阅读说明：本技术 一种特种可消毒重复使用熔喷布材料及其制备方法 (Special type reusable melt-blown fabric material capable of being disinfected and preparation method thereof ) 是由 冯杰 陈云 刘洪� 于 2020-06-19 设计创作，主要内容包括：本发明公开了一种特种可消毒重复使用熔喷布材料及其制备方法,属于环境过滤技术领域,所述熔喷布材料以纤维级聚苯硫醚、氢氧化钠、一卤苯、水和N-甲基吡咯烷酮为原料聚合为聚苯硫醚树脂,再经挤出工艺和熔喷法制得,其中一卤苯为一氯苯、苯甲醇、苯酚和碘苯中的任意一种,纤维级聚苯硫醚为硫封端的纤维级聚苯硫醚；本发明利用纤维级聚苯硫醚和第三单体一卤苯的作用极大地提高了聚苯硫醚熔喷布材料的流动性,同时不影响可纺性和耐温性,得到的聚苯硫醚熔喷布材料稳定性好,用本发明的熔喷布材料制备的口罩过滤效果好,重复使用率高。(The invention discloses a special type reusable melt-blown fabric material capable of being disinfected and a preparation method thereof, belonging to the technical field of environmental filtration, wherein the melt-blown fabric material is prepared by polymerizing fiber-grade polyphenylene sulfide, sodium hydroxide, monohalobenzene, water and N-methyl pyrrolidone serving as raw materials into polyphenylene sulfide resin through an extrusion process and a melt-blowing method, wherein the monohalobenzene is any one of monochlorobenzene, benzyl alcohol, phenol and iodobenzene, and the fiber-grade polyphenylene sulfide is sulfur-terminated fiber-grade polyphenylene sulfide; the invention greatly improves the fluidity of the polyphenylene sulfide melt-blown fabric material by utilizing the effects of fiber-grade polyphenylene sulfide and third monomer-halobenzene, does not influence the spinnability and the temperature resistance, and the obtained polyphenylene sulfide melt-blown fabric material has good stability.)

1. A special type reusable melt-blown cloth material capable of being disinfected is characterized in that the melt-blown cloth material is prepared by polymerizing fiber-grade polyphenylene sulfide, sodium hydroxide, monohalobenzene, water and N-methylpyrrolidone serving as raw materials into polyphenylene sulfide resin and then performing an extrusion granulation process.

2. A specialty sterilizable reusable meltblown fabric material according to claim 1, wherein said monohalobenzene is any one of monochlorobenzene, benzyl alcohol, phenol and iodobenzene.

3. A special sterilizable reusable meltblown fabric material according to claim 1, wherein the weight average molecular weight of the fiber-grade polyphenylene sulfide is 10000-45000, and the melt viscosity is 100-300 Pa.s.

4. A specialty sterilizable reusable meltblown fabric material according to claim 1, wherein said fiber-grade polyphenylene sulfide is sulfur-terminated fiber-grade polyphenylene sulfide.

5. A method for preparing a special type sterilizable reusable melt-blown fabric material according to any one of claims 1 to 4, comprising the following preparation steps:

(1) feeding: adding N-methyl pyrrolidone into a reaction kettle, sequentially adding fiber-grade polyphenylene sulfide resin, sodium hydroxide, monohalobenzene and water into the reaction kettle, introducing nitrogen for replacement for 6-10 times, replacing the pressure with 1-5 bar, and starting stirring;

(2) ring-opening polymerization: heating the temperature of a reaction kettle of the system obtained in the step (1) to 250-270 ℃, and keeping the temperature for 1-6 hours;

(3) cooling: after the constant temperature in the step (2) is finished, cooling the reaction system to 190-230 ℃, and keeping the temperature of the system at 190-230 ℃;

(4) heating and repolymerization: heating the ring-opening polymerization reaction system obtained in the step (3) to 250-280 ℃ again, slowly adding water into the reaction kettle, keeping the temperature of the reaction kettle at 250-280 ℃, and reacting for 1-10 hours;

(5) separation and drying: after the reaction is finished, cooling to below 200 ℃, separating a product by using a centrifugal machine, and filtering, washing and drying to obtain the polyphenylene sulfide resin;

(6) and (3) heat treatment: carrying out heat treatment on the dried polyphenylene sulfide resin at 105-150 ℃ for 10-60 min, and heating to 150-200 ℃ for 10-60 min;

(7) melt extrusion: and (4) granulating the polyphenylene sulfide resin treated in the step (6) by using a double-screw extruder and a filter screen to obtain the melt-blown fabric material.

6. A method for preparing a special type of sterilizable and reusable meltblown fabric material according to claim 5, wherein in step (1), the molar ratio of the materials is, fibrous polyphenylene sulfide: sodium hydroxide: monohalobenzene: water: n-methylpyrrolidone ═ 1 (0.10-0.30): (0.01-0.05): (0.1-0.5): (2-11).

7. A preparation method of a special type sterilizable reusable melt-blown fabric material according to claim 5, wherein in the step (2), the temperature rise rate of the reaction kettle is 0.8-3 ℃/min, and in the step (3), the temperature drop rate of the reaction system is 2-3 ℃/min.

8. A special type of a sterilizable reusable meltblown fabric material according to claim 5, wherein in step (4), the water is ultrapure water, distilled water or deionized water, and the amount added is 1.5 to 10.5 moles.

9. A special type of a sterilizable reusable meltblown fabric material according to claim 5, wherein in step (4), the water is added at a rate of 0.2 to 0.5kg/min and the reaction pressure is controlled within 0.5 to 10 MPa.

10. A special type of a method for preparing a sterilizable reusable meltblown fabric material according to claim 5, wherein in step (7), the temperature of each zone of the twin-screw extruder is controlled within 260 to 350 ℃, and the mesh number of the filter screen is 100 to 1500.

Technical Field

The invention relates to the technical field of environmental filtration, in particular to a special type reusable melt-blown fabric material capable of being disinfected and a preparation method thereof.

Background

At present, along with the prevalence of SARS, H1N1, NCP and other viruses, harmful substances in the air are increased, the haze is more and more serious, the traditional disposable mask can not meet the isolation requirement of people on the viruses, and in addition, the polypropylene melt-blown material can be aged in the use process and can not be used for a long time. Meanwhile, the environment-friendly treatment problem is serious due to a large number of disposable masks, the melt-blown cloth material can be repeatedly sterilized and used, and the pollution of the disposable masks to the environment can be greatly reduced.

Polyphenylene sulfide is special engineering resin which is industrially produced by Philips in the last 60 th century, has the characteristics of high temperature resistance, radiation protection, self-flame retardance, high strength, high modulus and the like, has excellent comprehensive performance, and is widely applied to the fields of automobiles, environmental protection, war industry, aerospace and the like. Meanwhile, the melt-blown non-woven fabric made of the polyphenylene sulfide has excellent high temperature resistance, flame retardant property, chemical corrosion resistance and filtering property, and the polyphenylene sulfide is hardly dissolved in any organic solvent below 200 ℃, so that the melt-blown non-woven fabric is an excellent reusable melt-blown fabric material. But the polyphenylene sulfide is difficult to use in the melt-blown process, the melt-blown processing process is 40-80 ℃ higher than the processing temperature of a common polypropylene melt-blown material, and the processability of the polyphenylene sulfide resin is poor due to the high molecular weight and poor fluidity in a molten state in the melt-blown processing process, so that a spinneret orifice is easily blocked, and the subsequent processing of the non-woven fabric is extremely difficult; if ordinary low molecular weight polyphenylene sulfide is selected, crosslinking and carbonization easily occur during the melt blowing process due to the presence of a large amount of low molecular weight resin.

US patent US6110589 describes a method for making polyphenylene sulfide meltblown fibers and nonwovens. According to the method, a proper amount of polypropylene is added into the polyphenylene sulfide to improve the spinnability of the polyphenylene sulfide, and the addition amount of the polypropylene is 1-40%. The result shows that the flow spinnability of PPS can be obviously improved when more than 5 percent of polypropylene is added into the PPS, and the spinneret orifices are clean and have no blocking phenomenon. The addition of polypropylene improves the processability of polyphenylene sulfide, but causes the temperature resistance, the dimensional stability and the like of the polyphenylene sulfide non-woven fabric to be greatly reduced.

Therefore, how to improve the fluidity of the polyphenylene sulfide and ensure that the performance of the prepared melt-blown fabric material is not influenced is still a great technical problem, and based on the technical problem, a special type reusable melt-blown fabric material capable of being disinfected and a preparation method thereof are provided.

Summary yao

The invention aims to: the special type reusable melt-blown cloth material capable of being disinfected and the preparation method thereof are provided, the fluidity of the polyphenylene sulfide melt-blown material is greatly improved by utilizing the effects of fiber-grade polyphenylene sulfide and third monomer-halobenzene, the spinnability and the temperature resistance are not influenced, the obtained polyphenylene sulfide melt-blown material is good in stability, and a mask prepared from the melt-blown cloth material is good in filtering effect and high in reuse rate.

The technical scheme adopted by the invention is as follows:

in order to achieve the purpose, the invention provides a special type reusable melt-blown fabric material capable of being disinfected, which is prepared by polymerizing fiber-grade polyphenylene sulfide, sodium hydroxide, monohalobenzene, water and N-methylpyrrolidone serving as raw materials into polyphenylene sulfide resin and then performing an extrusion granulation process.

Preferably, the monohalobenzene is any one of monochlorobenzene, benzyl alcohol, phenol and iodobenzene.

Preferably, the weight-average molecular weight of the fiber-grade polyphenylene sulfide is 10000-45000, and the melt viscosity is 100-300 Pa.s.

Preferably, the fiber-grade polyphenylene sulfide is sulfur-terminated fiber-grade polyphenylene sulfide. The melt-blown filamentation is easy to break after the ring-opening polymerization of the polyphenylene sulfide of the injection molding grade and the coating grade, so that the performance is reduced, the filtering effect of the melt-blown cloth is gradually reduced in the using process, the repeated use effect is not good, the activity of the fiber grade polyphenylene sulfide after the sulfur end capping is higher, the molecular chain is easier to link after the third monomer, namely halogen benzene, is added, and the filtering effect is more excellent after the melt-blown filamentation.

The invention also provides a preparation method of the special type reusable melt-blown fabric material capable of being disinfected, which comprises the following preparation steps:

(1) feeding: adding N-methyl pyrrolidone into a reaction kettle, sequentially adding fiber-grade polyphenylene sulfide resin, sodium hydroxide, monohalobenzene and water into the reaction kettle, introducing nitrogen for replacement for 6-10 times, replacing the pressure with 1-5 bar, and starting stirring;

(2) ring-opening polymerization: heating the temperature of a reaction kettle of the system obtained in the step (1) to 250-270 ℃, and keeping the temperature for 1-6 hours;

(3) cooling: after the constant temperature in the step (2) is finished, cooling the reaction system to 190-230 ℃, and keeping the temperature of the system at 190-230 ℃;

(4) heating and repolymerization: heating the ring-opening polymerization reaction system obtained in the step (3) to 250-280 ℃ again, slowly adding water into the reaction kettle, keeping the temperature of the reaction kettle at 250-280 ℃, and reacting for 1-10 hours;

(5) separation and drying: after the reaction is finished, reducing the temperature to be below 200 ℃ at a cooling rate of 3-5 ℃/min, separating a product by using a centrifuge, and filtering, washing and drying to obtain polyphenylene sulfide resin;

(6) and (3) heat treatment: carrying out heat treatment on the dried polyphenylene sulfide resin at 105-150 ℃ for 10-60 min, then heating to 150-200 ℃ for 10-60 min, and enabling the polyphenylene sulfide melt-blown fabric material to have good toughness and oxidation resistance after heat treatment;

(7) melt extrusion: and (4) granulating the polyphenylene sulfide resin treated in the step (6) by using a double-screw extruder and a filter screen to obtain the melt-blown material.

Preferably, in the step (1), the molar ratio of each material is that the fiber-grade polyphenylene sulfide: sodium hydroxide: monohalobenzene: water: n-methylpyrrolidone ═ 1 (0.10-0.30): (0.01-0.05): (0.1-0.5): (2-11).

Preferably, in the step (2), the temperature rise rate of the reaction kettle is 0.8-3 ℃/min, and the temperature drop rate of the reaction system in the step (3) is 2-3 ℃/min.

Preferably, in the step (4), the added water is ultrapure water, distilled water or deionized water, and the adding amount is 1.5-10.5 mol.

Preferably, in the step (4), the adding rate of the water is 0.2-0.5 kg/min, and the reaction pressure is controlled within 0.5-10 MPa.

Preferably, in the step (7), the temperature of each zone of the twin-screw extruder is controlled within 260-350 ℃, and the mesh number of the filter screen is 100-1500 meshes.

In summary, due to the adoption of the technical scheme, the invention has the beneficial effects that:

1. according to the invention, a third monomer, namely, halobenzene, is introduced to be grafted with the open-loop fiber-grade polyphenylene sulfide macromolecules to form the melt-blown special material with good fluidity, so that the molecular weight of fiber-grade resin can be reduced in a balanced manner, the melt index can be increased to 500-2000 g/10min, the fluidity of fiber-grade polyphenylene sulfide is improved, the melt-blown fabric material is easier to melt-blow and form, the spinnability and the temperature resistance are not influenced, and the obtained polyphenylene sulfide melt-blown fabric has good stability.

2. The invention adopts fiber-grade polyphenylene sulfide as a raw material to synthesize the polyphenylene sulfide melt-blown material, the molecular weight is 10000-45000, the filtering effect is excellent after melt-blown filamentation, the resin impurity content is low, a melt-blown cloth equipment die head is not easy to block during preparation of melt-blown cloth, the production efficiency is improved, and the equipment failure rate is reduced.

3. The melt-blown filamentation is easy to break after the ring-opening polymerization of the polyphenylene sulfide of the injection molding grade and the coating grade, so that the performance is reduced, the filtering effect of the melt-blown cloth is gradually reduced in the using process, and the repeated use effect is poor.

4. After the filter mask prepared by the melt-blown cloth material is worn, the filter mask is processed by alcohol spraying, hot water soaking and 84 disinfectant soaking and then is reused, the filtering performance of the filter mask is still stable, the recycling frequency of the mask is improved, the environmental protection pressure and the use cost are greatly reduced, a polymerization system is single, a reaction solvent of the polymerization system is easy to recover, the recovery difficulty is reduced, and the pollution of the disposable mask to the environment is indirectly reduced.

Detailed Description

The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.