CN116200950B - Flame-retardant automobile interior material and production process thereof - Google Patents
Flame-retardant automobile interior material and production process thereof Download PDFInfo
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- CN116200950B CN116200950B CN202310320365.1A CN202310320365A CN116200950B CN 116200950 B CN116200950 B CN 116200950B CN 202310320365 A CN202310320365 A CN 202310320365A CN 116200950 B CN116200950 B CN 116200950B
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- retardant
- flame
- flame retardant
- foaming
- slurry
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- 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 title claims abstract description 119
- 239000003063 flame retardant Substances 0.000 title claims abstract description 89
- 239000000463 material Substances 0.000 title claims abstract description 46
- 238000004519 manufacturing process Methods 0.000 title abstract description 6
- 238000005187 foaming Methods 0.000 claims abstract description 42
- 239000010410 layer Substances 0.000 claims abstract description 13
- 239000004744 fabric Substances 0.000 claims abstract description 12
- 239000011159 matrix material Substances 0.000 claims abstract description 12
- 229920001410 Microfiber Polymers 0.000 claims abstract description 11
- 239000003658 microfiber Substances 0.000 claims abstract description 11
- 239000002344 surface layer Substances 0.000 claims abstract description 10
- 238000013329 compounding Methods 0.000 claims abstract 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 54
- 239000002002 slurry Substances 0.000 claims description 42
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 30
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 28
- 238000002156 mixing Methods 0.000 claims description 27
- 238000006243 chemical reaction Methods 0.000 claims description 25
- 238000003756 stirring Methods 0.000 claims description 25
- 238000002390 rotary evaporation Methods 0.000 claims description 24
- IBDMRHDXAQZJAP-UHFFFAOYSA-N dichlorophosphorylbenzene Chemical compound ClP(Cl)(=O)C1=CC=CC=C1 IBDMRHDXAQZJAP-UHFFFAOYSA-N 0.000 claims description 17
- 235000019441 ethanol Nutrition 0.000 claims description 17
- DYUWTXWIYMHBQS-UHFFFAOYSA-N n-prop-2-enylprop-2-en-1-amine Chemical compound C=CCNCC=C DYUWTXWIYMHBQS-UHFFFAOYSA-N 0.000 claims description 16
- 239000000758 substrate Substances 0.000 claims description 16
- RYHBNJHYFVUHQT-UHFFFAOYSA-N 1,4-Dioxane Chemical compound C1COCCO1 RYHBNJHYFVUHQT-UHFFFAOYSA-N 0.000 claims description 14
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims description 14
- LAMUXTNQCICZQX-UHFFFAOYSA-N 3-chloropropan-1-ol Chemical compound OCCCCl LAMUXTNQCICZQX-UHFFFAOYSA-N 0.000 claims description 13
- UUEWCQRISZBELL-UHFFFAOYSA-N 3-trimethoxysilylpropane-1-thiol Chemical compound CO[Si](OC)(OC)CCCS UUEWCQRISZBELL-UHFFFAOYSA-N 0.000 claims description 12
- 239000006260 foam Substances 0.000 claims description 11
- 239000004088 foaming agent Substances 0.000 claims description 11
- 239000003381 stabilizer Substances 0.000 claims description 11
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 10
- 230000035484 reaction time Effects 0.000 claims description 10
- 239000000741 silica gel Substances 0.000 claims description 10
- 229910002027 silica gel Inorganic materials 0.000 claims description 10
- 239000003085 diluting agent Substances 0.000 claims description 9
- 239000007788 liquid Substances 0.000 claims description 9
- 238000004321 preservation Methods 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 238000007865 diluting Methods 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 238000010992 reflux Methods 0.000 claims description 5
- 238000007790 scraping Methods 0.000 claims description 5
- 238000005034 decoration Methods 0.000 claims description 2
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 claims description 2
- SWWQTDXVMYFEFF-UHFFFAOYSA-N [Na].C(CCCCCCCCCCCCCCCCC)(=O)N Chemical group [Na].C(CCCCCCCCCCCCCCCCC)(=O)N SWWQTDXVMYFEFF-UHFFFAOYSA-N 0.000 claims 1
- KDYFGRWQOYBRFD-UHFFFAOYSA-L succinate(2-) Chemical compound [O-]C(=O)CCC([O-])=O KDYFGRWQOYBRFD-UHFFFAOYSA-L 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 8
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 4
- 125000002887 hydroxy group Chemical group [H]O* 0.000 abstract description 4
- 239000001301 oxygen Substances 0.000 abstract description 4
- 229910052760 oxygen Inorganic materials 0.000 abstract description 4
- 229910052698 phosphorus Inorganic materials 0.000 abstract description 4
- 239000011574 phosphorus Substances 0.000 abstract description 4
- 239000002649 leather substitute Substances 0.000 abstract description 3
- 238000002955 isolation Methods 0.000 abstract description 2
- 125000001477 organic nitrogen group Chemical group 0.000 abstract description 2
- 229910052710 silicon Inorganic materials 0.000 abstract description 2
- 239000010703 silicon Substances 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 14
- 230000000052 comparative effect Effects 0.000 description 8
- 238000010907 mechanical stirring Methods 0.000 description 7
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical group CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 6
- 238000001816 cooling Methods 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
- 238000007792 addition Methods 0.000 description 5
- 239000010985 leather Substances 0.000 description 5
- 238000012986 modification Methods 0.000 description 5
- 230000004048 modification Effects 0.000 description 5
- 239000002994 raw material Substances 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 238000009835 boiling Methods 0.000 description 4
- 235000013312 flour Nutrition 0.000 description 4
- 239000012796 inorganic flame retardant Substances 0.000 description 4
- 238000005452 bending Methods 0.000 description 3
- 238000002485 combustion reaction Methods 0.000 description 3
- 230000006837 decompression Effects 0.000 description 3
- VONWDASPFIQPDY-UHFFFAOYSA-N dimethyl methylphosphonate Chemical compound COP(C)(=O)OC VONWDASPFIQPDY-UHFFFAOYSA-N 0.000 description 3
- 238000009775 high-speed stirring Methods 0.000 description 3
- 239000005457 ice water Substances 0.000 description 3
- ARYZCSRUUPFYMY-UHFFFAOYSA-N methoxysilane Chemical group CO[SiH3] ARYZCSRUUPFYMY-UHFFFAOYSA-N 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 2
- YUWBVKYVJWNVLE-UHFFFAOYSA-N [N].[P] Chemical compound [N].[P] YUWBVKYVJWNVLE-UHFFFAOYSA-N 0.000 description 2
- ADCOVFLJGNWWNZ-UHFFFAOYSA-N antimony trioxide Chemical compound O=[Sb]O[Sb]=O ADCOVFLJGNWWNZ-UHFFFAOYSA-N 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 238000004132 cross linking Methods 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 description 2
- 239000000347 magnesium hydroxide Substances 0.000 description 2
- 229910001862 magnesium hydroxide Inorganic materials 0.000 description 2
- 238000005956 quaternization reaction Methods 0.000 description 2
- -1 sodium succinic acid mono-octadecanoyl amide Chemical group 0.000 description 2
- 238000007711 solidification Methods 0.000 description 2
- 230000008023 solidification Effects 0.000 description 2
- 150000003512 tertiary amines Chemical group 0.000 description 2
- 244000166124 Eucalyptus globulus Species 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
- 150000001263 acyl chlorides Chemical group 0.000 description 1
- 238000007259 addition reaction Methods 0.000 description 1
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 229910000410 antimony oxide Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000012650 click reaction Methods 0.000 description 1
- 238000009841 combustion method Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000004872 foam stabilizing agent Substances 0.000 description 1
- 230000000977 initiatory effect Effects 0.000 description 1
- 239000002932 luster Substances 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- VTRUBDSFZJNXHI-UHFFFAOYSA-N oxoantimony Chemical compound [Sb]=O VTRUBDSFZJNXHI-UHFFFAOYSA-N 0.000 description 1
- 150000003014 phosphoric acid esters Chemical class 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 230000003678 scratch resistant effect Effects 0.000 description 1
- 150000003335 secondary amines Chemical group 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 238000004513 sizing Methods 0.000 description 1
- FGBQETOZANEBSZ-UHFFFAOYSA-M sodium;4-octadecanoyloxy-4-oxo-3-sulfobutanoate Chemical compound [Na+].CCCCCCCCCCCCCCCCCC(=O)OC(=O)C(S(O)(=O)=O)CC([O-])=O FGBQETOZANEBSZ-UHFFFAOYSA-M 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- PXQLVRUNWNTZOS-UHFFFAOYSA-N sulfanyl Chemical class [SH] PXQLVRUNWNTZOS-UHFFFAOYSA-N 0.000 description 1
- 239000002341 toxic gas Substances 0.000 description 1
- DQWPFSLDHJDLRL-UHFFFAOYSA-N triethyl phosphate Chemical compound CCOP(=O)(OCC)OCC DQWPFSLDHJDLRL-UHFFFAOYSA-N 0.000 description 1
- WVLBCYQITXONBZ-UHFFFAOYSA-N trimethyl phosphate Chemical compound COP(=O)(OC)OC WVLBCYQITXONBZ-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/12—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof with macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. gelatine proteins
- D06N3/14—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof with macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. gelatine proteins with polyurethanes
- D06N3/145—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof with macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. gelatine proteins with polyurethanes two or more layers of polyurethanes
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/0002—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the substrate
- D06N3/0004—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the substrate using ultra-fine two-component fibres, e.g. island/sea, or ultra-fine one component fibres (< 1 denier)
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/0043—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by their foraminous structure; Characteristics of the foamed layer or of cellular layers
- D06N3/005—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by their foraminous structure; Characteristics of the foamed layer or of cellular layers obtained by blowing or swelling agent
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/0056—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the compounding ingredients of the macro-molecular coating
- D06N3/0059—Organic ingredients with special effects, e.g. oil- or water-repellent, antimicrobial, flame-resistant, magnetic, bactericidal, odour-influencing agents; perfumes
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N2209/00—Properties of the materials
- D06N2209/06—Properties of the materials having thermal properties
- D06N2209/067—Flame resistant, fire resistant
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N2211/00—Specially adapted uses
- D06N2211/12—Decorative or sun protection articles
- D06N2211/26—Vehicles, transportation
- D06N2211/261—Body finishing, e.g. headliners
Landscapes
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Dispersion Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention relates to a flame-retardant automobile interior material and a production process thereof, belonging to the technical field of PU synthetic leather. The interior material is formed by compounding a microfiber base cloth, a foaming layer and a surface layer, wherein self-made modified flame retardant is added into the foaming layer and the surface layer, the end part of the modified flame retardant is provided with branch-shaped hydroxyl groups, can participate in a cross-linked network of a PU matrix, is not easy to segregate and exude from the matrix, can play a stable flame retardant role, is essentially an organic nitrogen phosphorus silicon flame retardant, can form a flame retardant isolation layer to be inserted into the PU matrix when burning occurs, prevents the burning from being aggravated, achieves a good flame retardant effect, has a limiting oxygen index of more than 28 percent and has a flame retardant grade of V-1.
Description
Technical Field
The invention belongs to the technical field of PU synthetic leather, and particularly relates to a flame-retardant automobile interior material and a production process thereof.
Background
With the improvement of living standard and the development of automobile industry, people not only pay attention to the external shape and performance of the automobile when buying the automobile, but also more and more consumers pay attention to the aesthetic property and comfort of the automobile interior material, and the automobile interior material becomes an important factor affecting the quality and grade of the whole automobile. The traditional automobile interior material mainly comprises leather materials and cloth, wherein the leather materials are good in comfort, high in price and difficult to maintain, and are generally only used in high-grade automobiles, and the cloth is wide in source, low in price and poor in comfort, so that various synthetic leather materials are produced.
PU leather has soft luster and soft hand feeling, is similar to the texture of leather materials, is wear-resistant and scratch-resistant, and is widely applied to automotive interior materials; however, PU materials are inflammable, and a large amount of molten drops and toxic gases can be generated in the combustion process, so that great potential safety hazards exist; in the prior art, a certain amount of flame retardant is added into a PU matrix to improve the flame retardant performance, and the flame retardant applied to interior materials at present mainly comprises an inorganic flame retardant and an organic phosphorus flame retardant, wherein the inorganic flame retardant mainly comprises aluminum hydroxide, magnesium hydroxide, antimony oxide and other materials, and can exert good flame retardant performance under proper addition, but the inorganic flame retardant has poor compatibility with the PU matrix and poor dispersibility, so that the texture of PU leather is greatly reduced; compared with inorganic flame retardants, the organic phosphorus flame retardant mainly comprises phosphate esters, such as methyl dimethyl phosphate, ethyl diethyl phosphate and the like, has stronger flame retardant effect due to the compatibility with a PU matrix, but is easy to segregate in the matrix, has even exudation problem in a high-temperature environment, and has unstable flame retardant effect.
Disclosure of Invention
In order to solve the technical problems in the background art, the invention aims to provide a flame-retardant automobile interior material and a production process thereof.
The aim of the invention can be achieved by the following technical scheme:
the utility model provides a fire-retardant automotive interior material, is formed by microfiber base cloth, foaming layer and surface course complex, wherein, the foaming layer includes: PU sizing agent, modified flame retardant, foaming agent and foam stabilizer; the surface layer comprises: PU slurry, liquid silica gel, and modified flame retardant.
The production process of the flame-retardant automobile interior material specifically comprises the following steps:
step S1: premixing a modified flame retardant, a foaming agent, a foam stabilizer and a diluent, uniformly mixing the mixture with PU slurry in a stirring state, stirring and foaming at a high speed to obtain flame-retardant foaming slurry, arranging a microfiber base in a flat plate mold, injecting the flame-retardant foaming slurry, closing the mold and pressurizing to 1-1.2MPa, and curing at 88-95 ℃ for 20-25min to form a foaming layer to obtain a foaming substrate;
step S2: uniformly mixing PU slurry, liquid silica gel and a modified flame retardant to obtain flame-retardant surface slurry, then scraping the flame-retardant surface slurry on the surface of a foaming substrate, pre-baking for 15-20min at 50-60 ℃, then closing the mold, pressurizing to 1.5-1.8MPa, maintaining the temperature at 75-80 ℃, and curing for 30-40min to form a surface layer, thus obtaining the flame-retardant automobile interior decoration material.
Further, the flame-retardant foaming slurry comprises the following components in percentage by weight: 1.7-2.3wt% of modified flame retardant, 2-3wt% of foaming agent, 0.15-0.22wt% of foam stabilizer, 4-5wt% of diluent and the balance of PU slurry.
Further, the flame-retardant flour paste comprises the following components in percentage by weight: 8-12wt% of liquid silica gel, 2.5-3.5wt% of modified flame retardant and the balance of PU slurry.
Further, the foaming agent is sodium succinic acid mono-octadecanoyl amide sulfonate.
Further, the foam stabilizer is foam stabilizer MD-318.
Further, the diluent is ethyl acetate.
The modified flame retardant is prepared by the following method:
step A1: uniformly mixing diallyl amine, triethylamine and dioxane, keeping the temperature at 10-20 ℃, mechanically stirring at 180-240rpm, slowly adding phenylphosphonic dichloride, keeping the temperature and stirring for reaction after the complete addition, controlling the total reaction time of adding phenylphosphonic dichloride to be 1.5-2h, adding absolute ethyl alcohol for mixing, and removing low-boiling substances such as diallyl amine, dioxane and the like by reduced pressure rotary evaporation to obtain an intermediate a;
further, the dosage ratio of phenylphosphonic dichloride, diallylamine, triethylamine and dioxane was 0.1mol:0.21-0.23mol:3.5-4.5mL:80-100mL of secondary amine groups in the diallylamine react with acyl chloride groups in the phenylphosphonic acid dichloride to form a compound containing a phosphorus nitrogen element and a branched double bond end cap.
Step A2: diluting mercaptopropyl trimethoxysilane with cyclohexane, heating to 60-70deg.C with 300-400W/m 2 Ultraviolet irradiation and mechanical stirring at 120-180rpm, slowly adding the intermediate a, continuing to react after the intermediate a is completely added, controlling the total adding reaction time of the intermediate a to be 3-4h, and removing cyclohexane by rotary evaporation under reduced pressure after the reaction is finished to obtain an intermediate b;
further, the ratio of the amount of intermediate a, mercaptopropyl trimethoxysilane and cyclohexane was 0.1mol:0.42-0.43mol:220-280mL, wherein mercapto in mercaptopropyl trimethoxy silane and a terminal double bond of the intermediate a are subjected to click addition reaction under ultraviolet irradiation, and methoxy silane group modification is introduced into the intermediate a.
Step A3: mixing trimethylenechlorohydrine, an intermediate b, an ethanol solution and dimethyl sulfoxide, introducing nitrogen for protection, heating to 82-88 ℃, mechanically stirring at 80-120rpm, carrying out heat preservation stirring reflux reaction for 8-10h, removing the ethanol solution after the reaction is finished, adding deionized water, and carrying out reduced pressure rotary evaporation to remove the dimethyl sulfoxide to obtain a modified flame retardant;
further, the ratio of the amount of intermediate b, trimethylenechlorohydrin, ethanol solution and dimethyl sulfoxide was 0.1mol:40-50mL:150-200mL: and (3) 20-50mL of ethanol solution with the volume concentration of 20-30%, promoting the hydrolysis of methoxy silane at the end part of the intermediate b, introducing hydroxyl modification at the end part, and simultaneously carrying out quaternization treatment on a tertiary amine structure in the structure of the intermediate b by using trimethylenechlorohydrin.
The invention has the beneficial effects that:
the invention prepares a PU-based interior material, which consists of microfiber base cloth, a foaming layer and a surface layer, wherein self-made modified flame retardants are added in the foaming layer and the surface layer, diallyl amine and phenylphosphonyl dichloride are used as raw materials, a phosphorus-nitrogen element and a branched double bond end-capped intermediate a is prepared through substitution reaction, then mercaptopropyl trimethoxy silane is used for carrying out click reaction with the end double bond of the intermediate a under the initiation of ultraviolet irradiation, organosilicon modification is introduced to prepare an intermediate b, then alcohol water environment containing trimethylenechlorohydrin is used for activating, the hydrolysis of methoxysilane at the end part of the intermediate b is promoted, hydroxyl modification is introduced at the end part, and simultaneously the trimethylenechlorohydrin carries out quaternization treatment on a tertiary amine structure in the structure of the intermediate b, so that a certain antibacterial effect can be given; compared with the existing flame-retardant PU interior material, the branched hydroxyl at the end part of the modified flame retardant has good crosslinking activity with the PU matrix, can participate in a crosslinking network of the PU matrix, is not easy to segregate and exude from the matrix, can exert stable flame retardant effect, and is an organic nitrogen phosphorus silicon flame retardant, can form a flame retardant isolation layer to be penetrated in the PU matrix when burning, prevents the burning from being aggravated, achieves good flame retardant effect, has a limiting oxygen index of more than 28 percent, and has a flame retardant grade of V-1 grade.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The following raw materials are adopted in the implementation process:
PU paste, model XCB-20, supplied by XU Chuan chemical Co., ltd;
a foaming agent selected from sodium monooctadecanoyl sulfosuccinate, a chemical pure reagent;
the foam stabilizer is selected from commercial foam stabilizers, and the model is MD-318;
a diluent selected from ethyl acetate, a chemically pure reagent;
liquid silica gel, model TW-A40, of Ten-day eucalyptus silica gel technology Co., dongguan;
microfiber base cloth is provided by Shandong island New Material Co., ltd., microfiber Bei Siji cloth with thickness of 0.5mm.
Example 1
The preparation method of the flame-retardant automobile interior material comprises the following specific processes:
1) Preparing a modified flame retardant:
1.1, taking diallyl amine, triethylamine and dioxane for feeding, uniformly mixing by mechanical stirring, adopting ice water bath for constant temperature, controlling the temperature to be 10 ℃, controlling the stirring speed to be 180rpm, slowly adding phenylphosphonic dichloride within 50min, continuing to perform heat preservation stirring reaction after the complete addition, and controlling the total adding reaction time of the phenylphosphonic dichloride to be 2h, wherein the dosage ratio of the phenylphosphonic dichloride, the diallyl amine, the triethylamine and the dioxane is 0.1mol:0.21mol:3.5mL:80mL, adding absolute ethyl alcohol with the mass which is 0.2 times that of the reaction system for mixing and washing after the reaction is finished, and removing low-boiling substances including diallylamine and dioxane by reduced pressure rotary evaporation to obtain an intermediate a.
1.2, mixing and diluting mercaptopropyl trimethoxy silane and cyclohexane, heating to 60 ℃, mechanically stirring at 120rpm, and simultaneously adopting an ultraviolet lamp tube with 300W/m 2 Slowly adding the intermediate a in 1h during ultraviolet irradiation, and continuing to react after the intermediate a is completely added, wherein the total adding reaction time of the intermediate a is controlled to be 3h, and the dosage ratio of the intermediate a to mercaptopropyl trimethoxy silane to cyclohexane is 0.1mol:0.42mol:220mL, and after the reaction, cyclohexane is rapidly removed by rotary evaporation under reduced pressure to prepare an intermediate b.
1.3, taking and mixing trimethylenechlorohydrine, an intermediate b, an ethanol solution with the volume concentration of 20% and dimethyl sulfoxide, introducing nitrogen for protection, heating to 82 ℃, and carrying out mechanical stirring at 80rpm, and carrying out heat preservation, stirring and reflux reaction for 10 hours, wherein the dosage ratio of the intermediate b to the trimethylenechlorohydrine to the ethanol solution to the dimethyl sulfoxide is 0.1mol:40mL:150mL: and (3) 50mL, after the reaction, removing ethanol solution by rotary evaporation, adding deionized water with the mass which is 3 times that of the rotary evaporation substrate into the mixture for rotary evaporation twice, and removing dimethyl sulfoxide by decompression rotary evaporation to prepare the modified flame retardant.
2) Preparing a foaming substrate:
2.1, 1.7 weight percent of modified flame retardant, 3 weight percent of foaming agent, 0.22 weight percent of foam stabilizer, 5 weight percent of diluent and the balance of PU slurry are taken according to the weight proportion, all the raw materials are added into a mixing kettle, and high-speed stirring and foaming treatment at 600rpm are applied for 15min, so that the flame-retardant foaming slurry is prepared.
2.2, paving the microfiber base cloth in a flat plate mold, injecting flame-retardant foaming slurry, closing the mold, pressurizing to 1MPa, maintaining the temperature at 88 ℃, solidifying for 25min, opening the mold, and cooling to obtain the foaming substrate.
3) Preparing a flame-retardant automobile interior material:
3.1, taking 12 weight percent of liquid silica gel, 2.5 weight percent of modified flame retardant and the balance of PU slurry according to the weight ratio, and stirring and mixing for 7min at 80rpm to prepare flame-retardant flour slurry;
and 3.2, scraping the flame-retardant surface slurry on the surface of the foaming substrate, pre-baking for 20min at 50 ℃, then closing the mold, pressurizing to 1.5MPa, maintaining the pressure at 75 ℃, solidifying for 40min, opening the mold, and cooling to obtain the flame-retardant automobile interior material.
Example 2
The preparation method of the flame-retardant automobile interior material comprises the following specific processes:
1) Preparing a modified flame retardant:
1.1, taking diallyl amine, triethylamine and dioxane for feeding, uniformly mixing by mechanical stirring, adopting ice water bath for constant temperature, controlling the temperature to be 20 ℃, controlling the stirring speed to be 240rpm, slowly adding phenylphosphonic dichloride within 30min, continuing to perform heat preservation stirring reaction after the mixture is completely added, and controlling the total adding reaction time of the phenylphosphonic dichloride to be 1.5h, wherein the dosage ratio of the phenylphosphonic dichloride, the diallyl amine, the triethylamine and the dioxane is 0.1mol:0.23mol:4.5mL:100mL, adding absolute ethyl alcohol with the mass which is 0.3 times that of the reaction system for mixing and washing after the reaction is finished, and removing low-boiling substances including diallylamine and dioxane by reduced pressure rotary evaporation to obtain an intermediate a.
1.2, mixing and diluting mercaptopropyl trimethoxy silane and cyclohexane, heating to 70 ℃, mechanically stirring at 180rpm, and simultaneously adopting an ultraviolet lamp tube with 400W/m 2 Ultraviolet irradiation, slowly adding the intermediate a, and continuing to react after the intermediate a is completely added, wherein the total adding reaction time of the intermediate a is controlled to be 3 hours, and the dosage ratio of the intermediate a to mercaptopropyl trimethoxysilane to cyclohexane is 0.1mol:0.43mol:280mL, and after the reaction, cyclohexane is rapidly removed by rotary evaporation under reduced pressure to prepare an intermediate b.
1.3, taking and mixing trimethylenechlorohydrine, an intermediate b, an ethanol solution with the volume concentration of 30% and dimethyl sulfoxide, introducing nitrogen for protection, heating to 88 ℃, and carrying out mechanical stirring at 120rpm, and carrying out heat preservation, stirring and reflux reaction for 8 hours, wherein the dosage ratio of the intermediate b to the trimethylenechlorohydrine to the ethanol solution to the dimethyl sulfoxide is 0.1mol:50mL:200mL: and (3) 20mL, after the reaction, removing ethanol solution by rotary evaporation, adding deionized water with the mass 3 times that of the rotary evaporation substrate into the mixture for rotary evaporation twice, and removing dimethyl sulfoxide by decompression rotary evaporation to prepare the modified flame retardant.
2) Preparing a foaming substrate:
2.1, according to the weight proportion, 2.3 weight percent of modified flame retardant, 2 weight percent of foaming agent, 0.15 weight percent of foam stabilizer, 4 weight percent of diluent and the balance of PU slurry are taken, all raw materials are added into a mixing kettle, and high-speed stirring and foaming treatment at 700rpm are applied for 12min, so that the flame-retardant foaming slurry is prepared.
2.2, paving the microfiber base cloth in a flat plate mold, injecting flame-retardant foaming slurry, closing the mold, pressurizing to 1.2MPa, maintaining the temperature at 95 ℃, solidifying for 20min, opening the mold, and cooling to obtain the foaming substrate.
3) Preparing a flame-retardant automobile interior material:
3.1, taking 8 weight percent of liquid silica gel, 3.5 weight percent of modified flame retardant and the balance of PU slurry according to the weight ratio, and stirring and mixing for 5min at 120rpm to prepare flame-retardant flour slurry;
and 3.2, scraping the flame-retardant surface slurry on the surface of the foaming substrate, pre-baking for 15min at 60 ℃, then closing the mold, pressurizing to 1.8MPa, maintaining the pressure for solidification for 30min at 80 ℃, opening the mold, and cooling to obtain the flame-retardant automobile interior material.
Example 3
The preparation method of the flame-retardant automobile interior material comprises the following specific processes:
1) Preparing a modified flame retardant:
1.1, taking diallyl amine, triethylamine and dioxane for feeding, uniformly mixing by mechanical stirring, adopting ice water bath for constant temperature, controlling the temperature to be 12 ℃, controlling the stirring speed to be 240rpm, slowly adding phenylphosphonic dichloride within 40min, continuing to perform heat preservation stirring reaction after the complete addition, and controlling the total adding reaction time of the phenylphosphonic dichloride to be 1.8h, wherein the dosage ratio of the phenylphosphonic dichloride, the diallyl amine, the triethylamine and the dioxane is 0.1mol:0.22mol:4.2mL:100mL, adding absolute ethyl alcohol with the mass which is 0.3 times that of the reaction system for mixing and washing after the reaction is finished, and removing low-boiling substances including diallylamine and dioxane by reduced pressure rotary evaporation to obtain an intermediate a.
1.2, mixing and diluting mercaptopropyl trimethoxy silane and cyclohexane, heating to 62 ℃, mechanically stirring at 180rpm, and simultaneously adopting an ultraviolet lamp tube assisted by 360W/m 2 Ultraviolet irradiation, slowly adding the intermediate a, and continuing to react after the intermediate a is completely added, wherein the total adding reaction time of the intermediate a is controlled to be 3.8h, and the dosage ratio of the intermediate a to mercaptopropyl trimethoxy silane to cyclohexane is 0.1mol:0.42mol:260mL, and after the reaction, cyclohexane is rapidly removed by rotary evaporation under reduced pressure to prepare an intermediate b.
1.3, taking and mixing trimethylenechlorohydrine, an intermediate b, an ethanol solution with the volume concentration of 22% and dimethyl sulfoxide, introducing nitrogen for protection, heating to 85 ℃, and carrying out mechanical stirring at 100rpm, and carrying out heat preservation, stirring and reflux reaction for 8.5 hours, wherein the dosage ratio of the intermediate b to the trimethylenechlorohydrine to the ethanol solution to the dimethyl sulfoxide is 0.1mol:50mL:160mL:40mL, after the reaction, removing ethanol solution by rotary evaporation, adding deionized water with the mass 3 times of that of the rotary evaporation substrate into the mixture for rotary evaporation twice, and removing dimethyl sulfoxide by decompression rotary evaporation to prepare the modified flame retardant.
2) Preparing a foaming substrate:
2.1, according to the weight proportion, 2.1 percent of modified flame retardant, 2.5 percent of foaming agent, 0.18 percent of foam stabilizer, 4.5 percent of diluent and the balance of PU slurry are taken, each raw material is added into a mixing kettle, and the high-speed stirring foaming treatment at 700rpm is applied for 14 minutes, so that the flame-retardant foaming slurry is prepared.
2.2, paving the microfiber base cloth in a flat plate mold, injecting flame-retardant foaming slurry, closing the mold, pressurizing to 1MPa, maintaining the temperature at 92 ℃, solidifying for 22min, opening the mold, and cooling to obtain the foaming substrate.
3) Preparing a flame-retardant automobile interior material:
3.1, 10 weight percent of liquid silica gel, 3 weight percent of modified flame retardant and the balance of PU slurry are taken according to the weight proportion, and 120rpm is applied to stir and mix for 7min to prepare flame-retardant flour slurry;
and 3.2, scraping the flame-retardant surface slurry on the surface of the foaming substrate, pre-baking for 18min at 55 ℃, then closing the mold, pressurizing to 1.6MPa, maintaining the pressure for solidification for 46min at 78 ℃, opening the mold, and cooling to obtain the flame-retardant automobile interior material.
Comparative example 1
This comparative example was carried out in the same manner as in example 3, substituting 1.4wt% of DMMP (dimethyl methylphosphonate) as the flame retardant for the modified flame retardant in the flame retardant foaming slurry, and substituting 1.8wt% of DMMP as the flame retardant for the modified flame retardant in the flame retardant facing slurry.
Comparative example 2
This comparative example was carried out in the same manner as in example 3, substituting 1.6wt% of TDBPPE (tris (2, 4-dibromobenzene) phosphate) as a flame retardant for the modified flame retardant in the flame-retardant foamed slurry, and substituting 1wt% of magnesium hydroxide and 0.3wt% of antimony trioxide for the modified flame retardant in the flame-retardant foamed slurry.
The flame retardant automotive interior materials prepared in examples 1 to 3 and comparative examples 1 to 2 were sampled, tested for oxygen index with reference to ASTM D2863 standard, and tested for combustion by the UL-94 vertical combustion method, and specific test data are shown in table 1:
TABLE 1
As can be seen from the data in Table 1, the flame-retardant automobile interior material prepared by the invention belongs to flame-retardant materials, achieves V-1 flame-retardant grade, and has good flame retardant property.
To verify the flame-retardant durability of the flame-retardant automotive interior materials prepared in examples 1 to 3 and comparative examples 1 to 2, the test pieces were placed in an oven, left standing at a constant temperature of 65 ℃ for 30d, simulated a continuous high temperature environment in a summer automobile, and then subjected to an oxygen index test and a combustion test according to the above standards, and specific test data are shown in table 2:
TABLE 2
As can be seen from the data in Table 2, the flame retardant automotive interior material prepared by the invention has no obvious influence on flame retardant performance when baked for 30d at 65 ℃, wherein the flame retardant effect of comparative example 1 is obviously reduced, and the flame retardant effect is possibly related to segregation of an external flame retardant.
To verify the use properties of the flame retardant automotive interior materials prepared in examples 1 to 3 and comparative examples 1 to 2, bending test was performed with reference to FZ/T01054.1-1999 standard, and specific test data are shown in table 3:
TABLE 3 Table 3
As can be seen from the data in Table 3, the flame-retardant automobile interior material prepared by the invention has lower bending stiffness, good softness, lower bending hysteresis and good shape retention capability.
In the description of the present specification, the descriptions of the terms "one embodiment," "example," "specific example," and the like, mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present invention. In this specification, schematic representations of the above terms do not necessarily refer to the same embodiments or examples. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing is merely illustrative and explanatory of the invention, as various modifications and additions may be made to the particular embodiments described, or in a similar manner, by those skilled in the art, without departing from the scope of the invention or exceeding the scope of the invention as defined in the claims.
Claims (5)
1. The flame-retardant automobile interior material is formed by compounding a microfiber base cloth, a foaming layer and a surface layer, and is characterized in that the foaming layer and the surface layer take PU slurry as a matrix, and modified flame retardants are added in the foaming layer and the surface layer;
the modified flame retardant is prepared by the following method:
step A1: uniformly mixing diallylamine, triethylamine and dioxane, slowly adding phenylphosphonic acid dichloride under stirring at the constant temperature of 10-20 ℃, controlling the total adding reaction time of the phenylphosphonic acid dichloride to be 1.5-2h, adding absolute ethyl alcohol for mixing, and performing rotary evaporation under reduced pressure to obtain an intermediate a, wherein the dosage ratio of the phenylphosphonic acid dichloride, the diallylamine, the triethylamine and the dioxane is 0.1mol:0.21-0.23mol:3.5-4.5mL:80-100mL;
step A2: diluting mercaptopropyl trimethoxy silane with cyclohexane, heating to 60-70 ℃, slowly adding the intermediate a under ultraviolet irradiation and stirring, controlling the total adding reaction time of the intermediate a to be 3-4h, and performing reduced pressure rotary evaporation after the reaction is finished to obtain an intermediate b, wherein the dosage ratio of the intermediate a to mercaptopropyl trimethoxy silane to cyclohexane is 0.1mol:0.42-0.43mol:220-280mL;
step A3: mixing trimethylenechlorohydrine, an intermediate b, an ethanol solution and dimethyl sulfoxide, introducing nitrogen for protection, heating to 82-88 ℃, carrying out heat preservation, stirring and reflux reaction for 8-10h, removing the ethanol solution after the reaction is finished, and then adding deionized water for reduced pressure rotary evaporation to obtain a modified flame retardant, wherein the dosage ratio of the intermediate b to the trimethylenechlorohydrine to the ethanol solution to the dimethyl sulfoxide is 0.1mol:40-50mL:150-200mL:20-50mL.
2. The process for producing a flame retardant automotive interior material according to claim 1, comprising the steps of:
step S1: premixing a modified flame retardant, a foaming agent, a foam stabilizer and a diluent, uniformly mixing with PU slurry, stirring and foaming at a high speed to obtain flame-retardant foaming slurry, injecting the flame-retardant foaming slurry onto a microfiber base cloth, closing a mold, pressurizing to 1-1.2MPa, maintaining the temperature at 88-95 ℃, and curing for 20-25min to form a foaming layer to obtain a foaming substrate;
step S2: uniformly mixing PU slurry, liquid silica gel and a modified flame retardant to obtain flame-retardant surface slurry, then scraping the flame-retardant surface slurry on the surface of a foaming substrate, pre-baking for 15-20min at 50-60 ℃, then closing the mold, pressurizing to 1.5-1.8MPa, maintaining the temperature at 75-80 ℃, and curing for 30-40min to form a surface layer, thus obtaining the flame-retardant automobile interior decoration material.
3. The process for producing a flame-retardant automotive interior material according to claim 2, wherein the flame-retardant foaming slurry comprises the following components in percentage by weight: 1.7-2.3wt% of modified flame retardant, 2-3wt% of foaming agent, 0.15-0.22wt% of foam stabilizer, 4-5wt% of diluent and the balance of PU slurry.
4. The process for producing a flame-retardant automotive interior material according to claim 2, wherein the flame-retardant facestock comprises the following components in percentage by weight: 8-12wt% of liquid silica gel, 2.5-3.5wt% of modified flame retardant and the balance of PU slurry.
5. The process for producing a flame retardant automotive interior material according to claim 2, wherein the foaming agent is sodium monooctadecanoamide sulfonate succinate.
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| CN114605790A (en) * | 2022-03-15 | 2022-06-10 | 吴纪纪 | Preparation method of DOPO and MOSS-12 flame-retardant PET composite material |
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| GB1429531A (en) * | 1972-03-18 | 1976-03-24 | Stockhausen & Cie Chem Fab | Phosphoramidate flame-proofing agents |
| CN104611942A (en) * | 2015-02-10 | 2015-05-13 | 浙江佳阳塑胶新材料有限公司 | Thermoplastic polyurethane (TPU) physical foaming synthetic leather as well as production technology and application thereof |
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