Flame-retardant heat-insulating sound-absorbing cotton and preparation process thereof

Abstract

The application discloses a kind of fire-retardant heat-insulating sound-absorbing cotton and its preparation process, the raw material composition of sound-absorbing cotton product is strictly limited in the application, hollow fiber prepared by fire-retardant process is used as sound-absorbing cotton raw material, to ensure that sound-absorbing cotton fiber has sufficient fire-retardant performance and sound insulation and noise reduction ability, while the adhesive of sound-absorbing cotton is modified, and a strong cohesive force acrylic ester resin is prepared, which has strong adhesion, then in order to ensure the processability and fire resistance of acrylic ester resin, the application continues to prepare hyperbranched silicon-phosphorus flame retardant, silicon and phosphorus elements are introduced into the flame retardant, and the viscosity of acrylic ester resin is improved by the low viscosity characteristics of hyperbranched polymer, and the processability is enhanced.The fire-retardant heat-insulating sound-absorbing cotton prepared by the application has the characteristics of good fire resistance, strong heat insulation capacity and excellent noise reduction performance, and has a long service life, few safety hazards and wide application space.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of sound insulation and noise reduction, in particular to a flame-retardant heat-insulating sound-absorbing cotton and a preparation process thereof. BACKGROUND

[0002] The sound-absorbing cotton, as a commonly used automotive interior material, has developed for decades and has multiple functions of flame retardation, sound absorption and heat insulation, and has made important contributions to improving the driving comfort, aesthetics and practicality of automobiles; however, the existing sound-absorbing cotton process often adopts a post-flame-retardant process, which often leads to a problem of decreased flame-retardant effect after being wetted by water or being placed for too long, and most of the existing sound-absorbing cottons also face the problem of incompatibility of flame-retardant cotton adhesive in the preparation process, and often the phenomenon of flame-retardant sound-absorbing cotton and non-flame-retardant adhesive occurs, therefore, there is an urgent need for a sound-absorbing cotton product that can solve the above problems in the market to meet market demand. SUMMARY

[0003] The present application aims to provide a flame-retardant heat-insulating sound-absorbing cotton and a preparation process thereof to solve the problems raised in the background.

[0004] To solve the above technical problems, the present application provides the following technical solution: a flame-retardant heat-insulating sound-absorbing cotton, characterized in that the flame-retardant heat-insulating sound-absorbing cotton is composed of a flame-retardant sound-absorbing cotton layer and a flame-retardant acrylic adhesive film layer.

[0005] Among them, the flame-retardant sound-absorbing cotton layer includes the following components by weight: 30-50 parts of 4D low-melting-point fiber, 40-45 parts of hollow 6D long fiber and 40-45 parts of hollow 3D long fiber.

[0006] The flame-retardant acrylic adhesive film layer includes the following components: 49.5-68.5 parts of acrylic polymer, 10-15 parts of hyperbranched silicon-phosphorus flame retardant, 2-3 parts of thickening agent, 1-3 parts of crosslinking agent, 1.2-2.2 parts of emulsifier, 0.3-0.5 parts of stabilizer, 2-4 parts of antioxidant and 30-35 parts of pure water.

[0007] Further, the 4D low-melting-point fiber is a low-melting-point short fiber with a model number of LCF110-03 and a length of 49-52 mm; the hollow 6D long fiber is a flame-retardant hollow polyester short fiber with a model number of ZK9236.67dtex*60mm; and the hollow 3D long fiber is a flame-retardant polyester short fiber with a model number of GN4443.33dtex*65mm.

[0008] Further, the acrylic polymer includes the following components: 8.5-11.5 parts of methyl methacrylate, 5-7.5 parts of vinyl acetate, 21-27 parts of butyl acrylate and 15-22.5 parts of isooctyl acrylate.

[0009] Further, the emulsifier is sodium dodecyl benzene sulfonate; the stabilizer is allyl polyoxyethylene ether; the crosslinking agent is 2,2-azobis isobutyronitrile; the antioxidant is phosphite; and the thickening agent is sodium carboxymethyl cellulose.

[0010] A preparation method of a fire-retardant heat-insulating sound-absorbing cotton, comprising the following steps:

[0011] S1. preparing a fire-retardant sound-absorbing cotton layer:

[0012] S11. weighing and pre-stirring 4D low-melting-point fibers, hollow 6D long fibers and hollow 3D long fibers to mix them uniformly to obtain mixed fibers, pre-opening and mixing the mixed fibers, and then carrying out fluffy opening treatment;

[0013] S12. after the fluffy opening treatment is completed, carding the mixed fibers, laying and stacking them, heating the mixed fibers by hot air, and then winding after cooling to obtain the fire-retardant sound-absorbing cotton layer;

[0014] S2. preparing a hyperbranched silicon-phosphorus fire retardant:

[0015] S21. dissolving 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, triethylamine and 3-glycidyloxypropyltrimethoxysilane in N,N-dimethylformamide, treating with ice water bath, and filling with nitrogen protection;

[0016] S22. dropwise adding tetrachloromethane and continuously stirring for 24-48 h, spinning the reaction product after the reaction is completed, removing the excess solvent, and then cleaning with ethanol for 3-4 times to obtain a silicon-phosphorus polymer;

[0017] S23. dissolving 3-phenyl-2-propenoic acid in N,N-dimethylformamide, filling with nitrogen protection, and heating to 60-70 DEG C in a water bath, dissolving the silicon-phosphorus polymer in N,N-dimethylformamide, slowly adding into the 3-phenyl-2-propenoic acid solution, heating to 80-90 DEG C in a water bath after the dropwise adding is completed, filling with high-pressure nitrogen, maintaining pressure for 18-24 h, spinning the reaction product after the reaction is completed, and vacuum drying for 4-8 h to obtain the hyperbranched silicon-phosphorus fire retardant;

[0018] S3. preparing a fire-retardant acrylate water-based adhesive:

[0019] S31. mixing methyl methacrylate, vinyl acetate, butyl acrylate and isooctyl acrylate, and heating to 50-60 DEG C in a water bath, and stirring and mixing for 0.5-1 h to obtain mixed monomers;

[0020] S32. dissolving an emulsifier and a stabilizer in pure water, slowly adding the mixed monomers prepared in step S21, and stirring for 3-6 h to obtain an emulsion;

[0021] S33. Dissolve the crosslinking agent and antioxidant in pure water, and heat in a water bath to 80-90 DEG C. Slowly add the emulsion, and after the addition is complete, continue stirring for 6-8 hours, then stop heating. Add the thickening agent and the hyperbranched silicon-phosphorus flame retardant prepared in step S2, and stir until uniform, to obtain the flame-retardant acrylate water-based adhesive;

[0022] S4. Apply the flame-retardant acrylate water-based adhesive to form a film, and after baking at 100-110 DEG C. for 3-5 minutes, obtain the flame-retardant acrylate adhesive film layer.

[0023] S5. Cut the flame-retardant acrylate adhesive film layer to the same size as the flame-retardant sound-absorbing cotton layer, and adhere the flame-retardant acrylate adhesive film layer to the flame-retardant sound-absorbing cotton, and cold-press to obtain the flame-retardant heat-insulating sound-absorbing cotton.

[0024] The flame-retardant heat-insulating sound-absorbing cotton is prepared in the application, and to ensure the sound-absorbing effect and use performance of the sound-absorbing cotton, the raw material composition of the flame-retardant sound-absorbing cotton layer is strictly limited. The sound-absorbing cotton fiber used in the application is FES fiber prepared by a previous flame-retardant process. The previous flame-retardant process is a modification treatment of the raw material composition before the FES is processed into a fiber, and a flame-retardant component is added to the composition, so that the flame-retardant performance of the FES fiber can be maintained for a relatively long time, and the flame-retardant performance is prevented from decreasing in subsequent use, causing a safety hazard.

[0025] Meanwhile, the FES fiber is treated by a multi-channel stirring and mixing process, so that the 4D low-melting-point fiber can be uniformly dispersed in the FES fiber, and then the FES fiber is heated, and under the action of high temperature, the 4D low-melting-point fiber is melted, so that the fiber filaments are connected to each other to form a whole, and the debris generated during the preparation of the sound-absorbing cotton is coated, so that the sound-absorbing cotton is prevented from producing falling residues during use, and the bonding strength is enhanced, and the use comfort is increased.

[0026] Then, the adhesive film of the flame-retardant heat-insulating sound-absorbing cotton is modified in the application. In order to maintain the sufficient adhesion and strength of the adhesive film, a large amount of hard monomers is added during the preparation of the adhesive film, so that the acrylate resin has strong cohesion. However, the cohesion is too strong, which will cause deformation and shrinkage of the adhesive film, and affect the processing performance. Therefore, the flame retardant with a hyperbranched structure is prepared in the application.

[0027] The hyperbranched polymer has a spherical structure, and the spherical structure and numerous branched groups can effectively reduce the viscosity of the acrylate resin, and the spherical hyperbranched polymer is dispersed between the acrylate molecular chains, thereby reducing the crosslinking degree and the difficulty of coating processing. Meanwhile, the prepared flame retardant is introduced with silicon and phosphorus elements, and in the preparation process, first, 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide and 3-alkylene glycol propyl trimethoxysilane are used as reaction monomers to synthesize an alkane polymer with silicon and phosphorus elements, and then the alkane polymer and 3-phenyl-2-acrylic acid are used as monomers to synthesize a flame retardant with a hyperbranched structure, and by utilizing the properties of silicon and phosphorus elements, the silicon-carbon layer containing silicon is formed to assist the acrylate to form a flame retardant at high temperature, and the generated PO· free radicals react with the free radicals ·H and ·OH generated in the combustion reaction to terminate the combustion reaction.

[0028] Further, the heating temperature of the hot air heating is 150-200 DEG C, and the heating time is 5-10 min.

[0029] Further, in step S3, the molar ratio of 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, triethylamine, 3-alkylene glycol propyl trimethoxysilane, tetrachloromethane and 3-phenyl-2-acrylic acid is (2.4-3.2):(2.5-3.5):(2-2.8):(2-2.5):(1.2-1.8) in terms of molar fraction.

[0030] Further, in step S33, after the high-pressure nitrogen gas is filled, the reaction pressure is 0.5-2.0 MPa.

[0031] Further, in step S5, the cold pressing composite speed is 5-8 m / s.

[0032] Further, in step S5, the cold pressing roller gap is 10%-13% of the thickness of the flame-retardant heat-insulating sound-absorbing cotton.

[0033] Compared with the prior art, the present application has the following beneficial effects: the raw material composition of the sound-absorbing cotton product is strictly limited, the hollow fiber prepared by the flame retardant process before use is used as the sound-absorbing cotton raw material, the sound-absorbing cotton fiber is ensured to have sufficient flame retardant performance and sound insulation and noise reduction capacity, the sound-absorbing cotton adhesive is modified, the acrylate resin with strong cohesive force is prepared, the adhesion is strong, then in order to ensure the processability and flame retardancy of the acrylate resin, the present application further prepares a hyperbranched silicon-phosphorus flame retardant, introduces silicon and phosphorus elements into the flame retardant, and by means of the low viscosity characteristics of the hyperbranched polymer, the viscosity of the acrylate resin is improved, and the processability is enhanced. The flame-retardant heat-insulating sound-absorbing cotton prepared by the present application has the characteristics of good flame retardancy, strong heat insulation capacity and excellent noise reduction performance, has a long service life, has few safety hazards, and has a wide application space. Attached Figure Description

[0034] The accompanying drawings are provided to further illustrate the invention and form part of the specification. They are used in conjunction with embodiments of the invention to explain the invention and do not constitute a limitation thereof. In the drawings:

[0035] Figure 1 The present invention relates to a flame-retardant, heat-insulating, and sound-absorbing cotton product. Detailed Implementation

[0036] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0037] In the embodiments and comparative examples of this invention, the 4D low-melting-point fiber used is a low-melting-point short fiber with model number LCF110-03 and specification LMF4D*51mm; the hollow 6D long fiber is a flame-retardant hollow polyester short fiber with model number ZK9236.67dtex*60mm sold by Sinopec; and the hollow 3D long fiber is a flame-retardant polyester short fiber with model number GN4443.33dtex*65mm sold by Sinopec.

[0038] Example 1.

[0039] A method for preparing flame-retardant, heat-insulating, and sound-absorbing cotton includes the following steps:

[0040] S1. Preparation of flame-retardant sound-absorbing cotton layer:

[0041] S11. By weight, 30 parts of 4D low melting point fiber, 40 parts of hollow 6D long fiber and 40 parts of hollow 3D long fiber are pre-mixed evenly to obtain mixed fiber. Then, the mixed fiber is thoroughly mixed twice using a pre-opening bin and three times using a cotton mixing bin. Finally, the fiber is fluffed and opened using an opening machine.

[0042] S12. After the loosening and opening treatment is completed, the fiber is transferred into the carding machine for web laying and stacking. Finally, the mixed fibers are heated in a hot air oven at a temperature of 150°C for 5 minutes. After heating, the fiber is cooled to room temperature and then wound up to obtain the flame-retardant sound-absorbing cotton layer.

[0043] S2. Preparation of hyperbranched silicon-phosphorus flame retardant:

[0044] S21. 2.4 parts of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, 2.5 parts of triethylamine and 2 parts of 3-glycidoxypropyltrimethoxysilane were dissolved in 30 parts of N,N-dimethylformamide, treated with ice water bath, and filled with nitrogen protection;

[0045] S22. 2 parts of tetrachloromethane were added dropwise, and the reaction was continuously stirred for 24 h. After the reaction was completed, the reaction product was rotary evaporated, the excess solvent was removed, and after being washed with ethanol 4 times, a silicon phosphorus polymer was obtained;

[0046] S23. 1.2 parts of 3-phenyl-2-propenoic acid were dissolved in 10 parts of N,N-dimethylformamide, nitrogen was introduced for protection, and the water bath was warmed to 60°C. The silicon phosphorus polymer was dissolved in 20 parts of N,N-dimethylformamide, slowly added to the 3-phenyl-2-propenoic acid solution, after the addition was completed, the water bath was warmed to 80°C, and high-pressure nitrogen was filled, the pressure was maintained at 0.5 MPa, the reaction was carried out for 18 h, after the reaction was completed, the reaction product was rotary evaporated, and vacuum dried for 4 h, to obtain a hyperbranched silicon phosphorus flame retardant;

[0047] S3. Preparation of flame-retardant acrylate water-based glue:

[0048] S31. 8.5 parts of methyl methacrylate, 5 parts of vinyl acetate, 21 parts of butyl acrylate and 15 parts of isooctyl acrylate were mixed, and the water bath was warmed to 50°C. The mixture was stirred at a speed of 100 rpm for 0.5 h to obtain a mixed monomer;

[0049] S32. 1.2 parts of sodium dodecylbenzenesulfonate and 0.3 parts of allyl polyoxyethylene ether were dissolved in 15 parts of pure water, and the mixed monomer prepared in step S21 was slowly added. After stirring at a speed of 300 rpm for 3 h, an emulsion was obtained;

[0050] S33. 0.2 parts of 2,2-azobis (isobutyronitrile) initiator and 2 parts of phosphite were dissolved in 15 parts of pure water, the water bath was warmed to 80°C, and the emulsion was slowly added. After the addition was completed, the stirring reaction was continued at a speed of 100 rpm for 6 h, and then the heating was stopped. 10 parts of the hyperbranched silicon phosphorus flame retardant prepared in step S2 and 2 parts of carboxymethyl cellulose sodium thickener were added, mixed uniformly, and a flame-retardant acrylate water-based glue was obtained;

[0051] S4. The flame-retardant acrylate water-based glue was coated into a film, and after baking at 100°C for 3 min, a flame-retardant acrylate glue film layer was obtained;

[0052] S5. Cutting the flame-retardant acrylate adhesive film layer to have the same size as the flame-retardant sound-absorbing cotton layer, and then bonding the flame-retardant acrylate adhesive film layer with the flame-retardant sound-absorbing cotton, cold pressing and compounding at a speed of 5 m / s and a gap of 10% of the thickness of the flame-retardant sound-absorbing cotton, and then winding after cold pressing, to obtain the flame-retardant sound-absorbing cotton.

[0053] Example 2.

[0054] Compared with Example 1, the amount of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide added in step S31 is increased in this example.

[0055] A method for preparing a flame-retardant sound-absorbing cotton, comprising the following steps:

[0056] S1. Preparing a flame-retardant sound-absorbing cotton layer:

[0057] S11. Preparing a mixture of 30 parts of 4D low-melting-point fibers, 40 parts of hollow 6D long fibers and 40 parts of hollow 3D long fibers by mixing them uniformly, and then performing secondary sufficient stirring using a pre-opening large bin, tertiary sufficient stirring using a cotton mixing large bin, and finally fluffy opening treatment using an opening machine;

[0058] S12. After the fluffy opening treatment, the mixture is transferred into a carding machine for web laying and stacking, and then heated in a hot air oven, wherein the heating temperature is 150 DEG C, the heating time is 5 min, and the mixture is cooled to room temperature after heating, and then wound to obtain the flame-retardant sound-absorbing cotton layer.

[0059] S2. Preparing a hyperbranched silicon-phosphorus flame retardant:

[0060] S21. Dissolving 3.2 parts of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, 2.5 parts of triethylamine and 2 parts of 3-glycidoxypropyltrimethoxysilane in 30 parts of N,N-dimethylformamide, and then treating with ice water and protecting with nitrogen;

[0061] S22. Adding 2 parts of tetrachloromethane dropwise and continuously stirring for 24 h, and then rotary-evaporating the reaction product after the reaction, removing the excess solvent, and then washing with ethanol 4 times to obtain a silicon-phosphorus polymer.

[0062] S23. Dissolving 1.2 parts of 3-phenyl-2-propenoic acid in 10 parts of N,N-dimethylformamide, protecting with nitrogen, and then heating in a water bath to 60 DEG C, dissolving the silicon-phosphorus polymer in 20 parts of N,N-dimethylformamide, and then slowly adding dropwise into the 3-phenyl-2-propenoic acid solution, heating in a water bath to 80 DEG C after the dropwise addition is completed, and then protecting with high-pressure nitrogen, maintaining the pressure at 0.5 MPa, and then reacting for 18 h, and then rotary-evaporating the reaction product after the reaction, and then vacuum drying for 4 h to obtain the hyperbranched silicon-phosphorus flame retardant.

[0063] S3. preparing the fire-retardant acrylate water-based adhesive:

[0064] S31. 8.5 parts of methyl methacrylate, 5 parts of vinyl acetate, 21 parts of butyl acrylate and 15 parts of isooctyl acrylate were mixed, and the mixture was stirred at a speed of 100 rpm for 0.5 h in a water bath heated to 50℃ to obtain a mixed monomer;

[0065] S32. 1.2 parts of sodium dodecyl benzene sulfonate and 0.3 parts of allyl polyoxyethylene ether were dissolved in 15 parts of pure water, and the mixed monomer prepared in step S21 was slowly added and stirred at a speed of 300 rpm for 3 h to obtain an emulsion;

[0066] S33. 0.2 parts of 2,2-azobisdimethylamide initiator and 2 parts of phosphite were dissolved in 15 parts of pure water, and the emulsion was slowly added in a water bath heated to 80℃, and after the addition was completed, the stirring was continued at a speed of 100 rpm for 6 h, then the heating was stopped, 10 parts of the hyperbranched silicon-phosphorus fire-retardant prepared in step S2 and 2 parts of sodium carboxymethyl cellulose thickener were added, and after being mixed uniformly, the fire-retardant acrylate water-based adhesive was obtained;

[0067] S4. The fire-retardant acrylate water-based adhesive was coated into a film, and after baking at 100℃ for 3 min, a fire-retardant acrylate adhesive film layer was obtained;

[0068] S5. The fire-retardant acrylate adhesive film layer was cut to have the same size as the fire-retardant sound-absorbing cotton layer, and the fire-retardant acrylate adhesive film layer was laminated with the fire-retardant sound-absorbing cotton, and cold pressing was performed at a speed of 5 m / s and a gap of 10% of the thickness of the fire-retardant sound-absorbing cotton between the cold pressing rollers, and after the cold pressing was completed, the fire-retardant sound-absorbing cotton was wound up, and the fire-retardant sound-absorbing cotton was obtained.

[0069] Example 3.

[0070] Compared with example 1, the amount of 3-glycidoxypropyltrimethoxysilane added in step S31 is increased in example 3.

[0071] A preparation method of a fire-retardant sound-absorbing cotton, comprising the following steps:

[0072] S1. preparing a fire-retardant sound-absorbing cotton layer:

[0073] S11. 30 parts of 4D low-melting-point fibers, 40 parts of hollow 6D long fibers and 40 parts of hollow 3D long fibers were pre-stirred and mixed uniformly, and then secondary sufficient stirring was performed using a pre-opening large bin, and tertiary sufficient stirring was performed using a cotton mixing large bin, and finally, the fibers were subjected to fluffy opening treatment using an opening machine;

[0074] S12. After the fluffy loosening treatment is completed, it is moved into a carding machine to perform web laying and stacking, and finally a hot air oven is used to heat the mixed fibers, wherein the heating temperature is 150°C, the heating time is 5 min, and after the heating is completed, it is cooled to room temperature, and then it is wound up, so that the sound-absorbing cotton layer is obtained;

[0075] S2. Preparation of hyperbranched silicon-phosphorus flame retardant:

[0076] S21. 2.4 parts of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, 2.5 parts of triethylamine and 2.8 parts of 3-glycidyloxypropyltrimethoxysilane are dissolved in 30 parts of N,N-dimethylformamide, treated with ice water bath, and filled with nitrogen protection;

[0077] S22. 2 parts of tetrachloromethane are added dropwise, and the stirring reaction is continued for 24 h. After the reaction is completed, the reaction product is rotary evaporated to remove excess solvent, washed with ethanol 4 times, and then the silicon-phosphorus polymer is obtained;

[0078] S23. 1.2 parts of 3-phenyl-2-propenoic acid are dissolved in 10 parts of N,N-dimethylformamide, nitrogen is introduced for protection, and the water bath is heated to 60°C. The silicon-phosphorus polymer is dissolved in 20 parts of N,N-dimethylformamide, slowly added to the 3-phenyl-2-propenoic acid solution, after the addition is completed, the water bath is heated to 80°C, high-pressure nitrogen is filled, the pressure is maintained at 0.5 MPa, the reaction is carried out for 18 h, after the reaction is completed, the reaction product is rotary evaporated, and vacuum dried for 4 h, so that the hyperbranched silicon-phosphorus flame retardant is obtained;

[0079] S3. Preparation of flame-retardant acrylic water-based adhesive:

[0080] S31. 8.5 parts of methyl methacrylate, 5 parts of vinyl acetate, 21 parts of butyl acrylate and 15 parts of isooctyl acrylate are mixed, and the water bath is heated to 50°C. The mixture is stirred at a speed of 100 rpm for 0.5 h to obtain a mixed monomer;

[0081] S32. 1.2 parts of sodium dodecylbenzenesulfonate and 0.3 parts of allyl polyoxyethylene ether are dissolved in 15 parts of pure water, and the mixed monomer prepared in step S21 is slowly added. After stirring at a speed of 300 rpm for 3 h, an emulsion is obtained;

[0082] S33. 0.2 parts of 2,2-azobis(isobutyronitrile) initiator and 2 parts of phosphite are dissolved in 15 parts of pure water, the water bath is heated to 80°C, the emulsion is slowly added, after the addition is completed, the stirring reaction is continued at a speed of 100 rpm for 6 h, then the heating is stopped, 10 parts of the hyperbranched silicon-phosphorus flame retardant prepared in step S2 and 2 parts of carboxymethyl cellulose sodium thickener are added, and after being uniformly mixed, the flame-retardant acrylic water-based adhesive is obtained;

[0083] S4. Coating the fire-retardant acrylate water-based base adhesive into a film, baking at 100 DEG C for 3 min, to obtain a fire-retardant acrylate adhesive film layer;

[0084] S5. Cutting the fire-retardant acrylate adhesive film layer to have the same size as the fire-retardant sound-absorbing cotton layer, and laminating the fire-retardant acrylate adhesive film layer with the fire-retardant sound-absorbing cotton, with a cold pressing speed of 5 m / s and a cold pressing gap of 10% of the thickness of the fire-retardant sound-absorbing cotton, to obtain the fire-retardant sound-absorbing cotton after winding.

[0085] Example 4.

[0086] A preparation method of the fire-retardant sound-absorbing cotton comprises the following steps:

[0087] S1. Preparing a fire-retardant sound-absorbing cotton layer:

[0088] S11. Mixing 50 parts of 4D low-melting-point fibers, 45 parts of hollow 6D long fibers and 45 parts of hollow 3D long fibers in a weight ratio, to obtain mixed fibers, and then performing secondary sufficient stirring using a pre-opening large bin, performing three times of sufficient stirring using a cotton mixing bin, and finally performing fluffy opening treatment using an opening machine;

[0089] S12. After the fluffy opening treatment is completed, the mixed fibers are moved into a carding machine to perform web laying and stacking, and then heated using a hot air oven, wherein the heating temperature is 200 DEG C, the heating time is 10 min, and the mixed fibers are cooled to room temperature after the heating is completed, and then wound, to obtain the fire-retardant sound-absorbing cotton layer;

[0090] S2. Preparing a hyperbranched silicon-phosphorus fire-retardant agent:

[0091] S21. Dissolving 3.2 parts of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, 3.5 parts of triethylamine and 2.8 parts of 3-glycidoxypropyltrimethoxysilane in 30 parts of N,N-dimethylformamide, and performing ice water bath treatment and nitrogen protection;

[0092] S22. Dropping 2.5 parts of tetrachloromethane, and continuously stirring for 24 h, and then rotary-evaporating the reaction product after the reaction is completed, removing the excess solvent, and cleaning 4 times using ethanol, to obtain a silicon-phosphorus polymer;

[0093] S23. Dissolving 1.8 parts of 3-phenyl-2-propenoic acid in 10 parts of N,N-dimethylformamide, and performing nitrogen protection and water bath heating to 70 DEG C, dissolving the silicon-phosphorus polymer in 20 parts of N,N-dimethylformamide, slowly dropping into the 3-phenyl-2-propenoic acid solution, after the dropping is completed, water bath heating to 80 DEG C, and nitrogen protection with a high pressure of 2.0 MPa, and reacting for 24 h, and then rotary-evaporating the reaction product after the reaction is completed, and vacuum drying for 4 h, to obtain the hyperbranched silicon-phosphorus fire-retardant agent.

[0094] S3. Preparation of flame-retardant acrylate water-based adhesive:

[0095] S31. 11.5 parts of methyl methacrylate, 7.5 parts of vinyl acetate, 27 parts of butyl acrylate and 22.5 parts of isooctyl acrylate were mixed, and the mixture was stirred at 100 rpm for 1 h in a water bath heated to 60°C to obtain a mixed monomer;

[0096] S32. 2.2 parts of sodium dodecyl benzene sulfonate and 0.5 parts of allyl polyoxyethylene ether were dissolved in 20 parts of pure water, and the mixed monomer prepared in step S21 was slowly added and stirred at 450 rpm for 6 h to obtain an emulsion;

[0097] S33. 1.5 parts of 2,2-azobis isobutyronitrile initiator and 4 parts of phosphite were dissolved in 15 parts of pure water, and the emulsion was slowly added in a water bath heated to 90°C. After the addition was completed, the stirring was continued at 200 rpm for 8 h, and then 15 parts of the hyperbranched silicon phosphorus flame retardant prepared in step S2 and 3 parts of sodium carboxymethyl cellulose thickener were added. After mixing uniformly, the flame-retardant acrylate water-based adhesive was obtained;

[0098] S4. The flame-retardant acrylate water-based adhesive was coated into a film, and after baking at 100°C for 3 min, a flame-retardant acrylate adhesive film layer was obtained;

[0099] S5. The flame-retardant acrylate adhesive film layer was cut to have the same size as the flame-retardant sound-absorbing cotton layer, and the flame-retardant acrylate adhesive film layer was laminated with the flame-retardant sound-absorbing cotton, and cold pressing was performed at a speed of 8 m / s and a gap of 13% of the thickness of the flame-retardant sound-absorbing cotton. After cold pressing, the flame-retardant sound-absorbing cotton was wound up, and the flame-retardant sound-absorbing cotton was obtained.

[0100] Comparative Example 1.

[0101] Compared with Example 1, the flame-retardant EVA adhesive film disclosed in the patent CN201710845887.8 was used to replace the flame-retardant acrylate adhesive film prepared in the present application;

[0102] A preparation method of flame-retardant sound-absorbing cotton, comprising the following steps:

[0103] S1. Preparation of flame-retardant sound-absorbing cotton layer:

[0104] S11. 30 parts of 4D low-melting-point fibers, 40 parts of hollow 6D long fibers and 40 parts of hollow 3D long fibers were pre-stirred and mixed uniformly to obtain a mixed fiber, and then the mixed fiber was subjected to secondary sufficient stirring using a pre-opening large bin, three times of sufficient stirring using a cotton mixing bin, and finally fluffy opening treatment using an opening machine;

[0105] S12. After the fluffy loosening treatment is completed, the mixture is moved into a carding machine to perform web laying and stacking, and finally heated using a hot air oven, wherein the heating temperature is 150 DEG C, the heating time is 5 min, and after the heating is completed, the mixture is cooled to room temperature and wound up, so that the flame-retardant sound-absorbing cotton layer is obtained;

[0106] S2. The adhesive film is prepared according to the technology disclosed in CN201710845887.8;

[0107] S5. The adhesive film is cut to have the same size as the flame-retardant sound-absorbing cotton layer, and the adhesive film is attached to the flame-retardant sound-absorbing cotton, and cold pressing is performed at a speed of 5 m / s, and the gap between the cold pressing rollers is 10% of the thickness of the flame-retardant sound-absorbing cotton, and after the cold pressing is completed, the flame-retardant sound-absorbing cotton is wound up, so that the flame-retardant sound-absorbing cotton is obtained.

[0108] Detection: The flame-retardant acrylic ester water-based adhesive of Examples 1-4 and the flame-retardant EVA of Comparative Example 1 are each prepared into a sample having a dry film thickness of 60 μm and an area of 10*10 cm, which is attached to a stainless steel plate and subjected to a 80 DEG C 500 g weight detection, and all can achieve 20 min without falling; and subjected to a 20 DEG C 500 g weight detection, and all can achieve 48 h without falling.

[0109] Examples 1-4 and Comparative Example 1 are each prepared into a flame-retardant sound-absorbing cotton layer having a thickness of 30 mm and an angle film thickness of 80 μm, and performance detection is performed thereon.

[0110] Detection: The flame-retardant effect of Examples 1-4 and Comparative Example 1 is detected according to GB8410-2006; the vertical combustion, oxygen index and smoke density grade of the product are detected according to GB38262-2019; the formaldehyde release amount is detected according to TB / T3139-2006; the 180 DEG peeling strength is detected according to GB / T2792-2014; the thermal conductivity is detected according to GB / T10294-2008; and the sound absorption coefficient of the product is detected, and the detection results are shown in the following table:

[0111]

[0112]

[0113] It can be seen from the comparison of Examples 1-4 and Comparative Example 1 that the sound-absorbing effect of the flame-retardant sound-absorbing cotton prepared by the present application is good, the sound absorption coefficient is generally greater than 0.6, and the thickness is low, so it is a good sound-absorbing material. In addition, the flame-retardant sound-absorbing cotton prepared by the present application has good heat insulation effect and low thermal conductivity, and has excellent heat insulation performance. It can be found from the comparison of Example 1 and Comparative Example 1 that the adhesive film prepared by the present application has good flame-retardant performance, low formaldehyde release amount, low smoke density during combustion, small harm to human body, and good flame-retardant effect.

[0114] It is to be noted that, in the present text, relational terms such as first and second and the like can be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Moreover, the terms "comprises", "comprising", or any other variations thereof, are intended to cover a non-exclusive inclusion such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but can include other elements not expressly listed or inherent to such process, method, article, or apparatus.

[0115] Finally, it should be noted that the above-mentioned only constitutes the preferred embodiments of the present application and is not intended to limit the present application. Although the present application has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that modifications, equivalent replacements, and improvements of the technical solutions described in the foregoing embodiments can be made. Any modifications, equivalent replacements, and improvements made within the spirit and principle of the present application shall fall within the scope of the present application.

Claims

1. A method for preparing a fire-retardant, heat-insulating, sound-absorbing cotton, characterized in that, Comprising the following steps: S1. Preparation of fire-retardant sound-absorbing cotton layer: S11. Weigh and pre-stir 4D low-melting-point fibers, hollow 6D long fibers, and hollow 3D long fibers to mix them evenly to obtain mixed fibers, and then pre-open the fibers, mix the fibers, and then perform fluffy open treatment; S12. After the fluffy open treatment is completed, card the fibers, perform web laying and stacking, heat the mixed fibers with hot air, and then cool and wind after rolling, to obtain the fire-retardant sound-absorbing cotton layer; S2. Preparation of hyperbranched silicon-phosphorus flame retardant: S21. Dissolve 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, triethylamine, and 3-glycidyloxypropyltrimethoxysilane in N,N-dimethylformamide, perform ice water bath treatment, and fill with nitrogen protection; S22. Drop 4-chloromethane, and continuously stir the reaction for 24-48 hours. After the reaction is completed, spin the reaction product, remove the excess solvent, and then clean with ethanol for 3-4 times to obtain the silicon-phosphorus polymer; S23. Dissolve 3-phenyl-2-propenoic acid in N,N-dimethylformamide, and then fill with nitrogen protection. Perform water bath heating to 60-70 DEG C. Dissolve the silicon-phosphorus polymer in N,N-dimethylformamide, and then slowly drop into the 3-phenyl-2-propenoic acid solution. After the dropping is completed, perform water bath heating to 80-90 DEG C, and then fill with high-pressure nitrogen. Maintain the pressure for 18-24 hours. After the reaction is completed, spin the reaction product, and then vacuum dry for 4-8 hours to obtain the hyperbranched silicon-phosphorus flame retardant; S3. Preparation of fire-retardant acrylic ester water-based glue: S31. Mix methyl methacrylate, vinyl acetate, butyl acrylate, and isooctyl acrylate, and then perform water bath heating to 50-60 DEG C. Stir and mix for 0.5-1 hour to obtain mixed monomers; S32. Dissolve the emulsifier and stabilizer in pure water, slowly add the mixed monomers prepared in step S21, and then stir for 3-6 hours to obtain an emulsion; S33. Dissolve the crosslinking agent and antioxidant in pure water, and then perform water bath heating to 80-90 DEG C. Slowly drop the emulsion. After the dropping is completed, continue to stir for 6-8 hours, and then stop heating. Add the thickening agent and the hyperbranched silicon-phosphorus flame retardant prepared in step S2, and then stir and mix evenly to obtain the fire-retardant acrylic ester water-based glue; S4. Coating the fire-retardant acrylic ester water-based glue to form a film, and then perform baking at 100-110 DEG C for 3-5 minutes to obtain a fire-retardant acrylic ester glue film layer; S5. Cut the fire-retardant acrylic ester glue film layer to have the same size as the fire-retardant sound-absorbing cotton layer, and then adhere the fire-retardant acrylic ester glue film layer to the fire-retardant sound-absorbing cotton layer, and then perform cold pressing to obtain the fire-retardant heat-insulating sound-absorbing cotton.

2. The method of claim 1, wherein the fire-retardant, heat-insulating, and sound-absorbing cotton is prepared by the steps of: In step S12, the heating temperature of the hot air heating is 150-200 DEG C, and the heating time is 5-10 minutes. ​ 3. The method of producing a fire-retardant, heat-insulating, and sound-absorbing cotton according to claim 1, characterized by: In step S2, according to the mole fraction, the mole ratio of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, triethylamine, 3-glycidyloxypropyltrimethoxysilane, 4-chloromethane, and 3-phenyl-2-propenoic acid is (2.4-3.2):(2.5-3.5):(2-2.8):(2-2.5):(1.2-1.8).

4. The method of producing a fire-retardant, heat-insulating, and sound-absorbing cotton according to claim 1, characterized in that: In step S23, after the high-pressure nitrogen is filled, the reaction pressure is 0.5-2.0 MPa.

5. The method of producing a fire-retardant, heat-insulating, and sound-absorbing cotton according to claim 1, characterized in that: In step S5, the cold-pressing composite speed is 5-8 m / s.

6. The method of producing a fire-retardant, heat-insulating, and sound-absorbing cotton according to claim 1, characterized in that: In step S5, the cold-pressing roller gap is 10%-13% of the thickness of the fire-retardant heat-insulating and sound-absorbing cotton.

7. A fire-retardant, heat-insulating, and sound-absorbing cotton prepared by the method of any one of claims 1 to 6, characterized in that: The fire-retardant heat-insulating and sound-absorbing cotton is composed of a fire-retardant sound-absorbing cotton layer and a fire-retardant acrylic ester adhesive film layer. The fire-retardant sound-absorbing cotton layer includes the following components by weight: 30-50 parts of 4D low-melting-point fibers, 40-45 parts of hollow 6D long fibers, and 40-45 parts of hollow 3D long fibers. The fire-retardant acrylic ester adhesive film layer includes the following components: 49.5-68.5 parts of acrylic polymers, 10-15 parts of hyperbranched silicon-phosphorus fire retardants, 2-3 parts of thickening agents, 1-3 parts of cross-linking agents, 1.2-2.2 parts of emulsifiers, 0.3-0.5 parts of stabilizers, 2-4 parts of antioxidants, and 30-35 parts of pure water.

8. The fire safety insulation and sound absorbing cotton according to claim 7, characterized in that: The thickness of the fire-retardant sound-absorbing cotton layer is 10-100 mm, and the thickness of the fire-retardant acrylic ester adhesive film layer is 20-100 μm.

9. The fire safety insulation and sound absorbing cotton according to claim 7, characterized in that: The acrylic polymers include the following components: 8.5-11.5 parts of methyl methacrylate, 5-7.5 parts of vinyl acetate, 21-27 parts of butyl acrylate, and 15-22.5 parts of isooctyl acrylate.

10. The fire safety insulation and sound absorbing cotton according to claim 7, characterized in that: The emulsifier is sodium dodecyl benzene sulfonate; the stabilizer is allyl polyoxyethylene ether; the cross-linking agent is 2,2-azobis isobutyronitrile; the antioxidant is phosphite; and the thickening agent is sodium carboxymethyl cellulose.

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