Preparation process of polypropylene antibacterial fiber material

By using diether catalysts and hydrogen adjustment methods in the process of polypropylene fiber materials, combined with uniform dispersion of organic antibacterial additives and composite antioxidants, the problem of poor antibacterial effect is solved, and the excellent mechanical properties and significant antibacterial effect of polypropylene antibacterial fiber materials are achieved.

CN120025628APending Publication Date: 2025-05-23PETROCHINA CO LTD
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Patent Information

Application Number
CN202311558279.0
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2023-11-21
Publication Date
2025-05-23

AI Technical Summary

Technical Problem

The antibacterial effect of polypropylene fiber materials produced by existing processes is not good, mainly due to the selection of antibacterial agents and the uneven dispersion of antibacterial agents in the base material.

Method used

The diether catalyst, external electron donor and activator are used to carry out prepolymerization reaction with refined propylene, and organic antibacterial additives and composite antioxidants are added. The antibacterial agent is uniformly dispersed in the polypropylene base through the hydrogen adjustment process and the extrusion granulation process.

Benefits of technology

The obtained polypropylene antibacterial fiber material has excellent mechanical properties and elasticity, and has excellent antibacterial effects. It can kill or inhibit bacterial proliferation within a certain period of time and improve people's health.

✦ Generated by Eureka AI based on patent content.

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Abstract

The invention belongs to the field of macromolecular antibacterial materials, and particularly relates to a preparation process of a polypropylene antibacterial material. According to the polypropylene antibacterial fiber particle prepared by the invention, propylene is taken as a main raw material, a diether catalyst, an external electron donor and an activating agent are added, polypropylene is produced by a hydrogen regulation process, then an organic antibacterial auxiliary agent and a composite antioxidant are added, a working section is switched to high-pressure operation, each parameter is a corresponding numerical value during high-pressure operation, and the polypropylene antibacterial fiber particle is obtained. The prepared polypropylene antibacterial fiber material has excellent mechanical properties and elasticity, and has an excellent antibacterial effect, the mildew-proof grade reaches the highest grade of 0, and the polypropylene antibacterial fiber material shows excellent long-acting antibacterial performance.
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Description

Technical Field

[0001] The invention belongs to the field of macromolecular antibacterial materials, and in particular relates to a preparation process of a polypropylene antibacterial material. Background Art

[0002] Antibacterial fiber plastic is a type of plastic that inhibits or kills bacteria, mold, yeast, algae, and even viruses that contaminate it in the environment where it is used. It is a well-known new material that is healthy and hygienic. The development of antibacterial fiber materials is closely related to the country's scientific and technological level, the degree of social progress, and whether laws, regulations, and standards are sound. The application of antibacterial polypropylene fiber is both economical and convenient, and can also improve people's health by killing or inhibiting bacterial proliferation, preventing or reducing disease transmission.

[0003] Polypropylene fiber is the most commonly used and important raw material for non-woven fabrics. According to the needs, giving non-woven fabrics antibacterial function can further inhibit the reproduction of bacteria and viruses and reduce the risk of cross infection. In practical applications, antibacterial materials are generally not required to quickly kill harmful microorganisms, but focus on inhibiting their growth and reproduction during long-term use to achieve the purpose of protecting the environment and improving personal hygiene and protection levels. The main method for producing antibacterial polypropylene fiber is to add antibacterial agents to the fiber base material. The main difficulty currently lies in the selection of antibacterial agents and the uniform dispersion of antibacterial agents in the base material. Summary of the invention

[0004] In order to solve the problem that the antibacterial effect of polypropylene fiber materials manufactured by existing processes is poor, which is mainly due to the selection of antibacterial agents and the uneven dispersion of antibacterial agents in base materials, a preparation process of polypropylene antibacterial material is provided.

[0005] A preparation process of polypropylene antibacterial fiber material comprises the following process steps:

[0006] A diether catalyst is mixed with vaseline oil and vaseline fat, and the mixture is kept warm for later use;

[0007] Refined propylene is obtained by removing free water, organic sulfur, sulfide, light components, bound water, arsenic and phosphorus from liquid propylene, and the refined propylene is subjected to polymerization reaction;

[0008] In a high-pressure environment, the heat-insulated diether catalyst, the external electron donor and the activator are mixed, and then prepolymerized with the refined propylene, the refined propylene is added in an amount of 1000-1100 kg / h, and the prepolymerization reaction is carried out after reaching the preset process parameters of the prepolymerization reaction;

[0009] The polymer produced by the prepolymerization reaction is continuously added with hydrogen and refined propylene for the first hydrogenation polymerization reaction, the amount of refined propylene added is 14500-15500 kg / h, the hydrogen concentration is 2200±50 ppm, and the hydrogenation polymerization reaction is performed after reaching the preset process parameters of the first hydrogenation polymerization reaction;

[0010] The polymer generated by the first hydrogenation polymerization reaction is continuously added with hydrogen and refined propylene for a second hydrogenation polymerization reaction, wherein the amount of refined propylene added is 8500-10500 kg / h, and the hydrogen is controlled to be 2200±50 ppm. After reaching the preset process parameters of the second hydrogenation polymerization reaction, the hydrogenation polymerization reaction is continued;

[0011] The polymer generated by the second hydrogenation polymerization reaction is separated after flashing, and the flashed propylene is recovered; the polypropylene slurry after flashing is deactivated by polymer steaming and then dried;

[0012] Adding an organic antibacterial additive, a composite antioxidant and calcium stearate to the dried polypropylene base material, adjusting the barrel temperature and the temperature of the heat transfer oil of the extrusion granulator, the rotation speed, the blade air pressure, the pelletizing water flow rate and the water temperature of the pelletizer to the preset process parameters, and performing extrusion granulation to obtain a polypropylene antibacterial fiber material;

[0013] The entire process conditions ensure that the powder melt index is controlled at 34-40g / 10min.

[0014] The mass ratio of the activator to the total propylene feed in the prepolymerization and polymerization process is 0.000014-0.000016:1, the mass ratio of the external electron donor to the total propylene feed in the prepolymerization and polymerization process is 0.0001-0.00017:1, and the mass ratio of the activator to the external electron donor is 100-150:1.

[0015] The diether catalyst controls the catalyst stroke at 8-18%.

[0016] The diether catalyst is ZN127 catalyst; the activator is triethylaluminum, and the purity of triethylaluminum is 100%; the external electron donor is cyclohexylmethyldimethoxysilane, and the purity of cyclohexylmethyldimethoxysilane is 3.5%.

[0017] The organic antibacterial additive is Micropel ZPT98, and the minimum addition concentration of Micropel ZPT98 is 200 ppm.

[0018] The composite antioxidant is 2,6-di-tert-butyl-4-methylphenol, and the minimum addition concentration of 2,6-di-tert-butyl-4-methylphenol is 1500 ppm.

[0019] The preset process parameters of the prepolymerization reaction are: reaction temperature of 20±1°C, pressure of 3.9±0.1Mpa, reaction time of 10-15 minutes, and catalyst stroke of 8-18%;

[0020] The preset process parameters of the first hydropolymerization reaction are: reaction temperature of 70±0.5°C, pressure of 3.85±0.1Mpa, reaction time of 1.5-2.0 hours, and power of the second axial flow pump of 170-205kw;

[0021] The preset process parameters of the second hydrogenation polymerization reaction are: reaction temperature of 70±0.5°C, pressure of 3.80±0.1Mpa, reaction time of 1.0-1.5 hours, and power of the third axial flow pump of 160-180kw.

[0022] During the drying process, the material level of the drying tank is controlled at 35-55%, and the material level of the steaming tank is controlled at 45-55%; during the steaming deactivation process, the steam flow rate in the steaming system is controlled at 650-800 kg / h, and the steam flow rate at the bottom of the steaming system is controlled at 200-250 kg / h.

[0023] The temperature of the heat transfer oil of the extrusion granulator is 235°C±2°C at the first outlet and 230°C±2°C at the second outlet; the rotation speed of the pelletizer is 680-850rpm, and the blade air pressure is 0.43-0.51Mpa; the pelletizing water flow rate is 240-255kg / h, and the water temperature is 45-50°C.

[0024] The production load of the entire preparation process is controlled at 11-13t / h.

[0025] Compared with the prior art, the present invention has the following beneficial effects:

[0026] The polypropylene antibacterial fiber particles prepared by the present invention use propylene as the main raw material, add a diether catalyst, an external electron donor and an activator, produce polypropylene through a hydrogen adjustment process, and then add an organic antibacterial auxiliary agent and a composite antioxidant. The preset reaction process parameters make the organic antibacterial auxiliary agent and the composite antioxidant uniformly dispersed in the polypropylene base material, and the structural properties of the organic antibacterial auxiliary agent are not affected under continuous high-temperature shearing. The prepared polypropylene antibacterial fiber material has excellent mechanical properties and elasticity, and has excellent antibacterial effect. The preparation process of the present invention is simple, the raw materials are easy to obtain, and it is easy to industrialize production. The prepared antibacterial fiber material and antibacterial non-woven fabric plastic can kill or inhibit the proliferation of bacteria contaminated on the fiber and the cloth surface within a certain period of time. Compared with the conventional chemical and physical disinfection methods, it is economical and convenient, and can prevent or reduce the spread of diseases by killing or inhibiting the proliferation of bacteria, thereby improving the health level of the people. When producing antibacterial fiber materials with a melt index of 34-40g / 10min, the amount of hydrogenation in the reaction system is smaller, and the conversion is faster. The antibacterial fiber material was tested for microorganisms by a third-party testing agency, and the results showed that the Escherichia coli was >99%, Staphylococcus aureus was >98%, and the Aspergillus niger, Chaetomium globosum, Paecilomyces variotii, Penicillium funiculosum, and Trichoderma longibrachiatum were tested, and the mildew resistance level all reached the highest level 0.

[0027] Furthermore, the main catalyst is selected as ZN127 high-efficiency catalyst, which has high activity, good hydrogen adjustment sensitivity and high catalytic efficiency. BRIEF DESCRIPTION OF THE DRAWINGS

[0028] In order to more clearly illustrate the technical solution of the embodiment of the present invention, the following briefly introduces the drawings required for use in the embodiment:

[0029] Figure 1 This is a process flow chart for preparing the polypropylene antibacterial fiber material of the present invention;

[0030] Figure 2 This is a process flow chart of 100,000 tons / year polypropylene antibacterial fiber material according to an embodiment of the present invention;

[0031] Figure 3 and Figure 4 This is a test report on the antibacterial properties of the non-woven fabric products produced by the present invention. DETAILED DESCRIPTION

[0032] The present invention will be further described below in conjunction with the accompanying drawings:

[0033] The present invention adopts the Spheripol-II generation polypropylene process device of Basell Company of Italy, with a designed production capacity of 100,000 tons / year of polypropylene, an annual operation of 8,000 hours, and can produce 37 grades of homopolymers. The future market application prospects of antibacterial polypropylene fiber are broad. With the in-depth promotion of high-quality economic development, antibacterial fibers will usher in a broad application market. Antibacterial polypropylene can be made into fibers and non-woven fabrics, which are mainly used in the medical and health fields. The end products are: (1) Protective medical supplies: surgical gowns, masks, face masks, patient gowns and bed sheets, gauze for disinfection, etc.; (2) Women's hygiene materials, baby diapers, elderly incontinence pads, etc.; (3) Antibacterial polypropylene non-woven fabric shoe materials: inhibit the reproduction of bacteria and fungi on the feet, and eliminate athlete's foot / foot odor caused by fungal and bacterial infections; (4) Filter materials for air conditioners: improve antibacterial ability and reduce product ash content.

[0034] Polypropylene fiber materials can be produced by oxide degradation method and hydrogen adjustment method. The peroxide method mainly adds peroxide during twin-screw extrusion granulation to break the molecular chains with larger molecular weight and degrade it into polypropylene with relatively lower molecular weight. The fiber materials prepared by the degradation method have the advantages of narrow molecular weight distribution and good fluidity, but the presence of peroxide residues may cause the fiber materials to have odor, fast aging and other problems. The hydrogen adjustment method is to add an appropriate concentration of hydrogen as a chain transfer agent in the polymerization system to reduce the relative molecular weight of polypropylene. Combined with the preferred catalyst system, by adjusting the appropriate polymerization process parameters, the production of high-fluidity fiber materials can also be achieved. Its products have the advantages of no peroxide residues and low odor.

[0035] In order to meet the requirements of processing and use performance, the melt index range of polypropylene antibacterial fiber material is 34-40g / 10min. The crystallization temperature needs to be higher than 110℃, the tensile yield stress should reach above 30.0MPa, the tensile fracture stress should reach above 8.0MPa, the antibacterial ability should be greater than 99%, and the mildew resistance level should be greater than level 1. The main method of production control is to add antibacterial agents to the fiber base material. The main difficulty lies in the selection of antibacterial agents and the uniform dispersion of antibacterial agents in the base material. In order to ensure the stability of the properties of polypropylene, it is required that the antibacterial agent does not react chemically with other polypropylene stabilizers and additives after addition, and the antibacterial agent does not change under high temperature shear, and the antibacterial agent particles do not agglomerate. The polypropylene reaction section is switched to high-pressure operation, and the alarm values ​​of each parameter are changed to the corresponding values ​​during high-pressure operation. The catalyst system was changed from CS-2-B to the corresponding diether catalyst, and the amount of hydrogenation was adjusted at the same time. The melt index of polypropylene powder was adjusted from 3g / 10min to the corresponding melt index using the hydrogen adjustment method. Organic zinc antibacterial additives, composite antioxidants, and calcium stearate were added in the granulation section to finally produce qualified new products.

[0036] like Figure 1 and Figure 2As shown, a specific process of preparing a polypropylene antibacterial fiber material includes the following steps:

[0037] Catalyst preparation: a diether catalyst was mixed with vaseline oil and vaseline fat, and kept warm for later use; 40 kg of the diether catalyst was mixed with 117.5 L of vaseline oil and 55 L of vaseline fat, and stored at 10°C for later use.

[0038] Propylene refining: free water, organic sulfur and sulfide contained in liquid propylene are removed by molecular sieve tower, and the total sulfur content of liquid propylene after desulfurization is less than 1ppm; light components such as carbon monoxide and bound water in the desulfurized liquid propylene are removed by propylene light component stripping tower, and finally, arsenic and phosphorus in liquid propylene are removed by catalyst tower to obtain refined propylene, which is sent to feed tank (D302) and sent to polymerization reaction system by high-speed pump for polymerization reaction;

[0039] Polymerization reaction: the mass ratio of the activator to the total propylene feed in the prepolymerization and polymerization process is 0.000014-0.000016:1, the mass ratio of the external electron donor to the total propylene feed in the prepolymerization and polymerization process is 0.0001-0.00017:1, the mass ratio of the activator to the external electron donor is 100-150:1, and the diether catalyst controls the catalyst stroke at 8-18%.

[0040] The reaction system is operated under high pressure, which is more difficult to operate and requires higher precision. The insulated diether catalyst, external electron donor and activator are mixed in the pre-contact tank (D201) and then enter the prepolymerization reactor (R200). The prepolymerization reactor is controlled to reach the preset process parameters, and the amount of refined propylene added is 1000-1100 kg / h; the preset process parameters of the prepolymerization reactor are: reaction temperature is 20±1°C, pressure is 3.9±0.1Mpa, reaction time is 10-15 minutes, and catalyst stroke is 8-18%;

[0041] The polymer in the prepolymerization reactor enters the first loop reactor (R201), and hydrogen and refined propylene are added. The amount of refined propylene added is 14500-15500 kg / h, and the hydrogen concentration is 2200±50 ppm. The first loop reactor is controlled to reach the preset process parameters before a hydrogenation polymerization reaction is carried out; the preset process parameters in the first loop reactor are: reaction temperature of 70±0.5°C, pressure of 3.85±0.1Mpa, reaction time of 1.5-2.0 hours, and the power of the second axial flow pump (P201) is 170-205kw.

[0042] The polymer produced in the first loop reactor enters the second loop reactor (R202), and hydrogen and refined propylene are added. The amount of refined propylene added is 8500-10500kg / h, and the hydrogen is controlled to 2200±50ppm. After the second loop reactor reaches the preset process parameters, the hydrogenation polymerization reaction continues; the preset process parameters in the second loop reactor are: reaction temperature of 70±0.5℃, pressure of 3.80±0.1Mpa, reaction time of 1.0-1.5 hours, and the power of the third axial flow pump (P202) is 160-180kw.

[0043] Flash evaporation and steam drying: the polymer generated in the second loop reactor is flashed and then enters the flash tank (D301) for separation, and the high-pressure propylene recovery system recovers the flashed propylene; the polypropylene slurry in the flash tank enters the low-pressure degassing system (F301) and then enters the steaming system (D501) for polymer steaming deactivation, and then enters the drying system for drying treatment to obtain ultra-high fluidity and high crystallinity polypropylene to the extrusion granulation system; the process parameters in the flash evaporation and steam drying steps are: the material level of the drying tank in the drying system is controlled at 35-55%, the material level of the steaming tank is controlled at 45-55%, the steam flow rate of the steaming system is controlled at 650-800kg / h, and the steam flow rate of the bottom of the steaming system is controlled at 200-250kg / h.

[0044] Extrusion granulation: Due to the high melt mass flow rate and very low melt strength of polypropylene antibacterial fiber material, the barrel temperature and heat transfer oil temperature of the extrusion granulator were appropriately lowered based on the drawing material, the speed of the pelletizer was increased, and the throttle valve opening, pelletizing water flow, water temperature, etc. were adjusted synchronously. Specifically, the dried polypropylene base material is sent to the extrusion granulation system, and organic antibacterial additives, composite antioxidants and calcium stearate are added to the polypropylene base material. The barrel temperature and heat transfer oil temperature of the extrusion granulator, the rotation speed of the pelletizer, the feed air pressure, pelletizing water flow rate and water temperature are adjusted to the preset process parameters, and extrusion granulation is carried out to obtain polypropylene antibacterial fiber material; the heat transfer oil temperature of the extrusion granulator is 235℃±2℃ at the first outlet (P808) and 230℃±2℃ at the second outlet (P809); the rotation speed of the pelletizer is 680-850rpm, the feed air pressure is 0.43-0.51Mpa, and the pelletizer rotation speed and feed air pressure are determined according to the pelletizer current and the shape and size of the pellets; the pelletizing water flow rate is 240-255kg / h, the water temperature is 45-50℃, and the pelletizing water flow rate and water temperature are determined according to the operation of the pelletizer.

[0045] The entire process conditions ensure that the powder melt index is controlled at 34-40g / 10min.

[0046] Catalyst system

[0047] Main catalyst: The diether catalyst is ZN127 produced by Basell. The diether catalyst has the advantages of high activity, good hydrogen adjustment sensitivity and high stereospecificity, which is conducive to the production by hydrogen adjustment method.

[0048] Activator: triethylaluminum (TEAl), 100% pure.

[0049] Electron donor: cyclohexylmethyldimethoxysilane (Donor-C), purity 3.5%.

[0050] Additive formula

[0051] In the preliminary test, the morphology of the collected antibacterial additives was analyzed for the initial extrusion particles, and three antibacterial additives were selected, including organic, high-efficiency silver and high-efficiency zinc. After further testing, it was found that the organic antibacterial additive MicropelZPT98 was the first choice, and the minimum addition concentration was 200ppm. The composite antioxidant can be a phenolic compound with a sterically hindered structure. The preferred composite antioxidant is 2,6-di-tert-butyl-4-methylphenol, and the minimum addition concentration of 2,6-di-tert-butyl-4-methylphenol is 1500ppm. The extrusion granulation process of polypropylene antibacterial fiber material still uses the composite antioxidant of non-woven fiber material, and the antibacterial agent is added at the same time. In actual production, the amount of additives added needs to be adjusted in time according to the test values ​​of mechanical properties.

[0052] Polymerization reaction process parameters

[0053] The polymerization process parameters of polypropylene antibacterial fiber material are shown in Table 1. The hydrogen concentration needs to be adjusted in time according to the melt mass flow rate, TEAL / Donor needs to be adjusted according to the isotacticity test results, and the control temperature and pressure of the loop reactor can be appropriately adjusted according to the actual reaction conditions.

[0054] Table 1 Polymerization process parameters of antibacterial fiber products

[0055]

[0056] Wherein, TEAL / FT2003 is the mass ratio of activator to the total propylene feed in the prepolymerization and polymerization process, DONOR / FT2003 is the mass ratio of external electron donor to the total propylene feed in the prepolymerization and polymerization process, TEAL / DONOR is the mass ratio of activator to external electron donor, FIC1501 stroke is the load of the catalyst metering pump, LIC5001 is the material level of the steaming tank, LIC5301 is the material level of the drying tank, FIC5001 is the intermediate steam flow rate of the steaming system, and FIC5002 is the bottom steam flow rate of the steaming system.

[0057] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. It should be pointed out that a person skilled in the art can make several improvements and modifications without departing from the technical principles of the present invention.

[0058] Application Examples

[0059] The 100,000 tons / year polypropylene unit of Qingyang Petrochemical Company adopts the Spheripol-II generation polypropylene process technology of Italy's Basell Company. It has a designed production capacity of 100,000 tons / year of polypropylene, an annual operation time of 8,000 hours, and can produce a total of 44 grades of homopolymers (34 grades) and random copolymers (10 grades).

[0060] Starting from 9:00 on December 14, 2021, the amount of hydrogen added was adjusted based on QY36S, the hydrogen concentration of AIC2001B was set to 2150ppm, the hydrogen concentration of AIC2002B was set to 2150ppm, the TEAL / FT2003 addition ratio was adjusted to 0.14g / kg, the TEAL / DONOR addition ratio was 130wt%, and the DONOR / FT2003 addition ratio was 1.4g / kg. At 10:00, the catalyst stroke was controlled at 11.5%, and the production load of the stable device was 12t / h. When adding organic antimicrobial agents in the later stage, attention should be paid to the uniform dispersion of the antimicrobial agents in the polypropylene base material, and at the same time, the structural properties of the antimicrobial agents should not be affected under continuous high-temperature shear. This requires more precise control of the barrel temperature control and throttle valve control of the extrusion granulator. 10:10 Adjust the temperature of the heat transfer oil, adjust the outlet of P808 to 235℃, and the outlet of P809 to 230℃; adjust the pelletizing water flow to 250kg / h, control the temperature at 47℃, adjust the pelletizer speed to 690rpm, and the air pressure of the blade to 0.47MPa. Control the barrel temperature of the extrusion granulator from the first to the seventh section to be 220℃, 225℃, 230℃, 240℃, 230℃, 225℃, and 220℃ respectively. 10:20 Add organic antibacterial additives Micropel ZPT98 and 2,6-di-tert-butyl-4-methylphenol, and the addition concentration of Micropel ZPT98 is 220ppm. 10:35 Cut the finished product silo and stabilize the operation of the granulator. To narrow the melt index, the amount of hydrogen needs to be adjusted in time according to the melt index. When the melt index of the pellets reaches the range of 34-40g / 10min, prepare to add antibacterial agents to produce polypropylene antibacterial fiber materials. At 12:30 on December 15, the hydrogen concentration in the reactor was adjusted, and the trial production of polypropylene antibacterial fiber material was completed, with a total of more than 300 tons of finished products produced. The Quality Inspection and Measurement Department coordinated a dedicated person to conduct quality inspection and analysis and guide production at any time; timely analyze the melt flow rate of powder and granular products, and adjust the amount of hydrogen added in time according to the analysis results to ensure that the product is qualified as soon as possible. When adjusting the hydrogen feed, closely monitor the density of the first and second loop reactors. If the density increases by more than 2kg / m per minute,3 This indicates that the hydrogen is adjusted too fast and should be slowed down. At the same time, the power and on-site current of the first axial flow pump (P200), the second axial flow pump (P201), and the third axial flow pump (P202) should be monitored. Increase the opening of the regulating valve position number for the exhaust system to discharge non-condensable gas and set its flow rate to 200-300kg / h to reduce the non-condensable gas content in the recovered propylene.

[0061] The antibacterial performance test of non-woven products is outsourced by the Lanzhou Chemical Research Center of PetroChina to contact qualified units for testing. When the antibacterial rate is ≥90%, the sample has an antibacterial effect; when the antibacterial rate is ≥99%, the sample has a good antibacterial effect. The test bacteria for the antibacterial rate are Escherichia coli and Staphylococcus aureus, and the test cycle is 10 days. The mildew resistance level of plastics is divided into 0, 1, 2, and 3 levels, with 0 being the highest level, and 3 and below being low-level mildew resistance levels. The test bacteria for the mildew resistance level are Aspergillus niger, Chaetomium globosum, Penicillium variotii, Penicillium funiculum and Trichoderma longibrachiatum, and the test cycle is 1 month. Figure 3 and Figure 4 As shown, after the first industrial product of the antibacterial fiber material was placed for 90 days, a third-party testing agency conducted a microbial test on the antibacterial fiber material, and the results showed that the Escherichia coli was greater than 99%, the Staphylococcus aureus was greater than 98%, and the Aspergillus niger, Chaetomium globosum, Paecilomyces variotii, Penicillium funiculum, and Trichoderma longibrachiatum were tested, and the mildew resistance level all reached the highest level 0, showing excellent long-term antibacterial performance.

[0062] The above embodiments are only used to illustrate the technical solutions of the present invention rather than to limit the same. Although the present invention has been described in detail with reference to the above embodiments, a person skilled in the art can still modify or make equivalent substitutions to the specific implementations of the present invention. Any modifications or equivalent substitutions that do not depart from the spirit and scope of the present invention are within the scope of protection of the claims of the present invention to be approved.

Claims

1. A process for preparing polypropylene antibacterial fiber material, It is characterized in that The process steps include: A diether catalyst is mixed with vaseline oil and vaseline fat, and the mixture is kept warm for later use; Refined propylene is obtained by removing free water, organic sulfur, sulfide, light components, bound water, arsenic and phosphorus from liquid propylene, and the refined propylene is subjected to polymerization reaction; In a high-pressure environment, the heat-insulated diether catalyst, the external electron donor and the activator are mixed, and then prepolymerized with the refined propylene, the refined propylene is added in an amount of 1000-1100 kg / h, and the prepolymerization reaction is carried out after reaching the preset process parameters of the prepolymerization reaction; The polymer produced by the prepolymerization reaction is continuously added with hydrogen and refined propylene for the first hydrogenation polymerization reaction, the amount of refined propylene added is 14500-15500 kg / h, the hydrogen concentration is 2200±50 ppm, and the hydrogenation polymerization reaction is performed after reaching the preset process parameters of the first hydrogenation polymerization reaction; The polymer generated by the first hydrogenation polymerization reaction is continuously added with hydrogen and refined propylene for a second hydrogenation polymerization reaction, wherein the amount of refined propylene added is 8500-10500 kg / h, and the hydrogen is controlled to be 2200±50 ppm. After reaching the preset process parameters of the second hydrogenation polymerization reaction, the hydrogenation polymerization reaction is continued; The polymer generated by the second hydrogenation polymerization reaction is separated after flashing, and the flashed propylene is recovered; the polypropylene slurry after flashing is deactivated by polymer steaming and then dried; Adding an organic antibacterial additive, a composite antioxidant and calcium stearate to the dried polypropylene base material, adjusting the barrel temperature and the temperature of the heat transfer oil of the extrusion granulator, the rotation speed, the blade air pressure, the pelletizing water flow rate and the water temperature of the pelletizer to the preset process parameters, and performing extrusion granulation to obtain a polypropylene antibacterial fiber material; The entire process conditions ensure that the powder melt index is controlled at 34-40g / 10min.

2. The preparation process of the polypropylene antibacterial fiber material according to claim 1, It is characterized in that The mass ratio of the activator to the total propylene feed in the prepolymerization and polymerization process is 0.000014-0.000016:1, the mass ratio of the external electron donor to the total propylene feed in the prepolymerization and polymerization process is 0.0001-0.00017:1, and the mass ratio of the activator to the external electron donor is 100-150:

1.

3. The preparation process of the polypropylene antibacterial fiber material according to claim 1, It is characterized in that The diether catalyst controls the catalyst stroke at 8-18%.

4. The process for preparing the polypropylene antibacterial fiber material according to claim 1, It is characterized in that The diether catalyst is ZN127 catalyst; the activator is triethylaluminum, and the purity of triethylaluminum is 100%; the external electron donor is cyclohexylmethyldimethoxysilane, and the purity of cyclohexylmethyldimethoxysilane is 3.5%.

5. The preparation process of the polypropylene antibacterial fiber material according to claim 1, It is characterized in that The organic antibacterial additive is Micropel ZPT98, and the minimum addition concentration of Micropel ZPT98 is 200 ppm.

6. The process for preparing the polypropylene antibacterial fiber material according to claim 1, It is characterized in that The composite antioxidant is 2,6-di-tert-butyl-4-methylphenol, and the minimum addition concentration of 2,6-di-tert-butyl-4-methylphenol is 1500 ppm.

7. The process for preparing the polypropylene antibacterial fiber material according to claim 1, It is characterized in that The preset process parameters of the prepolymerization reaction are: reaction temperature of 20±1°C, pressure of 3.9±0.1Mpa, reaction time of 10-15 minutes, and catalyst stroke of 8-18%; The preset process parameters of the first hydropolymerization reaction are: reaction temperature of 70±0.5°C, pressure of 3.85±0.1Mpa, reaction time of 1.5-2.0 hours, and power of the second axial flow pump of 170-205kw; The preset process parameters of the second hydrogenation polymerization reaction are: reaction temperature of 70±0.5°C, pressure of 3.80±0.1Mpa, reaction time of 1.0-1.5 hours, and power of the third axial flow pump of 160-180kw.

8. The process for preparing the polypropylene antibacterial fiber material according to claim 1, It is characterized in that During the drying process, the material level of the drying tank is controlled at 35-55%, and the material level of the steaming tank is controlled at 45-55%; during the steaming deactivation process, the steam flow rate in the steaming system is controlled at 650-800 kg / h, and the steam flow rate at the bottom of the steaming system is controlled at 200-250 kg / h.

9. The process for preparing the polypropylene antibacterial fiber material according to claim 1, It is characterized in that The temperature of the heat transfer oil of the extrusion granulator is 235°C±2°C at the first outlet and 230°C±2°C at the second outlet; the rotation speed of the pelletizer is 680-850rpm, and the blade air pressure is 0.43-0.51Mpa; the pelletizing water flow rate is 240-255kg / h, and the water temperature is 45-50°C.

10. The process for preparing the polypropylene antibacterial fiber material according to claim 1, It is characterized in that The production load of the entire preparation process is controlled at 11-13t / h.