Production process of high-performance hydrogenated polyethylene white rubber putty

Through the process of grafting acrylic chloride under a nitrogen atmosphere, introducing epoxy groups, catalytic hydrogenation and UV light source cross-linking, the problems of slow curing, loose cross-linking, insufficient tensile strength and poor high temperature stability are solved, and putty materials with fast curing, high strength and good toughness are achieved.

CN120365782APending Publication Date: 2025-07-25SICHUAN LONGSHENG TECH IND CO LTD
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Patent Information

Application Number
CN202510799206.3
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-06-16
Publication Date
2025-07-25

AI Technical Summary

Technical Problem

The existing hydrogenated polyethylene white rubber putty is slow in curing speed, loose crosslinking structure, insufficient tensile strength, poor high temperature stability, insufficient toughness, which affects construction efficiency and service life.

Method used

Acryloyl chloride is grafted by dissolving linear low-density polyethylene in an organic solvent under a nitrogen atmosphere, and then hydrogenation is catalyzed under supercritical fluid and ionic liquid conditions, and dynamic covalent bond-modified nanofillers are mixed, and dynamic cross-linking and photocuring reactions are triggered through a dual-band UV light source.

Benefits of technology

It significantly improves the curing rate and cross-linking density of putty, enhances tensile strength and thermal stability, improves the toughness and damage resistance of the material, and expands the application scenarios.

✦ Generated by Eureka AI based on patent content.

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Abstract

The invention relates to the technical field of polymer materials, and discloses a high-performance hydrogenated polyethylene white rubber putty production process, which comprises: dissolving linear low density polyethylene in an organic solvent in a nitrogen atmosphere to form a polyethylene solution, and adding acryloyl chloride; adding epoxy chloropropane into a reaction system, introducing an epoxy group, and removing a solvent and unreacted reagents through reduced pressure distillation to obtain a hydrogenated polyethylene prepolymer; carrying out catalytic hydrogenation reaction on the hydrogenated polyethylene prepolymer under the synergistic condition of supercritical fluid and ionic liquid; mixing and dispersing the hydrogenated polyethylene prepolymer and the dynamic covalent bond modified nanofiller to obtain a mixture; and triggering the dynamic crosslinking and photocuring reaction of the mixture by stages by using a dual-waveband UV light source. According to the invention, under the action of light energy, a polymerization reaction is rapidly started to form a stable cross-linked structure, so that the problem that the curing time of the material is too long in the construction process is effectively solved.
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Description

Technical Field

[0001] The present invention relates to the technical field of polymer materials, and particularly to a production process for a high-performance hydrogenated polyethylene white rubber putty. Background Art

[0002] In the prior art, hydrogenated polyethylene white rubber putty is widely used in the construction and decoration industries. Although such putty has good basic properties, there are some deficiencies in actual applications. First of all, traditional formulations usually rely on natural curing, resulting in a slow curing speed. During the construction process, the waiting time for the putty to cure is long, which affects the overall construction efficiency.

[0003] In addition, the cross-linking structure in existing putty products is relatively loose, directly resulting in insufficient tensile strength. Such materials are prone to cracking and peeling after construction, especially in areas with greater stress, and the service life of the material is thus affected, reducing consumer satisfaction; furthermore, traditional putty has poor stability under high-temperature conditions and is prone to softening or deformation. This performance limitation makes the putty unable to maintain stability in summer or high-temperature environments, thereby affecting the aesthetics and use effect of the coating. Customers hope to have a more durable use experience, but the prior art cannot meet this demand; finally, previous technologies also perform mediocrely in terms of toughness. The putty is prone to brittle cracking under external forces and lacks the necessary damage resistance.

[0004] In summary, the prior art has obvious deficiencies in terms of curing rate, mechanical properties, thermal stability, and toughness. These problems not only restrict the application effect of hydrogenated polyethylene putty but also affect its market competitiveness. To solve these problems, it is urgent to improve through new technical solutions to enhance the overall performance. Summary of the Invention

[0005] Aiming at the deficiencies of the prior art, the present invention provides a production process for a high-performance hydrogenated polyethylene white rubber putty, effectively solving the problem of excessive curing time of the material during the construction process.

[0006] To achieve the above objectives, the present invention is realized through the following technical solutions: A production process for a high-performance hydrogenated polyethylene white rubber putty, comprising:

[0007] S1: Under a nitrogen atmosphere, dissolve linear low-density polyethylene in an organic solvent to form a polyethylene solution and add acryloyl chloride to graft acrylate groups;

[0008] S2: Add epichlorohydrin to the reaction system to introduce epoxy groups, and remove the solvent and unreacted reagents by vacuum distillation to obtain a hydrogenated polyethylene prepolymer;

[0009] S3: Carry out catalytic hydrogenation reaction on the above hydrogenated polyethylene prepolymer under the synergistic condition of supercritical fluid and ionic liquid;

[0010] S4: Mix and disperse the hydrogenated polyethylene prepolymer with the nano-fillers modified by dynamic covalent bonds to obtain a mixture;

[0011] S5: Carry out staged triggering of dynamic crosslinking and photocuring reaction on the mixture by using a dual-band UV light source to form a high-performance final coating.

[0012] Preferably, the melt index range of the linear low-density polyethylene is 2-10 g / 10 min.

[0013] Preferably, the evaporation temperature of the vacuum distillation process is 60-80 °C, the degree of vacuum is 10-50 kPa, and the vacuum time is 1-3 hours.

[0014] Preferably, the supercritical fluid is supercritical carbon dioxide, the ionic liquid is 1-butyl-3-methylimidazolium hexafluorophosphate, the catalyst used for catalytic hydrogenation is supported ruthenium nanoparticles, the reaction conditions are a pressure of 7.0-8.0 MPa, a temperature of 75-85 °C, the reaction time is 1.5-2 hours, the catalyst loading is 1-5 wt%, and the concentration of the hydrogenated polyethylene prepolymer is 10-20 wt%.

[0015] Preferably, the dynamic covalent bond is formed by Diels-Alder reaction and modified on the surface of nano-silica, the particle size of the nano-fillers is 30-50 nm, and the addition amount of the nano-fillers is 5-20 wt%.

[0016] Preferably, the mixing and dispersion are carried out under vacuum conditions, the vacuum degree range is -0.06--0.1 MPa, the mixing temperature is 50-70 °C, and the mixing time is 30 minutes to 1 hour.

[0017] Preferably, the dual-band UV light source includes a first band of 285 nm and a second band of 365 nm, the irradiation time of the first band is 3-5 seconds, and the irradiation time of the second band is 8-12 seconds.

[0018] Preferably, the photoinitiator for the photocuring reaction is 2,4,6-trimethylbenzoyl-diphenylphosphine oxide, and the addition amount is 1-3 wt%.

[0019] Preferably, the hydrogen partial pressure is 2.5-3.5 MPa, the hydrogenation reaction time is 1.5-2.5 hours, and the hydrogenation degree ≥ 95%.

[0020] The molecular weight of the hydrogenated polyethylene prepolymer is 20,000-50,000 g / mol.

[0021] The present invention provides a production process for high-performance hydrogenated polyethylene white rubber putty, which has the following beneficial effects:

[0022] 1. The present invention adopts the technical solution of a photoinitiator, which significantly improves the curing rate of the hydrogenated polyethylene white rubber putty. Through the action of light energy, the polymerization reaction is quickly initiated to form a stable cross-linked structure. Compared with the prior art solutions with slower curing speeds, this improvement effectively solves the problem of excessive curing time of the material during construction.

[0023] 2. The present invention introduces a photoinitiator with high activity, which directly improves the tensile strength and adhesion of the putty. Research shows that the enhanced cross-linking degree brings better mechanical properties. Compared with the prior art solutions without a photoinitiator, the present invention solves the problems of insufficient bonding strength and material fragility, making the putty more durable in use.

[0024] 3. The present invention significantly improves the thermal stability of the putty by optimizing the combination of the hydrogenated polyethylene formula and the photoinitiator. This measure improves the performance of the putty in high-temperature environments, thereby expanding its application scenarios. Compared with the prior art formulas that are prone to failure at high temperatures, the present invention provides a more reliable user experience for customers.

[0025] 4. The present invention adopts an improved cross-linking mechanism to enhance the toughness of the hydrogenated polyethylene putty. This enhanced toughness effectively reduces the risk of brittle fracture of the material during actual application. Different from the prior art products with greater brittleness, the solution of the present invention greatly improves the damage resistance of the material, providing a higher cost-effective solution for users. BRIEF DESCRIPTION OF THE DRAWINGS

[0026] Figure 1 It is a schematic flow chart of the method of the present invention. DETAILED DESCRIPTION OF THE EMBODIMENTS

[0027] The following will clearly and completely describe the technical solutions in the embodiments of the present invention with reference to the accompanying drawings of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative efforts shall fall within the protection scope of the present invention.

[0028] Please refer to the appendix Figure 1 ;

[0029] Example 1: Preparation of Hydrogenated Polyethylene Putty

[0030] Materials and Basic Parameters:

[0031] Linear low-density polyethylene (LDPE): The melt index is 4 g / 10 min;

[0032] Organic solvent: a mixed solvent of deionized water and toluene;

[0033] Acryloyl chloride: 0.5 kg;

[0034] Epichlorohydrin: 0.3 kg;

[0035] Catalyst: supported ruthenium nanoparticles;

[0036] Supercritical fluid: supercritical carbon dioxide;

[0037] Detailed steps:

[0038] Dissolution and grafting of polyethylene:

[0039] Dissolve 2 kg of LDPE in 10 L of the mixed solvent of deionized water and toluene, keep nitrogen protection, set the temperature to 70 °C, and stir for 3 hours.

[0040] Add 0.5 kg of acryloyl chloride and continue the reaction for 4 hours to ensure the formation of polymer grafting.

[0041] Introduction of epoxy groups:

[0042] Add 0.3 kg of epichlorohydrin to the reaction system, keep the reaction temperature at 75 °C, and the reaction time is 1 hour. Remove the unreacted materials by vacuum distillation, set the vacuum degree to 25 kPa, and the evaporation temperature is 65 °C.

[0043] Catalytic hydrogenation reaction:

[0044] Transfer the prepolymer to a supercritical reactor, select supercritical carbon dioxide as the solvent, set the pressure to 7.5 MPa, and keep the temperature at 80 °C.

[0045] Add supported ruthenium nanoparticles, set the duration of the catalytic hydrogenation reaction to 2 hours, and the hydrogen partial pressure is 3.0 MPa.

[0046] Mixing and dispersion:

[0047] Mix the hydrogenated polyethylene prepolymer with 5 wt% modified nano-silica (particle size 30 - 50 nm), set the mixing temperature to 60 °C, the stirring speed to 800 rpm, and continue for 30 minutes.

[0048] Photocuring reaction:

[0049] Use a dual-band UV light source, irradiate with the first band at 285 nm for 4 seconds, and irradiate with the second band at 365 nm for 10 seconds. The addition amount of the photoinitiator is 2 wt%.

[0050] Example 2: Preparation of high-filled hydrogenated polyethylene putty

[0051] Materials and Basic Parameters:

[0052] Linear low density polyethylene (LDPE): The melt index is 8 g / 10 min;

[0053] Organic solvent: n - hexane;

[0054] Acryloyl chloride: 0.4 kg;

[0055] Epichlorohydrin: 0.2 kg;

[0056] Catalyst: Supported ruthenium nanoparticles;

[0057] Supercritical fluid: Supercritical carbon dioxide;

[0058] Detailed Steps:

[0059] Dissolution and Grafting of Polyethylene:

[0060] Dissolve 3 kg of LDPE in 15 L of n - hexane, stir under a nitrogen atmosphere, keep the temperature at 75 °C, and the reaction time is 3 hours.

[0061] Add 0.4 kg of acryloyl chloride and continue the reaction for 5 hours to achieve effective grafting.

[0062] Introduction of Epoxy Groups:

[0063] Add 0.2 kg of epichlorohydrin to the reaction system, keep the reaction temperature at 78 °C, and the time is set to 1 hour. Subsequently, perform vacuum distillation treatment, with the evaporation temperature at 70 °C and the degree of vacuum set to 30 kPa.

[0064] Catalytic Hydrogenation Reaction:

[0065] Transfer the obtained substance to a supercritical reactor, set the pressure to 8.0 MPa, carry out the catalytic hydrogenation reaction at 85 °C, the reaction time is 2 hours, and the partial pressure of hydrogen is 2.8 MPa.

[0066] Mixing and Dispersion:

[0067] Mix the hydrogenated polyethylene prepolymer with 5 wt% of modified nano - silica, set the stirring speed to 600 rpm, the mixing time is 1 hour, and the mixing temperature is 65 °C.

[0068] Photocuring Reaction:

[0069] Use a dual - band UV light source, the irradiation time of the first band at 285 nm is 5 seconds, the irradiation time of the second band at 365 nm is 12 seconds, and the addition amount of the photoinitiator is 1.5 wt%.

[0070] Example 3: Preparation of Low - Viscosity Hydrogenated Polyethylene Putty

[0071] Materials and Basic Parameters:

[0072] Linear low-density polyethylene (LDPE): The melt index is 10 g / 10 min;

[0073] Organic solvent: Alcohol solvent (such as isopropyl alcohol);

[0074] Acryloyl chloride: 0.6 kg;

[0075] Epichlorohydrin: 0.4 kg;

[0076] Catalyst: Supported ruthenium nanoparticles;

[0077] Supercritical fluid: Supercritical carbon dioxide.

[0078] Detailed Steps:

[0079] Dissolution and Grafting of Polyethylene:

[0080] Dissolve 2.5 kg of LDPE in 12 L of isopropyl alcohol and stir at 70 °C for 3 hours under a nitrogen atmosphere.

[0081] Add 0.6 kg of acryloyl chloride and keep the reaction time for 4 hours to achieve an ideal grafting effect.

[0082] Introduction of Epoxy Group:

[0083] Add 0.4 kg of epichlorohydrin to the reaction system, react for 1.5 hours, and keep the temperature at 80 °C. Remove the unreacted reagents by vacuum distillation, set the vacuum degree to 20 kPa, and the evaporation temperature to 65 °C.

[0084] Catalytic Hydrogenation Reaction:

[0085] Transfer the obtained substance to a supercritical reactor, set the pressure to 7.0 MPa, and carry out catalytic hydrogenation at 75 °C. Set the catalytic reaction time to 1.5 hours to ensure that the hydrogen partial pressure is 3.5 MPa.

[0086] Mixing and Dispersion:

[0087] Mix the hydrogenated polyethylene prepolymer with 10 wt% of modified nano-silica, control the mixing temperature at 55 °C, the stirring speed at 500 rpm, and the duration for 45 minutes.

[0088] Photocuring Reaction

[0089] Use a dual-band UV light source, irradiate for 3 seconds at the first band of 285 nm and 8 seconds at the second band of 365 nm, and add 2 wt% of the photoinitiator.

[0090] Comparative Example 1:

[0091] Compared with Example 1, the difference lies in the cancellation of the use of acryloyl chloride, and the rest are the same.

[0092] Comparative Example 2:

[0093] Compared with Example 2, the difference lies in reducing the temperature of the catalytic hydrogenation reaction to 70 °C, and the rest are the same.

[0094] Comparative Example 3:

[0095] Compared with Example 3, the difference lies in the cancellation of the use of supercritical fluid, and the rest are the same.

[0096] Experiment 1: Viscosity test experiment of Example 1 and Comparative Example 1

[0097] Experiment purpose:

[0098] Evaluate the effect of removing acryloyl chloride on the viscosity in hydrogenated polyethylene white rubber putty.

[0099] Experiment materials:

[0100] Sample of Example 1: Hydrogenated polyethylene putty containing acryloyl chloride;

[0101] Sample of Comparative Example 1: Hydrogenated polyethylene putty without acryloyl chloride;

[0102] Rotary viscometer.

[0103] Experiment steps:

[0104] Sample preparation:

[0105] Prepare the hydrogenated polyethylene samples of Example 1 and Comparative Example 1, ensuring that each sample has the same experimental conditions (such as thickness and temperature).

[0106] Preheat the samples at 70 °C for 30 minutes to ensure uniformity.

[0107] Viscosity measurement:

[0108] Immerse the rotor of the rotary viscometer into each sample, ensuring no bubbles.

[0109] Set the rotation speed of the rotary viscometer to 100 rpm, and select an appropriate temperature control system to keep the sample temperature at 60 °C.

[0110] Record the viscosity values of each sample, and conduct three repeated experiments to ensure the accuracy of the data.

[0111] Data recording:

[0112] Record and organize the results of each measurement, including the sample name, measurement time, and corresponding viscosity values.

[0113] Data analysis:

[0114] Calculate the average viscosity values of Example 1 and Comparative Example 1, and conduct a comparative analysis.

[0115] Viscosity test experimental data of Example 1 and Comparative Example 1

[0116] Sample Name Measurement Times Viscosity (mPa·s) Remarks Example 1 1 320 Test 1 Example 1 2 310 Test 2 Example 1 3 325 Test 3 Comparative Example 1 1 410 Test 1 Comparative Example 1 2 395 Test 2 Comparative Example 1 3 420 Test 3 Example 1 1 315 Test 1 Comparative Example 1 1 405 Test 1 Example 1 2 300 Test 2 Comparative Example 1 3 390 Test 3 Example 1 3 330 Test 3 Comparative Example 1 2 410 Test 2

[0117] Summary: In the viscosity test experiments of Example 1 and Comparative Example 1, from a mechanistic perspective, the introduction of acryloyl chloride had a significant impact on the fluidity and processing properties of the hydrogenated polyethylene white rubber putty. As a graft monomer, acryloyl chloride can react with the polyethylene chain to form a polymer chain with hydrophilic functional groups. The introduction of these hydrophilic groups increases the internal freedom of movement of the polymer. However, in some cases, too many polar groups may lead to an increase in the interaction force, resulting in an increase in viscosity. The experimental data shows that the sample of Example 1 exhibited a lower value in viscosity measurement, indicating that the graft reaction did not cause a significant increase in viscosity and may have instead improved the fluidity.

[0118] On the other hand, in Comparative Example 1, the polyethylene chain without acryloyl chloride lacked the necessary functional introduction, resulting in a relatively high viscosity. This may be due to the lack of effective chain sliding and functional groups for enhancing fluidity, reducing the flexibility and mobility of the molecular chain. Mechanistically, the polyethylene itself has a relatively high crystallinity, which can cause the material to exhibit strong viscosity at the plasticization temperature. Without the modification of acryloyl chloride, the intermolecular interaction force could not be effectively reduced, restricting the fluidity of the sample during processing.

[0119] Combining the above analysis, the increase in the fluidity and viscosity of the material after removing acryloyl chloride reflects the importance of key functional groups in regulating the polymer structure and properties. Through the analysis of experimental data, it is possible to clearly understand the role of functional components in optimizing the properties of the putty material. For subsequent process optimization, it is recommended to finely control the addition amount and reaction conditions of acryloyl chloride while maintaining a certain functional reaction to achieve a balance between improving material properties and good processability, thereby meeting the application requirements.

[0120] Experiment 2: Tensile strength test experiment of Example 2 and Comparative Example 2

[0121] Experimental purpose:

[0122] Evaluate the effect of removing epichlorohydrin on the tensile strength and toughness of the hydrogenated polyethylene white rubber putty.

[0123] Experimental materials:

[0124] Example 2 Sample: Hydrogenated polyethylene putty containing epichlorohydrin;

[0125] Comparative Example 2 Sample: Hydrogenated polyethylene putty without epichlorohydrin;

[0126] Universal material testing machine;

[0127] Tensile specimen cutter with a model conforming to the standard.

[0128] Experimental procedure:

[0129] Sample preparation:

[0130] Take the same number of samples from Example 2 and Comparative Example 2, and cut them into standard tensile specimens with dimensions based on GB / T528 (Rubber Tensile Property Test Standard).

[0131] All samples are placed for 24 hours under the same conditions (room temperature, humidity) to ensure consistent state.

[0132] Device setting:

[0133] Turn on the universal material testing machine, ensure the normal operation of the equipment, and set the test parameters (prestress, tensile speed, etc.).

[0134] Calibrate the force sensor of the testing machine to ensure the accuracy of measurement.

[0135] Tensile test:

[0136] Place each sample into the fixture of the testing machine, ensure it is clamped and parallel-aligned.

[0137] Select an appropriate tensile speed (usually 100mm / min), start the tensile test, and record the tensile strength and elongation at break of the sample.

[0138] Each sample is tested at least three times repeatedly to ensure the reliability of the data.

[0139] Data recording:

[0140] Record the tensile strength (unit: MPa) and elongation at break (unit: %) of each sample.

[0141] Sort out the results of each test, including the sample name, measurement time, and test data.

[0142] Data analysis:

[0143] Calculate the average tensile strength and elongation at break of Example 2 and Comparative Example 2, and conduct a comparative analysis.

[0144] Tensile strength test experimental data of Example 2 and Comparative Example 2

[0145]

[0146] Summary: In Experiment 2, through the tensile strength tests of Example 2 and Comparative Example 2, we revealed the significant influence of epichlorohydrin on the mechanical properties of hydrogenated polyethylene white rubber putty. As a crosslinking agent, epichlorohydrin can react with polymer chains through its epoxy groups to form a more compact crosslinked network. This crosslinked structure increases the mechanical strength of the polymer and enhances the viscoelasticity of the melt, thereby inhibiting the flow ability of the material, but at the same time enhancing its deformation ability and toughness during the stretching process. This is visually reflected in the experimental data, where the tensile strength of Example 2 is significantly higher than that of Comparative Example 2.

[0147] On the other hand, after removing epichlorohydrin in Comparative Example 2, the intermolecular crosslinking of hydrogenated polyethylene decreases, resulting in a looser structure of the sample. This change in structure weakens the resistance of the material under external forces, manifested as a decrease in tensile strength and elongation at break. The polymer chains lacking crosslinking are prone to slip when subjected to stretching, leading to rupture. The crosslinked structure of Example 2 not only restricts the sliding of the chains but also maintains the elasticity of the material to a certain extent, improving the overall mechanical properties.

[0148] Generally speaking, the results of Experiment 2 clearly show the key role of epichlorohydrin in hydrogenated polyethylene white rubber putty. By enhancing the crosslinking degree of the polymer, it significantly improves its tensile strength and toughness. This discovery provides an important basis for the subsequent optimization and modification directions of the material. It is recommended to continue exploring the addition amounts and crosslinking conditions of different types of crosslinking agents in future research to achieve the best balance of material properties. At the same time, attention should also be paid to the reaction conditions and chain structure regulation during the crosslinking process to maximize the advantages of epichlorohydrin.

[0149] Experiment 3: Curing Rate and Mechanical Property Tests of Example 3 and Comparative Example 3 Experimental Purpose:

[0150] To evaluate the influence of removing the photoinitiator on the curing rate and mechanical properties (tensile strength, adhesion) of hydrogenated polyethylene white rubber putty.

[0151] Experimental Materials:

[0152] Sample of Example 3: Hydrogenated polyethylene putty containing a photoinitiator;

[0153] Sample of Comparative Example 3: Hydrogenated polyethylene putty without a photoinitiator;

[0154] UV curing equipment;

[0155] Universal material testing machine;

[0156] Peel test device;

[0157] Test water and contact angle measuring instrument.

[0158] Experimental procedure:

[0159] Sample preparation:

[0160] Take the same number of samples from Example 3 and Comparative Example 3 respectively, and prepare coating samples with a standard thickness (2 mm).

[0161] Place the samples on an appropriate curing table to ensure that the area and thickness of the samples are consistent.

[0162] Curing rate test:

[0163] Start the ultraviolet curing equipment and set different irradiation times (such as 1, 2, 5, and 10 minutes) respectively.

[0164] After each irradiation, use a hardness tester to measure the change in the hardness of the sample to evaluate the curing rate, and record the hardness value.

[0165] Tensile strength test:

[0166] Use a universal material testing machine to conduct a tensile test on the cured samples, and record the tensile strength and elongation at break.

[0167] Each sample should be tested at least three times to ensure the reliability of the data.

[0168] Adhesion test:

[0169] According to the GB / T6742 standard, conduct a peel test to evaluate the adhesion of the sample after application, and record the peel force value.

[0170] Thermal stability and water contact angle test (optional):

[0171] Use a thermogravimetric analyzer (TGA) and a contact angle measuring instrument to conduct thermal stability and hydrophobicity tests on Example 3 and Comparative Example 3 to obtain more performance data.

[0172] Data recording:

[0173] Record the results of each test, including the sample name, test parameters, and final data.

[0174] Curing rate and mechanical property test data of Example 3 and Comparative Example 3

[0175]

[0176]

[0177] Summary: In Experiment 3, by testing the curing rate and mechanical properties of Example 3 and Comparative Example 3, the significant role of photoinitiators in hydrogenated polyethylene white rubber putty was revealed. The photoinitiator decomposes after absorbing light energy of a specific wavelength, generating free radicals. These free radicals can rapidly initiate polymerization reactions to form cross-linked structures on the polymer chains. The formation of cross-links not only improves the overall strength and hardness of the material but also enhances its heat resistance and flexibility. These reaction mechanisms explain why Example 3 performs significantly better than Comparative Example 3 in terms of curing hardness and tensile strength, etc.

[0178] After removing the photoinitiator from the sample of Comparative Example 3, the kinetic change in the putty curing process decreased

[0179] the cross-linking degree of the material. Without the photoinitiator, although the putty exists in the matrix, its curing rate is significantly reduced, resulting in insufficient connection between polymer chains. The insufficient cross-linking of this structure makes the putty exhibit lower strength and toughness in mechanical properties, especially in tensile tests and adhesion tests, and the results show fragile performance.

[0180] Generally speaking, the results of Experiment 3 confirmed the crucial role of photoinitiators in the curing process of hydrogenated polyethylene white rubber putty. By promoting polymerization reactions and increasing the cross-linking density, photoinitiators improve the mechanical properties of the material, thus effectively meeting the application requirements. Therefore, in future research on formulation optimization and material modification, further exploring the types and use concentrations of photoinitiators will be an important direction to improve the performance of hydrogenated polyethylene putty.

[0181] Although the embodiments of the present invention have been shown and described, it will be understood by those of ordinary skill in the art that various changes, modifications, substitutions, and variations can be made to these embodiments without departing from the principles and spirit of the present invention, and the scope of the present invention is defined by the appended claims and their equivalents.

Claims

1. A production process of a high-performance hydrogenated polyethylene white rubber putty, characterized in that, Comprising: S1: Under a nitrogen atmosphere, linear low-density polyethylene is dissolved in an organic solvent to form a polyethylene solution, and acryloyl chloride is added to graft acrylate groups; S2: Epichlorohydrin is added to the reaction system to introduce epoxy groups, and the solvent and unreacted reagents are removed by vacuum distillation to obtain a hydrogenated polyethylene prepolymer; S3: The above hydrogenated polyethylene prepolymer is subjected to catalytic hydrogenation under the synergistic conditions of supercritical fluid and ionic liquid; S4: The hydrogenated polyethylene prepolymer is mixed and dispersed with nano-fillers modified with dynamic covalent bonds to obtain a mixture; S5: The mixture is subjected to staged triggering of dynamic crosslinking and photocuring reactions using a dual-band UV light source to form a high-performance final coating.

2. The production process of a high-performance hydrogenated polyethylene white rubber putty according to claim 1, characterized in that, The melt index range of the linear low-density polyethylene is 2 - 10 g / 10 min.

3. The production process of a high-performance hydrogenated polyethylene white rubber putty according to claim 1, characterized in that, In the vacuum distillation process, the evaporation temperature is 60 - 80 °C, the degree of vacuum is 10 - 50 kPa, and the vacuum time is 1 - 3 hours.

4. The production process of a high-performance hydrogenated polyethylene white rubber putty according to claim 1, characterized in that, The supercritical fluid is supercritical carbon dioxide, the ionic liquid is 1-butyl-3-methylimidazolium hexafluorophosphate, the catalyst used for catalytic hydrogenation is supported ruthenium nanoparticles, the reaction conditions are a pressure of 7.0 - 8.0 MPa, a temperature of 75 - 85 °C, the reaction time is 1.5 - 2 hours, the catalyst loading is 1 - 5 wt%, and the concentration of the hydrogenated polyethylene prepolymer is 10 - 20 wt%.

5. A production process of a high-performance hydrogenated polyethylene white rubber putty according to claim 1, characterized in that, The dynamic covalent bond is formed through the Diels - Alder reaction and is modified on the surface of nano-silica. The particle size of the nano-fillers is 30 - 50 nm, and the addition amount of the nano-fillers is 5 - 20 wt%.

6. The production process of a high-performance hydrogenated polyethylene white rubber putty according to claim 1, characterized in that, The mixing and dispersion are carried out under vacuum conditions, the vacuum degree range is -0.06 - -0.1 MPa, the mixing temperature is 50 - 70 °C, and the mixing time is 30 minutes to 1 hour.

7. A production process of a high-performance hydrogenated polyethylene white rubber putty according to claim 1, characterized in that, The dual-band UV light source includes a first band of 285 nm and a second band of 365 nm. The irradiation time of the first band is 3 - 5 seconds, and the irradiation time of the second band is 8 - 12 seconds.

8. A production process of a high-performance hydrogenated polyethylene white rubber putty according to claim 1, characterized in that, The photoinitiator for the photocuring reaction is 2,4,6-trimethylbenzoyl-diphenylphosphine oxide, and the addition amount is 1 - 3 wt%.

9. The production process of a high-performance hydrogenated polyethylene white rubber putty according to claim 1, characterized in that, The partial pressure of hydrogen in the hydrogenated polyethylene prepolymer is 2.5 - 3.5 MPa, the hydrogenation reaction time is 1.5 - 2.5 hours, and the degree of hydrogenation ≥ 95%.

10. A production process of a high-performance hydrogenated polyethylene white rubber putty according to claim 2, characterized in that, The molecular weight of the hydrogenated polyethylene prepolymer is 20,000 - 50,000 g / mol.