CN110396825B - Preparation method of fireproof fabric - Google Patents
Preparation method of fireproof fabric Download PDFInfo
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- CN110396825B CN110396825B CN201910730457.0A CN201910730457A CN110396825B CN 110396825 B CN110396825 B CN 110396825B CN 201910730457 A CN201910730457 A CN 201910730457A CN 110396825 B CN110396825 B CN 110396825B
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- 239000004744 fabric Substances 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims abstract description 66
- 239000004745 nonwoven fabric Substances 0.000 claims abstract description 64
- 239000005054 phenyltrichlorosilane Substances 0.000 claims abstract description 31
- ORVMIVQULIKXCP-UHFFFAOYSA-N trichloro(phenyl)silane Chemical compound Cl[Si](Cl)(Cl)C1=CC=CC=C1 ORVMIVQULIKXCP-UHFFFAOYSA-N 0.000 claims abstract description 31
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000003063 flame retardant Substances 0.000 claims abstract description 30
- 238000005273 aeration Methods 0.000 claims abstract description 27
- 238000006243 chemical reaction Methods 0.000 claims abstract description 26
- 239000011248 coating agent Substances 0.000 claims abstract description 25
- 238000000576 coating method Methods 0.000 claims abstract description 25
- 239000000835 fiber Substances 0.000 claims abstract description 24
- 238000001125 extrusion Methods 0.000 claims abstract description 20
- 238000001816 cooling Methods 0.000 claims abstract description 18
- 239000000413 hydrolysate Substances 0.000 claims abstract description 18
- 238000003756 stirring Methods 0.000 claims abstract description 17
- 239000007788 liquid Substances 0.000 claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000012153 distilled water Substances 0.000 claims abstract description 14
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 13
- 238000001035 drying Methods 0.000 claims abstract description 12
- 238000010438 heat treatment Methods 0.000 claims abstract description 12
- 238000007789 sealing Methods 0.000 claims abstract description 12
- 239000002253 acid Substances 0.000 claims abstract description 8
- 238000002791 soaking Methods 0.000 claims abstract description 8
- 230000002378 acidificating effect Effects 0.000 claims abstract description 6
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 20
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 12
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 10
- 229920005989 resin Polymers 0.000 claims description 9
- 239000011347 resin Substances 0.000 claims description 9
- 239000004760 aramid Substances 0.000 claims description 7
- 229920003235 aromatic polyamide Polymers 0.000 claims description 7
- NBVXSUQYWXRMNV-UHFFFAOYSA-N fluoromethane Chemical compound FC NBVXSUQYWXRMNV-UHFFFAOYSA-N 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 239000007789 gas Substances 0.000 claims description 6
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 claims description 6
- 239000000347 magnesium hydroxide Substances 0.000 claims description 6
- 229910001862 magnesium hydroxide Inorganic materials 0.000 claims description 6
- 239000011787 zinc oxide Substances 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 239000000463 material Substances 0.000 abstract description 10
- 229920002050 silicone resin Polymers 0.000 abstract description 9
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 abstract description 5
- 230000004048 modification Effects 0.000 abstract description 4
- 238000012986 modification Methods 0.000 abstract description 4
- 239000010410 layer Substances 0.000 description 7
- 239000004753 textile Substances 0.000 description 5
- 239000002131 composite material Substances 0.000 description 4
- 238000002604 ultrasonography Methods 0.000 description 4
- 230000006378 damage Effects 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000011148 porous material Substances 0.000 description 3
- 238000001132 ultrasonic dispersion Methods 0.000 description 3
- 208000027418 Wounds and injury Diseases 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 208000014674 injury Diseases 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- 108010009736 Protein Hydrolysates Proteins 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000013043 chemical agent Substances 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 230000009970 fire resistant effect Effects 0.000 description 1
- 230000020169 heat generation Effects 0.000 description 1
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 1
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 238000012643 polycondensation polymerization Methods 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 239000005060 rubber Substances 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 230000002277 temperature effect Effects 0.000 description 1
Classifications
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
- D06M11/36—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
- D06M11/44—Oxides or hydroxides of elements of Groups 2 or 12 of the Periodic Table; Zincates; Cadmates
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/21—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/244—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of halogenated hydrocarbons
- D06M15/256—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of halogenated hydrocarbons containing fluorine
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/59—Polyamides; Polyimides
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/643—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/10—Repellency against liquids
- D06M2200/12—Hydrophobic properties
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/30—Flame or heat resistance, fire retardancy properties
Landscapes
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Fireproofing Substances (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
- Silicon Polymers (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
Abstract
The invention discloses a preparation method of a fireproof fabric, which comprises the following steps: adding phenyltrichlorosilane into anhydrous ether, and stirring at a low temperature until the phenyltrichlorosilane is completely dissolved to obtain ether dissolved solution; dropwise adding distilled water into the ether solution, sealing, ultrasonically dispersing at low temperature for 2-3h, and then cooling and standing to obtain acidic hydrolysate; soaking the fiber non-woven fabric into acid hydrolysate for high-density aeration reaction for 2-5h, and then putting the non-woven fabric into a reaction kettle for gradient heating reaction for 1-3h to obtain modified non-woven fabric; uniformly coating the flame-retardant coating liquid on the specific surface of the modified non-woven fabric, and drying to obtain a coated non-woven fabric; and adding the coated non-woven fabric into a mold, performing high-temperature extrusion polymerization reaction for 3-6h, and cooling to obtain the fireproof fabric. The invention utilizes the characteristic of high heat resistance of the polyaryl silicone resin to perform permeation modification on the fiber non-woven fabric, forms the three-dimensional trapezoidal total phenyl silicone resin on the fiber non-woven fabric, is assisted by the full-area coverage of the flame retardant material, improves the overall fireproof and flame retardant characteristics, and simultaneously has the electricity-proof and waterproof characteristics.
Description
Technical Field
The invention belongs to the field of garment materials, and particularly relates to a preparation method of a fireproof fabric.
Background
Garment materials widely exist and are applied to the life of everyone, and most of clothes, house curtains and the like are made of textile fabrics.
The clothing fabric is a composite material which takes various types of fibers, yarns and fabrics as a reinforcing phase and takes materials such as resin, rubber, metal, cement, ceramic and the like as a matrix phase. The structure and performance of the garment material, the bonding strength of the textile material and the interface of the substrate, the performance of the substrate and other factors determine the performance of the composite material. The garment fabric reinforcement is generally a flexible body, and the textile composite material can be either a flexible body or a rigid body. Since the fibers, yarns or fabrics within the garment shell may be oriented according to the application, the anisotropy of the textile reinforced composite may be formed.
At present, people live more intensively due to urbanization construction, many people live in the same building no matter work or life, the number of floors is usually large, people depend on elevators to go upstairs and downstairs, the knowledge of safety passages is very little, fire-fighting knowledge is generally lacked, and almost no escape experience exists. In case of fire, people usually have great disconcerting value, the safety channel is blocked, personnel are difficult to evacuate in time, great personnel injury is caused, property is difficult to preserve, so the injury of fire is extremely great, how to prevent the fire, and how to eliminate the fire after the fire happens is very important. At present, people do not have special, can relax portable and can be used for fire-fighting articles, and many chemical agent conflagrations, electric fires, gas fires at present are all unsuitable to put out a fire with water, so, to normal work and life, do not have the people that article can help to put out a fire, and the fire hydrant also needs to be changed regularly, often is ignored or forgotten by people.
In view of the above, there is a need for a better fire-resistant garment material to overcome the deficiencies of the prior art.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a preparation method of a fireproof fabric, which utilizes the characteristic of high heat resistance of polyaryl silicone resin to perform permeation modification on fiber non-woven fabric, forms three-dimensional trapezoidal total phenyl silicone resin on the fiber non-woven fabric, is assisted with full-area coverage of a flame retardant material, improves the overall fireproof and flame retardant characteristics, and has electricity-proof and waterproof characteristics.
In order to achieve the technical purpose, the technical scheme of the invention is as follows:
a preparation method of a fireproof fabric comprises the following steps:
step 1, adding phenyltrichlorosilane into anhydrous ether, and stirring at a low temperature until the phenyltrichlorosilane is completely dissolved to obtain ether dissolved solution;
step 2, dropwise adding distilled water into the ether solution, sealing, ultrasonically dispersing at low temperature for 2-3h, and then cooling and standing to obtain acidic hydrolysate;
step 3, soaking the fiber non-woven fabric into acid hydrolysate for high-density aeration reaction for 2-5h, and then putting the non-woven fabric into a reaction kettle for gradient heating reaction for 1-3h to obtain a modified non-woven fabric;
step 4, uniformly coating the flame-retardant coating liquid on the specific surface of the modified non-woven fabric, and drying to obtain a coated non-woven fabric;
and 5, adding the coated non-woven fabric into a mold, performing high-temperature extrusion polymerization reaction for 3-6h, and cooling to obtain the fireproof fabric.
The concentration of the phenyltrichlorosilane in the anhydrous ether in the step 1 is 20-50g/L, the stirring speed of low-temperature stirring is 500-1000r/min, and the low-temperature is 5-15 ℃.
The adding amount of the distilled water in the step 2 is 5-10 times of the molar amount of the phenyltrichlorosilane, the dropping speed is 1-2mL/min, the sealing low-temperature ultrasonic temperature is not higher than 20 ℃, the ultrasonic frequency is 40-80kHz, and the temperature for cooling and standing is 1-3 ℃.
And 3, the aeration gas of the high-density aeration reaction in the step 3 is nitrogen, the aeration speed is 15-30mL/min, and the aeration area covers the whole fiber non-woven fabric.
The gradient heating in the step 3 comprises the following procedures:
temperature of | |
50-60℃ | 10-20min |
110-150℃ | Time remaining |
。
The coating amount in the step 4 is 1-5mL/cm2The drying temperature is 120-130 ℃.
The temperature of the high-temperature extrusion polymerization reaction in the step 5 is 200-250 ℃, and the extrusion pressure is 2-3 MPa.
The flame-retardant coating liquid comprises the following components in parts by mass:
2-5 parts of magnesium hydroxide, 10-20 parts of zinc oxide, 5-10 parts of powdery fluorocarbon resin, 10-15 parts of aramid pulp, 5-10 parts of ethylene glycol and 20-40 parts of absolute ethyl alcohol.
Step 1, adding phenyl trichlorosilane into anhydrous ether, utilizing the solubility of phenyl trichlorosilane in ether, and matching with a low-temperature stirring mode to achieve the complete dissolution of phenyl trichlorosilane, and simultaneously, the low temperature can reduce the self-volatility of ether, so as to ensure the integrity of ether solution.
Step 2, dropwise adding distilled water into ether, and forming fast in the slow dropwise adding process to obtain a hydrolysate of phenyltrichlorosilane; the low-temperature ultrasound can uniformly disperse the distilled water into the ether, ensure the distilled water to be fully contacted with the phenyltrichlorosilane, and improve the hydrolysis rate of the phenyltrichlorosilane; the mode of sealing low-temperature ultrasound not only utilizes low temperature to reduce heat energy brought by ultrasound, prevents the heat energy from raising the whole temperature to cause condensation polymerization and solidification of hydrolysate in advance, but also seals the ether which is vaporized due to instant heat generation of ultrasound, and can be stored to prevent the ether from being dissipated to cause reduction of ether content and reduce pollution; the vaporized ether can be recovered into ether liquid at low temperature by subsequent cooling and standing.
Step 3, soaking the fiber non-woven fabric into acid hydrolysate to form a soaking permeation system, adsorbing a large amount of hydrolysate of phenyl trichlorosilane inside and outside the fiber non-woven fabric by utilizing the good permeability of diethyl ether and the adhesiveness of the acid hydrolysate, accelerating the permeation of diethyl ether to the inside of the fiber non-woven fabric by virtue of high-density aeration reaction, reducing the lyophobicity of monofilaments of the non-woven fabric and improving the permeation effect; gradient heating reaction can form secondary gradient constant temperature reaction, ether is got rid of fast to the temperature of first gradient, also can get rid of the hydrogen chloride who dissolves in the ether simultaneously, form the phenyltrichlorosilane hydrolysate that contains moisture, the second gradient can get rid of unnecessary moisture fast to utilize the temperature effect to impel phenyltrichlorosilane hydrolysate to take place polycondensation, obtain the total phenyl silicone resin with inside and outside cladding of non-woven fabrics, the heat resistance of whole non-woven fabrics has been promoted, give the non-woven fabrics good insulating nature and weatherability.
Step 4, uniformly coating the flame-retardant coating liquid on the surface of the non-woven fabric to form a flame-retardant coating layer, and simultaneously forming good permeation of the flame-retardant coating liquid through pores on the non-woven fabric to ensure the tightness of the non-woven fabric; the anhydrous ethanol can be quickly removed in the drying process, and the viscous liquid taking the glycol as the solvent is ensured to be formed.
And 5, in the high-temperature extrusion process, the ethylene glycol can be evaporated by the rise of the temperature, meanwhile, the magnesium hydroxide and the zinc oxide are used as fillers, the aramid pulp and the powdery fluorocarbon resin are used as resin binders, a stable bonding effect is formed, the aramid pulp and the powdery fluorocarbon resin are laid on the surface of the non-woven fabric to form a flame-retardant fireproof layer, and the overall compactness of the fabric can be increased by extrusion.
From the above description, it can be seen that the present invention has the following advantages:
1. the invention utilizes the characteristic of high heat resistance of the polyaryl silicone resin to perform permeation modification on the fiber non-woven fabric, forms the three-dimensional trapezoidal total phenyl silicone resin on the fiber non-woven fabric, is assisted by the full-area coverage of the flame retardant material, improves the overall fireproof and flame retardant characteristics, and simultaneously has the electricity-proof and waterproof characteristics.
2. The invention ensures that the outer layer of the modified non-woven fabric forms the flame-retardant layer by using a high-temperature extrusion polymerization mode, and the flame-retardant layer completely plugs the pores on the modified non-woven fabric, thereby preventing the improvement of the integral compactness.
Detailed Description
The present invention is described in detail with reference to examples, but the present invention is not limited to the claims.
Example 1
A preparation method of a fireproof fabric comprises the following steps:
step 1, adding phenyltrichlorosilane into anhydrous ether, and stirring at a low temperature until the phenyltrichlorosilane is completely dissolved to obtain ether dissolved solution;
step 2, dropwise adding distilled water into the ether solution, sealing, performing low-temperature ultrasonic dispersion for 2 hours, and then cooling and standing to obtain an acidic hydrolysate;
step 3, soaking the fiber non-woven fabric into acid hydrolysate for high-density aeration reaction for 2 hours, and then putting the non-woven fabric into a reaction kettle for gradient heating reaction for 1 hour to obtain a modified non-woven fabric;
step 4, uniformly coating the flame-retardant coating liquid on the specific surface of the modified non-woven fabric, and drying to obtain a coated non-woven fabric;
and 5, adding the coated non-woven fabric into a mold, performing high-temperature extrusion polymerization reaction for 3 hours, and cooling to obtain the fireproof fabric.
The concentration of the phenyltrichlorosilane in the anhydrous ether in the step 1 is 20g/L, the stirring speed of low-temperature stirring is 500r/min, and the low-temperature is 5 ℃.
The adding amount of the distilled water in the step 2 is 5 times of the molar amount of the phenyltrichlorosilane, the dropping speed is 1mL/min, the sealing low-temperature ultrasonic temperature is 20 ℃, the ultrasonic frequency is 40kHz, and the temperature for cooling and standing is 1 ℃.
And 3, the aeration gas of the high-density aeration reaction in the step 3 is nitrogen, the aeration speed is 15mL/min, and the aeration area covers the whole fiber non-woven fabric.
The gradient heating in the step 3 comprises the following procedures:
temperature of | |
50℃ | 10min |
110℃ | Time remaining |
。
The coating amount in the step 4 is 1mL/cm2The drying temperature is 120 ℃.
The temperature of the high-temperature extrusion polymerization reaction in the step 5 is 200 ℃, and the extrusion pressure is 2 MPa.
The flame-retardant coating liquid comprises the following components in parts by mass:
2 parts of magnesium hydroxide, 10 parts of zinc oxide, 5 parts of powdery fluorocarbon resin, 10 parts of aramid pulp, 5 parts of ethylene glycol and 20 parts of absolute ethyl alcohol.
Example 2
A preparation method of a fireproof fabric comprises the following steps:
step 1, adding phenyltrichlorosilane into anhydrous ether, and stirring at a low temperature until the phenyltrichlorosilane is completely dissolved to obtain ether dissolved solution;
step 2, dropwise adding distilled water into the ether solution, sealing, performing low-temperature ultrasonic dispersion for 3 hours, and then cooling and standing to obtain an acidic hydrolysate;
step 3, soaking the fiber non-woven fabric into acid hydrolysate for high-density aeration reaction for 5 hours, and then putting the non-woven fabric into a reaction kettle for gradient heating reaction for 3 hours to obtain modified non-woven fabric;
step 4, uniformly coating the flame-retardant coating liquid on the specific surface of the modified non-woven fabric, and drying to obtain a coated non-woven fabric;
and 5, adding the coated non-woven fabric into a mold, performing high-temperature extrusion polymerization reaction for 6 hours, and cooling to obtain the fireproof fabric.
The concentration of the phenyltrichlorosilane in the anhydrous ether in the step 1 is 50g/L, the stirring speed of low-temperature stirring is 1000r/min, and the temperature at low temperature is 15 ℃.
The adding amount of the distilled water in the step 2 is 10 times of the molar amount of the phenyltrichlorosilane, the dropping speed is 2mL/min, the sealing low-temperature ultrasonic temperature is 10 ℃, the ultrasonic frequency is 80kHz, and the temperature for cooling and standing is 3 ℃.
And 3, the aeration gas of the high-density aeration reaction in the step 3 is nitrogen, the aeration speed is 30mL/min, and the aeration area covers the whole fiber non-woven fabric.
The gradient heating in the step 3 comprises the following procedures:
temperature of | |
60℃ | 20min |
150℃ | Time remaining |
. The coating amount in the step 4 is 5mL/cm2The drying temperature is 130 ℃.
The temperature of the high-temperature extrusion polymerization reaction in the step 5 is 250 ℃, and the extrusion pressure is 3 MPa.
The flame-retardant coating liquid comprises the following components in parts by mass:
5 parts of magnesium hydroxide, 20 parts of zinc oxide, 10 parts of powdery fluorocarbon resin, 15 parts of aramid pulp, 10 parts of ethylene glycol and 40 parts of absolute ethyl alcohol.
Example 3
A preparation method of a fireproof fabric comprises the following steps:
step 1, adding phenyltrichlorosilane into anhydrous ether, and stirring at a low temperature until the phenyltrichlorosilane is completely dissolved to obtain ether dissolved solution;
step 2, dropwise adding distilled water into the ether solution, sealing, performing low-temperature ultrasonic dispersion for 2 hours, and then cooling and standing to obtain an acidic hydrolysate;
step 3, soaking the fiber non-woven fabric into acid hydrolysate for high-density aeration reaction for 4 hours, and then putting the non-woven fabric into a reaction kettle for gradient heating reaction for 2 hours to obtain a modified non-woven fabric;
step 4, uniformly coating the flame-retardant coating liquid on the specific surface of the modified non-woven fabric, and drying to obtain a coated non-woven fabric;
and 5, adding the coated non-woven fabric into a mold, performing high-temperature extrusion polymerization for 5 hours, and cooling to obtain the fireproof fabric.
The concentration of the phenyltrichlorosilane in the anhydrous ether in the step 1 is 40g/L, the stirring speed of low-temperature stirring is 800r/min, and the low-temperature is 10 ℃.
The adding amount of the distilled water in the step 2 is 8 times of the molar amount of the phenyltrichlorosilane, the dropping speed is 2mL/min, the sealing low-temperature ultrasonic temperature is 5 ℃, the ultrasonic frequency is 60kHz, and the temperature for cooling and standing is 2 ℃.
And 3, the aeration gas of the high-density aeration reaction in the step 3 is nitrogen, the aeration speed is 20mL/min, and the aeration area covers the whole fiber non-woven fabric.
The gradient heating in the step 3 comprises the following procedures:
temperature of | |
55℃ | 15min |
140℃ | Time remaining |
。
In said step 4The coating amount was 4mL/cm2The drying temperature is 125 ℃.
The temperature of the high-temperature extrusion polymerization reaction in the step 5 is 230 ℃, and the extrusion pressure is 3 MPa.
The flame-retardant coating liquid comprises the following components in parts by mass:
4 parts of magnesium hydroxide, 15 parts of zinc oxide, 8 parts of powdery fluorocarbon resin, 12 parts of aramid pulp, 8 parts of ethylene glycol and 30 parts of absolute ethyl alcohol.
Performance detection
The detection method is a GB/T5455 textile combustion performance test: vertical method
The detection data are as follows:
the flame-retardant cloth obtained by the invention has excellent flame-retardant effect, and the indexes of after-flame time, smoldering time and damage length all reach the B-level requirements in the international GB 8965.1-2009 flame-retardant protective clothing.
In summary, the invention has the following advantages:
1. the invention utilizes the characteristic of high heat resistance of the polyaryl silicone resin to perform permeation modification on the fiber non-woven fabric, forms the three-dimensional trapezoidal total phenyl silicone resin on the fiber non-woven fabric, is assisted by the full-area coverage of the flame retardant material, improves the overall fireproof and flame retardant characteristics, and simultaneously has the electricity-proof and waterproof characteristics.
2. The invention ensures that the outer layer of the modified non-woven fabric forms the flame-retardant layer by using a high-temperature extrusion polymerization mode, and the flame-retardant layer completely plugs the pores on the modified non-woven fabric, thereby preventing the improvement of the integral compactness.
It should be understood that the detailed description of the invention is merely illustrative of the invention and is not intended to limit the invention to the specific embodiments described. It will be appreciated by those skilled in the art that the present invention may be modified or substituted equally as well to achieve the same technical result; as long as the use requirements are met, the method is within the protection scope of the invention.
Claims (7)
1. A preparation method of a fireproof fabric is characterized by comprising the following steps: the method comprises the following steps:
step 1, adding phenyltrichlorosilane into anhydrous ether, and stirring at a low temperature until the phenyltrichlorosilane is completely dissolved to obtain ether dissolved solution;
step 2, dropwise adding distilled water into the ether solution, sealing, ultrasonically dispersing at low temperature for 2-3h, and then cooling and standing to obtain acidic hydrolysate;
step 3, soaking the fiber non-woven fabric into acid hydrolysate for high-density aeration reaction for 2-5h, and then putting the non-woven fabric into a reaction kettle for gradient heating reaction for 1-3h to obtain a modified non-woven fabric;
step 4, uniformly coating the flame-retardant coating liquid on the surface of the modified non-woven fabric, and drying to obtain a coated non-woven fabric; the flame-retardant coating liquid comprises the following components in parts by mass: 2-5 parts of magnesium hydroxide, 10-20 parts of zinc oxide, 5-10 parts of powdery fluorocarbon resin, 10-15 parts of aramid pulp, 5-10 parts of ethylene glycol and 20-40 parts of absolute ethyl alcohol;
and 5, adding the coated non-woven fabric into a mold, performing high-temperature extrusion polymerization reaction for 3-6h, and cooling to obtain the fireproof fabric.
2. The preparation method of the fireproof fabric according to claim 1, wherein: the concentration of the phenyltrichlorosilane in the anhydrous ether in the step 1 is 20-50g/L, the stirring speed of low-temperature stirring is 500-1000r/min, and the low-temperature is 5-15 ℃.
3. The preparation method of the fireproof fabric according to claim 1, wherein: the adding amount of the distilled water in the step 2 is 5-10 times of the molar amount of the phenyltrichlorosilane, the dropping speed is 1-2mL/min, the sealing low-temperature ultrasonic temperature is not higher than 20 ℃, the ultrasonic frequency is 40-80kHz, and the temperature for cooling and standing is 1-3 ℃.
4. The preparation method of the fireproof fabric according to claim 1, wherein: and 3, the aeration gas of the high-density aeration reaction in the step 3 is nitrogen, the aeration speed is 15-30mL/min, and the aeration area covers the whole fiber non-woven fabric.
5. The preparation method of the fireproof fabric according to claim 1, wherein: the gradient heating in the step 3 comprises the following procedures:
。
6. The preparation method of the fireproof fabric according to claim 1, wherein: the coating amount in the step 4 is 1-5mL/cm2The drying temperature is 120-130 ℃.
7. The preparation method of the fireproof fabric according to claim 1, wherein: the temperature of the high-temperature extrusion polymerization reaction in the step 5 is 200-250 ℃, and the extrusion pressure is 2-3 MPa.
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