Preparation method of nylon elastomer

Through multi-copolymerization, nitrogen charge and vacuum technology, the problem of nylon elastomer's softness and hardness and low preparation quality is solved, and the adjustment of softness and hardness of nylon elastomer and the improvement of the preparation quality is achieved.

CN119931034APending Publication Date: 2025-05-06HENAN XIANNING NEW MATERIAL TECH RES INST CO LTD
View PDF 0 Cites 4 Cited by

Patent Information

Application Number
CN202510287190.8
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-03-12
Publication Date
2025-05-06

AI Technical Summary

Technical Problem

In the prior art, the softness and hardness of the nylon elastomer is unadjustable, and it is difficult to effectively eliminate moisture and impurities in the reaction system during the preparation process, which affects the preparation quality.

Method used

By using the multivariate copolymerization method, the types and proportions of dibasic acids and dibasic acids and dibasic acids, the types and molecular weights of polyether amines and polyether alcohols are adjusted, and nitrogen charge and vacuuming operations are carried out multiple times during the preparation process to ensure the oxygen-free environment inside the reactor and remove moisture and impurities.

Benefits of technology

It realizes the adjustable softness and hardness of nylon elastomers, improves the preparation quality, adapts to the needs of different usage environments, and improves the toughness and processing performance of the product.

✦ Generated by Eureka AI based on patent content.

Smart Images

  • Figure CN119931034A_ABST
    Figure CN119931034A_ABST
Patent Text Reader

Abstract

The invention discloses a nylon elastomer preparation method, which comprises: S1, weighing preparation raw materials of a nylon elastomer according to a feeding ratio, and weighing the preparation raw materials by using a weighing device, the nylon elastomer is prepared from the following raw materials: tridecane diamine, tridecane dibasic acid, dodecanediamine, dodecanedioic acid, undecanediamine, undecanedioic acid, decamethylene diamine, sebacic acid, pentamethylene diamine, glutaric acid, hexamethylenediamine, adipic acid, caprolactam, and one or more of polyether amine and polyether alcohol; and S2, feeding the preparation raw materials weighed in the step S1. In the preparation process of the nylon elastomer, the nylon elastomer with different melting points, different crystallization temperatures, different strengths and different elongation at break is produced by adopting a multi-component copolymerization mode and adjusting the types and the molecular weights of polyether amine and polyether alcohol by adjusting the types and the proportions of binary acid and diamine, so that the nylon elastomer is suitable for different use environments; the utilization rate is improved.
Need to check novelty before this filing date? Find Prior Art

Description

Technical Field

[0001] The invention relates to the field of nylon elastomer preparation, and in particular to a method for preparing a nylon elastomer. Background Art

[0002] Nylon elastomer is also known as thermoplastic polyamide elastomer or TPAE. Nylon elastomer is usually a block copolymer composed of a hard segment of polyamide and a soft segment of aliphatic polyester or polyether. Nylon elastomer has high tensile strength, good elastic recovery, high low-temperature impact strength, excellent low-temperature resistance and easy processing. The specific gravity of nylon elastomer is usually 0.98-1.08, and the melting point of nylon elastomer is 110℃-220℃. Nylon elastomer is translucent or white solid. Nylon elastomer usually needs to be prepared. Nylon elastomer prepared by prior art usually has the situation that the hardness cannot be adjusted, resulting in the use of nylon elastomer. In addition, the preparation process cannot well remove moisture and impurities in the reaction system, affecting the preparation quality of nylon elastomer. Therefore, it is necessary to make the hardness of the prepared nylon elastomer adjustable and improve the preparation quality. Summary of the invention

[0003] The object of the present invention is to provide a method for preparing a nylon elastomer to solve the problems raised in the above background technology.

[0004] To achieve the above object, the present invention provides the following technical solution: a method for preparing a nylon elastomer, comprising the following specific steps:

[0005] S1: weighing the raw materials for preparing nylon elastomer according to the feed ratio, using a weighing device to weigh the raw materials for preparing nylon elastomer, wherein the raw materials for preparing nylon elastomer include tridecanediamine, tridecanedioic acid, dodecanediamine, dodecanedioic acid, undecanediamine, undecanedioic acid, decanediamine, decanedioic acid, pentamethylenediamine, glutaric acid, hexamethylenediamine, adipic acid and caprolactam, and one or more of polyetheramine and polyether alcohol, and one or more of sodium hypophosphite, antioxidant 1010 and antioxidant 168;

[0006] S2: feeding the weighed raw materials in S1, so that the weighed tridecanediamine, tridecanedioic acid, dodecanediamine, dodecanedioic acid, undecanediamine, undecanedioic acid, decanediamine, decanedioic acid, pentamethylenediamine, glutaric acid, hexamethylenediamine, adipic acid and caprolactam, as well as one or more of polyetheramine and polyether alcohol, sodium hypophosphite, antioxidant 1010 and antioxidant 168 are sequentially fed into the reactor, and the reactor is sealed by closing the lid;

[0007] S3: Perform a sealing test on the reactor, use a nitrogen container to fill nitrogen into the reactor, and test the sealing of the reactor;

[0008] S4: heating and stirring the reactor after the sealing test in S3, so that the various nylon elastomer raw materials in the reactor are stirred at a first preset temperature;

[0009] S5: On the basis of step S4, the temperature inside the reactor is continued to be raised, and after the temperature reaches a second preset temperature, the gas is released and the pressure is reduced;

[0010] S6: Vacuum the interior of the reactor;

[0011] S7: discharging the reaction kettle in step S6 to obtain a nylon elastomer finished product;

[0012] S8: Perform necessary post-processing operations on the discharged products, including cooling, curing and cutting, and perform performance testing and quality inspection on the prepared nylon elastomer.

[0013] Preferably, the reactor sealing test in S3 includes the following specific steps:

[0014] S31: Filling nitrogen into the reactor using a nitrogen container;

[0015] S32: After nitrogen is charged in step S31, the reactor is allowed to stand for a preset time to observe whether there is leakage in the reactor;

[0016] S33: If there is no leakage in the reactor in step S32, the interior of the reactor is vented and vacuumed, and the inflation and vacuuming are repeated for a preset number of times to completely remove the air and impurities inside the reactor;

[0017] S34: After the air and impurities in the reactor are completely removed, the nitrogen in the nitrogen container is charged into the reactor, so that the pressure inside the reactor is charged to a preset positive pressure.

[0018] Preferably, the nitrogen container in S31 is a nitrogen bottle, the preset standing time of the reactor in S32 is 10 minutes, the preset number of repeated inflation and vacuuming of the reactor in step S32 is three times, and the inside of the reactor in step S34 is filled to a preset positive pressure of 0.2-0.5 MPa.

[0019] Preferably, the chemical equations generated in the reactor in S4, the reactor in S5 and the reactor in S6 include:

[0020]

[0021] Preferably, the chemical equations generated in the reactor in S4, the reactor in S5 and the reactor in S6 also include:

[0022]

[0023] Preferably, the heating and stirring in S4 include the following specific steps:

[0024] S41: Start heating the reactor to a first preset temperature, and monitor the temperature and pressure changes in the reactor during the heating process;

[0025] S42: When the reactor is heated to the first preset temperature, the stirring device is turned on to stir and mix the various raw materials in the reactor so that the various raw materials are evenly mixed.

[0026] Preferably, the first preset temperature of the reactor in S41 is 100° C.-140° C., the stirring device in S42 is a stirrer, and the stirring speed of the stirrer is adjusted according to the reaction conditions.

[0027] Preferably, the step of continuing to heat up the reactor and venting and reducing the pressure in S5 comprises the following specific steps:

[0028] S51: Continue heating the reactor to a second preset temperature, which is 180° C. to 220° C.; monitor temperature and pressure changes during the heating process, and ensure that the stirring device works normally;

[0029] S52: after the reactor in S51 is heated to the second preset temperature, the venting valve is opened to slowly vent the interior of the reactor to reduce the pressure inside the reactor to normal pressure;

[0030] S53: While the air inside the reactor is released and the pressure is reduced, the temperature inside the reactor is continued to rise to a third preset temperature, which is 200-250°C.

[0031] Preferably, the vacuum treatment inside the reactor in S6 comprises the following specific steps:

[0032] S61: Start the vacuum pump equipment, slowly open the exhaust valve, and start vacuuming. During the vacuuming process, the temperature in the reactor is maintained at 220-260° C., and the vacuuming time is 1 hour;

[0033] S62: After the reactor in S61 is evacuated for 1 hour, the stirring device is turned off, and after waiting for 10 minutes, the evacuation valve and the vacuum pump are closed.

[0034] Preferably, the discharging of the reactor in S7 comprises the following specific steps:

[0035] S71: nitrogen is charged into the reactor to make the interior of the reactor reach a set pressure, and the pressure is adjusted according to the viscosity of the discharged material;

[0036] S72: Then, the outlet valve is opened to discharge the prepared nylon elastomer.

[0037] Technical effects and advantages of the present invention:

[0038] (1) The present invention adopts a multi-polymerization method in the preparation process of nylon elastomer, and adjusts the types and ratios of dibasic acid and diamine, and the types and molecular weights of polyetheramine and polyether alcohol to produce nylon elastomers with different melting points, different crystallization temperatures, different strengths, different elongations at break, different resistivities, different hardnesses and different processing properties, so as to adapt to different use environments and improve utilization rate;

[0039] (2) The present invention performs nitrogen charging and vacuuming operations multiple times during the preparation process and strictly tests the sealing performance, thereby ensuring an oxygen-free environment inside the reactor, preventing oxidation reactions from occurring, and removing moisture and impurities in the reaction system, thereby improving the preparation quality of the nylon elastomer.

[0040] (3) The present invention precisely controls the pressure in the reactor by opening the vent valve and performing vacuum operation during the preparation process, which is beneficial to controlling the reaction rate and the molecular weight distribution of the product. The preparation heating process is carried out in stages, and stirring is started within a specific temperature range, which is beneficial to uniform mixing of the raw materials and sufficient reaction. BRIEF DESCRIPTION OF THE DRAWINGS

[0041] Figure 1 The figure is a schematic diagram of the preparation process of the nylon elastomer of the present invention.

[0042] Figure 2 This is a schematic diagram of the S3 process of the present invention.

[0043] Figure 3 This is a schematic diagram of the S4 process of the present invention.

[0044] Figure 4 This is a schematic diagram of the S5 process of the present invention.

[0045] Figure 5 This is a schematic diagram of the S6 process of the present invention.

[0046] Figure 6 This is a schematic diagram of the S7 process of the present invention. DETAILED DESCRIPTION

[0047] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0048] Embodiment 1

[0049] The present invention provides Figure 1-6 A method for preparing a nylon elastomer shown includes the following specific steps:

[0050] S1: weighing the raw materials for preparing nylon elastomer according to the feed ratio, using a weighing device to weigh the raw materials for preparing nylon elastomer, wherein the raw materials for preparing nylon elastomer include tridecanediamine, tridecanedioic acid, dodecanediamine, dodecanedioic acid, undecanediamine, undecanedioic acid, decanediamine, decanedioic acid, pentamethylenediamine, glutaric acid, hexamethylenediamine, adipic acid and caprolactam, and one or more of polyetheramine and polyether alcohol, and one or more of sodium hypophosphite, antioxidant 1010 and antioxidant 168;

[0051] S2: adding the weighed raw materials in S1 to the reactor in order, so that the weighed tridecanediamine, tridecanedioic acid, dodecanediamine, dodecanedioic acid, undecanediamine, undecanedioic acid, decanediamine, decanedioic acid, pentamethylenediamine, glutaric acid, hexamethylenediamine, adipic acid and caprolactam, one or more of polyetheramine and polyether alcohol, sodium hypophosphite, antioxidant 1010 and antioxidant 168 are added into the reactor in order, and the reactor is sealed by closing the lid;

[0052] S3: Perform a sealing test on the reactor. Use a nitrogen container to fill nitrogen into the reactor to test the sealing of the reactor. The reactor sealing test in S3 includes the following specific steps:

[0053] S31: Filling nitrogen into the reactor using a nitrogen container;

[0054] S32: After nitrogen is charged in step S31, the reactor is allowed to stand for a preset time to observe whether there is leakage in the reactor;

[0055] S33: If there is no leakage in the reactor in step S32, the interior of the reactor is vented and vacuumed, and the inflation and vacuuming are repeated for a preset number of times to completely remove the air and impurities inside the reactor;

[0056] S34: After the air and impurities inside the reactor are completely removed, the nitrogen inside the nitrogen container is filled into the reactor to fill the pressure inside the reactor to a preset positive pressure. The nitrogen container in S31 is a nitrogen bottle, the reactor in S32 is left to stand for a preset time of 10 minutes, the reactor in step S32 is repeatedly filled and vacuumed for a preset number of times three times, and the value of the preset positive pressure filled inside the reactor in step S34 is 0.2-0.5MPa;

[0057] S4: The reactor after the sealing test in S3 is heated and stirred internally, so that the various nylon elastomer raw materials in the reactor are stirred at a first preset temperature. The heating and stirring in S4 include the following specific steps:

[0058] S41: Start heating the reactor to a first preset temperature. During the heating process, monitor the temperature and pressure changes in the reactor. The first preset temperature of the reactor in S41 is 100° C.-140° C. The stirring device in S42 is a stirrer, and the stirring speed of the stirrer is adjusted according to the reaction conditions.

[0059] S42: when the temperature of the reactor is raised to the first preset temperature, the stirring device is turned on to stir and mix the various raw materials in the reactor so that the various raw materials are evenly mixed;

[0060] S5: On the basis of step S4, the temperature inside the reactor is continued to be raised, and after the temperature reaches the second preset temperature, the gas is released and the pressure is reduced. The further heating of the reactor and the release and pressure reduction in S5 include the following specific steps:

[0061] S51: Continue heating the reactor to a second preset temperature, which is 180° C. to 220° C.; monitor temperature and pressure changes during the heating process, and ensure that the stirring device works normally;

[0062] S52: after the reactor in S51 is heated to the second preset temperature, the venting valve is opened to slowly vent the interior of the reactor to reduce the pressure inside the reactor to normal pressure;

[0063] S53: while releasing air and reducing pressure inside the reactor, the temperature inside the reactor is continuously raised to a third preset temperature, which is 200-250° C.;

[0064] S6: The interior of the reactor is subjected to vacuum treatment. The vacuum treatment of the interior of the reactor in S6 includes the following specific steps:

[0065] S61: Start the vacuum pump equipment, slowly open the exhaust valve, and start vacuuming. During the vacuuming process, the temperature in the reactor is maintained at 220-260° C., and the vacuuming time is 1 hour;

[0066] S62: After the reactor is evacuated for 1 hour in S61, the stirring device is turned off, and after waiting for 10 minutes, the exhaust valve and the vacuum pump are turned off;

[0067] S7: discharging the reaction kettle in step S6 to obtain a nylon elastomer finished product. The discharging of the reaction kettle in step S7 includes the following specific steps:

[0068] S71: nitrogen is charged into the reactor to make the interior of the reactor reach a set pressure, and the pressure is adjusted according to the viscosity of the discharged material;

[0069] S72: then opening the outlet valve to discharge the prepared nylon elastomer;

[0070] S8: Perform necessary post-processing operations on the discharged products, including cooling, curing and cutting, and perform performance testing and quality inspection on the prepared nylon elastomer.

[0071] Specifically, the chemical equations generated in the reactor in S4, the reactor in S5, and the reactor in S6 include:

[0072]

[0073] Specifically, the chemical equations generated in the reactor in S4, the reactor in S5, and the reactor in S6 also include:

[0074]

[0075] Embodiment 2

[0076] A method for preparing a nylon elastomer comprises the following specific steps:

[0077] S1: weighing the raw materials for preparing nylon elastomer according to the feed ratio, using a weighing device to weigh the raw materials for preparing nylon elastomer, wherein the raw materials for preparing nylon elastomer include several of tridecanediamine, tridecanedioic acid, dodecanediamine, dodecanedioic acid, undecanediamine, undecanedioic acid, decanediamine, decanedioic acid, pentamethylenediamine, glutaric acid, hexamethylenediamine, adipic acid and caprolactam, and one or more of sodium hypophosphite, antioxidant 1010 and antioxidant 168;

[0078] S2: adding the weighed raw materials in S1 to the reactor in order, and adding the weighed tridecanediamine, tridecanedioic acid, dodecanediamine, dodecanedioic acid, undecanediamine, undecanedioic acid, decanediamine, decanedioic acid, pentamethylenediamine, glutaric acid, hexamethylenediamine, adipic acid and caprolactam, and one or more of sodium hypophosphite, antioxidant 1010 and antioxidant 168 to the reactor, and sealing the reactor by closing the lid;

[0079] S3: Perform a sealing test on the reactor, use a nitrogen container to fill nitrogen into the reactor, and test the sealing of the reactor;

[0080] S4: heating and stirring the reactor after the sealing test in S3, so that the various nylon elastomer raw materials in the reactor are stirred at a first preset temperature;

[0081] S5: On the basis of step S4, the temperature inside the reactor is continued to be raised, and after the temperature reaches a second preset temperature, the gas is released and the pressure is reduced;

[0082] S6: Vacuum the interior of the reactor;

[0083] S7: discharging the reaction kettle in step S6 to obtain a nylon elastomer finished product;

[0084] S8: Perform necessary post-processing operations on the discharged products, including cooling, curing and cutting, and perform performance testing and quality inspection on the prepared nylon elastomer.

[0085] The nylon elastomer prepared by the above method is a translucent solid, the hardness of the nylon elastomer is not adjustable and the flexibility is weak.

[0086] It can be seen that when preparing nylon elastomer, adding one or more polyetheramines or polyether alcohols into the raw materials can improve the toughness and processing properties of the nylon elastomer and make the hardness of the prepared nylon elastomer adjustable.

[0087] Embodiment 3

[0088] A method for preparing a nylon elastomer comprises the following specific steps:

[0089] S1: weighing the raw materials for preparing nylon elastomer according to the feed ratio, using a weighing device to weigh the raw materials for preparing nylon elastomer, wherein the raw materials for preparing nylon elastomer include tridecanediamine, tridecanedioic acid, dodecanediamine, dodecanedioic acid, undecanediamine, undecanedioic acid, decanediamine, decanedioic acid, pentamethylenediamine, glutaric acid, hexamethylenediamine, adipic acid and caprolactam, and one or more of polyetheramine and polyether alcohol, and one or more of sodium hypophosphite, antioxidant 1010 and antioxidant 168;

[0090] S2: adding the weighed raw materials in S1 to the reactor in order, so that the weighed tridecanediamine, tridecanedioic acid, dodecanediamine, dodecanedioic acid, undecanediamine, undecanedioic acid, decanediamine, decanedioic acid, pentamethylenediamine, glutaric acid, hexamethylenediamine, adipic acid and caprolactam, one or more of polyetheramine and polyether alcohol, sodium hypophosphite, antioxidant 1010 and antioxidant 168 are added into the reactor in order, and the reactor is sealed by closing the lid;

[0091] S3: Perform a sealing test on the reactor. Use a nitrogen container to fill nitrogen into the reactor to test the sealing of the reactor. Exhaust and vacuum the inside of the reactor, and repeat the filling and vacuuming once;

[0092] S4: heating and stirring the reactor after the sealing test in S3, so that the various nylon elastomer raw materials in the reactor are stirred at a first preset temperature;

[0093] S5: On the basis of step S4, the temperature inside the reactor is continued to be raised, and after the temperature reaches a second preset temperature, the gas is released and the pressure is reduced;

[0094] S6: Vacuum the interior of the reactor;

[0095] S7: discharging the reaction kettle in step S6 to obtain a nylon elastomer finished product;

[0096] S8: Perform necessary post-processing operations on the discharged products, including cooling, curing and cutting, and perform performance testing and quality inspection on the prepared nylon elastomer.

[0097] The nylon elastomer prepared by the above method is a translucent solid with a main content of 87.73% and a yield of 85.24%.

[0098] Embodiment 4

[0099] A method for preparing a nylon elastomer comprises the following specific steps:

[0100] S1: weighing the raw materials for preparing nylon elastomer according to the feed ratio, using a weighing device to weigh the raw materials for preparing nylon elastomer, wherein the raw materials for preparing nylon elastomer include tridecanediamine, tridecanedioic acid, dodecanediamine, dodecanedioic acid, undecanediamine, undecanedioic acid, decanediamine, decanedioic acid, pentamethylenediamine, glutaric acid, hexamethylenediamine, adipic acid and caprolactam, and one or more of polyetheramine and polyether alcohol, and one or more of sodium hypophosphite, antioxidant 1010 and antioxidant 168;

[0101] S2: adding the weighed raw materials in S1 to the reactor in order, so that the weighed tridecanediamine, tridecanedioic acid, dodecanediamine, dodecanedioic acid, undecanediamine, undecanedioic acid, decanediamine, decanedioic acid, pentamethylenediamine, glutaric acid, hexamethylenediamine, adipic acid and caprolactam, one or more of polyetheramine and polyether alcohol, sodium hypophosphite, antioxidant 1010 and antioxidant 168 are added into the reactor in order, and the reactor is sealed by closing the lid;

[0102] S3: Perform a sealing test on the reactor. Use a nitrogen container to fill nitrogen into the reactor to test the sealing of the reactor. Exhaust and vacuum the inside of the reactor, and repeat the filling and vacuuming twice.

[0103] S4: heating and stirring the reactor after the sealing test in S3, so that the various nylon elastomer raw materials in the reactor are stirred at a first preset temperature;

[0104] S5: On the basis of step S4, the temperature inside the reactor is continued to be raised, and after the temperature reaches a second preset temperature, the gas is released and the pressure is reduced;

[0105] S6: Vacuum the interior of the reactor;

[0106] S7: discharging the reaction kettle in step S6 to obtain a nylon elastomer finished product;

[0107] S8: Perform necessary post-processing operations on the discharged products, including cooling, curing and cutting, and perform performance testing and quality inspection on the prepared nylon elastomer.

[0108] The nylon elastomer prepared by the above method is a translucent solid with a main content of 90.73% and a yield of 92.24%.

[0109] Embodiment 5

[0110] A method for preparing a nylon elastomer comprises the following specific steps:

[0111] S1: weighing the raw materials for preparing nylon elastomer according to the feed ratio, using a weighing device to weigh the raw materials for preparing nylon elastomer, wherein the raw materials for preparing nylon elastomer include tridecanediamine, tridecanedioic acid, dodecanediamine, dodecanedioic acid, undecanediamine, undecanedioic acid, decanediamine, decanedioic acid, pentamethylenediamine, glutaric acid, hexamethylenediamine, adipic acid and caprolactam, and one or more of polyetheramine and polyether alcohol, and one or more of sodium hypophosphite, antioxidant 1010 and antioxidant 168;

[0112] S2: adding the weighed raw materials in S1 to the reactor in order, so that the weighed tridecanediamine, tridecanedioic acid, dodecanediamine, dodecanedioic acid, undecanediamine, undecanedioic acid, decanediamine, decanedioic acid, pentamethylenediamine, glutaric acid, hexamethylenediamine, adipic acid and caprolactam, one or more of polyetheramine and polyether alcohol, sodium hypophosphite, antioxidant 1010 and antioxidant 168 are added into the reactor in order, and the reactor is sealed by closing the lid;

[0113] S3: Perform a sealing test on the reactor. Use a nitrogen container to fill nitrogen into the reactor to test the sealing of the reactor. Exhaust and vacuum the inside of the reactor, and repeat the filling and vacuuming three times.

[0114] S4: heating and stirring the reactor after the sealing test in S3, so that the various nylon elastomer raw materials in the reactor are stirred at a first preset temperature;

[0115] S5: On the basis of step S4, the temperature inside the reactor is continued to be raised, and after the temperature reaches a second preset temperature, the gas is released and the pressure is reduced;

[0116] S6: discharging the reaction kettle in step S5 to obtain a nylon elastomer finished product;

[0117] S7: Carry out necessary post-processing operations on the discharged products, including cooling, curing and cutting, and carry out performance testing and quality inspection on the prepared nylon elastomer.

[0118] The nylon elastomer prepared by the above method is a translucent solid with a main content of 85.73% and a yield of 84.24%.

[0119] It can be seen that the repeated inflation and vacuuming times for preparing nylon elastomers are controlled to three times and vacuuming is performed before discharging, which can obtain higher yield and high content nylon elastomer. The effects of repeated inflation and vacuuming times and vacuuming of discharging are shown in the following table:

[0120]

[0121] Working principle of the present invention:

[0122] Firstly, the raw materials for preparing nylon elastomer are weighed according to the feed ratio, and the raw materials for preparing nylon elastomer are weighed using a weighing device. The raw materials for preparing nylon elastomer include tridecanediamine, tridecane dibasic acid, dodecanediamine, dodecane dibasic acid, undecanediamine, undecane dibasic acid, decanediamine, decanedioic acid, pentamethylenediamine, glutaric acid, hexamethylenediamine, adipic acid and caprolactam, and one or more of polyetheramine and polyether alcohol, and one or more of sodium hypophosphite, antioxidant 1010 and antioxidant 168. Then, the weighed tridecanediamine, Several of tridecanedioic acid, dodecanedioic acid, dodecanedioic acid, undecanedioic acid, undecanedioic acid, decanediamine, decanedioic acid, pentamethylenediamine, glutaric acid, hexamethylenediamine, adipic acid and caprolactam, and one or more of polyetheramine and polyether alcohol, sodium hypophosphite, antioxidant 1010 and antioxidant 168 are sequentially put into the reactor, and the reactor is sealed with a lid, and a sealing test is performed on the inside of the reactor, and the test method is to use a nitrogen container to fill nitrogen into the inside of the reactor to test the sealing of the reactor;

[0123] Then after the sealing test of the reactor is completed, the interior of the reactor is heated and stirred, so that the various nylon elastomer raw materials inside the reactor are stirred at a first preset temperature, and then the interior of the reactor is continued to be heated, and after the temperature reaches a second preset temperature, the air is released and the pressure is reduced. After the pressure reduction is completed, the interior of the reactor is vacuumed, and the interior of the reactor is discharged to obtain a nylon elastomer finished product. Then, necessary post-processing operations are performed on the discharged products, including cooling, curing and cutting, and the prepared nylon elastomer is subjected to performance testing and quality inspection.

[0124] Finally, it should be noted that the above is only a preferred embodiment of the present invention and is not intended to limit the present invention. Although the present invention has been described in detail with reference to the aforementioned embodiments, it is still possible for those skilled in the art to modify the technical solutions described in the aforementioned embodiments or to make equivalent substitutions for some of the technical features therein. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention should be included in the protection scope of the present invention.

Claims

1. A method for preparing a nylon elastomer, characterized in that: The specific steps include: S1: weighing the raw materials for preparing nylon elastomer according to the feed ratio, using a weighing device to weigh the raw materials for preparing nylon elastomer, wherein the raw materials for preparing nylon elastomer include tridecanediamine, tridecanedioic acid, dodecanediamine, dodecanedioic acid, undecanediamine, undecanedioic acid, decanediamine, decanedioic acid, pentamethylenediamine, glutaric acid, hexamethylenediamine, adipic acid and caprolactam, and one or more of polyetheramine and polyether alcohol, and one or more of sodium hypophosphite, antioxidant 1010 and antioxidant 168; S2: feeding the weighed raw materials in S1, so that the weighed tridecanediamine, tridecanedioic acid, dodecanediamine, dodecanedioic acid, undecanediamine, undecanedioic acid, decanediamine, decanedioic acid, pentamethylenediamine, glutaric acid, hexamethylenediamine, adipic acid and caprolactam, as well as one or more of polyetheramine and polyether alcohol, sodium hypophosphite, antioxidant 1010 and antioxidant 168 are sequentially fed into the reactor, and the reactor is sealed by closing the lid; S3: Perform a sealing test on the reactor, use a nitrogen container to fill nitrogen into the reactor, and test the sealing of the reactor; S4: heating and stirring the reactor after the sealing test in S3, so that the various nylon elastomer raw materials in the reactor are stirred at a first preset temperature; S5: On the basis of step S4, the temperature inside the reactor is continued to be raised, and after the temperature reaches a second preset temperature, the gas is released and the pressure is reduced; S6: Vacuum the interior of the reactor; S7: discharging the reaction kettle in step S6 to obtain a nylon elastomer finished product; S8: Perform necessary post-processing operations on the discharged products, including cooling, curing and cutting, and perform performance testing and quality inspection on the prepared nylon elastomer.

2. The method for preparing a nylon elastomer according to claim 1, characterized in that: The reactor sealing test in S3 includes the following specific steps: S31: Filling nitrogen into the reactor using a nitrogen container; S32: After nitrogen is charged in step S31, the reactor is allowed to stand for a preset time to observe whether there is leakage in the reactor; S33: If there is no leakage in the reactor in step S32, the interior of the reactor is vented and vacuumed, and the inflation and vacuuming are repeated for a preset number of times to completely remove the air and impurities inside the reactor; S34: After the air and impurities in the reactor are completely removed, the nitrogen in the nitrogen container is charged into the reactor, so that the pressure inside the reactor is charged to a preset positive pressure.

3. The method for preparing a nylon elastomer according to claim 2, characterized in that: The nitrogen container in S31 is a nitrogen bottle, the reactor in S32 is left standing for a preset time of 10 minutes, the reactor in step S32 is repeatedly inflated and vacuumed for a preset number of times three times, and the reactor in step S34 is filled to a preset positive pressure of 0.2-0.5 MPa.

4. The method for preparing a nylon elastomer according to claim 1, characterized in that: The chemical equations generated in the reactor of S4, the reactor of S5 and the reactor of S6 include:

5. The method for preparing a nylon elastomer according to claim 1, characterized in that: The chemical equations generated in the reactor in S4, the reactor in S5 and the reactor in S6 also include:

6. The method for preparing a nylon elastomer according to claim 1, characterized in that: The heating and stirring in S4 include the following specific steps: S41: Start heating the reactor to a first preset temperature, and monitor the temperature and pressure changes in the reactor during the heating process; S42: When the reactor is heated to the first preset temperature, the stirring device is turned on to stir and mix the various raw materials in the reactor so that the various raw materials are evenly mixed.

7. The method for preparing a nylon elastomer according to claim 6, characterized in that: The first preset temperature for heating the reactor in S41 is 100° C.-140° C., the stirring device in S42 is a stirrer, and the stirring speed of the stirrer is adjusted according to the reaction conditions.

8. The method for preparing a nylon elastomer according to claim 1, characterized in that: The step of continuing to heat up the reactor and venting and reducing the pressure in S5 includes the following specific steps: S51: Continue heating the reactor to a second preset temperature, which is 180° C. to 220° C.; monitor temperature and pressure changes during the heating process, and ensure that the stirring device works normally; S52: after the reactor in S51 is heated to the second preset temperature, the venting valve is opened to slowly vent the interior of the reactor to reduce the pressure inside the reactor to normal pressure; S53: While the air inside the reactor is released and the pressure is reduced, the temperature inside the reactor is continued to rise to a third preset temperature, which is 200-250°C.

9. The method for preparing a nylon elastomer according to claim 1, characterized in that: The vacuuming treatment inside the reactor in S6 comprises the following specific steps: S61: Start the vacuum pump equipment, slowly open the exhaust valve, and start vacuuming. During the vacuuming process, the temperature in the reactor is maintained at 220-260° C., and the vacuuming time is 1 hour; S62: After the reactor in S61 is evacuated for 1 hour, the stirring device is turned off, and after waiting for 10 minutes, the evacuation valve and the vacuum pump are closed.

10. The method for preparing a nylon elastomer according to claim 1, characterized in that: The discharge of the reactor in S7 comprises the following specific steps: S71: nitrogen is charged into the reactor to make the interior of the reactor reach a set pressure, and the pressure is adjusted according to the viscosity of the discharged material; S72: Then, the outlet valve is opened to discharge the prepared nylon elastomer.

Citation Information

Cited By

  • Bio-based nylon 12 elastomer prepared by one-step method as well as preparation method and application of bio-based nylon 12 elastomer

    CN120309925A

  • One-step prepared bio-based nylon 12 elastomer and its preparation method and application

    CN120309925B

  • Polyamide elastomer and method for preparing polyamide elastomer by one-pot method

    CN120775185A

  • Polyamide elastomers and a one-pot method for preparing polyamide elastomers

    CN120775185B