CN114517011B - Waterproof breathable material and preparation method thereof - Google Patents

Waterproof breathable material and preparation method thereof Download PDF

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CN114517011B
CN114517011B CN202111586003.4A CN202111586003A CN114517011B CN 114517011 B CN114517011 B CN 114517011B CN 202111586003 A CN202111586003 A CN 202111586003A CN 114517011 B CN114517011 B CN 114517011B
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waterproof
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breathable material
coupling agent
antioxidant
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CN114517011A (en
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严亮
陈文旭
徐赢斐
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Ningbo Jeeao Chuangyi New Materials Co ltd
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J5/00Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/18Manufacture of films or sheets
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2377/00Characterised by the use of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Derivatives of such polymers
    • C08J2377/06Polyamides derived from polyamines and polycarboxylic acids
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/01Use of inorganic substances as compounding ingredients characterized by their specific function
    • C08K3/013Fillers, pigments or reinforcing additives
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00Use of organic ingredients
    • C08K5/04Oxygen-containing compounds
    • C08K5/13Phenols; Phenolates
    • C08K5/134Phenols containing ester groups
    • C08K5/1345Carboxylic esters of phenolcarboxylic acids
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00Use of organic ingredients
    • C08K5/16Nitrogen-containing compounds
    • C08K5/20Carboxylic acid amides
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00Use of organic ingredients
    • C08K5/54Silicon-containing compounds
    • C08K5/544Silicon-containing compounds containing nitrogen

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Abstract

The invention discloses a waterproof breathable material which is prepared from the following components in parts by weight: 60-80 parts of quinolyl phenylsulfonyl phenoxy fluorine-containing polyamide polycondensate, 20-30 parts of volcanic rock, 3-5 parts of coupling agent, 0.5-2 parts of antioxidant and 0.3-0.8 part of lubricant; the quinolinyl phenyl sulfone phenoxy fluorine-containing polyamide polycondensate is prepared from 2, 3-quinolinedicarboxylic acid, 4 ˈ -diamino diphenyl sulfone and 2, 2-bis [4- (4-aminophenoxy) phenyl ] -1, 3-hexafluoropropane through polycondensation reaction. The invention also discloses a preparation method of the waterproof breathable material. The waterproof breathable material disclosed by the invention has the advantages of good waterproof and breathable properties, good mechanical properties, excellent performance stability and environmental friendliness and long service life.

Description

Waterproof breathable material and preparation method thereof
Technical Field
The invention relates to the technical field of waterproof materials, in particular to a waterproof breathable material and a preparation method thereof.
Background
With the development of Chinese economy, the packaging material has increasingly appeared in promoting the construction of national economy and improving the status of mass culture life of people. The waterproof and breathable material is used as a common packaging material and is widely applied to industries such as pesticides, fertilizers, industrial chemicals, foods and the like. The waterproof and breathable materials are the materials which can block water molecules but allow gas to pass through, but the materials with the functions of the waterproof and breathable materials are few in the prior art, and only some materials are enough in waterproof property and poor in breathability, so that the application of the waterproof and breathable materials is limited.
At present, the waterproof and breathable material mostly adopts a structural mode of non-woven fabrics, breathable polymer materials and non-woven fabrics, but the waterproof and breathable material produced at home and abroad has the following problems: 1) The non-woven fabric is made of polyacrylate (PP), and the non-woven fabric made of the material has the advantages of low strength and poor durability, and is easy to age under long-term ultraviolet irradiation; 2) Polytetrafluoroethylene (EPTFE) is mostly adopted as the breathable polymer material, and although the EPTFE enjoys a lot of reputation in the industry, ammonium Perfluorooctanoate (PFOA) is used as a raw material in the production process of the EPTFE, and the PFOA is a strong carcinogen and is easy to bring great harm to operators in the production line.
To solve the above problems, chinese patent application CN105268013a discloses a breathable waterproof casting film material comprising: the breathable waterproof casting film comprises, by weight, high-pressure polyethylene, low-pressure polyethylene, linear polyethylene, metallocene, polypropylene and additives, wherein the high-pressure polyethylene, the low-pressure polyethylene, the linear polyethylene, the metallocene, the polypropylene and the additives account for 26%, 35%, 17%, 10%, 5% and 7% of the breathable waterproof casting film material respectively, and the additives comprise color concentrates and opening agents. Through the mode, the breathable waterproof casting film material disclosed by the invention is heated and melted after being mixed according to the proportion, and is matched with a waterproof and breathable film processing technology, so that the casting film with waterproof and breathable functions is easy to produce, and the produced casting film is light and thin in texture, soft in touch, high in tensile strength, suitable for being used as a back material of a sanitary towel, and capable of improving the comfort of a user. However, the puncture resistance and the air permeability are still further improved.
Therefore, the waterproof and breathable material with good waterproof and breathable properties, good mechanical properties, excellent performance stability and environmental protection and long service life and the preparation method thereof are still needed in the field.
Disclosure of Invention
The invention mainly aims to provide a waterproof breathable material with good waterproof breathability, good mechanical properties, excellent performance stability and environmental protection and long service life and a preparation method thereof.
In order to achieve the aim, the invention provides a waterproof breathable material which is characterized by being prepared from the following components in parts by weight: 60-80 parts of quinolyl phenylsulfonyl phenoxy fluorine-containing polyamide polycondensate, 20-30 parts of volcanic rock, 3-5 parts of coupling agent, 0.5-2 parts of antioxidant and 0.3-0.8 part of lubricant; the quinolinyl phenyl sulfone phenoxy fluorine-containing polyamide polycondensate is prepared from 2, 3-quinolinedicarboxylic acid, 4 ˈ -diamino diphenyl sulfone and 2, 2-bis [4- (4-aminophenoxy) phenyl ] -1, 3-hexafluoropropane through polycondensation reaction.
Preferably, the preparation method of the quinolinyl phenyl sulfonyl phenoxy fluorine-containing polyamide polycondensate comprises the following steps: 2, 3-quinoline dicarboxylic acid, 4- ˈ -diaminodiphenyl sulfone 2, 2-bis [4- (4-aminophenoxy) phenyl ] -1, 3-hexafluoropropane, N, N-diisopropylethylamine, 4-dimethylaminopyridine and a high boiling point solvent are uniformly mixed to form a solution, then the solution is added into a reaction kettle, the air in the kettle is replaced by inert gas, the reaction is carried out for 4 to 6 hours at the normal pressure of 125 to 140 ℃, heating to 235-245 ℃, carrying out polycondensation reaction for 15-22 hours under 300-600Pa, cooling to room temperature, adjusting to normal pressure, precipitating in water, washing the precipitated polymer with ethanol for 3-7 times, and drying to constant weight under 85-95 ℃ in a vacuum drying oven to obtain the quinolyl phenylsulfonyl phenoxy fluorine-containing polyamide polycondensate.
Preferably, the molar ratio of the 2, 3-quinoline dicarboxylic acid, the 4,4 ˈ -diamino diphenyl sulfone, the 2, 2-bis [4- (4-aminophenoxy) phenyl ] -1, 3-hexafluoropropane, the N, N-diisopropylethylamine, the 4-dimethylaminopyridine and the high boiling point solvent is 2:1:1 (0.8-1.2): 0.6-0.8): 15-20.
Preferably, the high boiling point solvent is at least one of dimethyl sulfoxide, N-dimethylformamide, N-dimethylacetamide and N-methylpyrrolidone.
Preferably, the inert gas is any one of nitrogen, helium, neon and argon.
Preferably, the volcanic rock has a particle size of 1000-1200 mesh.
Preferably, the coupling agent is at least one of a silane coupling agent KH550, a silane coupling agent KH560 and a silane coupling agent KH 570.
Preferably, the antioxidant is at least one of antioxidant 1010 and antioxidant 168.
Preferably, the lubricant is at least one of ethylene bis stearamide, stearic acid, calcium stearate and oxidized polyethylene wax.
Another object of the present invention is to provide a method for preparing the waterproof and breathable material, which is characterized by comprising the following steps: uniformly mixing the components in parts by weight to obtain a mixed material, and then adding the mixed material into a double-screw extruder for mixing, extruding and granulating; and casting to form a film, and finally stretching in two directions or one direction to obtain the waterproof breathable material.
Preferably, the temperature of the extrusion granulation is 230-260 ℃, and the screw rotating speed is 200-400 rpm.
Preferably, the temperature of the cast film is 230-245 ℃.
Due to the application of the technical scheme, the invention has the following beneficial effects:
(1) The preparation method of the waterproof and breathable material disclosed by the invention has the advantages of simple operation process, excellent product performance, good reproducibility, no need of expensive experimental equipment, and very good large-scale industrial production prospect, and remarkable economic benefit, social benefit and ecological benefit.
(2) According to the waterproof breathable material disclosed by the invention, through mutual matching and combined action of the components, the prepared waterproof breathable material is good in waterproof breathability, good in mechanical property, excellent in performance stability and environmental friendliness and long in service life.
(3) According to the waterproof breathable material disclosed by the invention, the quinolinyl, the phenylsulfonyl, the phenoxy, the fluorine-containing group and the amide are simultaneously introduced into the molecular chain of the quinolinyl phenylsulfonyl phenoxy fluorine-containing polyamide polycondensate, and under the multiple actions of an electronic effect, a steric effect and a conjugation effect, the puncture resistance, the ageing resistance and the waterproofness of the prepared waterproof breathable material are better; the volcanic rock can improve the mechanical property of the material, improve the performance stability and prolong the service life of the material.
(4) The invention discloses a waterproof breathable material, wherein a quinolinyl phenyl sulfone phenoxy fluorine-containing polyamide polycondensate is prepared from 2, 3-quinolinedicarboxylic acid, 4 ˈ -diaminodiphenyl sulfone and 2, 2-bis [4- (4-aminophenoxy) phenyl ] -1, 3-hexafluoropropane through polycondensation reaction; amidation polycondensation reaction is carried out between dicarboxyl functional groups on 2, 3-quinoline dicarboxylic acid and diamino functional groups respectively contained on 4,4 ˈ -diamino diphenyl sulfone and 2, 2-bis [4- (4-aminophenoxy) phenyl ] -1, 3-hexafluoropropane, and simultaneously quinoline groups, phenyl sulfonyl groups, phenoxy groups, fluorine-containing groups and amide groups are introduced into a polycondensate molecular chain at one time; by controlling the group proportion, the comonomers enter a polycondensate molecular chain, and corresponding structural units are formed in the molecular chain, so that the process is simple, and the operation and control are convenient; the catalytic dehydrating agent is N, N-diisopropylethylamine or 4-dimethylaminopyridine, so that the reaction rate is effectively improved, and the harsh requirements of the reaction on the reaction conditions are reduced.
Detailed Description
The following description is presented to enable one of ordinary skill in the art to make and use the invention. The preferred embodiments in the following description are by way of example only and other obvious variations will occur to those skilled in the art.
Example 1
The waterproof breathable material is prepared from the following components in parts by weight: 60 parts of quinolyl phenylsulfonyl phenoxy fluorine-containing polyamide polycondensate, 20 parts of volcanic rock, 3 parts of coupling agent, 0.5 part of antioxidant and 0.3 part of lubricant; the quinolinyl phenyl sulfone phenoxy fluorine-containing polyamide polycondensate is prepared from 2, 3-quinolinedicarboxylic acid, 4 ˈ -diamino diphenyl sulfone and 2, 2-bis [4- (4-aminophenoxy) phenyl ] -1, 3-hexafluoropropane through polycondensation reaction.
The preparation method of the quinolinyl phenylsulfonyl phenoxy fluorine-containing polyamide polycondensate comprises the following steps: 2, 3-quinoline dicarboxylic acid, 4- ˈ -diaminodiphenyl sulfone 2, 2-bis [4- (4-aminophenoxy) phenyl ] -1, 3-hexafluoropropane, N, uniformly mixing N-diisopropylethylamine, 4-dimethylaminopyridine and a high boiling point solvent to form a solution, adding the solution into a reaction kettle, replacing air in the kettle with inert gas, reacting at 125 ℃ for 4 hours under normal pressure, heating to 235 ℃, carrying out polycondensation reaction for 15 hours under 300Pa, cooling to room temperature, adjusting to normal pressure, precipitating in water, washing the precipitated polymer with ethanol for 3 times, and drying to constant weight at 85 ℃ in a vacuum drying oven to obtain the quinolyl phenylsulfonyl phenoxy fluorine-containing polyamide polycondensate.
The molar ratio of the 2, 3-quinoline dicarboxylic acid, the 4,4 ˈ -diamino diphenyl sulfone, the 2, 2-bis [4- (4-aminophenoxy) phenyl ] -1, 3-hexafluoropropane, the N, N-diisopropylethylamine, the 4-dimethylaminopyridine and the high boiling point solvent is 2:1:1:0.8:0.6:15; the high boiling point solvent is dimethyl sulfoxide; the inert gas is nitrogen.
The grain diameter of the volcanic rock is 1000 meshes; the coupling agent is a silane coupling agent KH550; the antioxidant is antioxidant 1010; the lubricant is ethylene bis stearamide.
The preparation method of the waterproof breathable material comprises the following steps: uniformly mixing the components in parts by weight to obtain a mixed material, and then adding the mixed material into a double-screw extruder for mixing, extruding and granulating; casting to form a film, and finally carrying out bidirectional or unidirectional stretching to obtain the waterproof breathable material; the temperature of extrusion granulation is 230 ℃, and the rotating speed of a screw is 200 revolutions per minute; the temperature of the cast film was 230 ℃.
Example 2
The waterproof breathable material is prepared from the following components in parts by weight: 65 parts of quinolyl phenylsulfonyl phenoxy fluorine-containing polyamide polycondensate, 22 parts of volcanic rock, 3.5 parts of coupling agent, 0.9 part of antioxidant and 0.4 part of lubricant; the quinolinyl phenyl sulfone phenoxy fluorine-containing polyamide polycondensate is prepared from 2, 3-quinolinedicarboxylic acid, 4 ˈ -diamino diphenyl sulfone and 2, 2-bis [4- (4-aminophenoxy) phenyl ] -1, 3-hexafluoropropane through polycondensation reaction.
The preparation method of the quinolinyl phenylsulfonyl phenoxy fluorine-containing polyamide polycondensate comprises the following steps: 2, 3-quinoline dicarboxylic acid, 4- ˈ -diaminodiphenyl sulfone 2, 2-bis [4- (4-aminophenoxy) phenyl ] -1, 3-hexafluoropropane, N, uniformly mixing N-diisopropylethylamine, 4-dimethylaminopyridine and a high boiling point solvent to form a solution, adding the solution into a reaction kettle, replacing air in the kettle with inert gas, reacting at 129 ℃ for 4.5 hours under normal pressure, heating to 239 ℃, carrying out polycondensation reaction for 17 hours under 400Pa, cooling to room temperature, adjusting to normal pressure, precipitating in water, washing the precipitated polymer with ethanol for 4 times, and drying to constant weight at 87 ℃ in a vacuum drying oven to obtain the quinolyl phenyl sulfone phenoxy fluorine-containing polyamide polycondensate.
The molar ratio of the 2, 3-quinoline dicarboxylic acid, the 4,4 ˈ -diamino diphenyl sulfone, the 2, 2-bis [4- (4-aminophenoxy) phenyl ] -1, 3-hexafluoropropane, the N, N-diisopropylethylamine, the 4-dimethylaminopyridine and the high boiling point solvent is 2:1:1:0.9:0.65:17; the high boiling point solvent is N, N-dimethylformamide; the inert gas is helium.
The particle size of the volcanic rock is 1050 meshes; the coupling agent is silane coupling agent KH560; the antioxidant is antioxidant 168; the lubricant is stearic acid.
The preparation method of the waterproof breathable material comprises the following steps: uniformly mixing the components in parts by weight to obtain a mixed material, and then adding the mixed material into a double-screw extruder for mixing, extruding and granulating; casting to form a film, and finally carrying out bidirectional or unidirectional stretching to obtain the waterproof breathable material; the temperature of extrusion granulation is 240 ℃, and the rotating speed of a screw is 250 revolutions per minute; the temperature of the cast film was 235 ℃.
Example 3
The waterproof breathable material is prepared from the following components in parts by weight: 70 parts of quinolyl phenylsulfonyl phenoxy fluorine-containing polyamide polycondensate, 25 parts of volcanic rock, 4 parts of coupling agent, 1.3 parts of antioxidant and 0.5 part of lubricant; the quinolinyl phenyl sulfone phenoxy fluorine-containing polyamide polycondensate is prepared from 2, 3-quinolinedicarboxylic acid, 4 ˈ -diamino diphenyl sulfone and 2, 2-bis [4- (4-aminophenoxy) phenyl ] -1, 3-hexafluoropropane through polycondensation reaction.
The preparation method of the quinolinyl phenylsulfonyl phenoxy fluorine-containing polyamide polycondensate comprises the following steps: 2, 3-quinoline dicarboxylic acid, 4- ˈ -diaminodiphenyl sulfone 2, 2-bis [4- (4-aminophenoxy) phenyl ] -1, 3-hexafluoropropane, N, uniformly mixing N-diisopropylethylamine, 4-dimethylaminopyridine and a high boiling point solvent to form a solution, adding the solution into a reaction kettle, replacing air in the kettle with inert gas, reacting at 133 ℃ for 5 hours under normal pressure, heating to 240 ℃, carrying out polycondensation reaction for 19 hours under 450Pa, cooling to room temperature, adjusting to normal pressure, precipitating in water, washing the precipitated polymer with ethanol for 5 times, and drying to constant weight at 90 ℃ in a vacuum drying oven to obtain the quinolyl phenylsulfonyl phenoxy fluorine-containing polyamide polycondensate.
The molar ratio of the 2, 3-quinoline dicarboxylic acid, the 4,4 ˈ -diamino diphenyl sulfone, the 2, 2-bis [4- (4-aminophenoxy) phenyl ] -1, 3-hexafluoropropane, the N, N-diisopropylethylamine, the 4-dimethylaminopyridine and the high boiling point solvent is 2:1:1:1:0.7:17; the high boiling point solvent is N, N-dimethylacetamide; the inert gas is neon.
The particle size of the volcanic rock is 1100 meshes; the coupling agent is a silane coupling agent KH570; the antioxidant is antioxidant 1010; the lubricant is calcium stearate.
The preparation method of the waterproof breathable material comprises the following steps: uniformly mixing the components in parts by weight to obtain a mixed material, and then adding the mixed material into a double-screw extruder for mixing, extruding and granulating; casting to form a film, and finally carrying out bidirectional or unidirectional stretching to obtain the waterproof breathable material; the temperature of extrusion granulation is 245 ℃, and the rotating speed of a screw is 300 revolutions per minute; the temperature of the cast film was 239 ℃.
Example 4
The waterproof breathable material is prepared from the following components in parts by weight: 75 parts of quinolyl phenylsulfonyl phenoxy fluorine-containing polyamide polycondensate, 28 parts of volcanic rock, 4.5 parts of coupling agent, 1.8 parts of antioxidant and 0.7 part of lubricant; the quinolinyl phenyl sulfone phenoxy fluorine-containing polyamide polycondensate is prepared from 2, 3-quinolinedicarboxylic acid, 4 ˈ -diamino diphenyl sulfone and 2, 2-bis [4- (4-aminophenoxy) phenyl ] -1, 3-hexafluoropropane through polycondensation reaction.
The preparation method of the quinolinyl phenylsulfonyl phenoxy fluorine-containing polyamide polycondensate comprises the following steps: 2, 3-quinoline dicarboxylic acid, 4- ˈ -diaminodiphenyl sulfone 2, 2-bis [4- (4-aminophenoxy) phenyl ] -1, 3-hexafluoropropane, N, uniformly mixing N-diisopropylethylamine, 4-dimethylaminopyridine and a high boiling point solvent to form a solution, adding the solution into a reaction kettle, replacing air in the kettle with inert gas, reacting at 138 ℃ under normal pressure for 5.5 hours, heating to 243 ℃, carrying out polycondensation reaction for 20 hours under 550Pa, cooling to room temperature, adjusting to normal pressure, precipitating in water, washing the precipitated polymer with ethanol for 6 times, and drying to constant weight at 93 ℃ in a vacuum drying oven to obtain the quinolyl phenyl sulfone phenoxy fluorine-containing polyamide polycondensate.
The molar ratio of the 2, 3-quinoline dicarboxylic acid, the 4,4 ˈ -diamino diphenyl sulfone, the 2, 2-bis [4- (4-aminophenoxy) phenyl ] -1, 3-hexafluoropropane, the N, N-diisopropylethylamine, the 4-dimethylaminopyridine and the high boiling point solvent is 2:1:1:1.1:0.75:19; the high boiling point solvent is N-methyl pyrrolidone; the inert gas is argon.
The grain diameter of the volcanic rock is 1150 meshes; the coupling agent is a mixture formed by mixing a silane coupling agent KH550, a silane coupling agent KH560 and a silane coupling agent KH570 according to a mass ratio of 1:3:5; the antioxidant is a mixture formed by mixing an antioxidant 1010 and an antioxidant 168 according to a mass ratio of 2:3; the lubricant is a mixture formed by mixing ethylene bis stearamide, stearic acid, calcium stearate and oxidized polyethylene wax according to a mass ratio of 1:1:3:2.
The preparation method of the waterproof breathable material comprises the following steps: uniformly mixing the components in parts by weight to obtain a mixed material, and then adding the mixed material into a double-screw extruder for mixing, extruding and granulating; casting to form a film, and finally carrying out bidirectional or unidirectional stretching to obtain the waterproof breathable material; the temperature of extrusion granulation is 255 ℃, and the rotating speed of a screw is 350 revolutions per minute; the temperature of the cast film was 242 ℃.
Example 5
The waterproof breathable material is prepared from the following components in parts by weight: 80 parts of quinolyl phenylsulfonyl phenoxy fluorine-containing polyamide polycondensate, 30 parts of volcanic rock, 5 parts of coupling agent, 2 parts of antioxidant and 0.8 part of lubricant; the quinolinyl phenyl sulfone phenoxy fluorine-containing polyamide polycondensate is prepared from 2, 3-quinolinedicarboxylic acid, 4 ˈ -diamino diphenyl sulfone and 2, 2-bis [4- (4-aminophenoxy) phenyl ] -1, 3-hexafluoropropane through polycondensation reaction.
The preparation method of the quinolinyl phenylsulfonyl phenoxy fluorine-containing polyamide polycondensate comprises the following steps: 2, 3-quinoline dicarboxylic acid, 4- ˈ -diaminodiphenyl sulfone 2, 2-bis [4- (4-aminophenoxy) phenyl ] -1, 3-hexafluoropropane, N, uniformly mixing N-diisopropylethylamine, 4-dimethylaminopyridine and a high boiling point solvent to form a solution, adding the solution into a reaction kettle, replacing air in the kettle with inert gas, and (3) reacting at 140 ℃ under normal pressure for 6 hours, heating to 245 ℃, carrying out polycondensation reaction at 600Pa for 22 hours, cooling to room temperature, adjusting to normal pressure, precipitating in water, washing the precipitated polymer with ethanol for 7 times, and drying to constant weight at 95 ℃ in a vacuum drying oven to obtain the quinolyl phenylsulfonyl phenoxy fluorine-containing polyamide polycondensate.
The molar ratio of the 2, 3-quinoline dicarboxylic acid, the 4,4 ˈ -diamino diphenyl sulfone, the 2, 2-bis [4- (4-aminophenoxy) phenyl ] -1, 3-hexafluoropropane, the N, N-diisopropylethylamine, the 4-dimethylaminopyridine and the high boiling point solvent is 2:1:1:1.2:0.8:20; the high boiling point solvent is N-methyl pyrrolidone; the inert gas is nitrogen; the particle size of the volcanic rock is 1200 meshes; the coupling agent is a silane coupling agent KH550; the antioxidant is antioxidant 1010; the lubricant is oxidized polyethylene wax.
The preparation method of the waterproof breathable material comprises the following steps: uniformly mixing the components in parts by weight to obtain a mixed material, and then adding the mixed material into a double-screw extruder for mixing, extruding and granulating; casting to form a film, and finally carrying out bidirectional or unidirectional stretching to obtain the waterproof breathable material; the temperature of extrusion granulation is 260 ℃, and the rotating speed of a screw is 400 rpm; the temperature of the cast film was 245 ℃.
Comparative example 1
A waterproof breathable material has a formula and a preparation method similar to those of the example 1, except that 4,4 ˈ -diaminodiphenyl sulfone is used for replacing 2, 2-bis [4- (4-aminophenoxy) phenyl ] -1, 3-hexafluoropropane in the preparation process of the quinolylphenyl phenoxy fluorine-containing polyamide polycondensate.
Comparative example 2
A waterproof breathable material has a formula and a preparation method similar to those of the example 1, except that 2, 2-bis [4- (4-aminophenoxy) phenyl ] -1, 3-hexafluoropropane is used for replacing 4,4 ˈ -diaminodiphenyl sulfone in the preparation process of the quinolylphenyl sulfone phenoxy fluorine-containing polyamide polycondensate.
In order to further illustrate the beneficial technical effects of the waterproof and breathable materials prepared in the embodiments of the present invention, the waterproof and breathable materials prepared in the embodiments 1 to 5 and the comparative examples 1 to 2 were subjected to the relevant performance test, and the test results are shown in table 1, and the test methods are as follows:
(1) Puncture resistance: the test was performed according to standard GB/T10004.
(2) Air permeability: the test was performed using GB/T21529.
(3) Ageing resistance: after the material is placed in hot air at 85 ℃ for 96 hours, the retention rate of the puncture resistance is tested and calculated, and the larger the value is, the better the ageing resistance is.
(4) Waterproof (hydrostatic pressure resistance): the measurement was performed by means of YG-812 type hydrostatic pressure meter (GB/T4744-1991, anti-water permeation measurement hydrostatic pressure test).
TABLE 1
Project Puncture resistance Air permeability Aging resistance Hydrostatic pressure resistance
Unit (B) N g/m 2 /24h % MPa
Example 1 38.3 2112 97.93 0.25
Example 2 39.0 2124 98.25 0.27
Example 3 39.5 2132 98.92 0.28
Example 4 40.4 2138 99.39 0.28
Example 5 40.8 2142 99.84 0.30
Comparative example 1 36.0 2111 94.23 0.23
Comparative example 2 35.6 2111 97.07 0.24
As can be seen from table 1, the waterproof breathable material disclosed in the examples of the present invention has more excellent puncture resistance, waterproof property, breathability and aging resistance.
The foregoing has shown and described the basic principles, principal features and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, and that the above embodiments and descriptions are merely illustrative of the principles of the present invention, and various changes and modifications may be made therein without departing from the spirit and scope of the invention, which is defined by the appended claims. The scope of the invention is defined by the appended claims and equivalents thereof.

Claims (8)

1. The waterproof breathable material is characterized by being prepared from the following components in parts by weight: 60-80 parts of quinolyl phenylsulfonyl phenoxy fluorine-containing polyamide polycondensate, 20-30 parts of volcanic rock, 3-5 parts of coupling agent, 0.5-2 parts of antioxidant and 0.3-0.8 part of lubricant;
the preparation method of the quinolinyl phenylsulfonyl phenoxy fluorine-containing polyamide polycondensate comprises the following steps: 2, 3-quinoline dicarboxylic acid, 4- ˈ -diaminodiphenyl sulfone 2, 2-bis [4- (4-aminophenoxy) phenyl ] -1, 3-hexafluoropropane, N, N-diisopropylethylamine, 4-dimethylaminopyridine and a high boiling point solvent are uniformly mixed to form a solution, then the solution is added into a reaction kettle, the air in the kettle is replaced by inert gas, the reaction is carried out for 4 to 6 hours at the normal pressure of 125 to 140 ℃, heating to 235-245 ℃, carrying out polycondensation reaction for 15-22 hours under 300-600Pa, cooling to room temperature, adjusting to normal pressure, precipitating in water, washing the precipitated polymer with ethanol for 3-7 times, and drying to constant weight under 85-95 ℃ in a vacuum drying oven to obtain quinolyl phenylsulfonyl phenoxy fluorine-containing polyamide polycondensate; the molar ratio of the 2, 3-quinoline dicarboxylic acid, the 4,4 ˈ -diamino diphenyl sulfone, the 2, 2-bis [4- (4-aminophenoxy) phenyl ] -1, 3-hexafluoropropane, the N, N-diisopropylethylamine, the 4-dimethylaminopyridine and the high boiling point solvent is 2:1:1: (0.8-1.2): (0.6-0.8): (15-20).
2. The waterproof and breathable material according to claim 1, characterized in that said high boiling solvent is at least one of dimethylsulfoxide, N-dimethylformamide, N-dimethylacetamide, N-methylpyrrolidone.
3. The waterproof and breathable material according to claim 1, characterized in that said inert gas is any one of nitrogen, helium, neon and argon.
4. The waterproof and breathable material according to claim 1, characterized in that said volcanic rock has a particle size of 1000-1200 mesh.
5. The waterproof and breathable material according to claim 1, characterized in that said coupling agent is at least one of a silane coupling agent KH550, a silane coupling agent KH560, a silane coupling agent KH 570.
6. The waterproof and breathable material according to claim 1, characterized in that said antioxidant is at least one of antioxidant 1010, antioxidant 168; the lubricant is at least one of ethylene bis stearamide, stearic acid, calcium stearate and oxidized polyethylene wax.
7. A method of producing a waterproof and breathable material according to any one of claims 1 to 6, comprising the steps of: uniformly mixing the components in parts by weight to obtain a mixed material, and then adding the mixed material into a double-screw extruder for mixing, extruding and granulating; and casting to form a film, and finally stretching in two directions or one direction to obtain the waterproof breathable material.
8. The method for producing a waterproof and breathable material according to claim 7, characterized in that said extrusion granulation temperature is 230-260 ℃ and the screw rotation speed is 200-400 rpm; the temperature of the casting film is 230-245 ℃.
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Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH05170900A (en) * 1991-12-20 1993-07-09 Mitsui Toatsu Chem Inc Aromatic polyamide resin and resin composition thereof

Family Cites Families (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4826955A (en) * 1988-01-21 1989-05-02 Allied-Signal Inc. Amorphous copolyamide article of manufacture with moisture-insensitive oxygen barrier properties
AU649710B2 (en) * 1990-09-11 1994-06-02 Mitsubishi Gas Chemical Company, Inc. Polyamide resin composition and film therefrom
JPH08120099A (en) * 1994-10-27 1996-05-14 Unitika Ltd Polyamide film and its preparation
JP2000273168A (en) * 1999-03-29 2000-10-03 Hitachi Chem Co Ltd Aromatic polyamide and film, sheet, and adhesive made therefrom
JP3847579B2 (en) * 2001-06-28 2006-11-22 セントラル硝子株式会社 Alicyclic fluorinated dicarboxylic acid and polymer or photosensitive material composition using the same
US7041773B2 (en) * 2003-09-26 2006-05-09 General Electric Company Polyimide sulfones, method and articles made therefrom
JP5465987B2 (en) * 2009-11-20 2014-04-09 ユニチカ株式会社 Hot water-resistant polyamide film and method for producing the same
JP6072767B2 (en) * 2011-04-12 2017-02-01 アーケマ・インコーポレイテッド Multilayer breathable film
JP2014062201A (en) * 2012-09-21 2014-04-10 Yamamoto Chem Inc Polyamide and production method thereof
CN103304994A (en) * 2013-06-21 2013-09-18 苏州新区佳合塑胶有限公司 Wearable and hydrolysis-resistant enhanced nylon 66 composite material
CN105176078B (en) * 2015-08-11 2017-08-01 东华大学 A kind of polyimide modified engineering plastic alloy of electrodepositable biphenyl type dimaleoyl imino and preparation method thereof
CN109503830A (en) * 2018-12-06 2019-03-22 浙江新力新材料股份有限公司 A kind of preparation method of the amorphous nylon of low water absorbable
CN112480659A (en) * 2020-12-02 2021-03-12 厦门长塑实业有限公司 Toughened biaxially oriented polyamide film and preparation method thereof

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH05170900A (en) * 1991-12-20 1993-07-09 Mitsui Toatsu Chem Inc Aromatic polyamide resin and resin composition thereof

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