阅读说明：本技术 防护口罩第一层和第二层改性pp粒料及纤维的制备方法 (Preparation method of first layer and second layer modified PP granules and fibers of protective mask ) 是由 关义臣 关义重 关建 李鹏 于 2020-05-26 设计创作，主要内容包括：本发明公开了一种防护口罩第一层和第二层改性PP粒料及纤维的制备方法,涉及防护口罩加工材料技术领域,本发明通过上述技术方案制备的PP改性粒料,不仅能有效抑制细菌和病毒在口罩表面的繁殖,而且能保证口罩对细菌和病毒的截留以及吸附容量,从而延长细菌和病毒在体外的停留时间而将其杀灭,结合口罩第一层所具有抗菌和抗病毒功效的有机基团和光催化的多孔无机纳米粒子吸收太阳光中5％的紫外光催化杀死残留细菌和病毒。同时所制PP改性粒料使口罩单次使用后只需在太阳下晾晒就可杀灭口罩第一层表面残留的细菌和病毒并恢复口罩第二层的荷电性。(The invention discloses a preparation method of modified PP granules and fibers of a first layer and a second layer of a protective mask, and relates to the technical field of protective mask processing materials. Meanwhile, the prepared PP modified granules can kill bacteria and viruses remained on the surface of the first layer of the mask and recover the charge property of the second layer of the mask only by airing the mask in the sun after single use.)

1. Modified PP aggregate of protective mask first layer, its characterized in that: the polypropylene modified polypropylene is prepared by modifying polypropylene, and the specific modification method comprises the following steps:

(1) dissolving anhydride and an initiator in an organic solvent, adding the mixture into a high-speed mixer, adding polypropylene into the high-speed mixer, uniformly mixing, feeding the obtained mixture into a double-screw extruder, and carrying out melt reaction to obtain anhydride grafted polypropylene;

(2) dissolving polyamine and a condensing agent in an organic solvent, adding the mixture into a high-speed mixer, adding the prepared anhydride grafted polypropylene into the high-speed mixer, uniformly mixing, feeding the obtained mixture into a double-screw extruder, and carrying out melt reaction to obtain amide grafted polypropylene;

(3) dissolving organic salt in water, adding an inorganic porous material, performing ultrasonic treatment, performing reduced pressure distillation to remove water, and grinding to obtain a carrier;

(4) adding an epoxy silane coupling agent into ethanol, adding a nano photocatalyst, carrying out ultrasonic treatment, then adding the prepared carrier, continuing ultrasonic treatment, carrying out suction filtration, washing with ethanol, drying, and grinding to obtain porous nanoparticles;

(5) and adding the prepared amide grafted polypropylene and the prepared porous nanoparticles into a high-speed mixer, uniformly mixing, feeding the obtained mixture into a double-screw extruder, and performing melt extrusion granulation to obtain the first-layer modified PP granules of the protective mask.

2. The modified PP granules for the first layer of protective mask according to claim 1, wherein: the mass ratio of the polypropylene to the acid anhydride is 100:5-20, the mass ratio of the organic salt, the inorganic porous material, the epoxy silane coupling agent to the nano photocatalyst is 1-10:5-20:1-10:1-10, and the molar ratio of the acid anhydride, the initiator, the polyamine, the condensing agent and the epoxy silane coupling agent is 1-2:0.01-0.1: 1-2: 1-2.

3. The modified PP granules for the first layer of protective mask according to claim 1, wherein: the acid anhydride is one of maleic anhydride, succinic anhydride and benzoic anhydride, the initiator is dicumyl peroxide, the polyamine is one of hexamethylene diamine, diethylenetriamine, triethylene tetramine, m-phenylenediamine and isophorone diamine, and the condensing agent is one or more of dicyclohexylcarbodiimide, 4-dimethylaminopyridine, 1-ethyl- (3-dimethylaminopropyl) carbonyl diimine hydrochloride and 1-hydroxybenzotriazole.

4. The modified PP granules for the first layer of protective mask according to claim 1, wherein: the organic solvent is selected from one of DMF, toluene and DMSO.

5. The modified PP granules for the first layer of protective mask according to claim 1, wherein: the temperature of each section from the feeding port to the machine head of the double-screw extruder is as follows: 190 ℃ at 160 ℃ at 170 ℃ at 200 ℃ at 170 ℃ at 180 ℃ at 210 ℃ at 180 ℃ at 170 ℃ at 200 ℃ at 170 ℃ at 250 r/min.

6. The modified PP granules for the first layer of protective mask according to claim 1, wherein: the organic salt is quaternary ammonium salt or pyridinium, the inorganic porous material is one of diatomite, molecular sieve, activated carbon and porous alumina, and the nano photocatalyst is nano titanium dioxide or nano zinc oxide.

7. The modified PP granules of the first layer of the protective mask prepared according to any one of claims 1 to 6 are subjected to alkali treatment to prepare modified PP granules of the second layer of the protective mask.

8. The modified PP pellet of the second layer of protective mask according to claim 7, wherein: the alkali is sodium hydroxide solution, and the concentration is 0.5-5 mol/L.

9. The first layer modified PP pellet of the protective mask prepared according to any one of claims 1 to 6 is used for preparing fibers through wet spinning.

10. The second layer modified PP pellet of the protective mask prepared according to claim 7 is used for preparing fibers through wet spinning.

The technical field is as follows:

the invention relates to the technical field of protective mask processing materials, in particular to a preparation method of modified PP granules and fibers of a first layer and a second layer of a protective mask.

Background art:

the protective mask is a respiratory protection article aiming at preventing the transmission of some respiratory infectious microorganisms and protecting the health. The protective mask is divided into a daily protective mask and a medical protective mask, the daily protective mask is made of a filtering material, and a wearer overcomes the resistance of the filtering material to air flow by autonomous respiration, so the protective mask is called a self-absorption filtering respirator; the medical protective mask consists of a mask surface body and a tightening belt, wherein the mask surface body is divided into an inner layer, a middle layer and an outer layer, the inner layer is common sanitary gauze or non-woven fabric, the middle layer is an ultra-fine polypropylene fiber melt-blown material layer, and the outer layer is a non-woven fabric or ultra-fine polypropylene melt-blown material layer.

Most of the existing masks are disposable masks, and under the condition, the applicant deeply develops processing materials of the reusable mask on the basis of the existing long-term research, successfully develops first-layer and second-layer modified PP granules of the protective mask, improves the protection performance of the mask through modification treatment of the existing PP and realizes the reusability of the mask.

The invention content is as follows:

the technical problem to be solved by the invention is to provide a preparation method of modified PP granules and fibers of a first layer and a second layer of a protective mask, which is used for improving the protective performance of the mask by modifying the existing PP and realizing the reusability of the mask, thereby solving the problem that the protective performance of the protective mask is easy to lose efficacy and cannot be reused to generate a large amount of medical wastes which are difficult to treat.

The technical problem to be solved by the invention is realized by adopting the following technical scheme:

the first layer of modified PP granules of the protective mask is formed by modifying polypropylene, and the specific modification method comprises the following steps:

(1) dissolving anhydride and an initiator in an organic solvent, adding the mixture into a high-speed mixer, adding polypropylene into the high-speed mixer, uniformly mixing, feeding the obtained mixture into a double-screw extruder, and carrying out melt reaction to obtain anhydride grafted polypropylene;

(2) dissolving polyamine and a condensing agent in an organic solvent, adding the mixture into a high-speed mixer, adding the prepared anhydride grafted polypropylene into the high-speed mixer, uniformly mixing, feeding the obtained mixture into a double-screw extruder, and carrying out melt reaction to obtain amide grafted polypropylene;

(3) dissolving organic salt in water, adding an inorganic porous material, performing ultrasonic treatment, performing reduced pressure distillation to remove water, and grinding to obtain a carrier;

(4) adding an epoxy silane coupling agent into ethanol, adding a nano photocatalyst, carrying out ultrasonic treatment, then adding the prepared carrier, continuing ultrasonic treatment, carrying out suction filtration, washing with ethanol, drying, and grinding to obtain porous nanoparticles;

(5) and adding the prepared amide grafted polypropylene and the prepared porous nanoparticles into a high-speed mixer, uniformly mixing, feeding the obtained mixture into a double-screw extruder, and performing melt extrusion granulation to obtain the first-layer modified PP granules of the protective mask.

The mass ratio of the polypropylene to the acid anhydride is 100:5-20, the mass ratio of the organic salt, the inorganic porous material, the epoxy silane coupling agent to the nano photocatalyst is 1-10:5-20:1-10:1-10, and the molar ratio of the acid anhydride, the initiator, the polyamine, the condensing agent and the epoxy silane coupling agent is 1-2:0.01-0.1: 1-2: 1-2.

The acid anhydride is one of maleic anhydride, succinic anhydride and benzoic anhydride, the initiator is dicumyl peroxide, the polyamine is one of hexamethylene diamine, diethylenetriamine, triethylene tetramine, m-phenylenediamine and isophorone diamine, and the condensing agent is one or more of dicyclohexylcarbodiimide, 4-dimethylaminopyridine, 1-ethyl- (3-dimethylaminopropyl) carbonyl diimine hydrochloride and 1-hydroxybenzotriazole.

The organic solvent is selected from one of DMF, toluene and DMSO.

The temperature of each section from the feeding port to the machine head of the double-screw extruder is as follows: 190 ℃ at 160 ℃ at 170 ℃ at 200 ℃ at 170 ℃ at 180 ℃ at 210 ℃ at 180 ℃ at 170 ℃ at 200 ℃ at 170 ℃ at 250 r/min.

The organic salt is quaternary ammonium salt or pyridinium, the inorganic porous material is one of diatomite, molecular sieve, activated carbon and porous alumina, and the nano photocatalyst is nano titanium dioxide or nano zinc oxide.

The second layer of modified PP granules of the protective mask is prepared by alkali treatment of the first layer of modified PP granules of the protective mask.

The alkali is sodium hydroxide solution, and the concentration is 0.5-5 mol/L.

And preparing fibers by wet spinning by using the first layer of modified PP granules of the protective mask prepared by the method.

And preparing fibers by wet spinning by using the prepared modified PP granules on the second layer of the protective mask.

In the technical scheme, the organic group with antibacterial and antiviral activities is introduced to the polypropylene by adding the quaternary ammonium salt or the pyridinium, and the quaternary ammonium salt or the pyridinium enters pores of the inorganic porous material through ions, so that the problem of falling off can be caused and the potential safety hazard of being inhaled by the mouth and the nose is formed. Aiming at the problem, the invention also selects the diamino quinazoline as the polyamine, the amino group contained in the diamino quinazoline can react with the carboxyl and the epoxy group to complete the grafting modification, and the contained quinazoline has antibacterial and antiviral activity, and simultaneously, the chemical bond connection is adopted, so the shedding problem is effectively solved.

The polyamine is a diaminoquinazoline.

According to the invention, organic groups with excellent antibacterial and antiviral properties and porous inorganic nanoparticles with photocatalytic effects are introduced through chemical grafting or doping to prepare the PP modified granules for the first layer of the protective mask, so that active sites for adsorbing viruses are further increased on the premise of not increasing filtration resistance and reducing hydrophobicity, and the PP grafted modified granules are subjected to alkali treatment to introduce charged functional groups to endow renewable electrostatic effects, so that the modified PP granules for the second layer of the protective mask are obtained.

The invention has the beneficial effects that: according to the PP modified granular material prepared by the technical scheme, the propagation of bacteria and viruses on the surface of the mask can be effectively inhibited, the interception and adsorption capacity of the mask to the bacteria and viruses can be ensured, so that the stay time of the bacteria and the viruses in vitro is prolonged and the bacteria and the viruses are killed, 5% of ultraviolet light in sunlight is absorbed by combining organic groups with antibacterial and antiviral effects on the first layer of the mask and photocatalytic porous inorganic nanoparticles to catalyze and kill residual bacteria and viruses, the defense effect of the mask is effectively improved, and the problem that the protective performance of the protective mask is easy to lose efficacy and cannot be reused to generate a large amount of medical waste which is difficult to treat is solved. Meanwhile, the prepared PP modified granules can kill bacteria and viruses remained on the surface of the first layer of the mask and recover the charge property of the second layer of the mask only by airing the mask in the sun after single use.

The specific implementation mode is as follows:

in order to make the technical means, the creation characteristics, the achievement purposes and the effects of the invention easily understood, the invention is further described with reference to the specific embodiments.

The polypropylene in the following examples and comparative examples is from Ningbo Taiwan 5090T; the diatomite is white diatomite from Yurun sea water purification materials Limited of consolidated city; the nano titanium dioxide is from Beijing German island gold science and technology Limited, and has an average grain diameter of 20 nm; the nanometer zinc oxide is from Beijing Deke island gold science and technology ltd, and has an average particle size of 50 nm.