CN114908479B - Production method of high-filtration low-resistance double-layer melt-blown non-woven fabric for medical and health materials - Google Patents
Production method of high-filtration low-resistance double-layer melt-blown non-woven fabric for medical and health materials Download PDFInfo
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- CN114908479B CN114908479B CN202210543187.4A CN202210543187A CN114908479B CN 114908479 B CN114908479 B CN 114908479B CN 202210543187 A CN202210543187 A CN 202210543187A CN 114908479 B CN114908479 B CN 114908479B
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- 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
- D04H13/00—Other non-woven fabrics
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/09—Addition of substances to the spinning solution or to the melt for making electroconductive or anti-static filaments
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/02—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from cellulose, cellulose derivatives, or proteins
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
- D01F8/14—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyester as constituent
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- 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
- D04H1/42—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 characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
- D04H1/4382—Stretched reticular film fibres; Composite fibres; Mixed fibres; Ultrafine fibres; Fibres for artificial leather
- D04H1/43825—Composite fibres
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- 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
- D04H1/70—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres
- D04H1/72—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged
- D04H1/728—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged by electro-spinning
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- D—TEXTILES; PAPER
- D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B2401/00—Physical properties
- D10B2401/16—Physical properties antistatic; conductive
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- D—TEXTILES; PAPER
- D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B2509/00—Medical; Hygiene
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- 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- 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
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Abstract
The invention discloses a production method of a high-filtration low-resistance double-layer melt-blown non-woven fabric for medical and health materials, which specifically comprises the following steps: step S1: adding modified polyester into the modified cellulose liquid, stirring, distilling to remove the solvent, adding the substrate into deionized water, continuously stirring, filtering again, and drying the substrate to obtain composite particles; step S2: uniformly mixing composite particles, porous filler, fluorocarbon resin and N, N-dimethylacetamide, carrying out electrostatic spinning, and collecting by using a PBT melt-blown non-woven fabric to prepare the double-layer melt-blown non-woven fabric. The modified cellulose liquid is blended with the modified polyester, and under alkaline conditions, amino groups on modified cellulose molecules react with epoxy groups on side chains of the modified polyester molecules to form a space structure with two kinds of molecular chains wrapped at intervals, and the structure greatly improves the mechanical effect of the non-woven fabric.
Description
Technical Field
The invention relates to the technical field of medical supplies, in particular to a production method of a high-filtration low-resistance double-layer melt-blown non-woven fabric for medical and sanitary materials.
Background
Nonwoven fabrics, also known as nonwovens, are constructed from oriented or random fibers, which are referred to as cloths because of their appearance and certain properties. The non-woven fabric has no warps and wefts, is very convenient to cut and sew, is light in weight and easy to shape, and is deeply favored by handcraftsmen. The non-woven fabric product is widely used, attractive and elegant in appearance, various in patterns and styles, light in weight, environment-friendly and recyclable, and is internationally recognized as an environment-friendly product for protecting the ecology of the earth due to rich colors, vividness, fashion and environment friendliness. Is widely applied to the fields of chemical industry, automobile industry, home building materials, life decoration, medical treatment and health, etc.
The medical non-woven fabric has excellent performance in the aspects of elasticity and wear resistance, can recover by itself after being deformed, has a certain waterproof function, and has a great market competitive advantage due to low production cost. Finally, the medical non-woven fabric has the antibacterial and anti-corrosion properties, which is the most critical characteristic of the medical non-woven fabric, other fabrics are difficult to replace the antibacterial and anti-corrosion properties, but the non-woven fabric has poor toughness and is easy to tear, so that the use of the non-woven fabric is affected.
Disclosure of Invention
The invention aims to provide a production method of a high-filtration low-resistance double-layer melt-blown non-woven fabric for medical and health materials, which solves the problem that the non-woven fabric is easy to tear and has a common filtration effect at the present stage.
The aim of the invention can be achieved by the following technical scheme:
the production method of the high-filtration low-resistance double-layer melt-blown non-woven fabric for the medical and health materials specifically comprises the following steps:
step S1: adding modified polyester into the modified cellulose liquid, stirring for 2-3 hours under alkaline conditions at the rotating speed of 200-300r/min and the temperature of 25-30 ℃, distilling to remove the solvent, adding the substrate into deionized water, continuously stirring for 3-5 minutes, filtering again, and drying the substrate to obtain composite particles;
step S2: uniformly mixing composite particles, porous filler, fluorocarbon resin and N, N-dimethylacetamide, carrying out electrostatic spinning under the conditions that the propelling speed is 0.001-0.003mm/s, the voltage is 18-20kV and the receiving distance is 15-18cm, and collecting by using PBT melt-blown non-woven fabrics to prepare the double-layer melt-blown non-woven fabrics.
Further, the molar ratio of the amino groups in the modified cellulose liquid to the epoxy groups in the modified polyester in the step S1 is 1:4.
Further, the mass ratio of the composite particles, the porous filler and the fluorocarbon resin in the step S2 is 5:0.02:2.
Further, the modified cellulose liquid is prepared by the following steps:
step A1: uniformly mixing 4,4' -dimethylbiphenyl and concentrated sulfuric acid, stirring and dropwise adding a nitric acid solution at the rotating speed of 120-150r/min and the room temperature, reacting for 4-6 hours, cooling to the temperature of 0-3 ℃, filtering to remove filtrate to obtain an intermediate 1, dissolving the intermediate 1 in carbon tetrachloride, introducing chlorine under the illumination condition, and reacting for 1-1.5 hours to obtain an intermediate 2;
the reaction process is as follows:
step A2: dissolving the intermediate 2 in toluene, adding concentrated hydrochloric acid, stirring and adding tin powder at the rotation speed of 120-150r/min and the temperature of 100-110 ℃, reacting for 30-40min, adjusting the pH value of the reaction solution to be alkaline to prepare an intermediate 3, mixing cellulose and N, N-dimethylacetamide, stirring for 2-3h at the rotation speed of 300-500r/min and the temperature of 130-140 ℃, cooling to the temperature of 90-100 ℃, adding lithium chloride, continuously stirring for 30-40min, cooling to the temperature of 50-60 ℃, adding the intermediate 3, and continuously stirring for 7-9h to prepare the cellulose solution.
The reaction process is as follows:
further, the dosage ratio of the 4,4' -dimethylbiphenyl, the concentrated sulfuric acid and the nitric acid solution in the step A1 is 0.01mol:20mL:6mL, the mass fraction of the concentrated sulfuric acid is 98%, the mass fraction of the nitric acid solution is 60%, and the molar ratio of the intermediate 1 to the chlorine is 1:1.
Further, the dosage ratio of the intermediate 2 to the concentrated hydrochloric acid to the tin powder in the step A2 is 3g to 20mL to 8g, the mass fraction of the concentrated hydrochloric acid is 36%, and the molar ratio of hydroxyl groups in cellulose to the intermediate 3 is 1 to 0.25.
The modified polyester is prepared by the following steps:
step B1: uniformly mixing 5-hydroxy isophthalic acid, methanol, concentrated sulfuric acid and hexane, carrying out reflux reaction for 5-7h at the temperature of 80-90 ℃ to obtain an intermediate 4, uniformly mixing the intermediate 4, acetic anhydride and pyridine, continuously stirring for 2-4h at the temperature of 90-100 ℃ to obtain an intermediate 5, uniformly mixing sodium borohydride, lithium chloride and tetrahydrofuran, stirring and adding the intermediate 5 at the rotating speed of 150-200r/min and the temperature of 80-90 ℃ to react for 3-5h, and regulating the pH value of a reaction solution to be acidic to obtain an intermediate 6;
the reaction process is as follows:
step B2: uniformly mixing the intermediate 6, terephthalic acid, ethylene glycol and antimony acetate, reacting for 4-6 hours at 220-250 ℃ and 0.3-0.4MPa, heating to 260-280 ℃, adjusting the pressure to 50-60Pa, continuously reacting for 1-2 hours to obtain polyester, dissolving the polyester in N, N-dimethylformamide, adding sodium carbonate and epichlorohydrin, reacting for 2-4 hours at the rotating speed of 200-300r/min and the temperature of 30-40 ℃, distilling to remove the solvent, adding deionized water, uniformly mixing, and filtering again to remove the filtrate to obtain the modified polyester.
Further, the dosage ratio of 5-hydroxy isophthalic acid, methanol, concentrated sulfuric acid and hexane in the step B1 is 0.2mol:100mL:5mL:100mL, the mass fraction of the concentrated sulfuric acid is the same as that in the step A1, the dosage ratio of the intermediate 4, acetic anhydride and pyridine is 0.1mol:25mL:1mL, and the molar ratio of sodium borohydride, lithium chloride and the intermediate 5 is 2.5:2.5:0.4.
Further, the molar ratio of the intermediate 6 to terephthalic acid to ethylene glycol in the step B2 is 0.05:1:1.5, the amount of antimony acetate is 0.05% of the mass of the reactants, and the molar ratio of hydroxyl groups of the polyester to epichlorohydrin is 1:1.
Further, the porous filler is prepared by the following steps:
mixing desilication high-alumina fly ash, alumina, kaolinite and carbon nano tube, ball milling, mixing with polyvinyl alcohol and ammonium bicarbonate, adding into a mould, maintaining pressure for 2-3min under the condition of 200-220MPa, and roasting for 2-3h under the condition of 1200-1500 ℃ to obtain porous filler.
Further, the mass ratio of the desilication high-alumina fly ash to the alumina to the kaolinite to the carbon nano tube is 6:2:1:0.5.
The invention has the beneficial effects that: the invention prepares modified cellulose liquid, modified polyester and porous filler in the process of preparing high-filtering low-resistance double-layer melt-blown non-woven fabric, the modified cellulose liquid takes 4,4' -dimethylbiphenyl as raw material to carry out nitrosation treatment to prepare intermediate 1, then intermediate 1 is substituted by chlorine to prepare intermediate 2, intermediate 2 is reduced to reduce nitro to amino to prepare intermediate 3, cellulose reacts with intermediate 3 to enable hydroxyl on cellulose to react with chlorine atom sites on intermediate 3 to further generate crosslinking, the modified polyester 5-hydroxyisophthalic acid is taken as raw material to carry out esterification with methanol to prepare intermediate 4, intermediate 4 reacts with acetic anhydride to prepare intermediate 5, intermediate 5 is reduced by sodium borohydride to prepare intermediate 6, terephthalic acid and ethylene glycol are subjected to esterification polycondensation, the polyester is prepared, the polyester reacts with epichlorohydrin to make phenolic hydroxyl of a polyester side chain react with chlorine atom sites on the epichlorohydrin to prepare modified polyester, modified cellulose liquid is blended with the modified polyester, amino on modified cellulose molecules reacts with epoxy groups on the side chain of the modified polyester molecules under alkaline condition to form a space structure with two molecular chains being packed at intervals, the structure greatly improves the mechanical effect of non-woven fabrics, porous filler is prepared by ball milling and roasting desilication high alumina fly ash, alumina, kaolinite and carbon nano tubes, the porous filler contains a large number of pore channels which are communicated with each other and have through surfaces, the filtering effect of the non-woven fabrics is greatly improved, the wear-resisting effect of the non-woven fabrics is increased, the conductivity of the non-woven fabrics is improved, and electrostatic adsorption of the non-woven fabrics is avoided, so that dust is adsorbed on the surface and the filtering effect is affected.
Detailed Description
The following description of the technical solutions in the embodiments of the present invention will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present invention, but 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.
Example 1
The production method of the high-filtration low-resistance double-layer melt-blown non-woven fabric for the medical and health materials specifically comprises the following steps:
step S1: adding modified polyester into the modified cellulose liquid, stirring for 2 hours under alkaline conditions at the rotation speed of 200r/min and the temperature of 25 ℃, distilling to remove the solvent, adding the substrate into deionized water, continuously stirring for 3 minutes, filtering again, and drying the substrate to obtain composite particles;
step S2: uniformly mixing composite particles, porous filler, fluorocarbon resin and N, N-dimethylacetamide, carrying out electrostatic spinning under the conditions of 0.001mm/s of propelling speed, 18kV of voltage and 15cm of receiving distance, and collecting by using a PBT melt-blown non-woven fabric to prepare the double-layer melt-blown non-woven fabric.
The molar ratio of the amino groups in the modified cellulose liquid to the epoxy groups in the modified polyester in the step S1 is 1:4.
The mass ratio of the composite particles, the porous filler and the fluorocarbon resin in the step S2 is 5:0.02:2.
The modified cellulose liquid is prepared by the following steps:
step A1: uniformly mixing 4,4' -dimethylbiphenyl and concentrated sulfuric acid, stirring and dropwise adding a nitric acid solution at the rotating speed of 120r/min and the room temperature, reacting for 4 hours, cooling to the temperature of 0 ℃, filtering to remove filtrate to obtain an intermediate 1, dissolving the intermediate 1 in carbon tetrachloride, introducing chlorine under the illumination condition, and reacting for 1 hour to obtain an intermediate 2;
step A2: dissolving the intermediate 2 in toluene, adding concentrated hydrochloric acid, stirring at a rotating speed of 120r/min and a temperature of 100 ℃, adding tin powder, reacting for 30min, adjusting the pH value of the reaction solution to be alkaline to obtain an intermediate 3, mixing cellulose and N, N-dimethylacetamide, stirring at a rotating speed of 300r/min and a temperature of 130 ℃ for 2h, cooling to 90 ℃, adding lithium chloride, continuously stirring for 30min, cooling to a temperature of 50 ℃, adding the intermediate 3, and continuously stirring for 7h to obtain a cellulose liquid.
The dosage ratio of the 4,4' -dimethylbiphenyl to the concentrated sulfuric acid to the nitric acid solution in the step A1 is 0.01mol:20mL:6mL, the mass fraction of the concentrated sulfuric acid is 98%, the mass fraction of the nitric acid solution is 60%, and the molar ratio of the intermediate 1 to the chlorine is 1:1.
The dosage ratio of the intermediate 2 to the concentrated hydrochloric acid to the tin powder in the step A2 is 3g to 20mL to 8g, the mass fraction of the concentrated hydrochloric acid is 36%, and the molar ratio of hydroxyl groups in cellulose to the intermediate 3 is 1 to 0.25.
The modified polyester is prepared by the following steps:
step B1: uniformly mixing 5-hydroxy isophthalic acid, methanol, concentrated sulfuric acid and hexane, carrying out reflux reaction for 5 hours at the temperature of 80 ℃ to obtain an intermediate 4, uniformly mixing the intermediate 4, acetic anhydride and pyridine, continuously stirring for 2 hours at the temperature of 90 ℃ to obtain an intermediate 5, uniformly mixing sodium borohydride, lithium chloride and tetrahydrofuran, stirring at the rotating speed of 150r/min at the temperature of 80 ℃, adding the intermediate 5, carrying out reaction for 3 hours, and regulating the pH value of a reaction solution to be acidic to obtain an intermediate 6;
step B2: uniformly mixing the intermediate 6, terephthalic acid, ethylene glycol and antimony acetate, reacting for 4 hours at 220 ℃ and 0.3MPa, heating to 260 ℃, adjusting the pressure to 50Pa, continuously reacting for 1 hour to obtain polyester, dissolving the polyester in N, N-dimethylformamide, adding sodium carbonate and epichlorohydrin, reacting for 2 hours at the speed of 200r/min and the temperature of 30 ℃, distilling to remove the solvent, adding deionized water, uniformly mixing, and filtering again to remove the filtrate, thus obtaining the modified polyester.
The dosage ratio of 5-hydroxy isophthalic acid, methanol, concentrated sulfuric acid and hexane in the step B1 is 0.2mol:100mL:5mL:100mL, the mass fraction of the concentrated sulfuric acid is the same as that in the step A1, the dosage ratio of the intermediate 4, acetic anhydride and pyridine is 0.1mol:25mL:1mL, and the molar ratio of sodium borohydride, lithium chloride and intermediate 5 is 2.5:2.5:0.4.
The molar ratio of the intermediate 6 to terephthalic acid to ethylene glycol in the step B2 is 0.05:1:1.5, the amount of antimony acetate is 0.05% of the mass of the reactants, and the molar ratio of hydroxyl groups of the polyester to epichlorohydrin is 1:1.
The porous filler is prepared by the following steps:
mixing desilication high-alumina fly ash, alumina, kaolinite and carbon nano tubes, ball milling uniformly, mixing with polyvinyl alcohol and ammonium bicarbonate uniformly, adding into a mould, carrying out pressure maintaining treatment for 2min under the condition of 200MPa, and roasting for 2h under the condition of 1200 ℃ to obtain the porous filler.
The mass ratio of the desilication high-alumina fly ash to the alumina to the kaolinite to the carbon nano tube is 6:2:1:0.5.
Example 2
The production method of the high-filtration low-resistance double-layer melt-blown non-woven fabric for the medical and health materials specifically comprises the following steps:
step S1: adding modified polyester into the modified cellulose liquid, stirring for 2.5 hours under alkaline conditions at the rotating speed of 200r/min and the temperature of 28 ℃, distilling to remove the solvent, adding the substrate into deionized water, continuously stirring for 4 minutes, filtering again, and drying the substrate to obtain composite particles;
step S2: uniformly mixing composite particles, porous filler, fluorocarbon resin and N, N-dimethylacetamide, carrying out electrostatic spinning under the conditions that the propelling speed is 0.002mm/s, the voltage is 19kV and the receiving distance is 16cm, and collecting by using a PBT melt-blown non-woven fabric to prepare the double-layer melt-blown non-woven fabric.
The molar ratio of the amino groups in the modified cellulose liquid to the epoxy groups in the modified polyester in the step S1 is 1:4.
The mass ratio of the composite particles, the porous filler and the fluorocarbon resin in the step S2 is 5:0.02:2.
The modified cellulose liquid is prepared by the following steps:
step A1: uniformly mixing 4,4' -dimethylbiphenyl and concentrated sulfuric acid, stirring and dropwise adding a nitric acid solution at a rotating speed of 150r/min and a room temperature, reacting for 5 hours, cooling to a temperature of 2 ℃, filtering to remove filtrate to obtain an intermediate 1, dissolving the intermediate 1 in carbon tetrachloride, introducing chlorine under an illumination condition, and reacting for 1.3 hours to obtain an intermediate 2;
step A2: dissolving the intermediate 2 in toluene, adding concentrated hydrochloric acid, stirring at a rotating speed of 150r/min and a temperature of 105 ℃, adding tin powder, reacting for 35min, adjusting the pH value of the reaction solution to be alkaline to obtain an intermediate 3, mixing cellulose and N, N-dimethylacetamide, stirring at a rotating speed of 300r/min and a temperature of 135 ℃ for 2.5h, cooling to a temperature of 95 ℃, adding lithium chloride, continuously stirring for 35min, cooling to a temperature of 55 ℃, adding the intermediate 3, and continuously stirring for 8h to obtain a cellulose solution.
The dosage ratio of the 4,4' -dimethylbiphenyl to the concentrated sulfuric acid to the nitric acid solution in the step A1 is 0.01mol:20mL:6mL, the mass fraction of the concentrated sulfuric acid is 98%, the mass fraction of the nitric acid solution is 60%, and the molar ratio of the intermediate 1 to the chlorine is 1:1.
The dosage ratio of the intermediate 2 to the concentrated hydrochloric acid to the tin powder in the step A2 is 3g to 20mL to 8g, the mass fraction of the concentrated hydrochloric acid is 36%, and the molar ratio of hydroxyl groups in cellulose to the intermediate 3 is 1 to 0.25.
The modified polyester is prepared by the following steps:
step B1: uniformly mixing 5-hydroxy isophthalic acid, methanol, concentrated sulfuric acid and hexane, carrying out reflux reaction for 6 hours at the temperature of 85 ℃ to obtain an intermediate 4, uniformly mixing the intermediate 4, acetic anhydride and pyridine, continuously stirring for 3 hours at the temperature of 95 ℃ to obtain an intermediate 5, uniformly mixing sodium borohydride, lithium chloride and tetrahydrofuran, stirring at the rotating speed of 180r/min and adding the intermediate 5, carrying out reaction for 4 hours, and regulating the pH value of a reaction solution to be acidic to obtain an intermediate 6;
step B2: uniformly mixing the intermediate 6, terephthalic acid, ethylene glycol and antimony acetate, reacting for 5 hours at the temperature of 230 ℃ and the pressure of 0.3MPa, heating to 270 ℃, adjusting the pressure to 55Pa, continuously reacting for 1.5 hours to obtain polyester, dissolving the polyester in N, N-dimethylformamide, adding sodium carbonate and epichlorohydrin, reacting for 3 hours at the temperature of 35 ℃ at the rotating speed of 200r/min, distilling to remove the solvent, adding deionized water, uniformly mixing, and filtering again to remove the filtrate, thus obtaining the modified polyester.
The dosage ratio of 5-hydroxy isophthalic acid, methanol, concentrated sulfuric acid and hexane in the step B1 is 0.2mol:100mL:5mL:100mL, the mass fraction of the concentrated sulfuric acid is the same as that in the step A1, the dosage ratio of the intermediate 4, acetic anhydride and pyridine is 0.1mol:25mL:1mL, and the molar ratio of sodium borohydride, lithium chloride and intermediate 5 is 2.5:2.5:0.4.
The molar ratio of the intermediate 6 to terephthalic acid to ethylene glycol in the step B2 is 0.05:1:1.5, the amount of antimony acetate is 0.05% of the mass of the reactants, and the molar ratio of hydroxyl groups of the polyester to epichlorohydrin is 1:1.
The porous filler is prepared by the following steps:
mixing desilication high-alumina fly ash, alumina, kaolinite and carbon nano tubes, ball milling uniformly, mixing with polyvinyl alcohol and ammonium bicarbonate uniformly, adding into a mould, carrying out pressure maintaining treatment for 2.5min under the condition of 210MPa, and roasting for 2.5h under the condition of 1300 ℃ to obtain the porous filler.
The mass ratio of the desilication high-alumina fly ash to the alumina to the kaolinite to the carbon nano tube is 6:2:1:0.5.
Example 3
The production method of the high-filtration low-resistance double-layer melt-blown non-woven fabric for the medical and health materials specifically comprises the following steps:
step S1: adding modified polyester into the modified cellulose liquid, stirring for 3 hours under alkaline conditions at the rotating speed of 300r/min and the temperature of 30 ℃, distilling to remove the solvent, adding the substrate into deionized water, continuously stirring for 5 minutes, filtering again, and drying the substrate to obtain composite particles;
step S2: uniformly mixing composite particles, porous filler, fluorocarbon resin and N, N-dimethylacetamide, carrying out electrostatic spinning under the conditions of 0.003mm/s of propelling speed, 20kV of voltage and 18cm of receiving distance, and collecting by using a PBT melt-blown non-woven fabric to prepare the double-layer melt-blown non-woven fabric.
The molar ratio of the amino groups in the modified cellulose liquid to the epoxy groups in the modified polyester in the step S1 is 1:4.
The mass ratio of the composite particles, the porous filler and the fluorocarbon resin in the step S2 is 5:0.02:2.
The modified cellulose liquid is prepared by the following steps:
step A1: uniformly mixing 4,4' -dimethylbiphenyl and concentrated sulfuric acid, stirring and dropwise adding a nitric acid solution at a rotating speed of 150r/min and a room temperature, reacting for 6 hours, cooling to a temperature of 3 ℃, filtering to remove filtrate to obtain an intermediate 1, dissolving the intermediate 1 in carbon tetrachloride, introducing chlorine under an illumination condition, and reacting for 1.5 hours to obtain an intermediate 2;
step A2: dissolving the intermediate 2 in toluene, adding concentrated hydrochloric acid, stirring at a rotating speed of 150r/min and a temperature of 110 ℃, adding tin powder, reacting for 40min, adjusting the pH value of the reaction solution to be alkaline to obtain an intermediate 3, mixing cellulose and N, N-dimethylacetamide, stirring at a rotating speed of 500r/min and a temperature of 140 ℃ for 3h, cooling to a temperature of 100 ℃, adding lithium chloride, continuously stirring for 40min, cooling to a temperature of 60 ℃, adding the intermediate 3, and continuously stirring for 9h to obtain a cellulose liquid.
The dosage ratio of the 4,4' -dimethylbiphenyl to the concentrated sulfuric acid to the nitric acid solution in the step A1 is 0.01mol:20mL:6mL, the mass fraction of the concentrated sulfuric acid is 98%, the mass fraction of the nitric acid solution is 60%, and the molar ratio of the intermediate 1 to the chlorine is 1:1.
The dosage ratio of the intermediate 2 to the concentrated hydrochloric acid to the tin powder in the step A2 is 3g to 20mL to 8g, the mass fraction of the concentrated hydrochloric acid is 36%, and the molar ratio of hydroxyl groups in cellulose to the intermediate 3 is 1 to 0.25.
The modified polyester is prepared by the following steps:
step B1: uniformly mixing 5-hydroxy isophthalic acid, methanol, concentrated sulfuric acid and hexane, carrying out reflux reaction for 7h at 90 ℃ to obtain an intermediate 4, uniformly mixing the intermediate 4, acetic anhydride and pyridine, continuously stirring for 4h at 100 ℃ to obtain an intermediate 5, uniformly mixing sodium borohydride, lithium chloride and tetrahydrofuran, stirring at 200r/min at 90 ℃ and adding the intermediate 5, carrying out reaction for 5h, and then regulating the pH value of a reaction solution to be acidic to obtain an intermediate 6;
step B2: uniformly mixing the intermediate 6, terephthalic acid, ethylene glycol and antimony acetate, reacting for 6 hours at the temperature of 250 ℃ and the pressure of 0.4MPa, heating to the temperature of 280 ℃, adjusting the pressure to 60Pa, continuously reacting for 2 hours to obtain polyester, dissolving the polyester in N, N-dimethylformamide, adding sodium carbonate and epichlorohydrin, reacting for 4 hours at the rotating speed of 300r/min and the temperature of 40 ℃, distilling to remove the solvent, adding deionized water, uniformly mixing, and filtering again to remove the filtrate to obtain the modified polyester.
The dosage ratio of 5-hydroxy isophthalic acid, methanol, concentrated sulfuric acid and hexane in the step B1 is 0.2mol:100mL:5mL:100mL, the mass fraction of the concentrated sulfuric acid is the same as that in the step A1, the dosage ratio of the intermediate 4, acetic anhydride and pyridine is 0.1mol:25mL:1mL, and the molar ratio of sodium borohydride, lithium chloride and intermediate 5 is 2.5:2.5:0.4.
The molar ratio of the intermediate 6 to terephthalic acid to ethylene glycol in the step B2 is 0.05:1:1.5, the amount of antimony acetate is 0.05% of the mass of the reactants, and the molar ratio of hydroxyl groups of the polyester to epichlorohydrin is 1:1.
The porous filler is prepared by the following steps:
mixing desilication high-alumina fly ash, alumina, kaolinite and carbon nano tubes, ball milling uniformly, mixing with polyvinyl alcohol and ammonium bicarbonate uniformly, adding into a mould, carrying out pressure maintaining treatment for 3min under the condition of 220MPa, and roasting for 3h under the condition of 1500 ℃ to obtain the porous filler.
The mass ratio of the desilication high-alumina fly ash to the alumina to the kaolinite to the carbon nano tube is 6:2:1:0.5.
Comparative example 1
The comparative example is a PBT melt blown nonwoven.
Comparative example 2
In this comparative example, as compared with example 1, the nonwoven fabric was obtained by directly electrospinning a cellulose liquid and collecting the same with a PBT melt-blown nonwoven fabric.
Comparative example 3
The comparative example is a nonwoven fabric disclosed in chinese patent CN112853619 a.
The nonwoven fabrics prepared in examples 1-3 and comparative examples 1-3 were measured for tensile strength of films by using an HD021NS electronic single yarn brute force instrument, and then a CLJ-03A laser dust particle counter, a TSI-8108 large-particle-size aerosol generator was used, the sampling flow rate was 2.83L/min, the film thickness was 0.1mm, and the filtration efficiency was detected, and the results were shown in the following table;
from the above table, it can be seen that the tensile strength of the nonwoven fabrics prepared in examples 1-3 is 83.6-84.3MPa, and the filtration has good filtration effect, indicating that the invention has good mechanical effect and filtration effect.
The foregoing is merely illustrative and explanatory of the principles of the invention, as various modifications and additions may be made to the specific embodiments described, or similar thereto, by those skilled in the art, without departing from the principles of the invention or beyond the scope of the appended claims.
Claims (7)
1. The production method of the high-filtration low-resistance double-layer melt-blown non-woven fabric for the medical and sanitary material is characterized by comprising the following steps of: the method specifically comprises the following steps:
step S1: adding modified polyester into the modified cellulose liquid, stirring, distilling to remove the solvent, adding the substrate into deionized water, continuously stirring, filtering again, and drying the substrate to obtain composite particles;
step S2: uniformly mixing composite particles, porous filler, fluorocarbon resin and N, N-dimethylacetamide, carrying out electrostatic spinning, and collecting by using a PBT melt-blown non-woven fabric to prepare a double-layer melt-blown non-woven fabric;
the modified cellulose liquid is prepared by the following steps:
step A1: mixing 4,4' -dimethylbiphenyl and concentrated sulfuric acid for reaction, cooling, filtering to remove filtrate to obtain an intermediate 1, dissolving the intermediate 1 in carbon tetrachloride, introducing chlorine under the illumination condition, and reacting to obtain an intermediate 2;
step A2: dissolving the intermediate 2 in toluene, adding concentrated hydrochloric acid, stirring, adding tin powder, reacting, adjusting the pH value of the reaction solution to be alkaline to obtain an intermediate 3, mixing and stirring cellulose and N, N-dimethylacetamide, cooling, adding lithium chloride, continuously stirring, cooling again, adding the intermediate 3, and continuously stirring to obtain a cellulose solution;
the modified polyester is prepared by the following steps:
step B1: mixing 5-hydroxy isophthalic acid, methanol, concentrated sulfuric acid and hexane for reflux reaction to obtain an intermediate 4, mixing and stirring the intermediate 4, acetic anhydride and pyridine to obtain an intermediate 5, mixing and stirring sodium borohydride, lithium chloride and tetrahydrofuran, adding the intermediate 5, reacting, and adjusting the pH value of a reaction solution to obtain an intermediate 6;
step B2: mixing intermediate 6, terephthalic acid, ethylene glycol and antimony acetate for reaction, heating, regulating the pressure, continuing to react to obtain polyester, dissolving the polyester in N, N-dimethylformamide, adding sodium carbonate and epichlorohydrin for reaction, distilling to remove solvent, adding deionized water for uniform mixing, and filtering again to remove filtrate to obtain modified polyester;
the porous filler is prepared by the following steps:
mixing desilication high-alumina fly ash, alumina, kaolinite and carbon nano tube, ball milling, mixing with polyvinyl alcohol and ammonium bicarbonate, adding into a mould, maintaining pressure for 2-3min under the condition of 200-220MPa, and roasting for 2-3h under the condition of 1200-1500 ℃ to obtain porous filler.
2. The method for producing a high-filtration low-resistance double-layer melt-blown nonwoven fabric for medical and sanitary materials according to claim 1, wherein: the molar ratio of the amino groups in the modified cellulose liquid to the epoxy groups in the modified polyester in the step S1 is 1:4, and the mass ratio of the composite particles, the porous filler and the fluorocarbon resin in the step S2 is 5:0.02:2.
3. The method for producing a high-filtration low-resistance double-layer melt-blown nonwoven fabric for medical and sanitary materials according to claim 1, wherein: the dosage ratio of the 4,4' -dimethylbiphenyl to the concentrated sulfuric acid to the nitric acid solution in the step A1 is 0.01mol:20mL:6mL, the mass fraction of the concentrated sulfuric acid is 98%, the mass fraction of the nitric acid solution is 60%, and the molar ratio of the intermediate 1 to the chlorine is 1:1.
4. The method for producing a high-filtration low-resistance double-layer melt-blown nonwoven fabric for medical and sanitary materials according to claim 1, wherein: the dosage ratio of the intermediate 2 to the concentrated hydrochloric acid to the tin powder in the step A2 is 3g to 20mL to 8g, the mass fraction of the concentrated hydrochloric acid is 36%, and the molar ratio of hydroxyl groups in cellulose to the intermediate 3 is 1 to 0.25.
5. The method for producing a high-filtration low-resistance double-layer melt-blown nonwoven fabric for medical and sanitary materials according to claim 1, wherein: the dosage ratio of 5-hydroxy isophthalic acid, methanol, concentrated sulfuric acid and hexane in the step B1 is 0.2mol:100mL:5mL:100mL, the mass fraction of the concentrated sulfuric acid is the same as that in the step A1, the dosage ratio of the intermediate 4, acetic anhydride and pyridine is 0.1mol:25mL:1mL, and the molar ratio of sodium borohydride, lithium chloride and intermediate 5 is 2.5:2.5:0.4.
6. The method for producing a high-filtration low-resistance double-layer melt-blown nonwoven fabric for medical and sanitary materials according to claim 1, wherein: the molar ratio of the intermediate 6 to terephthalic acid to ethylene glycol in the step B2 is 0.05:1:1.5, the amount of antimony acetate is 0.05% of the mass of the reactants, and the molar ratio of hydroxyl groups of the polyester to epichlorohydrin is 1:1.
7. The method for producing a high-filtration low-resistance double-layer melt-blown nonwoven fabric for medical and sanitary materials according to claim 1, wherein: the mass ratio of the desilication high-alumina fly ash to the alumina to the kaolinite to the carbon nano tube is 6:2:1:0.5.
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