Ionic liquid modified nano calcium carbonate / dipropyl aluminum hypophosphite flame-retardant nylon material

Abstract

The invention discloses an ionic liquid modified nano calcium carbonate / dipropyl aluminum hypophosphite flame-retardant nylon material, and relates to the technical field of flame-retardant materials, the ionic liquid modified nano calcium carbonate / dipropyl aluminum hypophosphite flame-retardant nylon material comprises, by weight, 68-85 parts of nylon 6 slices, 0.1-0.5 part of an antioxidant, 0.2-1 part of a lubricant, 10-25 parts of dipropyl aluminum hypophosphite, and 5-10 parts of ionic liquid modified nano calcium carbonate; wherein the ionic liquid modified nano calcium carbonate is obtained by mixing, dispersing and drying nano calcium carbonate and ionic liquid; the ionic liquid is prepared from 1-methyl-1H-imidazole, decane chloride and NaBF4 (NaBF4). The environment-friendly flame-retardant cable material has the effects of environment friendliness, efficient flame retardance and low cost.

Description

Technical Field

[0001] The present application relates to the technical field of flame retardant materials, and in particular to an ionic liquid modified nano calcium carbonate / dipropyl aluminum hypophosphite flame retardant nylon material. Background Art

[0002] Nylon (PA) is a thermoplastic engineering plastic containing an amide bond (-NHCO-) ​​in the main chain of the molecule. Due to its advantages such as heat resistance, wear resistance, chemical resistance and self-lubrication, it is widely used in the automotive industry, electronic appliances, synthetic fibers, construction and other fields. It is one of the engineering plastics with the largest output and the widest application range in the world today. PA mainly includes PA6, PA66, PA610, PA1010, PA11, etc. Among them, PA6 and PA66 are the most widely used nylon products. Nylon 6 chips are also called nylon 6 chips. They are the second largest chemical fiber of synthetic fibers and occupy an important position in industrial use. In the preparation process of nylon materials, in order to ensure that the materials have flame retardancy, halogen flame retardants are usually added to the raw materials. However, the existing halogen flame retardants are easy to harm the environment during use and are not conducive to environmental protection. Therefore, they are gradually replaced by halogen-free flame retardants.

[0003] Halogen-free flame retardants mainly include: inorganic flame retardants, phosphorus flame retardants, silicon flame retardants and phosphorus nitrogen flame retardants, etc. These flame retardants have their own advantages and disadvantages, so it is crucial to develop new material performance and avoid material defects.

[0004] Although various flame retardants are gradually being developed on the market, there are still problems such as high prices and difficult processing, which need to be improved. Summary of the invention

[0005] In view of this, the purpose of this application is to provide an ionic liquid modified nano calcium carbonate / dipropyl aluminum hypophosphite flame retardant nylon material to achieve the purpose of green environmental protection, high efficiency flame retardancy and low cost. The specific scheme is as follows:

[0006] An ionic liquid modified nano calcium carbonate / dipropyl aluminum hypophosphite flame retardant nylon material comprises 68-85 parts by weight of nylon 6 slices, 0.1-0.5 parts of an antioxidant, 0.2-1 parts of a lubricant, 10-25 parts of dipropyl aluminum hypophosphite, and 5-10 parts of ionic liquid modified nano calcium carbonate; wherein the ionic liquid modified nano calcium carbonate is obtained by mixing nano calcium carbonate and ionic liquid, dispersing and drying; and the ionic liquid is prepared from 1-methyl-1H-imidazole, decane chloride and NaBF4.

[0007] Preferably, the particle size of the nano calcium carbonate is 80-100 nm.

[0008] Preferably, the relative viscosity of the nylon 6 chips is 2.4-2.8.

[0009] Preferably: the antioxidant is at least one of a phosphite auxiliary antioxidant and a hindered phenol main antioxidant; the hindered phenol main antioxidant is 1076 antioxidant, 1098 antioxidant or 1010 antioxidant, and the phosphite auxiliary antioxidant is specifically 168 antioxidant or 619F antioxidant.

[0010] Preferably, the antioxidant is 168 antioxidant and 1098 antioxidant in a mass ratio of 2:1.

[0011] Preferably: the lubricant is pentaerythritol stearate; the dipropyl aluminum hypophosphite is purchased from Shanghai MacLean Biochemical Technology Co., Ltd.

[0012] The second object of the present invention is to provide a method for preparing the ionic liquid modified nano calcium carbonate / dipropyl aluminum hypophosphite flame retardant nylon material as described above, comprising the following steps:

[0013] Step 1, raw material preparation: weigh nylon 6 chips, antioxidant, lubricant, dipropyl aluminum hypophosphite and ionic liquid modified nano calcium carbonate according to weight;

[0014] Step 2, mixing treatment: put the raw materials into a mixer for mixing, control the stirring time to 8-15min, and the speed to 8-20Hz to obtain a premixed material;

[0015] Step 3, extrusion granulation: the premixed material is put into an extruder, and after melting, extrusion and granulation, a composite flame-retardant nylon material is obtained.

[0016] Preferably, in step 1, the nylon 6 chips are placed in a drying oven at 90-100° C. for drying, and the moisture content of the nylon 6 chips is controlled to be less than 0.02%.

[0017] Preferably: the preparation of the ionic liquid modified nano calcium carbonate includes an ionic liquid preparation part and a modification preparation part;

[0018] The ionic liquid preparation part includes the steps of ① weighing 10g of 1-methyl-1H-imidazole and placing it in a 100mL round-bottom flask, then slowly dropping 22g of decane chloride into the flask, wherein the flask is placed in a water bath, and the temperature of the water bath is controlled to be 45-55°C, until the liquid in the flask becomes clear and bright, then washing with polyethylene glycol ester, and taking the lower layer of liquid for standby use; step ② weighing 20g of the lower layer of liquid and 10g of NaBF4 into the flask, and adding reaction medium acetone for reaction treatment, wherein the flask is placed in a water bath, and the temperature of the water bath is controlled to be 55-60°C, and after the reaction is completed, the reaction liquid is vacuum filtered and dried to obtain the ionic liquid;

[0019] The modification preparation part comprises the steps of ① weighing 45g of nano calcium carbonate and placing it in a beaker, adding 40-50g of anhydrous ethanol to the beaker to obtain a suspension, placing the suspension in a warm water bath at 50-70°C and stirring for 10-15 minutes, and ultrasonically dispersing for 0.5h to obtain a dispersion; ② keeping the dispersion in the warm water bath and dropping 9g of ionic liquid, and continuing to stir for 30min and ultrasonically disperse for 30min in sequence after the dropping is completed to obtain an ultrasonic suspension; ③ placing the ultrasonic suspension in a drying oven for drying treatment, controlling the temperature of the drying oven to 60-70°C, and obtaining a dry crude product; and ④ grinding and sieving the dry crude product to obtain nano calcium carbonate modified by the ionic liquid, wherein a 200-mesh screen is used for sieving.

[0020] Preferably: in step 3, the screw speed of the extruder is 450 rpm, the screw aspect ratio is 44:1, the temperature of processing zone 1 is 205°C, the temperature of zone 2 is 210°C, the temperature of zone 3 is 215°C, the temperature of zone 4 is 220°C, the temperature of zone 5 is 225°C, the temperature of zone 6 is 225°C, the temperature of zone 7 is 230°C, the temperature of zone 8 is 225°C, the temperature of zone 9 is 220°C, the temperature of the die is 245°C, and a vacuum pump is used for extraction in the front zone of the die to control the vacuum pressure to be lower than 0.03MPa.

[0021] It can be seen from the above scheme that the present application provides an ionic liquid modified nano calcium carbonate / dipropyl aluminum hypophosphite flame retardant nylon material, and the ionic liquid modified nano calcium carbonate / dipropyl aluminum hypophosphite flame retardant nylon material has the following beneficial effects:

[0022] 1. Dipropyl aluminum hypophosphite decomposes to form non-volatile aluminum phosphate and promotes the carbonization of PA6, thereby forming an expansion layer and producing a flame retardant effect. At the same time, it decomposes to form volatile phosphides, which capture the free radicals generated by combustion in the gas phase to achieve the effect of inhibiting combustion;

[0023] 2. Nano flame retardants can effectively reduce the amount of smoke while improving the flame retardant effect, thereby improving environmental friendliness. Ionic liquids are mixed with nano calcium carbonate for modification, so that the obtained ionic liquid modified nano calcium carbonate will rapidly undergo thermal decomposition when stimulated by a heat source, and release carbon dioxide and water vapor, thereby effectively diluting oxygen to reduce the combustion reaction rate and the spread of the fire. At the same time, its decomposition products will form a coke substance on the surface of the material, thereby further reducing the combustion reaction rate by wrapping the surface of the material, thereby effectively improving the flame retardant properties of the material;

[0024] 3. By combining low-cost dipropyl aluminum hypophosphite with ionic liquid modified nano calcium carbonate, the flame retardancy of nylon 6 material can be effectively improved by synergizing with each other while effectively controlling the production cost, so that the ionic liquid modified nano calcium carbonate / dipropyl aluminum hypophosphite flame retardant nylon material has the effects of green environmental protection, high efficiency flame retardancy and low cost. DETAILED DESCRIPTION

[0025] The following will be clearly and completely described in conjunction with the technical solutions in the embodiments of the present application. Obviously, the described embodiments are only part of the embodiments of the present application, not all of the embodiments. Based on the embodiments in the present application, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of this application.

[0026] The ionic liquid modified nano calcium carbonate / dipropyl aluminum hypophosphite flame retardant nylon material of the present application will be specifically described below.

[0027] An ionic liquid modified nano calcium carbonate / dipropyl aluminum hypophosphite flame retardant nylon material comprises 68-85 parts by weight of nylon 6 slices, 0.1-0.5 parts of antioxidants, 0.2-1 parts of lubricants, 10-25 parts of dipropyl aluminum hypophosphites, and 5-10 parts of ionic liquid modified nano calcium carbonate; wherein the ionic liquid modified nano calcium carbonate is obtained by mixing, dispersing and drying nano calcium carbonate and ionic liquid. The ionic liquid is prepared from 1-methyl-1H-imidazole, decane chloride and NaBF4. The particle size of the nano calcium carbonate is 80-100 nm. The relative viscosity of the nylon 6 slices is 2.4-2.8. The antioxidant is at least one of a phosphite auxiliary antioxidant and a hindered phenol main antioxidant; the hindered phenol main antioxidant is 1076 antioxidant, 1098 antioxidant or 1010 antioxidant, and the phosphite auxiliary antioxidant is specifically 168 antioxidant or 619F antioxidant. In the embodiment of the present application, the lubricant is pentaerythritol stearate, and dipropyl aluminum hypophosphite is purchased from Shanghai McLean Biochemical Technology Co., Ltd. Of course, the type of lubricant is not specifically limited, and it will not be repeated here. The purchase source of dipropyl aluminum hypophosphite is not specifically limited, and it will not be repeated here.

[0028] A method for preparing an ionic liquid modified nano calcium carbonate / dipropyl aluminum hypophosphite flame retardant nylon material comprises the following steps:

[0029] Step 1, raw material preparation: weigh nylon 6 chips, antioxidant, lubricant, dipropyl aluminum hypophosphite and ionic liquid modified nano calcium carbonate according to weight;

[0030] Step 2, mixing treatment: put the raw materials into a mixer for mixing, control the stirring time to 8-15min, and the speed to 8-20Hz to obtain a premixed material;

[0031] Step 3, extrusion granulation: the premixed material is put into an extruder, and after melting, extrusion and granulation, a composite flame-retardant nylon material is obtained.

[0032] Among them, the moisture content of nylon 6 slices is controlled to be lower than 0.02%. And in the embodiment of the present application, the moisture content of nylon 6 slices is controlled by putting nylon 6 slices into a drying oven at 90-100°C for drying. In the parameter setting of the extruder, the screw speed of the extruder in the embodiment of the present application is 450rpm, the screw aspect ratio is 44:1, the processing zone 1 temperature is 205°C, the zone 2 temperature is 210°C, the zone 3 temperature is 215°C, the zone 4 temperature is 220°C, the zone 5 temperature is 225°C, the zone 6 temperature is 225°C, the zone 7 temperature is 230°C, the zone 8 temperature is 225°C, the zone 9 temperature is 220°C, the head temperature is 245°C, and a vacuum pump is used in the front zone of the head for extraction, and the vacuum pressure is controlled to be lower than 0.03MPa.

[0033] At the same time, in order to obtain ionic liquid-modified nano-calcium carbonate, the preparation of ionic liquid-modified nano-calcium carbonate in the embodiments of the present application includes an ionic liquid preparation part and a modification preparation part.

[0034] The ionic liquid preparation part includes the steps of ① weighing 10g of 1-methyl-1H-imidazole and placing it in a 100mL round-bottom flask, and then slowly dropping 22g of decane chloride into the flask, wherein the flask is placed in a water bath, and the temperature of the water bath is controlled to be 45-55°C, until the liquid in the flask becomes clear and bright, and then washing with polyethylene glycol ester, and taking the lower layer of liquid for standby use; step ② weighing 20g of the lower layer of liquid and 10g of NaBF4 into the flask, and adding the reaction medium acetone for reaction treatment, wherein the flask is placed in a water bath, and the temperature of the water bath is controlled to be 55-60°C, and after the reaction is completed, the reaction liquid is vacuum filtered and dried to obtain the ionic liquid;

[0035] The modification preparation part comprises the steps of ① weighing 45g of nano calcium carbonate and placing it in a beaker, adding 40-50g of anhydrous ethanol to the beaker to obtain a suspension, placing the suspension in a warm water bath at 50-70°C and stirring for 10-15 minutes, and ultrasonically dispersing for 0.5h to obtain a dispersion; ② keeping the dispersion in the warm water bath and dripping 9g of ionic liquid, and continuing to stir for 30min and ultrasonically disperse for 30min in sequence after the dripping is completed to obtain an ultrasonic suspension; ③ placing the ultrasonic suspension in a drying oven for drying treatment, controlling the temperature of the drying oven to 60-70°C, and obtaining a dry crude product; and ④ grinding and sieving the dry crude product to obtain nano calcium carbonate modified by the ionic liquid, wherein a 200-mesh screen is used for sieving.

[0036] Embodiment 1

[0037] An ionic liquid modified nano calcium carbonate / dipropyl aluminum hypophosphite flame retardant nylon material comprises 74.2 parts by weight of nylon 6 slices, 0.3 parts of antioxidants, 0.5 parts of lubricants, 20 parts of dipropyl aluminum hypophosphites, and 5 parts of ionic liquid modified nano calcium carbonate. The ionic liquid modified nano calcium carbonate is obtained by mixing, dispersing and drying nano calcium carbonate and ionic liquid. The ionic liquid is prepared from 1-methyl-1H-imidazole, decane chloride and NaBF4. The particle size of the nano calcium carbonate is 80-100nm. The relative viscosity of the nylon 6 slice is 2.4-2.8. The antioxidant is 0.1 parts of 1098 antioxidants and 0.2 parts of 168 antioxidants. In the embodiment of the present application, the lubricant is pentaerythritol stearate, and the dipropyl aluminum hypophosphite is purchased from Shanghai McLean Biochemical Technology Co., Ltd.

[0038] A method for preparing an ionic liquid modified nano calcium carbonate / dipropyl aluminum hypophosphite flame retardant nylon material comprises the following steps:

[0039] Step 1, raw material preparation: weigh nylon 6 chips, antioxidant, lubricant, dipropyl aluminum hypophosphite and ionic liquid modified nano calcium carbonate according to weight;

[0040] Step 2, mixing treatment: putting the raw materials into a mixer for mixing, controlling the stirring time to 8 minutes and the rotation speed to 20 Hz to obtain a premixed material;

[0041] Step 3, extrusion granulation: the premixed material is put into an extruder, and after melting, extrusion and granulation, a composite flame-retardant nylon material is obtained.

[0042] Among them, the moisture content of nylon 6 slices is controlled to be lower than 0.02 parts. And in the embodiment of the present application, the moisture content of nylon 6 slices is controlled by putting nylon 6 slices into a drying oven at 90°C for drying. In the parameter setting of the extruder, the screw speed of the extruder in the embodiment of the present application is 450rpm, the screw aspect ratio is 44:1, the processing zone 1 temperature is 205°C, the zone 2 temperature is 210°C, the zone 3 temperature is 215°C, the zone 4 temperature is 220°C, the zone 5 temperature is 225°C, the zone 6 temperature is 225°C, the zone 7 temperature is 230°C, the zone 8 temperature is 225°C, the zone 9 temperature is 220°C, the head temperature is 245°C, and a vacuum pump is used in the front zone of the head for extraction, and the vacuum pressure is controlled to be lower than 0.03MPa.

[0043] At the same time, in order to obtain ionic liquid-modified nano-calcium carbonate, the preparation of ionic liquid-modified nano-calcium carbonate in the embodiments of the present application includes an ionic liquid preparation part and a modification preparation part.

[0044] The ionic liquid preparation part includes the steps of ① weighing 10g of 1-methyl-1H-imidazole and placing it in a 100mL round-bottom flask, then slowly dropping 22g of decane chloride into the flask, wherein the flask is placed in a water bath, and the temperature of the water bath is controlled to be 45°C, until the liquid in the flask becomes clear and bright, then washing with polyethylene glycol ester, and taking the lower layer of liquid for standby use; step ② weighing 20g of the lower layer of liquid and 10g of NaBF4 into the flask, and adding the reaction medium acetone for reaction treatment, wherein the flask is placed in a water bath, and the temperature of the water bath is controlled to be 55°C, and after the reaction is completed, the reaction liquid is vacuum filtered and dried to obtain the ionic liquid;

[0045] The modification preparation part comprises the steps of ① weighing 45g of nano calcium carbonate and placing it in a beaker, adding 40g of anhydrous ethanol to the beaker to obtain a suspension, placing the suspension in a warm water bath at 50°C and stirring for 10 minutes, and obtaining a dispersion after ultrasonic dispersion for 0.5h; ② keeping the dispersion in the warm water bath and dropping 9g of ionic liquid, and continuing to stir for 30min and ultrasonic dispersion for 30min in sequence after the dropping is completed, to obtain an ultrasonic suspension; ③ placing the ultrasonic suspension in a drying oven for drying treatment, controlling the temperature of the drying oven to 60°C, to obtain a dry crude product; and ④ grinding and sieving the dry crude product to obtain nano calcium carbonate modified by the ionic liquid, wherein a 200-mesh screen is used for sieving.

[0046] Embodiment 2

[0047] The difference between Example 2 and Example 1 is that the ionic liquid modified nano calcium carbonate / dipropyl aluminum hypophosphite flame retardant nylon material in Example 2 includes 74.2 parts by weight of nylon 6 chips, 0.2 parts of antioxidant 168, 0.1 parts of antioxidant 1098, 0.5 parts of lubricant PETS, 17 parts of dipropyl aluminum hypophosphite and 8 parts of ionic liquid modified nano calcium carbonate.

[0048] Embodiment 3

[0049] The difference between Example 3 and Example 1 is that the ionic liquid modified nano calcium carbonate / dipropyl aluminum hypophosphite flame retardant nylon material in Example 3 includes 74.2 parts by weight of nylon 6 chips, 0.2 parts of antioxidant 168, 0.1 parts of antioxidant 1098, 0.5 parts of lubricant PETS, 15 parts of dipropyl aluminum hypophosphite and 10 parts of ionic liquid modified nano calcium carbonate.

[0050] Embodiment 4

[0051] The difference between Example 4 and Example 1 is that the ionic liquid modified nano calcium carbonate / dipropyl aluminum hypophosphite flame retardant nylon material in Example 4 includes 69.2 parts of nylon 6 chips, 0.2 parts of antioxidant 168, 0.1 parts of antioxidant 1098, 0.5 parts of lubricant PETS, 25 parts of dipropyl aluminum hypophosphite and 5 parts of ionic liquid modified nano calcium carbonate.

[0052] Embodiment 5

[0053] The difference between Example 5 and Example 1 is that the ionic liquid modified nano calcium carbonate / dipropyl aluminum hypophosphite flame retardant nylon material in Example 5 includes 69.2 parts of nylon 6 chips, 0.2 parts of antioxidant 168, 0.1 parts of antioxidant 1098, 0.5 parts of lubricant PETS, 22 parts of dipropyl aluminum hypophosphite and 8 parts of ionic liquid modified nano calcium carbonate.

[0054] Embodiment 6

[0055] The difference between Example 6 and Example 1 is that the ionic liquid modified nano calcium carbonate / dipropyl aluminum hypophosphite flame retardant nylon material in Example 6 includes 69.2 parts of nylon 6 chips, 0.2 parts of antioxidant 168, 0.1 parts of antioxidant 1098, 0.5 parts of lubricant PETS, 20 parts of dipropyl aluminum hypophosphite and 10 parts of ionic liquid modified nano calcium carbonate.

[0056] Comparative Example 1

[0057] The difference between Comparative Example 1 and Example 1 is that the ionic liquid modified nano calcium carbonate / dipropyl aluminum hypophosphite flame retardant nylon material in Comparative Example 1 includes 74.2 parts by weight of nylon 6 chips, 0.2 parts of antioxidant 168, 0.1 parts of antioxidant 1098, 0.5 parts of lubricant PETS and 25 parts of dipropyl aluminum hypophosphite.

[0058] Comparative Example 2

[0059] The difference between Comparative Example 2 and Example 1 is that the ionic liquid modified nano calcium carbonate / dipropyl aluminum hypophosphite flame retardant nylon material in Comparative Example 2 includes 69.2 parts of nylon 6 chips, 0.2 parts of antioxidant 168, 0.1 parts of antioxidant 1098, 0.5 parts of lubricant PETS, and 30 parts of dipropyl aluminum hypophosphite.

[0060] Comparative Example 3

[0061] The difference between Comparative Example 3 and Example 1 is that the ionic liquid modified nano calcium carbonate / dipropyl aluminum hypophosphite flame retardant nylon material in Comparative Example 3 includes 69.2 parts of nylon 6 chips, 0.2 parts of antioxidant 168, 0.1 parts of antioxidant 1098, 0.5 parts of lubricant PETS, 20 parts of dipropyl aluminum hypophosphite and 5 parts of nano calcium carbonate in parts by weight.

[0062] Performance Test:

[0063] Performance tests were conducted on the above embodiments 1 to 6 and comparative examples 1 to 3, and the test results are shown in Table 1 below.

[0064] Table 1 Performance test results

[0065]

[0066] It can be seen from Table 1 above that the ionic liquid modified nano calcium carbonate / dipropyl aluminum hypophosphite composite flame retardant nylon material of the present application achieves the purpose of effective flame retardancy and excellent mechanical properties while effectively controlling costs when mixed with nylon 6 chips by combining dipropyl aluminum hypophosphite and ionic liquid modified nano calcium carbonate, and obtains the optimal ratio as shown in Example 5.

[0067] In summary, the present application provides an ionic liquid modified nano calcium carbonate / dipropyl aluminum hypophosphite flame retardant nylon material, which first decomposes dipropyl aluminum hypophosphite to form non-volatile aluminum phosphate and promotes PA6 carbonization, thereby forming an expansion layer and producing a flame retardant effect, and decomposes to form volatile phosphides, and achieves the effect of inhibiting combustion by capturing free radicals generated by combustion in the gas phase. Secondly, the nano flame retardant is used to effectively reduce the smoke volume while improving the flame retardant effect, thereby improving environmental friendliness, and the ionic liquid is mixed with the nano calcium carbonate for modification, so that the ionic liquid modified nano calcium carbonate obtained is rapidly thermally decomposed when stimulated by a heat source, and releases carbon dioxide and water vapor, thereby effectively diluting oxygen to reduce the combustion reaction rate and reduce the degree of spread of the fire, and its decomposition product will form a coke substance on the surface of the material, thereby further reducing the speed of the combustion reaction by wrapping the surface of the material, thereby effectively improving the flame retardant properties of the material. Therefore, the ionic liquid modified nano calcium carbonate / dipropyl aluminum hypophosphite flame retardant nylon material combines low-cost dipropyl aluminum hypophosphite with ionic liquid modified nano calcium carbonate, thereby effectively controlling the production cost while synergizing with each other to effectively improve the flame retardancy of nylon 6 material, so that the ionic liquid modified nano calcium carbonate / dipropyl aluminum hypophosphite flame retardant nylon material has the effects of green environmental protection, high efficiency flame retardancy and low cost.

[0068] The "first", "second", "third", "fourth", etc. (if any) referred to in this application are used to distinguish similar objects, and are not necessarily used to describe a specific order or sequence. It should be understood that the data used in this way can be interchangeable where appropriate, so that the embodiments described herein can be implemented in an order other than that described herein. In addition, the terms "including" and "having" and any variations thereof are intended to cover non-exclusive inclusions, for example, a process, method or device comprising a series of steps or units is not necessarily limited to those steps or units clearly listed, but may include other steps or units that are not clearly listed or inherent to these processes, methods or devices.

[0069] It should be noted that the descriptions involving "first", "second", etc. in this application are only for descriptive purposes and cannot be understood as indicating or implying their relative importance or implicitly indicating the number of technical features indicated. Therefore, the features defined as "first" and "second" may explicitly or implicitly include at least one of the features. In addition, the technical solutions between the various embodiments can be combined with each other, but they must be based on the ability of ordinary technicians in this field to implement them. When the combination of technical solutions is contradictory or cannot be implemented, it should be deemed that such combination of technical solutions does not exist and is not within the scope of protection required by this application.

[0070] Specific examples are used herein to illustrate the principles and implementation methods of the present application. The description of the above embodiments is only used to help understand the method of the present application and its core idea. At the same time, for those skilled in the art, according to the idea of ​​the present application, there will be changes in the specific implementation methods and application scope. In summary, the content of this specification should not be understood as a limitation on the present application.

Claims

1. An ionic liquid modified nano calcium carbonate / dipropyl aluminum hypophosphite flame retardant nylon material, characterized in that: The invention comprises 68-85 parts by weight of nylon 6 chips, 0.1-0.5 parts of antioxidants, 0.2-1 parts of lubricants, 10-25 parts of dipropyl aluminum hypophosphite, and 5-10 parts of ionic liquid modified nano calcium carbonate; wherein the ionic liquid modified nano calcium carbonate is obtained by mixing nano calcium carbonate and ionic liquid, dispersing and drying; and the ionic liquid is prepared from 1-methyl-1H-imidazole, decane chloride and NaBF4.

2. The ionic liquid modified nano calcium carbonate / dipropyl aluminum hypophosphite flame retardant nylon material according to claim 1, characterized in that: The particle size of the nano calcium carbonate is 80-100 nm.

3. The ionic liquid modified nano calcium carbonate / dipropyl aluminum hypophosphite flame retardant nylon material according to claim 1, characterized in that: The relative viscosity of the nylon 6 chips is 2.4-2.

8.

4. The ionic liquid modified nano calcium carbonate / dipropyl aluminum hypophosphite flame retardant nylon material according to claim 1, characterized in that: The antioxidant is at least one of a phosphite auxiliary antioxidant and a hindered phenol main antioxidant; the hindered phenol main antioxidant is 1076 antioxidant, 1098 antioxidant or 1010 antioxidant, and the phosphite auxiliary antioxidant is specifically 168 antioxidant or 619F antioxidant.

5. The ionic liquid modified nano calcium carbonate / dipropyl aluminum hypophosphite flame retardant nylon material according to claim 4, characterized in that: The antioxidants are 168 antioxidant and 1098 antioxidant in a mass ratio of 2:

1.

6. The ionic liquid modified nano calcium carbonate / dipropyl aluminum hypophosphite flame retardant nylon material according to claim 1, characterized in that: The lubricant is pentaerythritol stearate; the dipropyl aluminum hypophosphite is purchased from Shanghai MacLean Biochemical Technology Co., Ltd.

7. A method for preparing the ionic liquid modified nano calcium carbonate / dipropyl aluminum hypophosphite flame retardant nylon material according to any one of claims 1 to 6, characterized in that: The steps include: Step 1, raw material preparation: weigh nylon 6 chips, antioxidant, lubricant, dipropyl aluminum hypophosphite and ionic liquid modified nano calcium carbonate according to weight; Step 2, mixing treatment: put the raw materials into a mixer for mixing, control the stirring time to 8-15min, and the speed to 8-20Hz to obtain a premixed material; Step 3, extrusion granulation: the premixed material is put into an extruder, and after melting, extrusion and granulation, a composite flame-retardant nylon material is obtained.

8. The method for preparing the ionic liquid modified nano calcium carbonate / dipropyl aluminum hypophosphite flame retardant nylon material according to claim 7, characterized in that: In step 1, the nylon 6 chips are placed in a drying oven at 90-100° C. for drying, and the moisture content of the nylon 6 chips is controlled to be less than 0.02%.

9. The method for preparing the ionic liquid modified nano calcium carbonate / dipropyl aluminum hypophosphite flame retardant nylon material according to claim 7, characterized in that: The preparation of the ionic liquid modified nano calcium carbonate includes an ionic liquid preparation part and a modification preparation part; The ionic liquid preparation part includes the steps of ① weighing 10g of 1-methyl-1H-imidazole and placing it in a 100mL round-bottom flask, then slowly dropping 22g of decane chloride into the flask, wherein the flask is placed in a water bath, and the temperature of the water bath is controlled to be 45-55°C, until the liquid in the flask becomes clear and bright, then washing with polyethylene glycol ester, and taking the lower layer of liquid for standby use; step ② weighing 20g of the lower layer of liquid and 10g of NaBF4 into the flask, and adding reaction medium acetone for reaction treatment, wherein the flask is placed in a water bath, and the temperature of the water bath is controlled to be 55-60°C, and after the reaction is completed, the reaction liquid is vacuum filtered and dried to obtain the ionic liquid; The modification preparation part includes the steps of ① weighing 45g of nano calcium carbonate and placing it in a beaker, and adding 40-50g of anhydrous ethanol to the beaker to obtain a suspension, placing the suspension in a warm water bath at 50-70°C and stirring for 10-15 minutes, and ultrasonically dispersing for 0.5h to obtain a dispersion; ② keeping the dispersion in the warm water bath and adding 9g of ionic liquid dropwise, and continuing to stir for 30min and ultrasonically disperse for 30min after the addition is completed, to obtain an ultrasonic suspension; Step ③: placing the ultrasonic suspension in a drying oven for drying, controlling the temperature of the drying oven to 60-70° C., and obtaining a dry crude product; Step ④: grinding and sieving the dry crude product to obtain ionic liquid-modified nano-calcium carbonate, wherein a 200-mesh screen is used for sieving.

10. The method for preparing the ionic liquid modified nano calcium carbonate / dipropyl aluminum hypophosphite flame retardant nylon material according to claim 7, characterized in that: In step 3, the screw speed of the extruder is 450 rpm, the screw aspect ratio is 44:1, the temperature of processing zone 1 is 205°C, the temperature of zone 2 is 210°C, the temperature of zone 3 is 215°C, the temperature of zone 4 is 220°C, the temperature of zone 5 is 225°C, the temperature of zone 6 is 225°C, the temperature of zone 7 is 230°C, the temperature of zone 8 is 225°C, the temperature of zone 9 is 220°C, the temperature of the die is 245°C, and a vacuum pump is used for extraction in the front zone of the die to control the vacuum pressure below 0.03MPa.

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