CN103114433A - Preparation method of open-fire resistance thermal insulation textile - Google Patents
Preparation method of open-fire resistance thermal insulation textile Download PDFInfo
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- CN103114433A CN103114433A CN2013100686651A CN201310068665A CN103114433A CN 103114433 A CN103114433 A CN 103114433A CN 2013100686651 A CN2013100686651 A CN 2013100686651A CN 201310068665 A CN201310068665 A CN 201310068665A CN 103114433 A CN103114433 A CN 103114433A
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Abstract
The invention discloses a preparation method of an open-fire resistance thermal insulation textile. The preparation method comprises the steps of: firstly modifying fiber surfaces, so that the fiber surfaces generate a plurality of-COOH groups so as to adsorb Mg(OH)2 seed crystals, then adopting a secondary growth method to enable the Mg(OH)2 seed crystals to grow for the second time on the fiber surfaces, preparing Mg(OH)2 crystal films which are completely coated on the fiber surfaces, then mixing a high-temperature resistance polymer solution and different dosages of organic pillar vermiculites by taking a high-temperature-resistant polymer phenolphthalein-based polyether sulphone as a continuous phase, so as to realize the uniform mixing of high-temperature-resistant polymers with different proportions and the organic pillar vermiculites by a physical means of supersonic wave cell smashing, coating fiber fabrics by the prepared high-temperature-resistant polymers and a vermiculite mixed liquid, wherein magnesium hydrate crystal films grow on the surfaces of the fiber fabrics, and forming vermiculite film protective layers with different thicknesses on the fiber surfaces through appropriate thermal treatment, so as to obtain the textile with strong open-fire resistance and thermal insulation property. The open-fire resistance thermal insulation textile prepared by using the preparation method has the advantages of improving the open-fire resistance and the thermal insulation property.
Description
Technical field
The present invention relates to by sheet Mg (OH) on fiber
2the acting in conjunction of crystal film and polyether sulphone/vermiculite composite membrane overcoat, cladding material for special protecting clothings such as fire-fighting fighting uniforms, improve the fire-proof and thermal-insulation ability of cladding material, exploitation is had can long-time anti-naked light, high heat insulation, fire-fighting fighting uniform that have comfortableness and flexibility concurrently has the preparation method of the thermal isolation of anti-naked light textiles of decisive role.
Background technology
Along with the quickening of Urbanization Process In China, high-rise, high-rise building increases gradually, and the people who works therein, lives is also more and more, and the fire problem of the skyscraper of the generation of following is also come to be attracted attention by the world.According to the fire statistics, learn: building fire generally accounts for 60% left and right of fire sum, and fire of high-rise building shared ratio in building fire is very large, and the fire probability is very high.Because current fire-fighting fighting uniform does not possess the ability of the thermal isolation of anti-the naked light, make fire fighters can not enter the scene of a fire, had a strong impact on fire fighters rescue and relief work ability.Develop the thermal isolation of anti-naked light fire-entry suit, improve the rescue and relief work ability of fire fighters and the survival ability in the scene of a fire, personal safety to the guarantee people is significant, and this material, except being endowed good fire-proof and thermal-insulation ability, also should have smoke suppressing preferably simultaneously.According to the analysis of current typical fire hazard consequence, generally can qualitatively think poison gas danger > danger of being fuming > intensity of a fire increases dangerous > heat release danger.In fire, about died more than 80% is because flue gas is lethal, and wherein major part is after having sucked flue dust and toxic gas (being mainly CO), and first stupor is scorched to death again, so this Technique Popularizing, to building trade, is also had to wide prospect as the building auxiliary material.
There is fire-resistant and fire-fighting fighting uniform thermal protection function and generally there is sandwich construction, be followed successively by from outside to inside flame-retardant material layer, waterproof ventilative layer, thermal insulation layer and comfort liner etc., wherein outermost material is to the structure of the selecting of the fire resistance of protective clothing, inner layer material, thermal insulation layer with thick and heavy etc. play conclusive effect, thereby affects practicality, comfortableness and the flexibility of protective clothing and fighting uniform.For cladding material, except difficulty combustion, fire-resistant, also should have fabulous heat-proof quality, improve the anti-naked light performance of material and thermal isolation performance thereof, exploitation is had can long-time anti-naked light, high fire-entry suit and fighting uniform heat insulation, that have comfortableness and flexibility concurrently have decisive role.
Whether the fire retardancy of appraisement system, except its flame retardant effect, has the good effect that presses down cigarette and the discharge of minimizing poison gas and is also paid close attention to gradually at present.The organic fire retardant, owing to there being the shortcoming that total smoke release is large, its catabolite toxicity is larger, is just progressively replaced by the mineral-type fire retardant.Mg (OH)
2typical Representative as the mineral-type fire retardant, because it decomposes caloric receptivity large (44.8 KJ/mol), the magnesia generated after decomposing is again high temperature resistant material, be attached to matrix surface and can further stop the carrying out of burning, have again simultaneously and do not produce harmful gas, the characteristics such as non-volatile, nontoxic, smokeless, therefore be widely used in the industries such as rubber, plastics, paint, coating, chemical industry.Mg (OH)
2obtained fairly large application as fire retardant and filler at polymeric material field, but its application report in textile field is less.
Industrial, a category mica mineral of expanding layer solution sharply when vermiculite refers to calcination as a kind of mineral products, comprise the interbed mineral that vermiculite on mineralogical significance and vermiculite crystal layer and phlogopite, biotite, chlorite crystal layer etc. form.Vermiculite usually in the form of sheets, is the product of the Mineral Weatherings such as biotite, phlogopite or hydrothermal alteration.From becoming the angle analysis in ore deposit, vermiculite should be the middle transition product of montmorillonite and gold (deceiving) mica.The primary mineral of vermiculite interlamellar spacing is 1.46 nm left and right, and wherein the crystal structure elementary layer of phyllosilicate (TOT layer) thickness is 0.93 nm, more than the intercalated vermiculite interlamellar spacing can reach 3 nm.The air wall is arranged between the vermiculite synusia, thereby can produce good effect of heat insulation, fusing point can reach 1370-1400 ℃, and its thermal conductivity factor is little, between (0.047-0.07) w/mk.Polyethersulfone with cardo is a kind of novel heat-resistant polymer, and its vitrification point can be up to 260 ℃.Except thering is good mechanical performance, also there is excellent high temperature resistant hydrolysis, chemical stability and DIMENSIONAL STABILITY.Thereby polyethersulfone with cardo is widely used in the every field such as Aeronautics and Astronautics, machinery.The special performance of heat insulation, the low heat conduction of the height therefore vermiculite had is attached in the preparation research of polymer/inorganic thing nano composite material will have great potentiality.
summary of the invention:
The objective of the invention is in order to overcome above deficiency, provide a kind of heat-resistant polymer with preparation and the growth of organic-pillared vermiculite mixed liquor effects on surface to have the fabric of magnesium hydroxide crystal film to be applied, through suitable heat treatment, form the vermiculite film overcoat of different-thickness on the surface of fiber, thereby prepare the preparation method of the textiles with the stronger thermal isolation of anti-naked light performance.
Purpose of the present invention is achieved through the following technical solutions: a kind of preparation method of the thermal isolation of anti-naked light textiles comprises the following steps: first fiber surface is carried out to modification, make it to produce a large amount of-COOH group with absorption Mg (OH)
2crystal seed, then adopt the diauxic growth method to make Mg (OH)
2crystal seed, at the fiber surface diauxic growth, makes the Mg (OH) that fiber surface is coated fully
2crystal film, take the heat-resistant polymer polyethersulfone with cardo as continuous phase again, heat-resistant polymer solution and organic-pillared vermiculite are mixed, the physical means of pulverizing by supersonic cell is realized the even mixing of heat-resistant polymer and organic-pillared vermiculite, with heat-resistant polymer and the growth of vermiculite mixed liquor effects on surface of preparation, there is the fabric of magnesium hydroxide crystal film to be applied, through Overheating Treatment, surface at fiber forms the vermiculite film overcoat, thereby prepares the textiles with the stronger thermal isolation of anti-naked light performance.
Further improvement of the present invention is, comprises following concrete steps:
Sheet Mg (OH) on A, fiber
2the preparation of crystal film:
A, fiber carboxy-modified: be divided into the carboxy-modified of the carboxy-modified of cellulose fibre and polysulphonamide fiber fabric, during cellulose fibre carboxy-modified, cellulose base fiber fabric is cut into to the bulk of fixed size, remove grease and the wax of fabric face with ether, with solvent and solute preparation modification liquid, solvent is redistilled water, solute is the inferior sodium phosphate that accounts for the citric acid of modification liquid gross mass 1%-30% and account for modification liquid gross mass 1%-20%, citric acid is modifying agent, inferior sodium phosphate is catalyst, by cellulose base fiber fabric impregnated in modification liquid two soak two roll carry out carboxy-modified, during polysulphonamide fiber fabric carboxy-modified, the polysulphonamide fiber fabric is cut into to the bulk of fixed size, remove grease and the wax of fabric face with ether, take 1-30g/L NaOH as modifying agent, the preparation modification liquid, by the polysulphonamide fiber textile impregnation in modification liquid two soak two roll carry out carboxy-modified,
B, Mg (OH)
2the preparation of crystal seed: under 10-80 ℃ of condition, by the NH of 0.1-10 mol/L
3 .h
2o solution is added drop-wise in the polyvinylpyrrolidonesolution solution of 1-30 g/L, the pH to 10.0 of regulation system ± 0.2, then with the speed of 1-50mL/hr by the MgCl of 0.01-1mol/L
2solution is added dropwise to rare NH
3 .h
2in the mixed liquor of O solution and polyvinylpyrrolidone, liquid feeding time remaining 1-10 h, therebetween by continuing to add the NH of 0.1-10mol/L
3 .h
2the pH value of the O solution hierarchy of control, in the 10.0-10.5 scope, after liquid feeding completes makes the prepared reactant liquor of said process vigorous stirring 0.5-5h ageing 0.5-5h under 10-80 ℃ of condition containing Mg (OH)
2the mother liquor of crystal seed;
C, Mg (OH)
2the absorption of crystal seed: adopt infusion process or adopt padding method, get the mother liquor of 50-500ml magnesium hydroxide crystal seed in some beakers while adopting infusion process, add the fabric after 0.1-10.0g modification, put into constant temperature oscillation water-bath vibration absorption, during vibration absorption, rotating speed is 20-100r/min, 10-80 ° of C, adsorption time is 30-120 minute, after absorption, with redistilled water, carefully wash, standby after drying, while adopting padding method, the fabric after the 0.1-10.0g modification being impregnated in the mother liquor of 50-500ml magnesium hydroxide crystal seed to two soaks two and rolls, standby after drying,
D, Mg (OH)
2the diauxic growth of crystal seed: absorption is had to Mg (OH)
2the fabric 0.1-10g of crystal seed drops in the saturated magnesium hydroxide solution of 100-1000mL, then simultaneously to the NH that passes into 0.01-1 mol/L in system
3 .h
2the MgCl of O solution and 0.01-1 mol/L
2solution, NH
3 .h
2the speed of O solution is 0.1-10mL/h, MgCl
2the speed of solution is 0.1-10 mL/h, after 1-60 days, fabric is taken out, and uses the second distillation water washing, 60-160 ℃ of oven dry;
The preparation of B, polyethersulfone with cardo and organic-pillared vermiculite mixed liquor:
The preparation of a, organic-pillared vermiculite: the vermiculite that 1-50g is ground and crosses 200 mesh sieves evenly mixes with 100-2000ml distilled water, grind 1-12 h with 500-5000 r/min in disperseing sand mill, make the corase grind vermiculite, to roughly grind vermiculite drops in distilled water again, the alkyl quaternary ammonium salts that the carbon chain lengths that adds 1-10 times of CEC cation exchange capacity (CEC) is 4-36, at 20-90 ℃ of lower stirring reaction 1-12h, then the vermiculite reacted completely with the distilled water cyclic washing is until without Cl
-, Br
-exist, use AgNO
3detected Cl
-, Br
–have situation, final drying, to constant weight, makes organic-pillared vermiculite;
B, the preparation of polyethersulfone with cardo and organic-pillared vermiculite mixed liquor: the 1-50g organic-pillared vermiculite is joined in the METHYLPYRROLIDONE of 50-2000ml, and add therein the CATION of 0.1-10g/L, anion, non-ionic dispersing agent, for the butanone 1-100ml of polyethersulfone with cardo solubilizer with for the butyl glycol ether 1-100ml of polyethersulfone with cardo cosolvent, fully stir 1-12 h, then add the 10-300g polyethersulfone with cardo, finally utilizing ultrasonic wave to process fully dissolves it, make polyethersulfone with cardo and organic-pillared vermiculite mixed liquor,
C, the preparation of the thermal isolation of anti-naked light textiles: adopt wet method film forming or dry method film forming during preparation, while adopting the wet method film forming, with coating device, the polyethersulfone with cardo of preparation and organic-pillared vermiculite mixed liquor are had in superficial growth on the fabric of magnesium hydroxide crystal film and filmed, immerse in coagulating bath, the DMAc aqueous solution that coagulating bath is mass fraction 10-60 %, under 20-60 ℃, 0.5-5h is solidified in displacement, again fabric is put into to distilled water and soak 6-48h, with the remaining METHYLPYRROLIDONE except in striping, butanone and butyl glycol ether, 60-160 ℃ of oven dry, make the thermal isolation of anti-naked light textiles, while adopting the dry method film forming, with coating device, the polyethersulfone with cardo of preparation and organic-pillared vermiculite mixed liquor are had in superficial growth on the fabric of magnesium hydroxide crystal film and filmed, 60-160 ℃ of oven dry, make the thermal isolation of anti-naked light textiles.
D, performance test: test the flame retarding and smoke suppressing properties of textiles by taper calorimeter and normal beam technique fabrics flame resistance ability meter, and test the thermal stability of textiles by thermogravimetric analyzer, by the heat-proof quality of thermal conductivity factor instrument test textiles.
The present invention compared with prior art has the following advantages: the thin slice of the nanometer grade thickness that vermiculite is separated by air layer forms, existence due to high porosity, the surface of vermiculite material has good heat radiation albedo in addition, therefore vermiculite has high heat-proof quality, for magnesium hydroxide sheet crystal layer, can and decompose the effect that refractory heat-insulating is played in heat-absorbing action by reflex, for fibrous material, be mainly the mode reflective thermal radiation by scattering.The present invention is by the compound system of vermiculite thin layer/flat crystal layer/fibrous material, improve its anti-naked light, thermal isolation performance, thermal isolation performance particularly, can be used for the fire-entry suit in the safety discrepancy scene of a fire or the cladding material of fighting uniform, can also be for building trade, improve the fire insulation performance of building auxiliary material, reduce the building fire incidence.
The accompanying drawing explanation:
The process chart that Fig. 1 is preparation method of the present invention;
the specific embodiment:
in order to deepen the understanding of the present invention, below in conjunction with embodiment and accompanying drawing, the invention will be further described, and this embodiment only, for explaining the present invention, does not form limiting the scope of the present invention.
As Fig. 1 shows the preparation method's of a kind of thermal isolation of anti-naked light textiles of the present invention the specific embodiment, first fiber surface is carried out to modification, make it to produce a large amount of-COOH group with absorption Mg (OH)
2crystal seed, then adopt the diauxic growth method to make Mg (OH)
2crystal seed, at the fiber surface diauxic growth, makes the Mg (OH) that fiber surface is coated fully
2crystal film, take the heat-resistant polymer polyethersulfone with cardo as continuous phase again, heat-resistant polymer solution and organic-pillared vermiculite are mixed, the physical means of pulverizing by supersonic cell is realized the even mixing of heat-resistant polymer and organic-pillared vermiculite, with heat-resistant polymer and the growth of vermiculite mixed liquor effects on surface of preparation, there is the fabric of magnesium hydroxide crystal film to be applied, through Overheating Treatment, surface at fiber forms the vermiculite film overcoat, thereby prepares the textiles with the stronger thermal isolation of anti-naked light performance.
Embodiment mono-: (1) is cut into COTTON FABRIC the bulk of fixed size, removes grease and the wax of fabric face with ether.Take citric acid as modifying agent, inferior sodium phosphate is catalyst, the preparation modification liquid, wherein the content of citric acid in modification liquid is the 9wt%(citric acid: inferior sodium phosphate=3:2), COTTON FABRIC be impregnated in modification liquid to two and soak two and roll and carry out carboxy-modifiedly, it is above to reach balance that the fabric of modification must be placed 12 h.
(2) under 35 ± 0.5 ℃ of conditions, by rare NH of 0.1 mol/L
3 .h
2o solution is added drop-wise in 200 mL polyvinylpyrrolidonesolution solution (10 g/L), the pH to 10.0 of regulation system ± 0.2, then with the speed of 10 mL/hr by the MgCl of 0.05 mol/L
2solution is added dropwise to rare NH
3 .h
2in the mixed liquor of O solution and polyvinylpyrrolidone, liquid feeding time remaining 2 h, therebetween by continuing to add the NH of 0.1mol/L
3 .h
2the pH value of the O solution hierarchy of control, in the 10.0-10.5 scope, after liquid feeding completes makes reactant liquor vigorous stirring 1 h ageing 1 h under 35 ± 0.5 ℃ of conditions containing Mg (OH)
2the mother liquor of crystal seed.
(3) get the Mg (OH) of 50mL
2the mother liquor of crystal seed, in some 400mL beakers, then adds respectively the 1.0g modified fabric through accurately weighing, and (rotating speed is 80r/min to put into constant temperature oscillation water-bath vibration absorption, 35 ° of C), adsorption time is 60 minutes, after absorption, through redistilled water, carefully wash, standby after drying.
(4) absorption is had to Mg (OH)
2cOTTON FABRIC 1.0 g of crystal seed drop in the saturated magnesium hydroxide solution of 500 mL, then pass into NH in system simultaneously
3 .h
2o solution (0.1 mol/L, speed are 1 mL/h) and MgCl
2solution (0.025 mol/L, speed are 2 mL/h) took out COTTON FABRIC after 30 days, used the second distillation water washing, and 80 ℃ of oven dry, observe surface of cotton fabric Mg (OH) by SEM
2form after the crystal seed diauxic growth.
(5) vermiculite that 10g is ground and crosses 200 mesh sieves evenly mixes with distilled water, in disperseing sand mill, with 2000 r/min, grinds 6h, makes the corase grind vermiculite.To roughly grind vermiculite again and drop in distilled water, and add the softex kw of 4 times of CEC, at 80 ℃ of lower stirring reaction 6h, then the vermiculite reacted completely with the distilled water cyclic washing is until without Br
-exist and (use AgNO
3detected), be dried to constant weight, make organic-pillared vermiculite.
(6) organic-pillared vermiculite of 2g is joined in the METHYLPYRROLIDONE of 90ml, and add therein dispersing agent C H-10S(1g/L), the butanone (solubilizer of polyethersulfone with cardo) of 5ml and the butyl glycol ether (cosolvent of polyethersulfone with cardo) of 5ml, fully stir 2 h, then add polyethersulfone with cardo 18g, utilize ultrasonic wave to process it is fully dissolved, make polyethersulfone with cardo/organic-pillared vermiculite mixed liquor.
(7) with coating device, the polyethersulfone with cardo of preparation and organic-pillared vermiculite mixed liquor are had in superficial growth on the COTTON FABRIC of magnesium hydroxide crystal film and filmed, immerse in coagulating bath (the DMAc aqueous solution that coagulating bath is mass fraction 50%), under 25 ℃, 1h is solidified in displacement, again fabric is put into to distilled water and soak 24h, with remaining METHYLPYRROLIDONE, butanone and butyl glycol ether except in striping, 50 ℃ of vacuum dryings, make the thermal isolation of anti-naked light textiles.
(8) finally naked light thermal isolation textiles is carried out to Performance Detection.
embodiment bis-:
(1) fragrant sulfone synthetic fibre fabric is cut into to the bulk of fixed size, remove the finish of fabric face with ether, take 7.5g/l NaOH as modifying agent, fragrant sulfone synthetic fibre textile impregnation two is soaked to two and rolls and carry out carboxy-modifiedly in modification liquid, it is above to reach balance that the fabric of modification must be placed 12 h.
(2) under 35 ± 0.5 ℃ of conditions, by rare NH of 0.1 mol/L
3 .h
2o solution is added drop-wise in 200 mL polyvinylpyrrolidonesolution solution (10 g/L), the pH to 10.0 of regulation system ± 0.2, then with the speed of 10 mL/hr by the MgCl of 0.05 mol/L
2solution is added dropwise to rare NH
3 .h
2in the mixed liquor of O solution and polyvinylpyrrolidone, liquid feeding time remaining 2 h, therebetween by continuing to add the NH of 0.1mol/L
3 .h
2the pH value of the O solution hierarchy of control, in the 10.0-10.5 scope, after liquid feeding completes makes reactant liquor vigorous stirring 1 h ageing 1 h under 35 ± 0.5 ℃ of conditions containing Mg (OH)
2the mother liquor of crystal seed.
(3) the fragrant sulfone synthetic fibre textile impregnation after the 1.0g modification two is soaked to two and rolls in the mother liquor of magnesium hydroxide crystal seed, standby after drying.
(4) absorption is had to Mg (OH)
2fragrant sulfone synthetic fibre fabric 1.0 g of crystal seed drop in the saturated magnesium hydroxide solution of 500 mL, then pass into NH in system simultaneously
3 .h
2o solution (0.2 mol/L, speed are 2 mL/h) and MgCl
2solution (0.05 mol/L, speed are 4 mL/h) took out fragrant sulfone synthetic fibre fabric after 21 days, used the second distillation water washing, and 80 ℃ of oven dry, observe fragrant sulfone synthetic fibre fabric face Mg (OH) by SEM
2form after the crystal seed diauxic growth.
(5) vermiculite that 10g is ground and crosses 200 mesh sieves evenly mixes with distilled water, grind 6 h with 2000 r/min in disperseing sand mill, make the corase grind vermiculite, to roughly grind vermiculite drops in distilled water again, the INCROQUAT TMC-80 that adds 2 times of CEC, at 80 ℃ of lower stirring reaction 6 h, then the vermiculite reacted completely with the distilled water cyclic washing is until without Cl
-exist and (use AgNO
3detected), be dried to constant weight, make organic-pillared vermiculite.
(6) organic-pillared vermiculite of 1g is joined in the METHYLPYRROLIDONE of 180ml, and add therein dispersing agent C H-10S(1g/L), the butanone (solubilizer of polyethersulfone with cardo) of 10ml and the butyl glycol ether (cosolvent of polyethersulfone with cardo) of 10ml, fully stir 2 h, then add polyethersulfone with cardo 19g, utilize ultrasonic wave to process it is fully dissolved, make polyethersulfone with cardo/organic-pillared vermiculite mixed liquor.
(7) 15% polyethersulfone with cardo that will prepare with coating device and organic-pillared vermiculite mixed liquor have in superficial growth on the fragrant sulfone synthetic fibre fabric of magnesium hydroxide crystal film is filmed, and 80 ℃ of oven dry, make the thermal isolation of anti-naked light textiles.
(8) finally naked light thermal isolation textiles is carried out to Performance Detection.
Claims (2)
1. the preparation method of the thermal isolation of anti-a naked light textiles, is characterized in that, comprises the following steps: first fiber surface is carried out to modification, make it to produce a large amount of-COOH group with absorption Mg (OH)
2crystal seed, then adopt the diauxic growth method to make Mg (OH)
2crystal seed, at the fiber surface diauxic growth, makes the Mg (OH) that fiber surface is coated fully
2crystal film, take the heat-resistant polymer polyethersulfone with cardo as continuous phase again, heat-resistant polymer solution and organic-pillared vermiculite are mixed, the physical means of pulverizing by supersonic cell is realized the even mixing of heat-resistant polymer and organic-pillared vermiculite, with heat-resistant polymer and the growth of vermiculite mixed liquor effects on surface of preparation, there is the fabric of magnesium hydroxide crystal film to be applied, through Overheating Treatment, surface at fiber forms the vermiculite film overcoat, thereby prepares the textiles with the stronger thermal isolation of anti-naked light performance.
2. according to claim 1 a kind of preparation method of the thermal isolation of anti-naked light textiles, is characterized in that, comprises following concrete steps:
Sheet Mg (OH) on A, fiber
2the preparation of crystal film:
A, fiber carboxy-modified: be divided into the carboxy-modified of the carboxy-modified of cellulose fibre and polysulphonamide fiber fabric, during cellulose fibre carboxy-modified, cellulose base fiber fabric is cut into to the bulk of fixed size, remove grease and the wax of fabric face with ether, with solvent and solute preparation modification liquid, solvent is redistilled water, solute is the inferior sodium phosphate that accounts for the citric acid of modification liquid gross mass 1%-30% and account for modification liquid gross mass 1%-20%, citric acid is modifying agent, inferior sodium phosphate is catalyst, by cellulose base fiber fabric impregnated in modification liquid two soak two roll carry out carboxy-modified, during polysulphonamide fiber fabric carboxy-modified, the polysulphonamide fiber fabric is cut into to the bulk of fixed size, remove grease and the wax of fabric face with ether, take 1-30g/L NaOH as modifying agent, the preparation modification liquid, by the polysulphonamide fiber textile impregnation in modification liquid two soak two roll carry out carboxy-modified,
B, Mg (OH)
2the preparation of crystal seed: under 10-80 ℃ of condition, by the NH of 0.1-10 mol/L
3 .h
2o solution is added drop-wise in the polyvinylpyrrolidonesolution solution of 1-30 g/L, the pH to 10.0 of regulation system ± 0.2, then with the speed of 1-50mL/hr by the MgCl of 0.01-1mol/L
2solution is added dropwise to rare NH
3 .h
2in the mixed liquor of O solution and polyvinylpyrrolidone, liquid feeding time remaining 1-10 h, therebetween by continuing to add the NH of 0.1-10mol/L
3 .h
2the pH value of the O solution hierarchy of control, in the 10.0-10.5 scope, after liquid feeding completes makes the prepared reactant liquor of said process vigorous stirring 0.5-5h ageing 0.5-5h under 10-80 ℃ of condition containing Mg (OH)
2the mother liquor of crystal seed;
C, Mg (OH)
2the absorption of crystal seed: adopt infusion process or adopt padding method, get the mother liquor of 50-500ml magnesium hydroxide crystal seed in some beakers while adopting infusion process, add the fabric after 0.1-10.0g modification, put into constant temperature oscillation water-bath vibration absorption, during vibration absorption, rotating speed is 20-100r/min, 10-80 ° of C, adsorption time is 30-120 minute, after absorption, with redistilled water, carefully wash, standby after drying, while adopting padding method, the fabric after the 0.1-10.0g modification being impregnated in the mother liquor of 50-500ml magnesium hydroxide crystal seed to two soaks two and rolls, standby after drying,
D, Mg (OH)
2the diauxic growth of crystal seed: absorption is had to Mg (OH)
2the fabric 0.1-10g of crystal seed drops in the saturated magnesium hydroxide solution of 100-1000mL, then simultaneously to the NH that passes into 0.01-1 mol/L in system
3 .h
2the MgCl of O solution and 0.01-1 mol/L
2solution, NH
3 .h
2the speed of O solution is 0.1-10mL/h, MgCl
2the speed of solution is 0.1-10 mL/h, after 1-60 days, fabric is taken out, and uses the second distillation water washing, 60-160 ℃ of oven dry;
The preparation of B, polyethersulfone with cardo and organic-pillared vermiculite mixed liquor:
The preparation of a, organic-pillared vermiculite: the vermiculite that 1-50g is ground and crosses 200 mesh sieves evenly mixes with 100-2000ml distilled water, grind 1-12 h with 500-5000 r/min in disperseing sand mill, make the corase grind vermiculite, to roughly grind vermiculite drops in distilled water again, the alkyl quaternary ammonium salts that the carbon chain lengths that adds 1-10 times of CEC cation exchange capacity (CEC) is 4-36, at 20-90 ℃ of lower stirring reaction 1-12h, then the vermiculite reacted completely with the distilled water cyclic washing is until without Cl
-, Br
-exist, use AgNO
3detected Cl
-, Br
–have situation, final drying, to constant weight, makes organic-pillared vermiculite;
B, the preparation of polyethersulfone with cardo and organic-pillared vermiculite mixed liquor: the 1-50g organic-pillared vermiculite is joined in the METHYLPYRROLIDONE of 50-2000ml, and add therein the CATION of 0.1-10g/L, anion, non-ionic dispersing agent, for the butanone 1-100ml of polyethersulfone with cardo solubilizer with for the butyl glycol ether 1-100ml of polyethersulfone with cardo cosolvent, fully stir 1-12 h, then add the 10-300g polyethersulfone with cardo, finally utilizing ultrasonic wave to process fully dissolves it, make polyethersulfone with cardo and organic-pillared vermiculite mixed liquor,
C, the preparation of the thermal isolation of anti-naked light textiles: adopt wet method film forming or dry method film forming during preparation, while adopting the wet method film forming, with coating device, the polyethersulfone with cardo of preparation and organic-pillared vermiculite mixed liquor are had in superficial growth on the fabric of magnesium hydroxide crystal film and filmed, immerse in coagulating bath, the DMAc aqueous solution that coagulating bath is mass fraction 10-60 %, under 20-60 ℃, 0.5-5h is solidified in displacement, again fabric is put into to distilled water and soak 6-48h, with the remaining METHYLPYRROLIDONE except in striping, butanone and butyl glycol ether, 60-160 ℃ of oven dry, make the thermal isolation of anti-naked light textiles, while adopting the dry method film forming, with coating device, the polyethersulfone with cardo of preparation and organic-pillared vermiculite mixed liquor are had in superficial growth on the fabric of magnesium hydroxide crystal film and filmed, 60-160 ℃ of oven dry, make the thermal isolation of anti-naked light textiles,
D, performance test: test the flame retarding and smoke suppressing properties of textiles by taper calorimeter and normal beam technique fabrics flame resistance ability meter, and test the thermal stability of textiles by thermogravimetric analyzer, by the heat-proof quality of thermal conductivity factor instrument test textiles.
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