of the crosslinking agent BIPB. The presence of BaSO4 improves the activity of the crosslinking agent, accelerates the crosslinking reaction, and improves the dispersibility of BaSO4, the compatibility of the two in the crosslinking agent, and the uniform distribution of the crosslinking agent. The addition of the BaSO4 / 4A zeolite composite material improves the barrier property of the material and thus the stability. The crosslinking reaction is usually accompanied by volume shrinkage, and the addition of BaSO4 as a volume filler reduces the volume shrinkage during the crosslinking process, thereby reducing internal stress. The composite of 4A zeolite and BaSO4 affects the rheological properties of the crosslinking agent, thereby improving its flowability and processing performance during processing. The composite of 4A zeolite and BaSO4 helps to reduce the migration of the crosslinking agent in the rubber or plastic matrix, thereby improving the long-term stability of the product. The crosslinking agent BIPB prepared by the present application can increase the mechanical properties of rubber and plastic, improve the efficiency of crosslinking, and has potential application prospects.

[0005] In order to achieve the above technical purpose, the technical scheme adopted by the present application is as follows:

[0006] The present application provides a crosslinking agent BIPB with strong stability, which is prepared from the following raw materials 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.

[0007] The preparation raw materials of the BaSO4 / 4A zeolite composite material are sodium sulfate, barium chloride, and 4A zeolite.

[0008] The preparation method of the BaSO4 / 4A zeolite composite material specifically includes the following steps:

[0009] (1) Dissolve sodium sulfate in deionized water to form solution A, add barium chloride to solution A, and stir at 400 rpm for 30 min to form a mixture;

[0010] (2) Rinse the 4A zeolite with deionized water, dry it in an oven, and then calcine it in a muffle furnace. Heat to 500 ℃ at a rate of 5 ℃ / min and keep at 500 ℃ for 2 h to obtain activated 4A zeolite;

[0011] (3) The activated 4A zeolite obtained in step (2) is slowly added to the mixture obtained in step (1), and then transferred to a 100 mL polytetrafluoroethylene-lined autoclave, 160-200 ℃, 24 h, washing, drying to obtain a powder material;

[0012] (4) The powder material obtained in step (3) is calcined, heated to 300 ℃ at a rate of 3 ℃ / min at room temperature, and kept at 300 ℃ for 1-3 h, and then cooled to room temperature to obtain a BaSO4 / 4A zeolite composite material.

[0013] Further, the mass ratio of the sodium sulfate, the barium chloride and the deionized water is 1:1:20.

[0014] Further, the mass ratio of the activated 4A zeolite and the mixture is 1-4:20.

[0015] The application also provides a preparation method of the strong-stability crosslinking agent BIPB, which specifically comprises the following steps:

[0016] S1, tert-butyl hydroperoxide is weighed by weight parts and added to a reaction kettle, and acetic anhydride is added to the reaction kettle by weight parts for dehydration reaction, and the mixture is fully stirred and dispersed uniformly, the temperature is 30-50 ℃, and the time is 5-30 min, to obtain a mixed solution;

[0017] S2, a,a'-dihydroxy-1,3-diisopropylbenzene is added to the mixed solution obtained in step S1 by weight parts, and stirred and mixed, and then BaSO4 / 4A zeolite composite material is added by weight parts, and condensation reaction is carried out at 50-60 ℃, and the reaction time is 10-30 min, to obtain a reaction liquid;

[0018] S3, polypropylene and poly-4-methyl-1-pentene are taken by weight parts, mixed, put into a ball mill for grinding, and then sieved through a 70-mesh sieve, added to the reaction liquid obtained in step S2, stirred and mixed, and a reaction mixture is obtained;

[0019] S4, the reaction mixture is washed, then separated by a separatory funnel to obtain an organic layer solution, and then the organic layer solution is washed with a 15% sodium hydroxide aqueous solution by mass concentration, and then separated to obtain an organic phase;

[0020] S5, the organic phase obtained in step S4 is vacuum flash dried for 1-2 h, the vacuum flash drying temperature is 50 ℃, and the pressure is-0.095-0 MPa, and then cooled and solidified at room temperature to obtain the strong-stability crosslinking agent BIPB.

[0021] Compared with the prior art, the application has the following beneficial effects:

[0022] The application introduces BaSO4 / 4A zeolite composite material in the preparation of crosslinking agent BIPB with strong stability, increases the stability of crosslinking agent BIPB, 4A zeolite has high specific surface area and unique pore structure, when used as filler, the water content is too high to affect its performance, after the 4A zeolite is compounded with BaSO4, the BaSO4 will partially fill the pore of the zeolite, changes the pore size distribution and specific surface area of the 4A zeolite, so that the water content is reduced, the stability of the BaSO4 / 4A zeolite composite material is further increased, the large specific surface area and good adsorption performance of the 4A zeolite enable it to help BaSO4 to be better dispersed in the crosslinking agent BIPB, so as to improve the uniformity of the crosslinking agent BIPB, BaSO4 as filler can enhance the hardness and wear resistance of the composite material, the addition of 4A zeolite further optimizes the hardness and wear resistance, BaSO4 is a high-temperature-resistant compound, its addition can improve the thermal stability of the crosslinking agent, so that BIPB is more stable at high temperature, which is necessary for rubber or plastic products used in high-temperature environment; the compounding of 4A zeolite and BaSO4 helps to accelerate the crosslinking reaction of the crosslinking agent BIPB, the presence of BaSO4 improves the activity of the crosslinking agent and accelerates the crosslinking reaction by affecting the pore size structure of the 4A zeolite, BaSO4 alone is easy to agglomerate in the crosslinking agent BIPB, the compounding with 4A zeolite can improve the dispersibility of BaSO4 and improve the compatibility of the two in the crosslinking agent, BaSO4 has excellent barrier properties, which helps to prevent the penetration of gas and liquid, in the crosslinking agent BIPB, the addition of BaSO4 / 4A zeolite composite material can improve the barrier properties of the crosslinking material, and further improve the stability, the crosslinking reaction is usually accompanied by volume shrinkage, and the addition of BaSO4 as a volume filler can reduce the volume shrinkage during the crosslinking process, thereby reducing internal stress and improving stability, the compounding of 4A zeolite and BaSO4 can affect the rheological properties of the crosslinking agent BIPB, thereby improving its flowability and processing performance during processing, the compounding of 4A zeolite and BaSO4 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. BaSO4 and 4A zeolite are low in price, and their use can reduce the cost of the crosslinking agent BIPB, thereby reducing the cost of the final product. In the preparation process of the crosslinking agent BIPB of the application, polypropylene and poly-4-methyl-1-pentene are also added, which helps to improve the stability of the crosslinking agent BIPB in combination with the BaSO4 / 4A zeolite composite material, and improves the crosslinking efficiency during the crosslinking process.The preparation method of the crosslinking agent BIPB has mild reaction conditions, small corrosion to reaction equipment, high safety, excellent quality of the obtained crosslinking agent BIPB, and low toxicity. The preparation method of the crosslinking agent BIPB shortens the reaction period, and is more simple and easy to operate. The obtained acetic acid from acetic anhydride and water is directly used as a catalyst for the next dehydration condensation reaction, thereby saving the raw material cost. The excessive acetic anhydride further reacts with the water generated in the dehydration condensation reaction, promotes the forward reaction, accelerates the reaction rate, and makes the dehydration condensation reaction more thorough, thereby helping to improve the product yield. The strong and stable crosslinking agent BIPB prepared by the method has potential application prospects. BRIEF DESCRIPTION OF DRAWINGS

[0023] Figure 1 A purity diagram of the strong and stable crosslinking agent BIPB prepared by the method;

[0024] Figure 2 A yield diagram of the strong and stable crosslinking agent BIPB prepared by the method;

[0025] Figure 3 A stability diagram of the strong and stable crosslinking agent BIPB prepared by the method. DETAILED DESCRIPTION

[0026] In order to enable the person skilled in the art to better understand the technical solutions of the present application, and to make the above-mentioned features, objects and advantages of the present application more clear and easy to understand, the present application will be further described below in combination with examples. The examples are only used to illustrate the present application and not to limit the scope of the present application.

[0027] It should be noted that, unless otherwise specified, the chemical reagents involved in the present application are purchased through commercial channels.

[0028] Example 1: The present example provides a strong and stable crosslinking agent BIPB, which is prepared from the following raw materials by weight: 20 parts of tert-butyl hydroperoxide, 10 parts of BaSO4 / 4A zeolite composite material, 0.1 part of polypropylene, 10 parts of a,a'-dihydroxy-1,3-diisopropylbenzene, 40 parts of acetic anhydride, and 0.1 part of poly-4-methyl-1-pentene.

[0029] The preparation method of the BaSO4 / 4A zeolite composite material specifically includes the following steps:

[0030] (1) 5 parts of sodium sulfate are dissolved in deionized water to form a solution A, barium chloride is added to the solution A, and the mass ratio of sodium sulfate, barium chloride and deionized water is 1:1:20, and stirred at 400 rpm for 30 min to form a mixture;

[0031] (2) The 4A zeolite is repeatedly washed with deionized water, dried in a 70 ℃ oven for 24 h, and then calcined in a muffle furnace, heated to 500 ℃ at a rate of 5 ℃ / min and kept at 500 ℃ for 2 h, to obtain activated 4A zeolite;

[0032] (3) The activated 4A zeolite obtained in step (2) is slowly added to the mixture obtained in step (1), and the mass ratio of the activated 4A zeolite to the mixture is 1:20, and then transferred to a 100 mL polytetrafluoroethylene-lined autoclave, and hydrothermally reacted at 160 ℃ for 24 h, washed with deionized water and anhydrous ethanol alternately for 3 times, and dried in an oven at 70 ℃ for 12 h to obtain a powder material;

[0033] (4) The powder material obtained in step (3) is calcined, heated to 300 ℃ at a rate of 3 ℃ / min and kept at 300 ℃ for 1 h, and then cooled to room temperature to obtain a BaSO4 / 4A zeolite composite material.

[0034] The embodiment also provides a preparation method of the strong-stability crosslinking agent BIPB, and specifically includes the following steps:

[0035] S1, 20 parts of tert-butyl hydroperoxide are weighed into a glass reaction kettle, 40 parts of acetic anhydride are further added to the glass reaction kettle for dehydration reaction, fully stirred, mixed and dispersed, the temperature is 50 ℃, the time is 30 min, and the stirring speed is 300 rpm to obtain a mixed solution;

[0036] S2, 10 parts of a,a'-dihydroxy-1,3-diisopropylbenzene are added to the mixed solution obtained in step S1, stirred at a speed of 200 rpm, and then 10 parts of BaSO4 / 4A zeolite composite material are added, and a condensation reaction is carried out at 50 ℃ for 10 min to obtain a reaction solution;

[0037] S3, 0.1 parts of polypropylene and 0.1 parts of poly-4-methyl-1-pentene are mixed, put into a ball mill for grinding, sieved through a 70-mesh sieve after grinding, added to the reaction solution obtained in step S2, and stirred to obtain a reaction mixture;

[0038] S4, the reaction mixture is washed with water at 45 ℃, then separated by a separatory funnel to obtain an organic layer solution, and then the organic layer solution is washed with a 15% sodium hydroxide aqueous solution at a temperature of 45 ℃, and then separated to obtain an organic phase;

[0039] S5, vacuum flash drying the organic phase obtained in step S4 for 1 h, the temperature of vacuum flash drying is 50 ℃, the pressure is -0.095 MPa, and then cooling and solidifying at room temperature to obtain the strong stability crosslinking agent BIPB.

[0040] Embodiment 2: The embodiment provides a strong stability crosslinking agent BIPB, which is prepared from the following raw materials in parts by weight: 25 parts of t-butyl hydroperoxide, 8 parts of BaSO4 / 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.

[0041] The preparation method of the BaSO4 / 4A zeolite composite material specifically includes the following steps:

[0042] (1) 5 parts of sodium sulfate are dissolved in deionized water to form a solution A, barium chloride is added to the solution A, the mass ratio of sodium sulfate, barium chloride and deionized water is 1:1:20, and stirring is performed at 400 rpm for 30 min to form a mixture;

[0043] (2) The 4A zeolite is repeatedly washed with deionized water, dried in a 70 ℃ oven for 24 h, and then calcined in a muffle furnace, heated to 500 ℃ at a rate of 5 ℃ / min and kept at 500 ℃ for 2 h to obtain activated 4A zeolite;

[0044] (3) The activated 4A zeolite obtained in step (2) is slowly added to the mixture obtained in step (1), and the mass ratio of the activated 4A zeolite to the mixture is 3:20, and then transferred to a 100 mL polytetrafluoroethylene-lined autoclave, hydrothermally reacted at 180 ℃ for 24 h, washed with deionized water and anhydrous ethanol alternately for 3 times, and dried in an oven at 70 ℃ for 12 h to obtain a powder material;

[0045] (4) The powder material obtained in step (3) is calcined, heated to 300 ℃ at a rate of 3 ℃ / min and kept at 300 ℃ for 2 h, and then cooled to room temperature to obtain the BaSO4 / 4A zeolite composite material.

[0046] The embodiment also provides a preparation method of the strong stability crosslinking agent BIPB, which specifically includes the following steps:

[0047] S1, 25 parts of t-butyl hydroperoxide are weighed and added to a glass reaction kettle, 60 parts of acetic anhydride are further added to the glass reaction kettle for dehydration reaction, fully stirred, mixed and dispersed uniformly, the temperature is 40 ℃, the time is 20 min, and the stirring speed is 300 rpm to obtain a mixed solution;

[0048] S2, 15 parts of a,a'-dihydroxy-1,3-diisopropylbenzene were added to the mixed solution obtained in step S1, stirred at a speed of 200 rpm to mix uniformly, then 8 parts of BaSO4 / 4A zeolite composite material was added, and condensation reaction was carried out at 55 ℃, and the reaction time was 20 min, to obtain a reaction liquid;

[0049] S3, 1 part of polypropylene and 1 part of poly-4-methyl-1-pentene were mixed and put into a ball mill for grinding, and after grinding, a 70-mesh sieve was used, and the mixture was added to the reaction liquid obtained in step S2, stirred and mixed uniformly, to obtain a reaction mixture;

[0050] S4, the reaction mixture was washed with water at 45 ℃, then liquid separation was carried out with a separatory funnel, to obtain an organic layer solution, and then the organic layer solution was washed with a 15% sodium hydroxide aqueous solution at a temperature of 45 ℃, and then liquid separation was carried out, to obtain an organic phase;

[0051] S5, the organic phase obtained in step S4 was vacuum flash dried for 1.5-2 h, the vacuum flash drying temperature was 50 ℃, and the pressure was-0.082 MPa, and then the strong stability crosslinking agent BIPB was obtained by cooling and solidifying at room temperature.

[0052] Example 3: The present embodiment provides a strong stability crosslinking agent BIPB, which is prepared from the following raw materials in parts by weight: tert-butyl hydroperoxide 30 parts, BaSO4 / 4A zeolite composite material 5 parts, polypropylene 2 parts, a,a'-dihydroxy-1,3-diisopropylbenzene 20 parts, acetic anhydride 70 parts, and poly-4-methyl-1-pentene 1 part;

[0053] The preparation method of the BaSO4 / 4A zeolite composite material specifically includes the following steps:

[0054] (1) 5 parts of sodium sulfate were dissolved in deionized water to form solution A, barium chloride was added to solution A, and the mass ratio of sodium sulfate, barium chloride and deionized water was 1:1:20, and stirred at 400 rpm for 30 min to form a mixture;

[0055] (2) The 4A zeolite was repeatedly washed with deionized water, dried in a 70 ℃ oven for 24 h, and then calcined in a muffle furnace, heated to 500 ℃ at a rate of 5 ℃ / min at room temperature, and kept at 500 ℃ for 2 h, to obtain activated 4A zeolite;

[0056] (3) The activated 4A zeolite obtained in step (2) is slowly added to the mixture obtained in step (1), and the mass ratio of the activated 4A zeolite to the mixture is 1:5, and then transferred to a 100 mL polytetrafluoroethylene-lined autoclave, and hydrothermally reacted at 200 ℃ for 24 h, washed with deionized water and anhydrous ethanol alternately for 3 times, and dried in an oven at 70 ℃ for 12 h to obtain a powder material;

[0057] (4) The powder material obtained in step (3) is calcined, heated to 300 ℃ at a rate of 3 ℃ / min at room temperature, and kept at 300 ℃ for 3 h, and then cooled to room temperature to obtain a BaSO4 / 4A zeolite composite material.

[0058] The embodiment also provides a preparation method of the strong-stability crosslinking agent BIPB, and specifically comprises the following steps:

[0059] S1, 30 parts of tert-butyl hydroperoxide is weighed and added into a glass reaction kettle, 70 parts of acetic anhydride is further added into the glass reaction kettle for dehydration reaction, fully stirred, mixed and dispersed uniformly, the temperature is 30 ℃, the time is 5 min, and the stirring speed is 300 rpm to obtain a mixed solution;

[0060] S2, 20 parts of a,a'-dihydroxy-1,3-diisopropylbenzene is added into the mixed solution obtained in step S1, stirred and mixed uniformly at a speed of 200 rpm, and then 10 parts of BaSO4 / 4A composite material is added, and a condensation reaction is carried out at 60 ℃, and the reaction time is 30 min to obtain a reaction solution;

[0061] S3, 2 parts of polypropylene and 2 parts of poly-4-methyl-1-pentene are taken, mixed, put into a ball mill for grinding, sieved through a 70-mesh sieve after grinding, added into the reaction solution obtained in step S2, stirred and mixed uniformly to obtain a reaction mixture;

[0062] S4, the reaction mixture is washed with water at 45 ℃, then separated by a separatory funnel to obtain an organic layer solution, and then the organic layer solution is washed with a 15% sodium hydroxide aqueous solution at a temperature of 45 ℃, and then separated to obtain an organic phase;

[0063] S5, the organic phase obtained in step S4 is vacuum flash dried for 2 h, the vacuum flash drying temperature is 50 ℃, and the pressure is 0 MPa, and then cooled and solidified at room temperature to obtain the strong-stability crosslinking agent BIPB.

[0064] The difference between Comparative Example 1 and Example 1 is that the addition of the BaSO4 / 4A zeolite composite material is cancelled, and the rest is the same as that in Example 1.

[0065] The difference between Comparative Example 2 and Example 1 is that acetic anhydride is replaced by toluene, and the rest is the same as Example 1.

[0066] The difference between Comparative Example 3 and Example 1 is that the preparation method of the crosslinking agent BIPB is as follows: tert-butyl hydroperoxide is weighed by weight parts and added into a reaction kettle, diisopropylbenzene is added into the reaction kettle by weight parts to carry out a dehydration reaction, the mixture is fully stirred and dispersed uniformly, the temperature is 30-50 DEG C, and the time is 5-30 min to obtain a mixed solution; nickel bromide powder is added into the obtained mixed solution by weight parts, and the mixture is stirred uniformly to obtain a reaction liquid; the reaction liquid is washed, and then separated by a separatory funnel to obtain an organic layer solution, and the organic layer solution is dried to obtain the crosslinking agent BIPB.

[0067] The strong stability crosslinking agent BIPB prepared by Examples 1-3 and Comparative Examples 1-3 of the application is used to prepare an elastomer-plastic synthetic crosslinking body, and the required raw materials are as follows: natural rubber 80 parts, polyethylene 12 parts, crosslinking agent BIPB 3 parts, and antioxidant 2 parts.

[0068] The preparation method of the elastomer-plastic synthetic crosslinking body is as follows: the natural rubber and the polyethylene are respectively plasticized, the natural rubber is heated to 80 DEG C and kept for 15 h for standby, and the polyethylene is heated to 140 DEG C; the plasticized natural rubber, polyethylene, initiator and antioxidant are added into a banbury mixer and mixed for 10 min, the crosslinking agent is added and mixed for 5 min, then the temperature of the banbury mixer is 95-100 DEG C, and then the mixture is opened, extruded and cut into particles to obtain the elastomer-plastic synthetic crosslinking body.

[0069] The control group is not added with the strong stability crosslinking agent BIPB prepared by the application, and the rest is the same as the preparation method of the elastomer-plastic synthetic crosslinking body.

[0070] Then, the performance of the prepared elastomer-plastic synthetic crosslinking body is tested, and the elastomer-plastic synthetic crosslinking body is divided into Examples 1-3, Comparative Examples 1-3 and the control group.

[0071] Experimental Example 1: The tensile properties of the elastomer-plastic synthetic crosslinking body are tested according to GB / T528-2009, a TCS-2000 type computer system tensile testing machine of China High-speed Rail Testing Instrument Co., Ltd. is used, the test is carried out at a tensile speed of 5 mm / min, Examples 1-3, Comparative Examples 1-3 and the control group are tested, the initial sample is cut from the middle, then the test sample is prepared by natural splicing, the test sample is repaired at 30 DEG C for 20 min, then the tensile test is carried out, the tensile test is carried out for 3 times, the average value of the tensile strength is calculated, and the calculation result is recorded in Table 1.

[0072] Experimental Example 2: The tear strength was tested according to GB-T 529-2008 "Determination of tear strength of vulcanized rubber or thermoplastic rubber", the sample was cut from the test piece by a punch using a cutting tool, the pant-shaped sample, the cut was located at the center of the sample width, the depth was (40±5) mm, the right-angle shaped sample, the cut depth was (1.0±0.2) mm, the crescent-shaped sample, the cut depth was (1.0±0.2) mm, located at the center of the concave inner edge of the sample, the sample cut, measurement and test were continuously carried out. The sample was installed on a tensile testing machine, and stretched at the following moving speed of the clamps: (500±50) mm / min for the right-angle and crescent-shaped samples, and (100±10) mm / min for the pant-shaped sample, until the sample was broken. The maximum force value of the right-angle and crescent-shaped samples was recorded. When the pant-shaped sample was used, the force value of the entire tearing process should be automatically recorded. The tear strength was calculated according to the formula Ta=F / d, wherein, in the formula, Ta is the tear strength, the unit is kilonewton per meter (KN / m), F is the force required when the sample is torn, the unit is newton (N), and d is the median of the thickness of the sample, the unit is millimeter (mm), and the results are recorded in Table 1.

[0073] Experimental Example 3: The Shore A hardness was tested according to GB / T 2411-2008, the sample was placed on a hard, solid horizontal plane, the hardness tester was held in a vertical position, the tip of the pressure needle was 10 mm away from the edge of the sample, the pressure seat was immediately applied to the sample without impact, the pressure seat was parallel to the sample and sufficient pressure was applied, the pressure seat was in close contact with the sample, the value indicated by the indicating device was read after 15 s, 5 hardness values were measured on the same sample with a distance of 6 mm, and the average value was calculated, and the calculated hardness average value was recorded in Table 1.

[0074] Table 1

[0075]

[0076] The results in Table 1 show that the tensile strength, tear strength and Shore hardness of Examples 1-3 are higher than those of the control group and Comparative Examples 1-3, indicating that the rubber-plastic synthetic cross-linked body added with the strong stability cross-linking agent BIPB prepared in the application increases the mechanical properties and mechanical properties, indicating that the cross-linking agent BIPB prepared in the application can significantly improve the performance of the rubber,

[0077] Figure 1 The purity of the cross-linking agent BIPB prepared in the application is 99.28%, indicating that the addition of BaSO4 / 4A zeolite composite material in the application increases the purity of the cross-linking agent BIPB, indicating that the impurities in the target product are less during the preparation process, so that the purity is higher, Figure 2The yield of the crosslinking agent BIPB prepared by the present application reaches 93.26%, which shows that the crosslinking agent BIPB prepared by the present application has less by-products, thereby keeping the yield of the crosslinking agent BIPB at a high level, Figure 3 The anti-aging performance of the crosslinking agent BIPB prepared by the present application over time is shown, and it can be obviously seen that the crosslinking agent BIPB prepared by the present application still has an anti-aging performance of more than 90% after being placed for one week, which shows that the BaSO4 / 4A zeolite composite material added can strengthen the stability of the crosslinking agent BIPB, and make the practicability good in various cases.

[0078] In summary, by introducing the BaSO4 / 4A zeolite composite material into the crosslinking agent BIPB, the stability of the crosslinking agent is significantly improved, the crosslinking efficiency is improved, the same crosslinking effect can be achieved with a smaller amount of addition, and the mechanical performance of the rubber-plastic combined body synthesized by using the crosslinking agent BIPB prepared by the present application is significantly increased, and the stability at high temperature is enhanced. By adding the BaSO4 / 4A zeolite composite material, the performance of the crosslinking agent BIPB is significantly improved, thereby enabling the crosslinking agent BIPB prepared by the present application to be widely applied to more fields such as rubber, plastic, wire and cable, etc.

[0079] The above description is only the preferred embodiment of the present application, and does not limit the other forms of the present application. Any person skilled in the art can modify or change the above disclosed technical content to equivalent embodiments applied to other fields, but any simple modification, equivalent change and modification made according to the technical essence of the present application to the above embodiments still belongs to the protection scope of the technical solution of the present application.

Claims

1. A strong stability crosslinking agent BIPB, characterized in that, The strong stability crosslinking agent BIPB is prepared from the following raw materials by weight: t-butyl hydroperoxide 20-30 parts, BaSO4 / 4A zeolite composite 5-10 parts, polypropylene 0.1-2 parts, a,a'-dihydroxy-1,3-diisopropylbenzene 10-20 parts, acetic anhydride 40-70 parts, and poly-4-methyl-1-pentene 0.1-2 parts; The preparation raw materials of the BaSO4 / 4A zeolite composite are sodium sulfate, barium chloride and 4A zeolite; The preparation method of the BaSO4 / 4A zeolite composite specifically includes the following steps: (1) Dissolve sodium sulfate in deionized water to form solution A, add barium chloride to solution A, and stir to form a mixture; (2) Rinse 4A zeolite repeatedly with deionized water, dry, and then calcine to obtain activated 4A zeolite; (3) Slowly add the activated 4A zeolite obtained in step (2) to the mixture obtained in step (1), then perform a hydrothermal reaction, wash, and dry to obtain a powder material; (4) Calcine the powder material obtained in step (3), and then cool to room temperature to obtain the BaSO4 / 4A zeolite composite; The preparation method of the strong stability crosslinking agent BIPB specifically includes the following steps: S1, weigh t-butyl hydroperoxide and acetic anhydride by weight parts, add t-butyl hydroperoxide to acetic anhydride, perform a dehydration reaction, and fully stir and mix to obtain a mixed solution; S2, add a,a'-dihydroxy-1,3-diisopropylbenzene to the mixed solution obtained in step S1 according to the weight parts, stir to mix, then add BaSO4 / 4A zeolite composite according to the weight parts, perform a condensation reaction, and obtain a reaction liquid; S3, take polypropylene and poly-4-methyl-1-pentene by weight parts, mix them, grind, and add to the reaction liquid obtained in step S2, stir to mix, and obtain a reaction mixture; S4, wash the reaction mixture, then perform liquid separation to obtain an organic layer solution, continue to wash the organic layer solution, then perform liquid separation to obtain an organic phase; S5, vacuum flash dry the organic phase obtained in step S4, then cool and solidify at room temperature to obtain the strong stability crosslinking agent BIPB.

2. The crosslinking agent BIPB of claim 1, wherein, In step (1), the mass ratio of sodium sulfate, barium chloride and deionized water is 1:1:

20.

3. The crosslinking agent BIPB of claim 1, wherein, In step (3), the mass ratio of activated 4A zeolite to the mixture is 1-4:

20.

4. The crosslinking agent BIPB of claim 1, wherein, In step (3), the temperature of the hydrothermal reaction is set to 160-200 ℃, and the time is set to 24 h.

5. The crosslinking agent BIPB of claim 1, wherein, In step S2, the temperature of the condensation reaction is 50-60 ℃, and the reaction time is 10-30 min.

6. The crosslinking agent BIPB of claim 1, wherein, In step S5, the conditions of the vacuum flash are set to a temperature of 50 ℃, a pressure of -0.095-0 MPa, and a time of 1-2 h.

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