CN114163732B - Melt-blown polypropylene material and preparation method and application thereof - Google Patents

Melt-blown polypropylene material and preparation method and application thereof Download PDF

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CN114163732B
CN114163732B CN202111675506.9A CN202111675506A CN114163732B CN 114163732 B CN114163732 B CN 114163732B CN 202111675506 A CN202111675506 A CN 202111675506A CN 114163732 B CN114163732 B CN 114163732B
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melt
component
blown
parts
polypropylene material
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CN114163732A (en
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李振华
杨友强
丁超
丁敏
魏金刚
张龙飞
杨方强
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Guangdong Kingfa Science and Technology Co Ltd
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Guangdong Kingfa Science and Technology Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
    • C08J9/06—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent
    • C08J9/08—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent developing carbon dioxide
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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    • C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/0061—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof characterized by the use of several polymeric components
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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    • C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/0066—Use of inorganic compounding ingredients
    • C—CHEMISTRY; METALLURGY
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    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
    • C08J9/06—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent
    • C08J9/10—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent developing nitrogen, the blowing agent being a compound containing a nitrogen-to-nitrogen bond
    • C08J9/102—Azo-compounds
    • C08J9/103—Azodicarbonamide
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
    • C08J9/06—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent
    • C08J9/10—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent developing nitrogen, the blowing agent being a compound containing a nitrogen-to-nitrogen bond
    • C08J9/104—Hydrazines; Hydrazides; Semicarbazides; Semicarbazones; Hydrazones; Derivatives thereof
    • C08J9/105—Hydrazines; Hydrazides; Semicarbazides; Semicarbazones; Hydrazones; Derivatives thereof containing sulfur
    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
    • D04H1/54—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties by welding together the fibres, e.g. by partially melting or dissolving
    • D04H1/541—Composite fibres, e.g. sheath-core, sea-island or side-by-side; Mixed fibres
    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
    • D04H1/54—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties by welding together the fibres, e.g. by partially melting or dissolving
    • D04H1/56—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties by welding together the fibres, e.g. by partially melting or dissolving in association with fibre formation, e.g. immediately following extrusion of staple fibres
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2203/00—Foams characterized by the expanding agent
    • C08J2203/02—CO2-releasing, e.g. NaHCO3 and citric acid
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2203/00—Foams characterized by the expanding agent
    • C08J2203/04—N2 releasing, ex azodicarbonamide or nitroso compound
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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    • C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
    • C08J2323/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
    • C08J2323/10—Homopolymers or copolymers of propene
    • C08J2323/12—Polypropene
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
    • C08J2323/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
    • C08J2323/10—Homopolymers or copolymers of propene
    • C08J2323/14—Copolymers of propene
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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    • C08J2423/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
    • C08J2423/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
    • C08J2423/10—Homopolymers or copolymers of propene
    • C08J2423/12—Polypropene
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2423/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
    • C08J2423/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
    • C08J2423/10—Homopolymers or copolymers of propene
    • C08J2423/14—Copolymers of propene
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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    • Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
    • Y02P70/62—Manufacturing or production processes characterised by the final manufactured product related technologies for production or treatment of textile or flexible materials or products thereof, including footwear

Abstract

The invention relates to a melt-blown polypropylene material, a preparation method and application thereof. The melt-blown polypropylene material comprises a component A and a component B; the component A comprises polypropylene resin, a free radical initiator, a nucleating agent, an antioxidant and the like; the component B comprises a component A, foaming electret master batches and the like. According to the invention, through the regulation and control of a specific formula and a processing process, a large number of micropores and pits exist on the surface of the melt-blown fiber obtained by stretching the melt-blown polypropylene material, after the melt-blown fabric is manufactured, bacteria and oily particles remain on a melt-blown layer and are collected in holes on the surface of the melt-blown fiber when being filtered, compared with the smooth surface of a common fiber, more bacteria and oily particles are difficult to load by electrostatic adsorption, the melt-blown polypropylene material disclosed by the invention can obviously improve the specific surface area and the filtering capability, has an excellent oily filtering effect and an oily filtering efficiency retention rate, and has a great application prospect in the aspect of preparing labor protection articles suitable for severe environments.

Description

Melt-blown polypropylene material and preparation method and application thereof
Technical Field
The invention belongs to the field of high polymer materials, and particularly relates to a melt-blown polypropylene material, and a preparation method and application thereof.
Background
The mask is used as an important protective article for daily protection and virus protection of people, the melt-blown cloth playing a role of core protection is called as a heart of a medical surgical mask and an N95 mask, a melt-blown non-woven process is adopted, high-pressure and high-heat air is adopted to draft polymers into superfine fibers with average diameter less than 5 mu m, the fibers in a filter material are randomly arranged and formed by crossing interlayer, a fiber filter layer with multiple bending channels is formed, and the fibers are provided with enough charges by applying an electric field to the fibers, so that particles entering the filter layer can be adsorbed.
Improving the filtering effect of the melt-blown cloth is an important way for effectively improving the filtering performance of the mask. At present, the prior patent discloses a melt-blown polypropylene material, a preparation method and application thereof, wherein a peroxide master batch is obtained by utilizing a micro-foaming polypropylene and peroxide to carry out blending modification, and then the melt-blown polypropylene material is obtained by blending extrusion modification with water electret powder and other additives, so that a melt-blown polypropylene product which is easy to spin is obtained, and the obtained polypropylene non-woven fabric has the characteristics of low resistance and high filtration efficiency, and the filtration efficiency is kept for a long time. Although the oily filtration efficiency is improved to more than 95.5%, a certain lifting space is still provided.
Therefore, developing a melt-blown cloth material with better oily filtering effect has important research significance and application value.
Disclosure of Invention
The invention aims to overcome the defect or defect that a certain lifting space still exists in the oily filtering effect of melt-blown cloth in the prior art, and provides a melt-blown polypropylene material. According to the invention, through the regulation and control of a specific formula and a processing process, a large number of micropores and pits exist on the surface of the melt-blown fiber obtained by stretching the melt-blown polypropylene material, after the melt-blown fabric is manufactured, bacteria and oily particles remain on a melt-blown layer and are collected in holes on the surface of the melt-blown fiber when being filtered, compared with the smooth surface of a common fiber, more bacteria and oily particles are difficult to load by electrostatic adsorption, the specific surface area of the melt-blown polypropylene material can be remarkably improved, the filtering capacity of the oily particles of the melt-blown fabric is greatly improved, the excellent oily filtering effect and oily filtering efficiency retention rate are realized, and the melt-blown polypropylene material has great application prospect in the aspect of preparing labor protection articles suitable for severe environments.
It is another object of the present invention to provide a process for preparing the above melt blown polypropylene material.
It is another object of the present invention to provide a meltblown web.
It is another object of the present invention to provide the use of the above melt blown polypropylene material or melt blown cloth for the manufacture of protective articles.
In order to achieve the aim of the invention, the invention adopts the following technical scheme:
a melt-blown polypropylene material comprising a component a and a component B; wherein:
the component A comprises the following components in parts by weight: 93-99 parts of polypropylene resin, 0.1-1 part of free radical initiator, 0.1-0.5 part of nucleating agent, 0.01-3 parts of antioxidant and 0-3 parts of lubricant;
the component B comprises the following components in parts by weight: 80-95 parts of component A and 5-20 parts of foaming electret master batch;
the foaming electret master batch comprises the following components in parts by weight: 30-95 parts of polypropylene resin, 10-30 parts of foaming agent, 5-30 parts of electret, 0.1-3 parts of hyperdispersant, 0.1-1 part of antioxidant and 0-3 parts of lubricant; the processing temperature of the foaming electret master batch is 130-160 ℃;
the weight ratio of the component A to the component B is 1 (0.3-0.8).
It has been found that after meltblown fibers are formed into meltblown webs, bacterial and oily particulates are supported primarily by electrostatic adsorption, and the filtration results are limited and the retention of the filtration results is poor. If the specific surface area of the melt-blown cloth can be greatly improved, the oil filtering effect and the retention rate of the melt-blown cloth can be obviously greatly improved.
The inventors of the present invention tried to add a blowing agent to a melt blown polypropylene material to make holes, but there were two problems with direct addition: firstly, the foaming agent is partially decomposed under the high temperature condition in the processing process of melt-blown polypropylene material, so that the pore-forming effect is limited, and the oily filtering effect cannot be effectively improved; secondly, the foaming agent can have aggregation bursting phenomenon in the processing process of melt-blown polypropylene material, so that the processing performance and the filtering effect are affected instead of being processed or being too much in local pore-forming.
Through repeated researches, on one hand, the foaming agent, polypropylene resin, electret, hyperdispersant and other components are prepared into foaming electret master batches in advance at a lower processing temperature of 130-160 ℃, the hyperdispersant is utilized to realize the dispersion of the foaming agent in the foaming electret master batches, and meanwhile, the dispersion temperature is regulated and controlled, so that the decomposition of the foaming agent is avoided to a large extent; on the other hand, the melt-blown polypropylene material is designed into a component A and a component B, the component A is processed by using two components, the component A mainly provides structural strength support for the fiber, the component B is loaded on the component A fiber in a coextrusion mode, and the burst of the fiber caused by aggregation of the foaming agent is avoided by adjusting the proportion of the component A and the component B.
According to the invention, through the regulation and control of a specific formula and a processing process, a large number of micropores and pits exist on the surface of the melt-blown fiber obtained by stretching the melt-blown polypropylene material, after the melt-blown fabric is manufactured, the porosity is high, bacteria and oily particles remain on a melt-blown layer when being filtered and are collected in holes on the surface of the melt-blown fiber, and compared with the smooth surface of a common fiber, the melt-blown polypropylene material has the advantages that more bacteria and oily particles are difficult to load only by electrostatic adsorption, the specific surface area of the melt-blown polypropylene material can be obviously improved, and the filtering capacity of the oily particles of the melt-blown fabric is greatly improved, so that the melt-blown fabric has great application prospect in preparing labor protection articles suitable for severe environments.
Polypropylene resins conventionally used in the art for preparing meltblown webs, free radical initiators, nucleating agents, antioxidants, lubricants are useful in the present invention.
Preferably, the polypropylene resin is one or more of homo-polypropylene or co-polypropylene.
Preferably, the polypropylene resin has a melt flow rate of 1 to 200g/10min under 230 ℃/2.16kg test conditions according to GB/T3682.1-2018 standard. Further preferably 15 to 45g/10min.
Preferably, the free radical initiator is one or more of dicumyl peroxide, 2, 5-dimethyl-2, 5-bis (tert-butyl peroxy) hexane, 3,6, 9-triethyl-3, 6, 9-trimethyl-1, 4, 7-triperoxidonane or bis (tert-butyl peroxide) dicumyl peroxide.
Preferably, the antioxidant is one or more of pentaerythritol tetra [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate (1010), tris (2, 4-di-tert-butylphenyl) phosphite (168), 1,3, 5-tris (4-tert-butyl-3-hydroxy-2, 6-dimethylbenzyl) -1,3, 5-triazine-2, 4,6- (1H, 3H, 5H) -trione or pentaerythritol tetra-3-laurylthiopropionate.
Preferably, the lubricant is one or more of erucamide, oleamide, EBS amide, PE wax or stearate.
Preferably, the foaming agent is one or more of bicarbonate foaming agent, azo foaming agent or sulfonate foaming agent.
More preferably, the bicarbonate foaming agent is one or two of sodium citrate or sodium bicarbonate.
More preferably, the azo foaming agent is one or more of azobisisobutyronitrile, azodicarbonamide, azodiisoheptonitrile, barium azodicarboxylate or azo amine benzene.
More preferably, the sulfonate foaming agent is one or more of benzenesulfonyl hydrazine, p-toluenesulfonyl hydrazine or 4,4' -oxidized bis-benzenesulfonyl hydrazine.
Preferably, the electret is one or more of an organic electret material or an inorganic electret material.
More preferably, the organic electret material is one or more of polytetrafluoroethylene, polyvinylidene fluoride or copolymer fluoride.
More preferably, the inorganic electret material is one or more of tourmaline, silicon-based silicon nitride or silicon-based silicon dioxide.
Preferably, the hyper-dispersant is one or more of ethoxyamide wax, stearic acid amide with ester group functional group, hydroxyl-terminated hyperbranched polyester and carboxyl-terminated hyperbranched polyester.
It should be noted that the amounts and types of the individual components of component a, the amounts and types of the individual components of component B, and the amounts and types of the individual components of the foam master batch may be the same or different. Taking polypropylene resin as an example, the polypropylene resin in the independent component A is homopolymerized polypropylene resin, and the dosage is 96 parts; the polypropylene resin in the component A contained in the component B can be homo-polypropylene resin or other types of polypropylene resin, and the dosage of the polypropylene resin can be 96 parts or other proper dosage parts; as does the foaming electret master batch.
Preferably, the foaming electret master batch is prepared by the following steps: uniformly mixing polypropylene resin, a foaming agent, electret, hyperdispersant, antioxidant and lubricant, extruding at 130-160 ℃, and granulating to obtain the foaming electret master batch. The preparation method of the melt-blown polypropylene material comprises the following steps:
s1: uniformly mixing polypropylene resin, a free radical initiator, a nucleating agent, an antioxidant and a lubricant, and then extruding, bracing and granulating to obtain a component A; and uniformly mixing the component A and the foaming electret master batch to obtain a component B.
Preferably, the S1 is extruded by a double-screw extruder, the temperature of a screw cylinder of the double-screw extruder is 170-220 ℃, the length-diameter ratio is 36-52:1, and the rotating speed is 300-600 revolutions/min.
The melt-blown polypropylene material can be spun to obtain melt-blown cloth.
And (3) carrying out bicomponent spinning on the component A and the component B to obtain the melt-blown fabric.
Preferably, the meltblown web has a porosity of 86.6 to 91.5%.
The porosity n is determined by the following procedure: the thickness δ of the meltblown fabric was measured by a fabric thickness tester, and the density ρ of the meltblown polypropylene material was taken (based on the PP material basic physical properties ρ=0.9 g/cm 3 ) The basis weight M (g/M) was measured using a basis weight meltblown fabric 2 ) The unit of the porosity n is shown as the following formula:
Figure BDA0003451837370000041
preferably, the spinning process is as follows: spinning by using a double-component melt-blowing device, wherein the temperature of a screw cylinder of a double-screw extruder is 170-250 ℃, the length-diameter ratio is 36-52:1, the rotating speed is 300-600 revolutions per minute, and the temperature of a spinning die head is 190-260 ℃.
The use of the above melt blown polypropylene materials or melt blown webs in the manufacture of protective articles, such as masks, is also within the scope of the present invention.
Compared with the prior art, the invention has the following beneficial effects:
the melt-blown polypropylene material can remarkably improve the specific surface area, further greatly improve the filtering capability of melt-blown cloth oily particles, has excellent oily filtering effect and oily filtering efficiency retention rate, and has great application prospect in preparing labor protection articles suitable for severe environments.
Detailed Description
The invention is further illustrated below with reference to examples. These examples are only for illustrating the present invention and are not intended to limit the scope of the present invention. The experimental procedures in the examples below, without specific details, are generally performed under conditions conventional in the art or recommended by the manufacturer; the raw materials, reagents and the like used, unless otherwise specified, are those commercially available from conventional markets and the like. Any insubstantial changes and substitutions made by those skilled in the art in light of the above teachings are intended to be within the scope of the invention as claimed.
The reagents selected for the examples and comparative examples of the present invention are described below:
polypropylene resin No. 1: homo-polypropylene, PP Z30S, medium petrochemical, melt flow rate 30g/10min (GB/T3682.1-2018 standard, 230 ℃/2.16kg, supra).
Polypropylene resin # 2: homo-polypropylene, PP L5E89 (Guangxi), medium petroleum, melt flow rate 1g/10min.
Polypropylene resin 3#: homo-polypropylene, PP BX3950, korean SK, melt flow rate 200g/10min.
Polypropylene resin # 4: the melt flow rate of the polypropylene copolymer, shell petrochemical PP EP548R is 30g/10min.
Polypropylene resin No. 5: homo-polypropylene, PP H9018, medium petrochemical, melt flow rate 45g/10min.
Polypropylene resin No. 6: homo-polypropylene, PP HJ4012, medium petrochemical and melt flow rate of 15g/10min.
Radical initiator: dicumyl peroxide, commercially available.
Nucleating agent: aryl phosphate nucleating agents, TMP-5, commercially available.
An antioxidant: an antioxidant 1010 and an antioxidant 168 are compounded according to the weight ratio of 1:1 to obtain a compound; antioxidant 1010, commercially available; antioxidant 168, commercially available.
And (3) a lubricant: erucamide, WK1890, commercially available.
Foaming agent # 1: bicarbonate foaming agent, Y3008, perseveration.
Foaming agent # 2: azo foaming agent, F-54, nippon Yonghe Co., ltd.
Foaming agent 3#: sulfonate foaming agent, 4-oxo-bis-benzenesulfonyl hydrazide, available from Jinhe Utility Co., ltd.
Electret: inorganic electret material, tourmaline, commercially available.
Hyperdispersant: ethoxylated amide wax, acomax.
Foaming electret master batches 1-14 #: and (5) self-making. The amounts of the components in the formulation are shown in Table 1. The preparation process is as follows: and uniformly mixing the components to obtain a mixture, and extruding the mixture through an extensional rheological extruder, bracing and granulating to obtain the foaming electret master batch. The processing temperatures of the extensional rheo-extruder are shown in Table 1. The foaming electret master batch 14# cannot be extruded and molded due to the fact that the selected extrusion temperature is too low, and therefore subsequent preparation of melt-blown polypropylene materials and related performance tests are not carried out.
Electret master batches: the self-made material has the formula without foaming agent, and the other components, the dosage and the extrusion temperature are consistent with those of the foaming electret master batch 1 #.
Table 1 formulation and extrusion temperature of foam electret master batches 1 to 14#
Figure BDA0003451837370000061
It should be understood that the same commercial product was used for one of the components in each of the examples and comparative examples unless otherwise specified.
The melt blown polypropylene materials in examples 1 to 22 and comparative examples 1 to 4 of the present invention were prepared by the following processes:
(1) Weighing the components (polypropylene resin, free radical initiator, nucleating agent, antioxidant and lubricant) in the component A according to the formula, uniformly mixing, and extruding by adopting a double-screw extruder; wherein the extrusion temperature is 170-220 ℃, the length-diameter ratio is 40:1, the rotation speed of the extruder is 500rpm, and the component A is obtained after the extrusion, bracing and cooling and granulating.
(2) And uniformly mixing the component A and the foaming electret master batch by adopting particle mixing equipment to obtain a component B for standby.
(3) Adding the component A and the component B into an extruder for bi-component spinning, wherein the barrel temperature of the twin-screw extruder is 170-250 ℃, the length-diameter ratio is 40:1, and the rotating speed is 500 revolutions per minute; and (3) adopting an electrostatic electret electrode to spray the obtained nonwoven web material, wherein the electret voltage is 15kV, and the temperature of a spinning die head is 190-260 ℃, so as to obtain the melt-blown fabric.
The test method of the melt-blown polypropylene material of the embodiment and the comparative example is as follows:
porosity: the thickness δ of the meltblown fabric was measured by a fabric thickness tester, and the density ρ of the meltblown polypropylene material was taken (based on the PP material basic physical properties ρ=0.9 g/cm 3 ) The basis weight M (g/M) was measured using a basis weight meltblown fabric 2 ) The unit of the porosity n is shown as the following formula:
Figure BDA0003451837370000071
oil filtration efficiency and retention rate: the oily filtration efficiency was tested according to EN 149:2001 test standard, the medium DOP was tested, and oily filtration efficiency P of oily particles, and oily filtration efficiency Px after loading with 1H,3H and 5H, oily filtration efficiency retention = Px/p1 x 100%.
Examples 1 to 22
This example provides a series of melt blown polypropylene materials with the amounts of the components in the formulation shown in tables 2-4.
Table 2 formulations (parts) of Components A1# to 8#
Figure BDA0003451837370000072
Table 3 formulations (parts) of Components B1# through 18#
Figure BDA0003451837370000081
Table 4 formulations (parts) of examples 1 to 22
Figure BDA0003451837370000082
Figure BDA0003451837370000091
Comparative examples 1 to 6
This comparative example provides a series of melt blown polypropylene materials with the amounts of the components in the formulation as shown in Table 5.
Table 5 formulations of comparative examples 1 to 4
Figure BDA0003451837370000092
Comparative example 5 provides a melt blown polypropylene material having the same a component as in example 1; the total amount of each component in the B component is the same as that in example 1, except that the foaming electret master batch is not prepared in advance in the B component, but each component is directly and uniformly mixed according to the same process conditions in step (2) of example 1, and then extruded, bracing and granulating are carried out.
Comparative example 6 provides a melt blown polypropylene material which is a one component design, the total amount of each component being equal to the total amount of each component in example 1, prepared as follows: adding the components into an extruder for single-component spinning to obtain a melt-blown polypropylene material, wherein the extrusion temperature is 170-250 ℃, the length-diameter ratio is 40:1, and the rotation speed of the extruder is 500 revolutions per minute; the spinning conditions are as follows: static electret, 15kV electret voltage and 190-260 ℃ of spinning die head temperature.
The properties of the melt blown polypropylene materials provided in the examples and comparative examples were tested according to the performance test methods described above and the results are shown in table 6.
Table 6 results of performance testing of the melt blown polypropylene materials provided in examples 1-22 and comparative examples 1-6
Figure BDA0003451837370000101
Figure BDA0003451837370000111
From the above test results, it is found that the melt-blown polypropylene materials provided in examples 1 to 22 have an oil filtration efficiency of 99% or more, and have excellent oil filtration efficiency after loading the oil particles with 1H,3H and 5H, and a high retention of filtration efficiency. The foaming electret master batch in the comparative example 1 is obtained through higher processing temperature, the foaming agent loss is serious due to the higher processing temperature, the oily filtration efficiency is low, and the oily filtration efficiency retention rate after the oily particles are loaded is low; the electret master batch added in the comparative example 2 is not added with a foaming agent, and basically cannot provide a rough surface after foaming, the specific surface area is greatly reduced, and the storage capacity of oily particles is poorer; the amount of component B in comparative example 3 is too low to form an effective particulate storage cross section, and the initial oily filtration efficiency and the oily filtration efficiency after loading of oily particles are not high; the amount of the component B in the comparative example 4 is too high, a large amount of discontinuous foaming components are formed, more long fibers cannot be formed like the embodiment, the interception efficiency of particles is greatly reduced, the foaming agent in the comparative example 5 is not prepared into foaming electret master batches in advance, and the problem of premature loss of the foaming electret master batches also exists in the scheme; in comparative example 6, the foaming agent was directly added and a one-component design was adopted, the foaming component could not be effectively dispersed, and a melt-blown polypropylene material (melt-blown nonwoven polypropylene material) of good quality could not be obtained basically in the spinning process.
Those of ordinary skill in the art will recognize that the embodiments herein are intended to assist the reader in understanding the principles of the invention and should be understood that the scope of the invention is not limited to such specific statements and embodiments. Those of ordinary skill in the art can make various other specific modifications and combinations from the teachings of the present disclosure without departing from the spirit thereof, and such modifications and combinations remain within the scope of the present disclosure.

Claims (12)

1. A melt-blown polypropylene material, characterized by comprising a component a and a component B; wherein:
the component A comprises the following components in parts by weight: 93-99 parts of polypropylene resin, 0.1-1 part of free radical initiator, 0.1-0.5 part of nucleating agent, 0.01-3 parts of antioxidant and 0-3 parts of lubricant;
the component B comprises the following components in parts by weight: 80-95 parts of component A and 5-20 parts of foaming electret master batch;
the foaming electret master batch comprises the following components in parts by weight: 30-95 parts of polypropylene resin, 10-30 parts of foaming agent, 5-30 parts of electret, 0.1-3 parts of hyperdispersant, 0.1-1 part of antioxidant and 0-3 parts of lubricant; the processing temperature of the foaming electret master batch is 130-160 ℃;
the weight ratio of the component A to the component B is 1 (0.3-0.8).
2. The melt-blown polypropylene material according to claim 1, wherein the polypropylene resin is one or more of homo-polypropylene or co-polypropylene; the melt flow rate of the polypropylene resin under the test condition of 230 ℃/2.16kg is 1-200 g/10min according to the GB/T3682.1-2018 standard.
3. The melt blown polypropylene material according to claim 1, wherein the free radical initiator is one or more of dicumyl peroxide, 2, 5-dimethyl-2, 5-bis (t-butylperoxy) hexane, 3,6, 9-triethyl-3, 6, 9-trimethyl-1, 4, 7-triperoxidonane or bis (t-butylperoxy) dicumyl peroxide.
4. The melt blown polypropylene material of claim 1, wherein the nucleating agent is one or more of a dibenzylidene sorbitol nucleating agent, an aryl phosphate salt nucleating agent, an aromatic carboxylate metal salt nucleating agent, or an aromatic organic phosphate metal salt nucleating agent;
the antioxidant is one or more of pentaerythritol tetra [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate, tris (2, 4-di-tert-butylphenyl) phosphite, 1,3, 5-tris (4-tert-butyl-3-hydroxy-2, 6-dimethylbenzyl) -1,3, 5-triazine-2, 4,6- (1H, 3H, 5H) -trione or pentaerythritol tetra-3-laurylthiopropionate;
the lubricant is one or more of erucamide, oleamide, EBS amide, PE wax or stearate.
5. The melt-blown polypropylene material according to claim 1, wherein the foaming agent is one or more of a bicarbonate foaming agent, an azo foaming agent or a sulfonate foaming agent.
6. The melt blown polypropylene material according to claim 1, wherein the electret is one or more of an organic electret material or an inorganic electret material.
7. The melt-blown polypropylene material according to claim 1, wherein the hyper-dispersant is one or more of an ethoxylated amide wax, an ester functional group-containing stearic acid amide, a hydroxyl-terminated hyperbranched polyester, and a carboxyl-terminated hyperbranched polyester.
8. The melt blown polypropylene material of claim 1, wherein the foamed electret master batch is prepared by the process of: uniformly mixing polypropylene resin, a foaming agent, electret, hyperdispersant, antioxidant and lubricant, extruding at 130-160 ℃, and granulating to obtain the foaming electret master batch.
9. The method for preparing the melt-blown polypropylene material according to any one of claims 1 to 8, comprising the steps of:
s1: uniformly mixing polypropylene resin, a free radical initiator, a nucleating agent, an antioxidant and a lubricant, and then extruding, bracing and granulating to obtain a component A;
s2: and uniformly mixing the component A and the foaming electret master batch to obtain a component B.
10. A meltblown web, comprising the steps of: and (3) spinning the component A and the component B according to any one of claims 1 to 8 to obtain the melt-blown fabric.
11. The meltblown web according to claim 10, wherein the meltblown web has a porosity of 86.6 to 91.5%.
12. Use of the meltblown polypropylene material according to any one of claims 1 to 8 or the meltblown fabric according to any one of claims 10 to 11 for the manufacture of protective articles.
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