CN115785573B - Durable antibacterial EPDM (ethylene-propylene-diene monomer) particles and preparation method thereof - Google Patents
Durable antibacterial EPDM (ethylene-propylene-diene monomer) particles and preparation method thereof Download PDFInfo
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Abstract
The invention discloses durable antibacterial EPDM particles, which comprise the following raw materials in parts by weight: (a) at least one ethylene propylene diene monomer; (b) at least (2-mercaptoethyl) -guanidine sulfate; (c) at least comprising coal slag, asbestos powder and a vulcanizing agent. The durable antibacterial EPDM particles provided by the invention adopt the (2-mercaptoethyl) -guanidine sulfate as an antibacterial agent, and are mixed into a formula rest system in the banburying process, when EPDM vulcanization is carried out, mercapto in the (2-mercaptoethyl) -guanidine sulfate and double bonds in the EPDM are subjected to click reaction, and an antibacterial group guanidine is introduced into the EPDM particles, so that the durable antibacterial EPDM particles have better antibacterial activity and antibacterial durability.
Description
Technical Field
The invention belongs to the technical field of plastic track particle production and processing, and particularly relates to durable antibacterial EPDM particles and a preparation method thereof.
Background
EPDM, ethylene propylene diene monomer is a terpolymer of ethylene, propylene and non-conjugated diene, can produce a plurality of colors, can resist ultraviolet irradiation and general chemical reaction by virtue of the excellent performance, and can show the superiority of EPDM color particles especially in patterned construction. The novel anti-skid sports ground is mainly used for sports grounds such as stadium runways, football stadiums, tennis courts, basketball courts and the like, and is widely used for places such as highways, hospitals, hotels, kindergartens, nursing homes, highways, factories and the like which need shock absorption, noise reduction and skid resistance.
At present, the plastic particles are widely applied to sports fields, the plastic particles and the adhesive can be mixed and paved into the plastic fields in the plastic track, and in the artificial lawn, the elasticity of the lawn is increased due to the filling of the plastic particles, and the impact of athletes on the bottom surface can be buffered. The EPDM plastic track mainly comprises a colored sizing material layer and a black rubber bottom layer, and is a fixed type racing track material. The plastic track has the characteristics of good flatness, high compressive strength, proper hardness and elasticity and stable physical properties, is beneficial to the exertion of athlete speed and technology, effectively improves the athletic performance and reduces the injury rate.
The current plastic track is composed of rubber particles or polyurethane particles, pigment, auxiliary agent and filler, most of the plastic tracks are paved outdoors, however, under natural conditions, the surfaces of the rubber particles are cracked under the actions of rain washing, sunlight irradiation and the like, and meanwhile, bacteria are easily generated in the rubber tracks and cause mildew under the long-time moist action, so that the health of a human body is influenced. The Chinese patent application number 201710529359.1 discloses a preparation method of modified rubber particles, which has the technical key points that: firstly, adding organic butyl titanate into a certain amount of sulfuric acid solution, slowly adding ferric oxide and zinc oxide under a severe stirring condition, and performing severe stirring to obtain a clear solution A, and secondly, adding polypropylene fibers, sodium lignin sulfonate and hydroxyethyl cellulose into a certain amount of water, and stirring to obtain a solution B; then, transferring the solution B into the solution A under the water bath condition, reacting for a period of time, and dropwise adding a saturated calcium hydroxide solution to adjust the pH value of the system to be neutral to obtain a solution C; and finally, adding water, rubber particles, polyvinyl alcohol and gelatin into the solution C, stirring, naturally cooling to room temperature, filtering to obtain a filter cake, and drying in an oven to obtain modified rubber particles D. The rubber particles are environment-friendly, and have multiple functions of good ultraviolet resistance, aging resistance, crack resistance, weather resistance, sterilization, deodorization and the like. Although the comprehensive performance of the rubber particles is improved, the method is characterized in that the rubber particles are modified by a chemical method, the steps are compounded, a large amount of waste water and waste gas are generated, the environment is not protected, the added antibacterial substances are inorganic particles such as titanium dioxide, ferric oxide and zinc oxide, the compatibility of the antibacterial agents with the rubber particles is limited, the antibacterial agents are easy to separate out from the rubber particles after long-time use, and the antibacterial performance of the rubber particles is possibly reduced, so that whether the rubber particles have antibacterial durability is still to be purchased.
Thus, it is of great interest to the art to prepare EPDM particles that are durable in antimicrobial activity.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a durable antibacterial EPDM particle and a preparation method thereof, wherein the EPDM particle adopts (2-mercaptoethyl) -guanidine sulfate as an antibacterial agent and is mixed into a formula rest system in the banburying process, when EPDM vulcanization is carried out, mercapto in the (2-mercaptoethyl) -guanidine sulfate and double bonds in the EPDM are subjected to click reaction, and an antibacterial group guanidine is introduced into the EPDM particle, so that the EPDM particle has better antibacterial activity and antibacterial durability.
In order to achieve the above purpose, the present invention provides the following technical solutions:
a durable antimicrobial EPDM particulate comprising the following ingredients:
(a) At least one ethylene propylene diene monomer;
(b) At least containing (2-mercaptoethyl) -guanidine sulfate;
(c) At least contains coal slag, asbestos powder and vulcanizing agent.
Preferably, the (a) component is 15-65 parts by weight, the (b) component is 1-3 parts by weight, and the (c) component is 25-50 parts by weight.
Preferably, the ethylene content in the ethylene propylene diene monomer in the component (a) is 60-75%, and the Mooney viscosity is 60-70.
Preferably, the mass ratio of the coal slag, the asbestos powder and the vulcanizing agent in the component (c) is 10-20:10-20:5-10.
Preferably, the vulcanizing agent in the component (c) is one or more of sulfur, dicumyl peroxide and octyl phenol-formaldehyde vulcanizing resin; the mesh number of the coal slag is 300-400 mesh; the mesh number of the asbestos powder is 600-800 meshes.
Preferably, component (c) further comprises a vulcanization accelerator, an antioxidant and mineral oil; 2-4 parts of vulcanization accelerator, 1-3 parts of antioxidant and 10-25 parts of mineral oil.
Preferably, the vulcanization accelerator is one or more of accelerator TMTD, accelerator D and accelerator M; the antioxidant is one or more of 1010, 1098 or an antioxidant DPPD; the mineral oil is naphthenic oil or white oil.
The invention also provides a preparation method of the durable antibacterial EPDM particles, which comprises the following steps:
S1, weighing raw materials according to a formula, and adding the component (c) into a high-speed mixer for uniform mixing to obtain a mixture;
s2, adding the mixture, the component (a) and the component (b) in the step S1 into a mixing chamber of an internal mixer, and carrying out internal mixing to obtain a mixture after the internal mixing is finished;
S3, placing the mixture in the step S2 on a conveyor, conveying the mixture into a feed hopper of an extruder by using the conveyor, and extruding the mixture to prepare a rubber plate for later use;
s4, placing the rubber plate in the step S3 into a vulcanizing tank for vulcanizing, opening a valve after vulcanizing is completed, and discharging steam to obtain a vulcanized rubber plate;
S5, putting the vulcanized rubber plate obtained in the step S4 into a pulverizer for pulverizing, and sieving by a vibrating screen, wherein the sieving particle size is 1mm-3mm, so that the durable antibacterial EPDM particles are obtained.
Preferably, the banburying in the step S2 is carried out at the temperature of 95-105 ℃ for 20-30min;
Preferably, the vulcanization temperature in the step S4 is 170-190 ℃, the vulcanization time is 70-100min, and the vulcanization pressure is 0.7-1MPa.
Compared with the prior art, the invention has the following beneficial effects:
(1) The (2-mercaptoethyl) -guanidine sulfate is adopted as an antibacterial agent and is mixed into a formula rest system in the banburying process, when EPDM vulcanization is carried out, mercapto in the (2-mercaptoethyl) -guanidine sulfate and double bonds in the EPDM are subjected to click reaction, and an antibacterial group guanidine is introduced into the EPDM particles; meanwhile, the antibacterial activity of the polymer antibacterial agent containing the guanidine group is weaker than that of the guanidine group hung by the corresponding small molecule due to the steric hindrance of the polymer skeleton, so that the (2-mercaptoethyl) -guanidine sulfate introduced by the invention has better antibacterial activity and antibacterial durability.
(2) According to the durable antibacterial EPDM particles prepared by the invention, the coal slag is added into the formula as the filler, so that the utilization of waste is facilitated, the production cost is reduced, the heat resistance and the flame retardance of the product are improved, the condition that the EPDM particles are melted at high temperature is avoided, the heat stability of the EPDM particles is improved, and the comprehensive performance of the EPDM particles is improved.
Detailed Description
The technical solutions of the present invention will be clearly and completely described in connection with the embodiments, and it is obvious that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The ethylene propylene diene monomer is purchased from Dongguan city Shandong feather plastic raw material Co., ltd, and the brand is American Cheng Xiao EPDM (Tao Shidu Bunt) IP 4785HM, and the Mooney viscosity is [ ML (1+4) 100 ℃ C. ]60-70; the naphthenic oil is naphthenic oil 4010; the white oil is purchased from Shandong Help friend lubrication technology Co., ltd and is No. 32 white oil; the polyhexamethylene guanidine phosphate was purchased from Lifan chemical Co., ltd.
Example 1
A durable antimicrobial EPDM particulate comprising the following raw materials: 400g of ethylene propylene diene monomer, (2-mercaptoethyl) -guanidine sulfate 20g, 150g of coal mine slag, 150g of asbestos powder, 80g of dicumyl peroxide, 30g of accelerator D, 1098 g of accelerator D and 200g of naphthenic oil.
A method for preparing durable antimicrobial EPDM particles, comprising the steps of:
S1, weighing raw materials according to a formula, and adding coal slag, asbestos powder, a vulcanizing agent, a vulcanization accelerator, an antioxidant and mineral oil into a high-speed mixer for uniform mixing to obtain a mixture;
S2, adding the mixture obtained in the step S1, ethylene propylene diene monomer rubber and (2-mercaptoethyl) -guanidine sulfate into a mixing chamber of an internal mixer, and carrying out internal mixing at the temperature of 100 ℃ for 25min to obtain a mixture after the internal mixing is completed;
S3, placing the mixture in the step S2 on a conveyor, conveying the mixture into a feed hopper of an extruder by using the conveyor, and extruding the mixture to prepare a rubber plate for later use;
s4, putting the rubber plate in the step S3 into a vulcanizing tank for vulcanization, wherein the vulcanization temperature is 180 ℃, the vulcanization time is 90min, the vulcanization pressure is 0.9MPa, and after the vulcanization is finished, opening a valve and discharging steam to obtain a vulcanized rubber plate;
S5, putting the vulcanized rubber plate obtained in the step S4 into a pulverizer for pulverizing, and sieving by a vibrating screen, wherein the sieving particle size is 1mm-3mm, so that the durable antibacterial EPDM particles are obtained.
Example 2
A durable antimicrobial EPDM particulate comprising the following raw materials: 500g of ethylene propylene diene monomer, (2-mercaptoethyl) -guanidine sulfate, 15g of coal mine slag, 150g of asbestos powder, 70g of sulfur, 30g of accelerator TMTD, 1098, 15g of white oil and 150g of white oil.
A method for preparing durable antimicrobial EPDM particles, comprising the steps of:
S1, weighing raw materials according to a formula, and adding coal slag, asbestos powder, a vulcanizing agent, a vulcanization accelerator, an antioxidant and mineral oil into a high-speed mixer for uniform mixing to obtain a mixture;
S2, adding the mixture obtained in the step S1, ethylene propylene diene monomer rubber and (2-mercaptoethyl) -guanidine sulfate into a mixing chamber of an internal mixer, and carrying out internal mixing at the temperature of 100 ℃ for 25min to obtain a mixture after the internal mixing is completed;
S3, placing the mixture in the step S2 on a conveyor, conveying the mixture into a feed hopper of an extruder by using the conveyor, and extruding the mixture to prepare a rubber plate for later use;
S4, putting the rubber plate in the step S3 into a vulcanizing tank for vulcanization, wherein the vulcanization temperature is 180 ℃, the vulcanization time is 80min, the vulcanization pressure is 0.8MPa, and after the vulcanization is finished, opening a valve and discharging steam to obtain a vulcanized rubber plate;
S5, putting the vulcanized rubber plate obtained in the step S4 into a pulverizer for pulverizing, and sieving by a vibrating screen, wherein the sieving particle size is 1mm-3mm, so that the durable antibacterial EPDM particles are obtained.
Example 3
A durable antimicrobial EPDM particulate comprising the following raw materials: 300g of ethylene propylene diene monomer, (2-mercaptoethyl) -guanidine sulfate, 10g of coal mine slag, 100g of asbestos powder, 50g of sulfur, 20g of accelerator TMTD, 1010 10g of naphthenic oil and 100g of naphthenic oil.
A method for preparing durable antimicrobial EPDM particles, comprising the steps of:
S1, weighing raw materials according to a formula, and adding coal slag, asbestos powder, a vulcanizing agent, a vulcanization accelerator, an antioxidant and mineral oil into a high-speed mixer for uniform mixing to obtain a mixture;
S2, adding the mixture obtained in the step S1, ethylene propylene diene monomer rubber and (2-mercaptoethyl) -guanidine sulfate into a mixing chamber of an internal mixer, and carrying out internal mixing at the temperature of 95 ℃ for 30min to obtain a mixture after the internal mixing is completed;
S3, placing the mixture in the step S2 on a conveyor, conveying the mixture into a feed hopper of an extruder by using the conveyor, and extruding the mixture to prepare a rubber plate for later use;
S4, putting the rubber plate in the step S3 into a vulcanizing tank for vulcanization, wherein the vulcanization temperature is 170 ℃, the vulcanization time is 100min, the vulcanization pressure is 0.7MPa, and opening a valve after the vulcanization is completed, and discharging steam to obtain a vulcanized rubber plate;
S5, putting the vulcanized rubber plate obtained in the step S4 into a pulverizer for pulverizing, and sieving by a vibrating screen, wherein the sieving particle size is 1mm-3mm, so that the durable antibacterial EPDM particles are obtained.
Example 4
A durable antimicrobial EPDM particulate comprising the following raw materials: 650g of ethylene propylene diene monomer, (2-mercaptoethyl) -guanidine sulfate 30g, 200g of coal mine slag, 200g of asbestos powder, 100g of octyl phenol sulfide resin, 40g of accelerator M, 30g of antioxidant DPPD and 250g of white oil.
A method for preparing durable antimicrobial EPDM particles, comprising the steps of:
S1, weighing raw materials according to a formula, and adding coal slag, asbestos powder, a vulcanizing agent, a vulcanization accelerator, an antioxidant and mineral oil into a high-speed mixer for uniform mixing to obtain a mixture;
S2, adding the mixture obtained in the step S1, ethylene propylene diene monomer rubber and (2-mercaptoethyl) -guanidine sulfate into a mixing chamber of an internal mixer, and carrying out internal mixing at 105 ℃ for 20min to obtain a mixture after the internal mixing is completed;
S3, placing the mixture in the step S2 on a conveyor, conveying the mixture into a feed hopper of an extruder by using the conveyor, and extruding the mixture to prepare a rubber plate for later use;
s4, putting the rubber plate in the step S3 into a vulcanizing tank for vulcanization, wherein the vulcanization temperature is 190 ℃, the vulcanization time is 70min, the vulcanization pressure is 1MPa, and after the vulcanization is completed, opening a valve and discharging steam to obtain a vulcanized rubber plate;
S5, putting the vulcanized rubber plate obtained in the step S4 into a pulverizer for pulverizing, and sieving by a vibrating screen, wherein the sieving particle size is 1mm-3mm, so that the durable antibacterial EPDM particles are obtained.
Comparative example
A durable antimicrobial EPDM particulate comprising the following raw materials: 400g of ethylene propylene diene monomer, 20g of polyhexamethylene guanidine phosphate, 150g of coal mine slag, 150g of asbestos powder, 80g of dicumyl peroxide, 30g of accelerator D, 1098 and 20g of naphthenic oil.
A method for preparing durable antimicrobial EPDM particles, comprising the steps of:
S1, weighing raw materials according to a formula, and adding coal slag, asbestos powder, a vulcanizing agent, a vulcanization accelerator, an antioxidant and mineral oil into a high-speed mixer for uniform mixing to obtain a mixture;
S2, adding the mixture obtained in the step S1, ethylene propylene diene monomer and polyhexamethylene guanidine phosphate into a mixing chamber of an internal mixer, and carrying out internal mixing at a temperature of 100 ℃ for 25min to obtain a mixture after the internal mixing is completed;
S3, placing the mixture in the step S2 on a conveyor, conveying the mixture into a feed hopper of an extruder by using the conveyor, and extruding the mixture to prepare a rubber plate for later use;
s4, putting the rubber plate in the step S3 into a vulcanizing tank for vulcanization, wherein the vulcanization temperature is 180 ℃, the vulcanization time is 90min, the vulcanization pressure is 0.9MPa, and after the vulcanization is finished, opening a valve and discharging steam to obtain a vulcanized rubber plate;
S5, putting the vulcanized rubber plate obtained in the step S4 into a pulverizer for pulverizing, and sieving by a vibrating screen, wherein the sieving particle size is 1mm-3mm, so that the durable antibacterial EPDM particles are obtained.
Cutting the durable antibacterial EPDM vulcanized rubber plates prepared in the examples 1-4 and the comparative example S4 into samples with the size of 5cm multiplied by 5cm and the thickness of 6mm, placing the samples in 75% alcohol for sterilization for 30min, washing off the alcohol on the surfaces of the materials in sterilized PBS, placing the sterilized PBS into a sterilization plate, taking bacterial suspensions of prepared staphylococcus aureus ATCC6538P and escherichia coli ATTC8739, respectively dripping 100 microliters on each sample to be tested and each sample to be tested, uniformly coating, after action for 6h, respectively putting the sample into a test tube containing 5ml of PBS by using sterile forceps, fully mixing and eluting bacteria, adding PBS buffer solution for dilution to 100 times, respectively sucking 0.5ml of the samples, placing the plates in two plates, pouring the plates in 15ml of LB solid culture medium cooled to 40 ℃, rotating the plates to enable the plates to be fully uniform, overturning the plates after agar solidification, culturing the plates at 37 ℃ for 24h, and counting viable bacteria.
The bacteriostasis rate was calculated as follows: x=100% × (a-B)/a
Wherein, X-antibacterial rate,%; a-average colony count of control samples; b-average colony count of samples tested.
The control sample was a pure EPDM rubber sheet.
The test method of the antibacterial durability comprises the following steps: after the test pieces were left outdoors for 180 days, the antibacterial activity was again measured, and the test results were as shown in table 1 below:
TABLE 1
As can be seen from the above Table 1, the durable antimicrobial EPDM particles prepared by the present invention have good antimicrobial properties, and compared with the polyhexamethylene guanidine phosphate antimicrobial agent added in the comparative example, the EPDM particles of the present invention have better antimicrobial durability and good application prospects.
Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made therein without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (8)
1. The durable antibacterial EPDM particles are characterized by being prepared from the following raw materials in parts by weight:
(a) At least one ethylene propylene diene monomer;
(b) At least containing (2-mercaptoethyl) -guanidine sulfate;
(c) At least comprises coal slag, asbestos powder and vulcanizing agent;
The composition (a) comprises, by weight, 15-65 parts of a composition (b) 1-3 parts of a composition (c) 25-50 parts of a composition (c); (a) The ethylene content in the ethylene propylene diene monomer in the components is 60-75%, and the Mooney viscosity is 60-70;
The preparation method of the durable antibacterial EPDM particles comprises the following steps:
s1, weighing raw materials according to a formula, and adding the component (c) into a high-speed mixer for uniform mixing to obtain a mixture;
S2, adding the mixture, the component (a) and the component (b) in the step S1 into a mixing chamber of an internal mixer, and carrying out internal mixing to obtain a mixture after the internal mixing is finished;
S3, placing the mixture in the step S2 on a conveyor, conveying the mixture into a feed hopper of an extruder by using the conveyor, and extruding the mixture to prepare a rubber plate for later use;
s4, placing the rubber plate in the step S3 into a vulcanizing tank for vulcanizing, opening a valve after vulcanizing is completed, and discharging steam to obtain a vulcanized rubber plate;
S5, putting the vulcanized rubber plate obtained in the step S4 into a pulverizer for pulverizing, and sieving by a vibrating screen, wherein the sieving particle size is 1mm-3mm, so that the durable antibacterial EPDM particles are obtained.
2. The durable antimicrobial EPDM granule as claimed in claim 1, wherein the mass ratio of the coal slag, the asbestos powder and the vulcanizing agent in the component (c) is 10 to 20:10-20:5-10.
3. The durable antimicrobial EPDM particles of claim 1, wherein the vulcanizing agent in component (c) is one or more of sulfur, dicumyl peroxide, and octyl phenol-formaldehyde vulcanizing resin; the mesh number of the coal slag is 300-400 mesh; the mesh number of the asbestos powder is 600-800 meshes.
4. A durable antimicrobial EPDM particle as claimed in claim 1, wherein component (c) further comprises a vulcanization accelerator, an antioxidant and mineral oil; 2-4 parts of vulcanization accelerator, 1-3 parts of antioxidant and 10-25 parts of mineral oil.
5. The durable antimicrobial EPDM particles of claim 4, wherein the vulcanization accelerator is one or more of accelerator TMTD, accelerator D, and accelerator M; the antioxidant is one or more of 1010, 1098 or an antioxidant DPPD; the mineral oil is naphthenic oil or white oil.
6. A process for the preparation of the durable, antimicrobial EPDM particles as claimed in any one of claims 1 to 5, comprising the steps of:
s1, weighing raw materials according to a formula, and adding the component (c) into a high-speed mixer for uniform mixing to obtain a mixture;
S2, adding the mixture, the component (a) and the component (b) in the step S1 into a mixing chamber of an internal mixer, and carrying out internal mixing to obtain a mixture after the internal mixing is finished;
S3, placing the mixture in the step S2 on a conveyor, conveying the mixture into a feed hopper of an extruder by using the conveyor, and extruding the mixture to prepare a rubber plate for later use;
s4, placing the rubber plate in the step S3 into a vulcanizing tank for vulcanizing, opening a valve after vulcanizing is completed, and discharging steam to obtain a vulcanized rubber plate;
S5, putting the vulcanized rubber plate obtained in the step S4 into a pulverizer for pulverizing, and sieving by a vibrating screen, wherein the sieving particle size is 1mm-3mm, so that the durable antibacterial EPDM particles are obtained.
7. The method according to claim 6, wherein the internal mixing in step S2 is carried out at a temperature of 95-105℃for 20-30min.
8. The method according to claim 6, wherein the vulcanizing temperature in the step S4 is 170-190 ℃, the vulcanizing time is 70-100min, and the vulcanizing pressure is 0.7-1MPa.
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