CN114517011A - Waterproof breathable material and preparation method thereof - Google Patents
Waterproof breathable material and preparation method thereof Download PDFInfo
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- CN114517011A CN114517011A CN202111586003.4A CN202111586003A CN114517011A CN 114517011 A CN114517011 A CN 114517011A CN 202111586003 A CN202111586003 A CN 202111586003A CN 114517011 A CN114517011 A CN 114517011A
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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
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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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
- C08J2377/00—Characterised by the use of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Derivatives of such polymers
- C08J2377/06—Polyamides derived from polyamines and polycarboxylic acids
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/01—Use of inorganic substances as compounding ingredients characterized by their specific function
- C08K3/013—Fillers, pigments or reinforcing additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/13—Phenols; Phenolates
- C08K5/134—Phenols containing ester groups
- C08K5/1345—Carboxylic esters of phenolcarboxylic acids
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/16—Nitrogen-containing compounds
- C08K5/20—Carboxylic acid amides
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/54—Silicon-containing compounds
- C08K5/544—Silicon-containing compounds containing nitrogen
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 quinolyl phenylsulfonyl phenoxy fluorine-containing polyamide polycondensate is prepared from 2, 3-quinoline dicarboxylic acid, 4' -diamino diphenyl sulfone and 2, 2-bis [4- (4-aminophenoxy) phenyl ] -1,1,1,3,3, 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 breathability, good mechanical property, excellent performance stability and environmental friendliness and long service life.
Description
Technical Field
The invention relates to the technical field of waterproof materials, in particular to a waterproof and breathable material and a preparation method thereof.
Background
Along with the development of economy of China, the status of the packaging material in promoting the construction of national economy and improving the material culture life of people is increasingly shown. The waterproof and breathable material is widely applied to the industries of pesticides, chemical fertilizers, industrial chemicals, foods and the like as a common packaging material. The waterproof breathable material is just a material capable of blocking water molecules and allowing gas to pass through as the name suggests, in the prior art, a plurality of waterproof materials and breathable materials are provided, but the number of materials with the functions of both materials is small and few, and only some materials have enough waterproofness and poor breathability, so that the application of the material is limited.
At present, the waterproof and breathable material mostly adopts a structural mode of non-woven fabric, breathable high polymer material and non-woven fabric, but the waterproof and breathable material produced at home and abroad has the following problems: 1) the non-woven fabric is mostly made of polyacrylate (PP), although the non-woven fabric made of the material also has the advantages of the non-woven fabric, the non-woven fabric is low in strength and poor in durability, and is easy to age under long-term ultraviolet irradiation; 2) polytetrafluoroethylene (EPTFE) is mostly adopted as a breathable high polymer material, although EPTFE is popular in the industry, ammonium Perfluorooctanoate (PFOA) is required to be used as a raw material in the production process, and PFOA is a strong carcinogenic substance and brings great harm to operators in the production line.
In order to solve the above problems, chinese patent application CN105268013A discloses a breathable waterproof casting film material comprising: the high-pressure polyethylene, the low-pressure polyethylene, the linear polyethylene, the metallocene, the polypropylene and the additive account for 26 percent, 35 percent, 17 percent, 10 percent, 5 percent and 7 percent of the breathable waterproof casting film material in percentage by weight respectively, and the additive comprises a color masterbatch and an opening agent. Through the mode, the breathable waterproof cast film material is mixed according to a proportion, then is heated and melted, is matched with a waterproof breathable film processing technology, is easy to produce the cast film with the waterproof and breathable functions, is light and thin in texture, soft in touch and high in tensile strength, is suitable for being used as a sanitary towel back material, and improves the comfort of a user. However, both the puncture resistance and the air permeability are still to be improved.
Therefore, the waterproof and breathable material with good waterproof and breathable properties, good mechanical properties, excellent performance stability and environmental protection property 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 which is good in waterproof breathability, good in mechanical property, excellent in performance stability and environmental friendliness and long in service life and a preparation method thereof.
In order to achieve the purpose, 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 quinolyl phenylsulfonyl phenoxy fluorine-containing polyamide polycondensate is prepared from 2, 3-quinoline dicarboxylic acid, 4' -diaminodiphenyl sulfone and 2, 2-bis [4- (4-aminophenoxy) phenyl ] -1,1,1,3,3, 3-hexafluoropropane through polycondensation.
Preferably, the preparation method of the quinolyl phenylsulfonyl phenoxy fluorine-containing polyamide polycondensate comprises the following steps: uniformly mixing 2, 3-quinolinedicarboxylic acid, 4' -diaminodiphenyl sulfone, 2-bis [4- (4-aminophenoxy) phenyl ] -1,1,1,3,3, 3-hexafluoropropane, N-diisopropylethylamine, 4-dimethylaminopyridine and a high-boiling-point solvent to form a solution, then adding the solution into a reaction kettle, replacing the air in the kettle with inert gas, reacting for 4-6 hours at the temperature of 125-140 ℃ under normal pressure, then heating to the temperature of 235-245 ℃, carrying out polycondensation reaction for 15-22 hours under the pressure of 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 in vacuum drying oven at 85-95 deg.C to constant weight to obtain the final product.
Preferably, the molar ratio of the 2, 3-quinolinedicarboxylic acid, the 4, 4' -diaminodiphenyl sulfone, the 2, 2-bis [4- (4-aminophenoxy) phenyl ] -1,1,1,3,3, 3-hexafluoropropane, the N, N-diisopropylethylamine, the 4-dimethylaminopyridine and the high boiling point solvent is 2:1:1 (0.8-1.2) to (0.6-0.8) to (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 particle size of the volcanic rock is 1000-1200 meshes.
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, adding the mixed material into a double-screw extruder, and carrying out mixing, extrusion and granulation; then casting to form a film, and finally performing bidirectional or unidirectional stretching to obtain the waterproof breathable material.
Preferably, the temperature of the extrusion granulation is 230-260 ℃, and the screw rotation speed is 200-400 rpm.
Preferably, the temperature of the casting 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 breathable material disclosed by the invention has the advantages of simple operation process, excellent product performance, good reproducibility, no need of expensive experimental equipment, very good prospect of large-scale industrial production, and remarkable economic, social and ecological benefits.
(2) The waterproof breathable material disclosed by the invention has the advantages that through the mutual matching and combined action of the components, the prepared waterproof breathable material has good waterproof breathability, good mechanical properties, excellent performance stability and environmental friendliness and long service life.
(3) According to the waterproof breathable material disclosed by the invention, quinolyl, phenylsulfonyl, phenoxy, fluorine-containing group and acylamino are simultaneously introduced into a molecular chain of the quinolyl phenylsulfonyl phenoxy fluorine-containing polyamide polycondensate, and under the multiple actions of an electronic effect, a steric effect and a conjugated effect, the prepared waterproof breathable material has better puncture resistance, aging resistance and waterproofness; the addition of the volcanic rock can improve the mechanical property of the material, improve the stability of the property and prolong the service life of the material.
(4) The invention discloses a waterproof breathable material, wherein the quinolyl phenylsulfonyl phenoxy fluorine-containing polyamide polycondensate is prepared by carrying out polycondensation reaction on 2, 3-quinoline dicarboxylic acid, 4' -diamino diphenyl sulfone and 2, 2-bis [4- (4-aminophenoxy) phenyl ] -1,1,1,3,3, 3-hexafluoropropane; the method comprises the steps of carrying out amidation polycondensation reaction on a dicarboxyl functional group on 2, 3-quinolinedicarboxylic acid and a diamino functional group respectively contained on 4, 4' -diaminodiphenyl sulfone and 2, 2-bis [4- (4-aminophenoxy) phenyl ] -1,1,1,3,3, 3-hexafluoropropane, and simultaneously introducing quinolyl, phenylsulfonyl, phenoxy, fluorine-containing group and amide group to a polycondensate molecular chain at one time; by controlling the proportion of the groups, the comonomers enter a molecular chain of the polycondensate and form corresponding structural units in the molecular chain, so that the process is simple and the operation and the control are convenient; the catalytic dehydrating agent is N, N-diisopropylethylamine and 4-dimethylaminopyridine, so that the reaction rate is effectively improved, and the harsh requirements of the reaction on reaction conditions are reduced.
Detailed Description
The following description is presented to disclose the invention so as to enable any person skilled in the art to practice the invention. The preferred embodiments in the following description are given 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 quinolyl phenylsulfonyl phenoxy fluorine-containing polyamide polycondensate is prepared from 2, 3-quinoline dicarboxylic acid, 4' -diamino diphenyl sulfone and 2, 2-bis [4- (4-aminophenoxy) phenyl ] -1,1,1,3,3, 3-hexafluoropropane through polycondensation reaction.
The preparation method of the quinolyl phenylsulfonyl phenoxy fluorine-containing polyamide polycondensate comprises the following steps: uniformly mixing 2, 3-quinolinedicarboxylic acid, 4' -diaminodiphenyl sulfone, 2-bis [4- (4-aminophenoxy) phenyl ] -1,1,1,3,3, 3-hexafluoropropane, N-diisopropylethylamine, 4-dimethylaminopyridine and a high-boiling-point solvent to form a solution, adding the solution into a reaction kettle, replacing the air in the kettle with inert gas, reacting at 125 ℃ under normal pressure for 4 hours, heating to 235 ℃, carrying out polycondensation reaction at 300Pa for 15 hours, cooling to room temperature, adjusting to normal pressure, precipitating in water, washing the precipitated polymer with ethanol for 3 times, and drying in a vacuum drying oven at 85 ℃ to constant weight to obtain the quinolyl phenylsulfonyl phenoxy fluorine-containing polyamide polycondensate polymer.
The molar ratio of the 2, 3-quinolinedicarboxylic acid to the 4, 4' -diaminodiphenyl sulfone to the 2, 2-bis [4- (4-aminophenoxy) phenyl ] -1,1,1,3,3, 3-hexafluoropropane to the N, N-diisopropylethylamine to the 4-dimethylaminopyridine to the high-boiling solvent is 2:1:1:0.8:0.6: 15; the high boiling point solvent is dimethyl sulfoxide; the inert gas is nitrogen.
The particle size of the volcanic rock is 1000 meshes; the coupling agent is a silane coupling agent KH 550; the antioxidant is 1010; the lubricant is ethylene bis stearamide.
A preparation method of the waterproof breathable material comprises the following steps: uniformly mixing the components in parts by weight to obtain a mixed material, adding the mixed material into a double-screw extruder, and carrying out mixing, extrusion and granulation; then casting to form a film, and finally performing bidirectional or unidirectional stretching to obtain the waterproof breathable material; the temperature of the extrusion granulation is 230 ℃, and the rotating speed of a screw is 200 r/min; the temperature of the cast film formation is 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 quinolyl phenylsulfonyl phenoxy fluorine-containing polyamide polycondensate is prepared from 2, 3-quinoline dicarboxylic acid, 4' -diamino diphenyl sulfone and 2, 2-bis [4- (4-aminophenoxy) phenyl ] -1,1,1,3,3, 3-hexafluoropropane through polycondensation reaction.
The preparation method of the quinolyl phenylsulfonyl phenoxy fluorine-containing polyamide polycondensate comprises the following steps: uniformly mixing 2, 3-quinolinedicarboxylic acid, 4' -diaminodiphenyl sulfone, 2-bis [4- (4-aminophenoxy) phenyl ] -1,1,1,3,3, 3-hexafluoropropane, N-diisopropylethylamine, 4-dimethylaminopyridine and a high-boiling-point solvent to form a solution, adding the solution into a reaction kettle, replacing the air in the kettle with inert gas, reacting at 129 ℃ under normal pressure for 4.5 hours, heating to 239 ℃, carrying out polycondensation reaction at 400Pa for 17 hours, cooling to room temperature, adjusting to normal pressure, precipitating in water, washing the precipitated polymer with ethanol for 4 times, and drying in a vacuum drying oven at 87 ℃ to constant weight to obtain the quinolyl phenylsulfonyl phenoxy fluorine-containing polyamide polycondensate.
The molar ratio of the 2, 3-quinolinedicarboxylic acid to the 4, 4' -diaminodiphenyl sulfone to the 2, 2-bis [4- (4-aminophenoxy) phenyl ] -1,1,1,3,3, 3-hexafluoropropane to the N, N-diisopropylethylamine to the 4-dimethylaminopyridine to the high-boiling 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 a silane coupling agent KH 560; the antioxidant is antioxidant 168; the lubricant is stearic acid.
A preparation method of the waterproof breathable material comprises the following steps: uniformly mixing the components in parts by weight to obtain a mixed material, adding the mixed material into a double-screw extruder, and carrying out mixing, extrusion and granulation; then casting to form a film, and finally performing bidirectional or unidirectional stretching to obtain the waterproof breathable material; the temperature of the extrusion granulation is 240 ℃, and the rotating speed of a screw is 250 r/min; the temperature of the casting film forming is 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 quinolyl phenylsulfonyl phenoxy fluorine-containing polyamide polycondensate is prepared from 2, 3-quinoline dicarboxylic acid, 4' -diaminodiphenyl sulfone and 2, 2-bis [4- (4-aminophenoxy) phenyl ] -1,1,1,3,3, 3-hexafluoropropane through polycondensation.
The preparation method of the quinolyl phenylsulfonyl phenoxy fluorine-containing polyamide polycondensate comprises the following steps: uniformly mixing 2, 3-quinolinedicarboxylic acid, 4' -diaminodiphenyl sulfone, 2-bis [4- (4-aminophenoxy) phenyl ] -1,1,1,3,3, 3-hexafluoropropane, N-diisopropylethylamine, 4-dimethylaminopyridine and a high-boiling-point solvent to form a solution, adding the solution into a reaction kettle, replacing the air in the kettle with inert gas, reacting at 133 ℃ under normal pressure for 5 hours, heating to 240 ℃, carrying out polycondensation reaction at 450Pa for 19 hours, cooling to room temperature, adjusting to normal pressure, precipitating in water, washing the precipitated polymer with ethanol for 5 times, and drying in a vacuum drying oven at 90 ℃ to constant weight to obtain the quinolyl phenylsulfonyl phenoxy fluorine-containing polyamide polycondensate polymer.
The molar ratio of the 2, 3-quinolinedicarboxylic acid to the 4, 4' -diaminodiphenyl sulfone to the 2, 2-bis [4- (4-aminophenoxy) phenyl ] -1,1,1,3,3, 3-hexafluoropropane to the N, N-diisopropylethylamine to the 4-dimethylaminopyridine to the high-boiling 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 KH 570; the antioxidant is 1010; the lubricant is calcium stearate.
A preparation method of the waterproof breathable material comprises the following steps: uniformly mixing the components in parts by weight to obtain a mixed material, adding the mixed material into a double-screw extruder, and carrying out mixing, extrusion and granulation; then casting to form a film, and finally performing bidirectional or unidirectional stretching to obtain the waterproof breathable material; the temperature of the extrusion granulation is 245 ℃, and the rotating speed of a screw is 300 r/min; the temperature of the casting film forming is 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 quinolyl phenylsulfonyl phenoxy fluorine-containing polyamide polycondensate is prepared from 2, 3-quinoline dicarboxylic acid, 4' -diamino diphenyl sulfone and 2, 2-bis [4- (4-aminophenoxy) phenyl ] -1,1,1,3,3, 3-hexafluoropropane through polycondensation reaction.
The preparation method of the quinolyl phenylsulfonyl phenoxy fluorine-containing polyamide polycondensate comprises the following steps: uniformly mixing 2, 3-quinolinedicarboxylic acid, 4' -diaminodiphenyl sulfone, 2-bis [4- (4-aminophenoxy) phenyl ] -1,1,1,3,3, 3-hexafluoropropane, N-diisopropylethylamine, 4-dimethylaminopyridine and a high-boiling-point solvent to form a solution, adding the solution into a reaction kettle, replacing the air in the kettle with inert gas, reacting at 138 ℃ for 5.5 hours under normal pressure, heating to 243 ℃, performing 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 at 93 ℃ in a vacuum drying oven to constant weight to obtain the quinolyl phenylsulfonyl phenoxy fluorine-containing polyamide polycondensate.
The molar ratio of the 2, 3-quinolinedicarboxylic acid to the 4, 4' -diaminodiphenyl sulfone to the 2, 2-bis [4- (4-aminophenoxy) phenyl ] -1,1,1,3,3, 3-hexafluoropropane to the N, N-diisopropylethylamine to the 4-dimethylaminopyridine to 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 particle size 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 in a mass ratio of 1:3: 5; the antioxidant is a mixture formed by mixing an antioxidant 1010 and an antioxidant 168 according to the 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 the mass ratio of 1:1:3: 2.
A preparation method of the waterproof breathable material comprises the following steps: uniformly mixing the components in parts by weight to obtain a mixed material, adding the mixed material into a double-screw extruder, and carrying out mixing, extrusion and granulation; then casting to form a film, and finally performing bidirectional or unidirectional stretching to obtain the waterproof breathable material; the temperature of the extrusion granulation is 255 ℃, and the rotating speed of a screw is 350 r/min; the temperature of the casting film forming is 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 quinolyl phenylsulfonyl phenoxy fluorine-containing polyamide polycondensate is prepared from 2, 3-quinoline dicarboxylic acid, 4' -diamino diphenyl sulfone and 2, 2-bis [4- (4-aminophenoxy) phenyl ] -1,1,1,3,3, 3-hexafluoropropane through polycondensation reaction.
The preparation method of the quinolyl phenylsulfonyl phenoxy fluorine-containing polyamide polycondensate comprises the following steps: uniformly mixing 2, 3-quinolinedicarboxylic acid, 4' -diaminodiphenyl sulfone, 2-bis [4- (4-aminophenoxy) phenyl ] -1,1,1,3,3, 3-hexafluoropropane, N-diisopropylethylamine, 4-dimethylaminopyridine and a high-boiling-point solvent to form a solution, adding the solution into a reaction kettle, replacing the air in the kettle with inert gas, reacting at 140 ℃ under normal pressure for 6 hours, then heating to 245 ℃, carrying out polycondensation reaction at 600Pa for 22 hours, then cooling to room temperature, adjusting to normal pressure, precipitating in water, washing the precipitated polymer with ethanol for 7 times, and then placing in a vacuum drying oven at 95 ℃ to constant weight to obtain the quinolyl phenylsulfonyl phenoxy fluorine-containing polyamide polycondensate.
The molar ratio of the 2, 3-quinolinedicarboxylic acid to the 4, 4' -diaminodiphenyl sulfone to the 2, 2-bis [4- (4-aminophenoxy) phenyl ] -1,1,1,3,3, 3-hexafluoropropane to the N, N-diisopropylethylamine to the 4-dimethylaminopyridine to the high-boiling 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 KH 550; the antioxidant is 1010; the lubricant is oxidized polyethylene wax.
A preparation method of the waterproof breathable material comprises the following steps: uniformly mixing the components in parts by weight to obtain a mixed material, adding the mixed material into a double-screw extruder, and carrying out mixing, extrusion and granulation; then casting to form a film, and finally performing bidirectional or unidirectional stretching to obtain the waterproof breathable material; the temperature of the extrusion granulation is 260 ℃, and the rotating speed of a screw is 400 r/min; the temperature of the casting film forming is 245 ℃.
Comparative example 1
A waterproof and breathable material, the formulation and the preparation method of which are similar to those of example 1, except that in the preparation process of the quinolyl phenylsulfonyl phenoxy fluorine-containing polyamide polycondensate, 2-bis [4- (4-aminophenoxy) phenyl ] -1,1,1,3,3, 3-hexafluoropropane is replaced by 4, 4' -diaminodiphenyl sulfone.
Comparative example 2
A waterproof and breathable material, the formulation and preparation method of which are similar to those of example 1, except that 2, 2-bis [4- (4-aminophenoxy) phenyl ] -1,1,1,3,3, 3-hexafluoropropane is used in place of 4, 4' -diaminodiphenyl sulfone in the preparation process of the quinolyl phenylsulfonyl phenoxy fluorine-containing polyamide polycondensate.
To further illustrate the beneficial technical effects of the waterproof and breathable materials made according to the embodiments of the present invention, the waterproof and breathable materials made according to the embodiments 1 to 5 and the comparative examples 1 to 2 were tested for their relevant performance, the test results are shown in table 1, and the test methods are as follows:
(1) puncture resistance: the test was carried out according to the standard GB/T10004.
(2) Air permeability: the test was carried out using GB/T21529.
(3) Aging 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 of the retention rate is, the better the aging resistance is.
(4) Water resistance (hydrostatic pressure resistance): measured with a model YG-812 hydrostatic pressure meter (GB/T4744-1991, hydrostatic pressure test for water impermeability).
TABLE 1
| Item | Puncture resistance | Air permeability | Aging resistance | Resistance to hydrostatic pressure |
| Unit of | N | g/m2/24h | % | 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 and breathable material disclosed in the embodiment of the present invention has more excellent puncture resistance, waterproofness, breathability and aging resistance.
The foregoing shows and describes the general principles, essential 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, which are merely illustrative of the principles of the invention, but that various changes and modifications may be made without departing from the spirit and scope of the invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (10)
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 quinolyl phenylsulfonyl phenoxy fluorine-containing polyamide polycondensate is prepared from 2, 3-quinoline dicarboxylic acid, 4' -diamino diphenyl sulfone and 2, 2-bis [4- (4-aminophenoxy) phenyl ] -1,1,1,3,3, 3-hexafluoropropane through polycondensation reaction.
2. The waterproof breathable material according to claim 1, wherein the preparation method of the quinolyl phenylsulfonyl phenoxy fluorine-containing polyamide polycondensate comprises the following steps: uniformly mixing 2, 3-quinolinedicarboxylic acid, 4' -diaminodiphenyl sulfone, 2-bis [4- (4-aminophenoxy) phenyl ] -1,1,1,3,3, 3-hexafluoropropane, N-diisopropylethylamine, 4-dimethylaminopyridine and a high-boiling-point solvent to form a solution, then adding the solution into a reaction kettle, replacing the air in the kettle with inert gas, reacting for 4-6 hours at the temperature of 125-140 ℃ under normal pressure, heating to the temperature of 235-245 ℃, carrying out polycondensation reaction for 15-22 hours under the pressure of 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 in vacuum drying oven at 85-95 deg.C to constant weight to obtain the final product.
3. The waterproof breathable material according to claim 2, characterized in that the molar ratio of 2, 3-quinolinedicarboxylic acid, 4' -diaminodiphenyl sulfone, 2-bis [4- (4-aminophenoxy) phenyl ] -1,1,1,3,3, 3-hexafluoropropane, N-diisopropylethylamine, 4-dimethylaminopyridine, high boiling point solvent is 2:1:1 (0.8-1.2) (0.6-0.8) to (15-20).
4. The waterproof breathable material of claim 2, wherein the high boiling point solvent is at least one of dimethylsulfoxide, N-dimethylformamide, N-dimethylacetamide, and N-methylpyrrolidone.
5. The waterproof breathable material of claim 2, wherein said inert gas is any one of nitrogen, helium, neon and argon.
6. The waterproof breathable material of claim 1, wherein the volcanic rock has a particle size of 1000-1200 meshes.
7. The waterproof breathable material according to claim 1, wherein said coupling agent is at least one of silane coupling agent KH550, silane coupling agent KH560, and silane coupling agent KH 570.
8. The waterproof breathable material of claim 1, wherein the antioxidant is at least one of antioxidant 1010 and antioxidant 168; the lubricant is at least one of ethylene bis stearamide, stearic acid, calcium stearate and oxidized polyethylene wax.
9. A method for preparing a waterproof and breathable material according to any one of claims 1 to 8, characterized in that it comprises the following steps: uniformly mixing the components in parts by weight to obtain a mixed material, adding the mixed material into a double-screw extruder, and carrying out mixing, extrusion and granulation; then casting to form a film, and finally performing bidirectional or unidirectional stretching to obtain the waterproof breathable material.
10. The method for preparing a waterproof and breathable material as claimed in claim 9, wherein the temperature of the extrusion granulation is 230-; the temperature of the casting film forming is 230-245 ℃.
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