CN111218839A - Preparation method of flame-retardant wallpaper - Google Patents
Preparation method of flame-retardant wallpaper Download PDFInfo
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- CN111218839A CN111218839A CN202010069656.4A CN202010069656A CN111218839A CN 111218839 A CN111218839 A CN 111218839A CN 202010069656 A CN202010069656 A CN 202010069656A CN 111218839 A CN111218839 A CN 111218839A
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21F—PAPER-MAKING MACHINES; METHODS OF PRODUCING PAPER THEREON
- D21F11/00—Processes for making continuous lengths of paper, or of cardboard, or of wet web for fibre board production, on paper-making machines
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H21/00—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties
- D21H21/14—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties characterised by function or properties in or on the paper
- D21H21/34—Ignifugeants
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H23/00—Processes or apparatus for adding material to the pulp or to the paper
- D21H23/02—Processes or apparatus for adding material to the pulp or to the paper characterised by the manner in which substances are added
- D21H23/22—Addition to the formed paper
- D21H23/32—Addition to the formed paper by contacting paper with an excess of material, e.g. from a reservoir or in a manner necessitating removal of applied excess material from the paper
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H25/00—After-treatment of paper not provided for in groups D21H17/00 - D21H23/00
- D21H25/04—Physical treatment, e.g. heating, irradiating
- D21H25/06—Physical treatment, e.g. heating, irradiating of impregnated or coated paper
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H27/00—Special paper not otherwise provided for, e.g. made by multi-step processes
- D21H27/18—Paper- or board-based structures for surface covering
- D21H27/22—Structures being applied on the surface by special manufacturing processes, e.g. in presses
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Abstract
The invention relates to the technical field of functional wallpaper base materials, in particular to a preparation method of flame-retardant wallpaper, which comprises the steps of selecting alginate fibers, coffee carbon fibers and whole wood pulp to carry out mixing and pulping, manufacturing and drying to obtain a wallpaper base layer, and carrying out impregnation treatment and drying on the wallpaper base layer by using a flame retardant I to obtain the flame-retardant base layer; and mixing the PVC resin and the 2, 5-furandicarboxylic acid di (trans-2 hexene) ester liquid plasticizer uniformly to obtain a PVC premix, mixing the PVC premix and the cyclotriphosphazene flame retardant II uniformly to obtain a PVC paste, coating the PVC paste on the surface of the flame-retardant base layer, and solidifying and forming to obtain the flame-retardant PVC paste. The flame-retardant wallpaper has the advantages of high temperature resistance, flame retardance, high smoke abatement, excellent sound insulation and noise reduction effects, excellent physical properties and excellent use experience.
Description
Technical Field
The invention relates to the technical field of functional wallpaper base materials, in particular to a preparation method of flame-retardant wallpaper.
Background
The wallpaper is also called as wall paper, is an interior decoration material for pasting wall surfaces, and is widely used for interior decoration of houses, offices, hotels, and the like. The material is not limited to paper, and may include other materials. The decorative material has the characteristics of various colors, rich patterns, luxury, safety, environmental protection, convenient construction, proper price and the like which are incomparable with various other interior decorative materials, so the decorative material is popularized to a great extent in developed countries and regions such as Europe, America, Japan and the like. Wallpaper is classified into various types, such as film-coated wallpaper, embossed wallpaper, and the like. The base paper is usually produced from bleached chemical wood pulp, and then is processed through different procedures, such as coating, printing, embossing or surface plastic coating, and finally is cut and packaged for delivery. Has certain strength, toughness, beautiful appearance and good water resistance. In the past, wallpaper only serves as a decorative material to enter the life of people, people have more requirements on the decoration and the aesthetic property, and along with the improvement of the living standard of people, people need high-quality wallpaper to set up their own life, and people have more and more requirements on other functions of the wallpaper.
With the improvement of living standard of people, the requirements on the flame retardant property of decorative wallpaper of rooms, restaurants, hotels and the like are higher and higher. From the aspects of fire safety and practicality, the requirement of flame retardance on the wallpaper is increasing day by day. Because the paper has the characteristic of being combustible, the actual highest flame retardant grade of the traditional flame-retardant wallpaper base paper can only reach B2 grade combustible or B3 grade combustible. When open fire exists, the conventional flame-retardant wallpaper base paper still can burn rapidly, so that the fireproof flame-retardant effect cannot be actually achieved, and great potential safety hazard exists. In the production of the existing flame-retardant wallpaper base paper, flame-retardant chemical fibers or flame-retardant latex are mostly adopted as raw materials to improve the flame retardance of the flame-retardant wallpaper base paper. However, the price of the flame-retardant chemical fiber and the flame-retardant latex is expensive, the price of the flame-retardant chemical fiber and the flame-retardant latex per ton can reach more than ten thousand yuan, and compared with the price of the cheap non-flame-retardant chemical fiber and the latex, the price has a huge difference, so that the production cost of the flame-retardant wallpaper base paper is too high, and the market competitiveness is lacked. The flame retardant effect of the wallpaper on the market is not uniform, and the environment-friendly wallpaper with high quality and high flame retardant property is few, so that the development of the environment-friendly flame retardant wallpaper is needed.
The above background disclosure is only for the purpose of assisting understanding of the inventive concept and technical solutions of the present invention, and does not necessarily belong to the prior art of the present patent application, and should not be used for evaluating the novelty and inventive step of the present application in the case that there is no clear evidence that the above content is disclosed at the filing date of the present patent application.
Disclosure of Invention
The invention aims to provide a preparation method of flame-retardant wallpaper, which is characterized in that fiber mixed pulp is used as a wallpaper base material, a flame-retardant base layer is obtained by soaking a flame retardant, and then PVC paste mixed with a plasticizer and the flame retardant is coated on the surface of the flame-retardant base layer, so that the flame-retardant wallpaper is obtained, has high temperature resistance, high smoke abatement, excellent sound insulation and noise reduction effects, excellent physical properties and excellent use experience.
The technical scheme adopted by the invention for realizing the purpose is as follows: the preparation method of the flame-retardant wallpaper comprises the steps of selecting alginate fibers, coffee carbon fibers and whole wood pulp to be mixed and pulped, making paper and drying to obtain a wallpaper base layer, and dipping the wallpaper base layer by using a flame retardant I and drying to obtain the flame-retardant base layer; and mixing the PVC resin and the 2, 5-furandicarboxylic acid di (trans-2 hexene) ester liquid plasticizer uniformly to obtain a PVC premix, mixing the PVC premix and the cyclotriphosphazene flame retardant II uniformly to obtain a PVC paste, coating the PVC paste on the surface of the flame-retardant base layer, and solidifying and forming to obtain the flame-retardant PVC paste.
The preparation method of the flame-retardant wallpaper specifically comprises the following steps:
1) mixing and pulping alginate fibers, coffee carbon fibers and whole wood pulp, brooming the fibers as much as possible, controlling the concentration of slurry to be 25-40 wt%, controlling the beating degree of the slurry to be 23-31 DEG SR, adding a dispersing agent, mixing and stirring for 35-40 min, and then making and drying the slurry to obtain a wallpaper base layer;
2) soaking the wallpaper base layer in the step 1) in a flame retardant I, performing ultrasonic dipping treatment and drying to obtain a flame retardant base layer;
3) uniformly mixing the PVC resin and a2, 5-furandicarboxylic acid di (trans-2 hexene) ester liquid plasticizer according to the weight ratio of 10-50: 1 to obtain a PVC premix;
4) uniformly mixing the PVC premix and the cyclotriphosphazene flame retardant II to obtain a PVC paste;
5) and (3) coating the PVC paste on the surface of the flame-retardant base layer in the step 2) through 60-mesh screen printing, drying at the temperature of 150-200 ℃ for 30-150 s, and solidifying and forming to obtain the flame-retardant PVC paste.
according to the method, firstly, alginate fibers, coffee carbon fibers and all wood pulp are mixed, beaten and manufactured into a wallpaper base material, the alginate fibers have excellent negative ion release characteristics and can purify indoor environment, the content of environmental negative ions is increased, the metabolism of organisms is promoted to be vigorous, the physical fitness is enhanced, mineral substances in the alginate fibers can release alpha waves, people feel happy and comfortable, the far infrared radiation effect of the alginate fibers and the heat storage and heat preservation effects of the coffee carbon are cooperated, the heat preservation and heat preservation performance and the antibacterial deodorization effect of the wallpaper are enhanced, in addition, the mixed pulp base layer wallpaper is soaked in the flame retardant I, the flame retardant characteristic of the wallpaper is increased, modified montmorillonite in the flame retardant I can further fill gaps among fibers in the base layer of the wallpaper, air storage is reduced, meanwhile, the modified montmorillonite contains more silicon dioxide, the modified montmorillonite has good moisture absorption and is not easy to burn, the flame retardant performance of the fiber base layer is further increased, in addition, the invention surprisingly discovers that the PVC resin base material is mixed with 2, 5-furan dicarboxylic acid di (trans-2 hexene) ester liquid plasticizer and cyclotriphosphazene paste to be compounded into a PVC flame retardant paste, the PVC base material is improved, the flame retardant property is more easily to be coated on the PVC resin base material, the PVC resin is more excellent in a high in a good in a way, the flame retardant and the flame retardant effect of reducing the flame retardant is.
Further, the preparation method of the flame-retardant wallpaper further comprises the working procedures of cooling, printing, embossing, inspecting and curling.
Further, the seaweed fiber in the step 1) is chopped seaweed fiber with the average length of 3-5 mm.
Further, the coffee carbon fiber obtained in the step 1) has the linear density of 1.67dtex, the length of 20-38 mm, the breaking strength of not less than 3.5cN/dtex, the limiting oxygen index of not less than 20%, the deodorization rate of not less than 90% and the moisture regain of 1.62%. The coffee carbon fiber heat-storage warm-keeping, antibacterial and deodorant wallpaper is green and environment-friendly, and has good warm-keeping property.
Further, the weight ratio of the alginate fibers, the coffee carbon fibers and the whole wood pulp in the step 1) is 15-30: 5-10: 100.
Further, the dispersant of step 1) is an anionic dispersant or a water-soluble polymeric dispersant.
Furthermore, the anionic dispersing agent is at least one of fatty alcohol-polyoxyethylene ether sodium sulfate, cellulose sodium sulfate, alkyl diphenyl ether sodium sulfonate or alkylphenol polyoxyethylene ether phosphate.
Further, the water-soluble polymer dispersing agent is sodium alginate.
Further, the basis weight of the wallpaper base material in the step 1) is 195-210 g/m2. The fiber mixed pulp wallpaper base material is made of fibers, the density of the fibers influences the adsorption effect of the flame retardant I and the adhesion effect of the PVC paste, and the quantitative amount is 195-210 g/m after multiple verification2The flame-retardant wallpaper formed by the wallpaper base material has better flame-retardant effect, mechanical property and sound insulation effect.
Further, the flame retardant I in the step 2) comprises the following components in parts by weight: 3.5 to 5.5 parts of formaldehyde, 0.2 to 0.3 part of dicyandiamide, 0.3 to 0.4 part of guanidine salt, 10 to 15 parts of phosphate and 12 to 17 parts of modified montmorillonite. Montmorillonite is added into the flame retardant I, so that gaps among fibers in the wallpaper base layer can be further filled, air storage is reduced, meanwhile, the montmorillonite contains more silicon dioxide, the montmorillonite has better hygroscopicity and is not easy to burn, and the flame retardant property of the fiber base layer is further improved.
Further, the guanidine salt in the flame retardant I is selected from at least one of guanidine hydrochloride, guanidine nitrate or guanidine carbonate.
Still further, the phosphate in the flame retardant I is selected from at least one of the following phosphates:
monobasic phosphates including sodium dihydrogen phosphate, potassium dihydrogen phosphate, and ammonium dihydrogen phosphate;
hydrogen phosphates including disodium hydrogen phosphate, dipotassium hydrogen phosphate, diammonium hydrogen phosphate;
orthophosphates include sodium orthophosphate, potassium orthophosphate, ammonium orthophosphate.
Further, the flame retardant I in the step 2) is prepared according to the following method:
1) adjusting the pH value of formaldehyde to 8.5-9.6 by using alkali liquor, and heating to 65-70 ℃;
2) dissolving formaldehyde and guanidine salt in a phosphate aqueous solution, and carrying out heat preservation reaction for 120-150 min;
3) then adding dicyandiamide and modified montmorillonite, and reacting at 65-70 ℃;
4) and after the guanidine salt and the dicyandiamide are dissolved, continuously reacting for 120-240 min to obtain the product.
Further, the concentration of the phosphate aqueous solution in the method for preparing the flame retardant I is 5.0-20.0%.
Further, the modified montmorillonite in the flame retardant I is prepared according to the following method:
1) after sodium-based montmorillonite is crushed into powder with the particle size of 80-100 meshes, one of water, ethanol or butyl acetate is added as a solvent to swell montmorillonite powder;
2) uniformly mixing the swelled nano montmorillonite and the silane coupling agent A151 according to the weight ratio of the sodium montmorillonite to the silane coupling agent of 60-100: 1;
3) carrying out modification reaction on the mixed material obtained in the step 2) at 82-85 ℃ for at least 3 h;
4) and (3) centrifuging the reactant in the step 3), continuously adding distilled water into the precipitate, centrifuging and washing until no bromide ion residue exists in the supernatant, drying the centrifuged product at 85-90 ℃, and grinding until the particle size is smaller than 200 meshes to obtain the product. After the wallpaper base material is soaked by the flame retardant I prepared by the method, the flame retardant property of the wallpaper is favorably improved, the modified montmorillonite in the flame retardant I can further fill gaps among fibers in the wallpaper base layer, air storage is reduced, meanwhile, the montmorillonite contains more silicon dioxide, has better hygroscopicity and is not easy to burn, and the flame retardant property of the fiber base layer is further improved.
Further, the bis (trans-2 hexene) -2, 5-furandicarboxylate liquid plasticizer of step 3) was prepared via the following steps:
1) slowly dripping excessive thionyl chloride into 2, 5-furandicarboxylic acid, carrying out reflux reaction at 40-50 ℃ for at least 5 hours, cooling to room temperature, and carrying out reduced pressure distillation to obtain white solid 2, 5-furandicarboxylic dichloride;
2) under ice bath, slowly dripping triethylamine into a dichloromethane solution containing trans-2-hexenol and 2, 5-furandicarboxyl dichloride, stirring for 45-60 min, removing the ice bath, slowly heating to room temperature, and reacting for at least 24 h;
3) and after the reaction is finished, washing the obtained product by using 1.2-1.5 mol/L hydrochloric acid, 3.0-5.0% sodium bicarbonate water solution and saturated sodium chloride water solution in sequence, and removing dichloromethane to obtain the compound. The reaction scheme is shown in figure 1. The 2, 5-furan dicarboxylic acid di (trans-2 hexene) ester liquid plasticizer prepared by the method has good compatibility with a PVC resin base material, is beneficial to improving the mechanical strength of the flame-retardant wallpaper of a final product, and more importantly, after the 2, 5-furan dicarboxylic acid di (trans-2 hexene) ester liquid plasticizer is compounded with the cyclotriphosphazene flame retardant II, the temperature resistance, the flame retardance, the smoke abatement and the sound insulation and noise reduction effects of the flame-retardant wallpaper can be obviously enhanced, and the use experience of the wallpaper is improved.
Furthermore, in the step of preparing the 2, 5-furandicarboxylic acid di (trans-2-hexene) ester liquid plasticizer, the molar weight ratio of triethylamine to trans-2-hexenol and 2, 5-furandicarboxylic dichloride is 2-3: 1.
Further, the cyclotriphosphazene flame retardant II of the step 3) is prepared by the following steps:
1) slowly dripping a tetrahydrofuran solution of hexachlorocyclotriphosphazene into the tetrahydrofuran solution containing p-hydroxybenzaldehyde and triethylamine, carrying out reflux reaction for at least 24 hours, adding water, rotatably evaporating out a solid, filtering, drying and recrystallizing with ethyl acetate to obtain hexa-p-formyl phenoxy cyclotriphosphazene;
2) carrying out reflux reaction on six pairs of aldehyde phenoxy cyclotriphosphazene, aniline and 1,4 dioxane for at least 24 h; then adding water to evaporate solids by rotary evaporation, filtering and drying to obtain hexa- (p-N-phenylmethyliminophenoxy) cyclotriphosphazene;
3) adding hexa- (p-N-phenylmethyliminophenoxy) cyclotriphosphazene and DOPO into a large amount of 1,4 dioxane according to the mass ratio of 1:7, carrying out reflux reaction for at least 24h, concentrating, pouring into a proper amount of ethanol, precipitating a large amount of white solid, carrying out ultrasonic treatment and washing for multiple times, and carrying out vacuum drying to obtain the cyclotriphosphazene flame retardant II. The reaction scheme is shown in FIG. 2. The cyclotriphosphazene flame retardant II prepared by the method can effectively reduce the release of heat and smoke when the final product flame-retardant wallpaper is burnt, the carbon residue is remarkably increased at high temperature, the further burning of the wallpaper is hindered, the flame retardant has a gas phase and a solidification phase for the flame retardant mechanism of the wallpaper, and the flame retardant has a good flame retardant effect for the fiber base material PVC wallpaper. Moreover, after the polyvinyl chloride paste is compounded with a PVC resin material containing 2, 5-furandicarboxylic acid di (trans-2 hexene) ester liquid plasticizer to form the PVC paste, the overall performance of the paste is improved, the paste is easy to be attached to a fiber mixed pulp wallpaper base material, the protective performance of the wallpaper base material is improved, the flame retardance, smoke abatement and sound insulation performance of the wallpaper are enhanced on the basis of maintaining higher mechanical performance, and the application experience is improved.
Furthermore, in the step 1) of preparing the cyclotriphosphazene flame retardant II, the amount ratio of the hexachlorocyclotriphosphazene to the p-hydroxybenzaldehyde and the triethylamine is 1: 8-10: 15-18.
Furthermore, in the step 2) of preparing the cyclotriphosphazene flame retardant II, the mass ratio of the six p-formyl phenoxy cyclotriphosphazene, the aniline and the 1,4 dioxane is 0.011-0.012: 0.13-0.15: 1.
Further, in the step 4), the weight ratio of the 2, 5-furandicarboxylic acid di (trans-2 hexene) ester liquid plasticizer to the cyclotriphosphazene flame retardant II is 3.5-4.0: 1. The 2, 5-furan dicarboxylic acid di (trans-2 hexene) ester liquid plasticizer and the cyclotriphosphazene flame retardant II in a specific weight ratio are added into the PVC resin base material, so that the overall physical and chemical properties of the PVC paste are improved, the PVC paste is more easily attached to a fiber mixed pulp wallpaper base material, the flame-retardant wallpaper can be endowed with high temperature resistance and flame retardance, high smoke abatement property and excellent sound insulation and noise reduction effects, and the use experience of the flame-retardant wallpaper is improved.
Additionally, the invention also provides flame-retardant wallpaper, which is prepared by any one of the methods.
The invention has the beneficial effects that:
1) the wallpaper base material is manufactured by mixing, pulping and papermaking of the alginate fibers, the coffee carbon fibers and the whole wood pulp, the alginate fibers have excellent anion release characteristics, can purify indoor environment, increase the content of environment anions, promote vigorous metabolism of organisms, strengthen physique, release α waves from mineral substances in the alginate fibers, make people happy and comfortable, and strengthen the heat preservation and heat preservation performance and antibacterial deodorization effect of the wallpaper by the mutual cooperation of the far infrared radiation effect of the alginate fibers and the heat storage and heat preservation effect of the coffee carbon;
2) the mixed pulp wallpaper base layer is soaked in the flame retardant I, so that the flame retardant property of the wallpaper is increased, the modified montmorillonite in the flame retardant I can further fill gaps among fibers in the wallpaper base layer, air storage is reduced, and meanwhile, the modified montmorillonite contains silicon dioxide, so that the modified montmorillonite has good hygroscopicity and is not easy to burn, and the flame retardant property of the fiber base layer is further increased;
3) after the PVC resin material, the 2, 5-furandicarboxylic acid di (trans-2 hexene) ester liquid plasticizer and the cyclotriphosphazene flame retardant II are sequentially compounded into the PVC paste, the overall physical and chemical properties of the PVC paste are improved, the PVC paste is more easily attached to a fiber mixed pulp wallpaper base material, the protective performance of the wallpaper base material is improved, and more importantly, after the compounded PVC paste is coated on the surface of the fiber mixed pulp wallpaper base material, the flame-retardant wallpaper can be endowed with high temperature resistance, flame retardance, high smoke abatement, excellent sound insulation and noise reduction effects, and the PVC paste is excellent in physical properties and use experience.
The invention adopts the technical scheme to provide the model essay, makes up the defects of the prior art, and has reasonable design and convenient operation.
Drawings
In order to make the aforementioned and other objects, features, and advantages of the invention, as well as others which will become apparent, reference is made to the following description taken in conjunction with the accompanying drawings in which:
FIG. 1 is a reaction scheme of a bis (trans-2 hexene) -2, 5-furandicarboxylate liquid plasticizer according to the present invention;
FIG. 2 is a reaction scheme of a cyclotriphosphazene flame retardant II of the present invention;
FIG. 3 is a schematic diagram of the mechanical property detection result of the flame-retardant wallpaper of the invention;
FIG. 4 is a schematic diagram of the sound insulation and noise reduction performance detection result of the flame-retardant wallpaper of the invention.
Detailed Description
Unless defined otherwise, technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The present invention uses the methods and materials described herein; other suitable methods and materials known in the art may be used. The materials, methods, and examples described herein are illustrative only and are not intended to be limiting. All publications, patent applications, patents, provisional applications, database entries, and other references mentioned herein, and the like, are incorporated by reference herein in their entirety. In case of conflict, the present specification, including definitions, will control.
All percentages, parts, ratios, etc., are by weight unless otherwise indicated; "wt%" means weight percent; "mol%" means mole percent; "vol%" and "v%" mean volume percent.
When an amount, concentration, or other value or parameter is given as either a range, preferred range or a list of upper preferable values and lower preferable values, this is to be understood as specifically disclosing all ranges formed from any pair of any upper range limit or preferred value and any lower range limit or preferred value, regardless of whether ranges are separately disclosed. For example, when a range of "1 to 5" is described, the described range should be understood to include ranges of "1 to 4", "1 to 3", "1 to 2 and 4 to 5", "1 to 3 and 5", and the like. Where numerical ranges are described herein, unless otherwise stated, the ranges are intended to include the endpoints of the ranges, and all integers and fractions within the ranges.
When the term "about" is used to describe a numerical value or an end point value of a range, the disclosure should be understood to include the specific value or end point referred to.
Furthermore, "or" means "or" unless expressly indicated to the contrary, rather than "or" exclusively. For example, condition a "or" B "applies to any of the following conditions: a is true (or present) and B is false (or not present), a is false (or not present) and B is true (or present), and both a and B are true (or present).
In addition, the indefinite articles "a" and "an" preceding an element or component of the invention are intended to mean no limitation on the number of occurrences (i.e., occurrences) of the element or component. Thus, "a" or "an" should be understood to include one or at least one and the singular forms of an element or component also include the plural unless the singular is explicitly stated.
The materials, methods, and examples described herein are illustrative only and not intended to be limiting unless otherwise specified. Although methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present invention, suitable methods and materials are described herein.
The present invention is described in detail below.
Example 1: a flame-retardant wallpaper comprises:
the embodiment provides flame-retardant wallpaper, and the preparation method specifically comprises the following steps A) -E).
A) Modifying montmorillonite, and the preparation steps specifically comprise:
A1) after sodium-based montmorillonite is crushed into powder with the particle size of 100 meshes, ethanol is added to swell the montmorillonite powder;
A2) uniformly mixing the swelled nano montmorillonite and the silane coupling agent A151 according to the weight ratio of the sodium montmorillonite to the silane coupling agent of 80: 1;
A3) modifying and reacting the mixed material obtained in the step A2) at 85 ℃ for 3 h;
A4) centrifuging the reaction product obtained in step A3), adding distilled water into the precipitate, centrifuging, and washing until the supernatant contains no bromide ion (AgNO)3Solution test), drying the centrifugal product at 88 ℃ and grinding the centrifugal product to a particle size of less than 200 meshes.
B) Preparing a flame retardant I: the flame retardant I comprises the following components in parts by weight: 4.0 parts of formaldehyde, 0.3 part of dicyandiamide, 0.4 part of guanidine hydrochloride, 12.0 parts of dipotassium hydrogen phosphate and 15.0 parts of modified montmorillonite; the preparation method specifically comprises the following steps:
B1) regulating the pH value of formaldehyde to 8.9 by using alkali liquor, and heating to 65 ℃;
B2) dissolving formaldehyde and guanidine hydrochloride in 10.0% dipotassium hydrogen phosphate water solution, and reacting for 120min under heat preservation;
B3) then adding dicyandiamide and modified montmorillonite, and reacting at 65 ℃;
B4) and (3) after the guanidine hydrochloride and the dicyandiamide are dissolved, continuing to react for 150min to obtain the guanidine hydrochloride/dicyandiamide compound.
C) The preparation method of the 2, 5-furan dicarboxylic acid di (trans-2 hexene) ester liquid plasticizer comprises the following steps:
C1) slowly dripping excessive thionyl chloride into 2, 5-furandicarboxylic acid, carrying out reflux reaction at 48 ℃ for 5 hours, cooling to room temperature, and carrying out reduced pressure distillation to obtain white solid 2, 5-furandicarboxylic dichloride;
C2) under ice bath, slowly dripping triethylamine into a dichloromethane solution containing trans-2-hexenol and 2, 5-furandicarboxyl dichloride, stirring for 60min, removing the ice bath, slowly heating to room temperature, and reacting for 24 h;
C3) after the reaction is finished, washing the mixture by using 1.3mol/L hydrochloric acid, 4.2% sodium bicarbonate water solution and saturated sodium chloride water solution in sequence to remove dichloromethane to obtain the compound;
wherein the molar weight ratio of triethylamine to the trans-2-hexenol and the 2, 5-furandicarboxylic dichloride is 3:2: 1.
D) Preparing a cyclotriphosphazene flame retardant II, which specifically comprises the following steps:
D1) slowly dripping a tetrahydrofuran solution of hexachlorocyclotriphosphazene into the tetrahydrofuran solution containing p-hydroxybenzaldehyde and triethylamine, carrying out reflux reaction for 30 hours, adding water, spirally distilling out a solid, filtering, drying and recrystallizing with ethyl acetate to obtain hexa-p-formyl phenoxy cyclotriphosphazene;
D2) carrying out reflux reaction on six pairs of aldehyde phenoxy cyclotriphosphazene, aniline and 1,4 dioxane for 24 hours; then adding water to evaporate solids by rotary evaporation, filtering and drying to obtain hexa- (p-N-phenylmethyliminophenoxy) cyclotriphosphazene;
D3) adding hexa- (p-N-phenylmethyliminophenoxy) cyclotriphosphazene and DOPO into a large amount of 1,4 dioxane according to the mass ratio of 1:7, carrying out reflux reaction for 24 hours, concentrating, pouring into a proper amount of ethanol, precipitating a large amount of white solid, carrying out ultrasonic treatment and washing for multiple times, and carrying out vacuum drying to obtain a cyclotriphosphazene flame retardant II;
in the step D1), the mass ratio of hexachlorocyclotriphosphazene to p-hydroxybenzaldehyde and triethylamine is 1:10: 16;
in the step D2), the ratio of the amounts of the six p-formyl phenoxy cyclotriphosphazene, aniline and 1,4 dioxane is 0.011:0.14: 1.
E) Preparing the flame-retardant wallpaper, which specifically comprises the following steps:
E1) mixing and pulping alginate fibers, coffee carbon fibers and whole wood pulp, brooming the fibers as much as possible, controlling the concentration of pulp to be 33 wt%, controlling the beating degree of the pulp to be 28 DEG SR, adding a dispersing agent, mixing and stirring for 40min, and then making and drying the pulp to obtain a wallpaper base layer;
E2) soaking the wallpaper base layer obtained in the step E1) in a flame retardant I, performing ultrasonic dipping treatment and drying to obtain a flame retardant base layer;
E3) uniformly mixing the PVC resin and the 2, 5-furan dicarboxylic acid di (trans-2 hexene) ester liquid plasticizer according to the weight ratio of 40:1 to obtain a PVC premix;
E4) uniformly mixing the PVC premix and the cyclotriphosphazene flame retardant II to obtain a PVC paste;
E5) coating the PVC paste on the surface of the flame-retardant base layer obtained in the step E2) through 60-mesh screen printing, drying at 180 ℃ for 120s, and then solidifying and forming to obtain the flame-retardant base layer;
wherein the content of the first and second substances,
the seaweed fiber of the step E1) is chopped seaweed fiber with the average length of about 4 mm;
the linear density of the coffee carbon fiber obtained in the step E1) is 1.67dtex, the length is about 25mm, the breaking strength is 3.5cN/dtex, the limited oxygen index is 20%, the deodorization rate is 93%, and the moisture regain is 1.62%;
the weight ratio of the alginate fibers, the coffee carbon fibers and the whole wood pulp in the step E1) is 2:1: 10;
the dispersant of the step E1) is water-soluble polymer dispersant sodium alginate;
step E1) the basis weight of the wallpaper substrate is 200g/m2；
The weight ratio of the bis (trans-2 hexene) 2, 5-furandicarboxylate liquid plasticizer to cyclotriphosphazene flame retardant II of step E4) was 3.8: 1.
Example 2: another flame retardant wallpaper:
the embodiment provides another flame-retardant wallpaper, the preparation steps and the formula of which are similar to those of embodiment 1, except that montmorillonite is not modified in the embodiment, namely sodium-based montmorillonite powder is directly used as a raw material to prepare a flame retardant I; and the flame-retardant wallpaper is prepared by the same steps and formula as in example 1.
Example 3: another flame retardant wallpaper:
the embodiment provides another flame-retardant wallpaper, the preparation steps and the formula of which are similar to those of embodiment 1, except that in the step A4) in the embodiment, the precipitate which is not subjected to bromide ion residue test in the step A3) is dried at 88 ℃ and ground to be 200 meshes smaller in particle size to be used as modified montmorillonite, and the modified montmorillonite is used as a raw material to prepare a flame retardant I; and the flame-retardant wallpaper is prepared by the same steps and formula as in example 1.
Example 4: another flame retardant wallpaper:
the embodiment provides another flame-retardant wallpaper, the preparation steps and the formula of which are similar to those of embodiment 1, except that clay is used as a raw material to replace modified montmorillonite powder to prepare a flame retardant I; and the flame-retardant wallpaper is prepared by the same steps and formula as in example 1.
Example 5: another flame retardant wallpaper:
the embodiment provides another flame-retardant wallpaper, the preparation steps and the formula of which are similar to those of embodiment 1, except that no montmorillonite component is added during the preparation of the flame retardant I in the embodiment; and the flame-retardant wallpaper is prepared by the same steps and formula as in example 1.
Example 6: another flame retardant wallpaper:
the embodiment provides another flame-retardant wallpaper, the preparation steps and the formula of which are similar to those of embodiment 1, except that in the step E1) of this embodiment, the alginate fibers and the whole wood pulp are mixed and beaten according to the weight ratio of 1:5, and the flame-retardant wallpaper is prepared by the remaining steps and the formula which are the same as those of embodiment 1, namely, the flame-retardant wallpaper is not added with the coffee carbon fibers.
Example 7: another flame retardant wallpaper:
this example provides another flame retardant wallpaper, which is prepared by the same steps and formulation as in example 1, except that the wallpaper base layer is not subjected to the impregnation treatment of the flame retardant I in this example, i.e. PVC paste is directly coated on the surface of the wallpaper base layer, and the flame retardant wallpaper is prepared by the same steps and formulation as in example 1.
Example 8: another flame retardant wallpaper:
the present example provides another flame retardant wallpaper, which is prepared by the steps and formulation similar to those of example 1, except that in the present example, dioctyl terephthalate is used as a liquid plasticizer to be uniformly mixed with PVC resin to prepare a PVC premix; and the flame-retardant wallpaper is prepared by the same steps and formula as in example 1.
Example 9: another flame retardant wallpaper:
this example provides another flame retardant wallpaper, which is prepared by the same steps and formulation as in example 1, except that in this example, step E3) is omitted, namely, PVC resin and cyclotriphosphazene flame retardant II are directly and uniformly mixed according to the weight ratio of 152:1 to obtain PVC paste, and flame retardant wallpaper is prepared by the same steps and formulation as in example 1.
Example 10: another flame retardant wallpaper:
the preparation steps and the formula of the flame-retardant wallpaper provided by the embodiment are similar to those of the wallpaper provided by the embodiment 1, except that the step E4) is omitted in the embodiment, namely, the PVC premix obtained in the step E3) is directly coated on the surface of the flame-retardant base layer obtained in the step E2) through 60-mesh screen printing, and the flame-retardant wallpaper is obtained after drying for 120s at 180 ℃ and solidification forming, wherein the other steps and the formula of the embodiment are the same as those of the wallpaper provided by the embodiment 1.
Example 11: another flame retardant wallpaper:
this example provides another flame retardant wallpaper, which was prepared by the same procedure and formulation as in example 1, except that in the procedure of E4) in this example, the weight ratio of the bis (trans-2 hexene) -2, 5-furandicarboxylate liquid plasticizer to the cyclotriphosphazene flame retardant II was 1:1, and the flame retardant wallpaper was prepared by the same procedure and formulation as in example 1.
Example 12: another flame retardant wallpaper:
this example provides another flame retardant wallpaper prepared by the same procedure and formulation as in example 1, except that in the procedure of E4) in this example, the weight ratio of the bis (trans-2 hexene) -2, 5-furandicarboxylate liquid plasticizer to the cyclotriphosphazene flame retardant II was 10:1, and the flame retardant wallpaper was prepared by the same procedure and formulation as in example 1.
Experimental example 1: and (3) mechanical property detection:
the tensile test samples of the wallpaper materials prepared in examples 1-12 are cut according to the standard QB/T4034-2010 in the light industry, the test samples are soaked in ultrapure water for 5min, the test samples are taken out and then are dried by using filter paper, the transverse and longitudinal wet tensile strengths of the test samples are measured by using a DCP-KZ (W)300 computer measurement and control horizontal tensile testing machine (Sichuan Yangtze river paper making instrument, Inc.), 10 parallel tests are carried out on each test sample, the average value is taken as the transverse and longitudinal wet tensile strength values of the sample, and the statistical result is shown in FIG. 3. As can be seen from the graph of fig. 3, the flame retardant wallpaper in the preferred embodiment 1 of the present application has a higher tensile strength, and the addition of a suitable inorganic filler (modified montmorillonite in the present application) in the wallpaper material is beneficial to improving the plastic deformation caused by the local stress concentration of the wallpaper material, so as to improve the mechanical properties thereof, and it can also be seen that the participation of the bis (trans-2 hexene) -2, 5-furandicarboxylate liquid plasticizer and the cyclotriphosphazene flame retardant II in the present application also has a gain effect on the mechanical properties of the wallpaper material.
Experimental example 2: and (3) detecting the flame retardant property:
the flame retardant performance of each flame retardant wallpaper sample in examples 1-12 was tested according to the following methods, and the statistical data are shown in table 1:
detection of A Limit oxygen index: with reference to national standard GB/T2406.2-2009, a JF-3 type oxygen index tester (Bright Leeb Instrument Co., Ltd.) is used for measuring the minimum oxygen concentration required by burning an 80mm sample; each sample was subjected to 3 replicates and the average was taken as the limiting oxygen index value of the sample.
B, measurement of smoke elimination performance: according to the national standard GB/T8627-2007, the smoke yield of static combustion of the material is measured by a JCY-1 type building material smoke density tester (Jianning district analytical instrument factory in Nanjing), and the smoke density data measured every 1 hour of 3 samples in each group are counted.
TABLE 1 flame retardant Properties of flame retardant wallpaper
As can be clearly seen from table 1, the flame retardant wallpaper in example 1 of the preferred embodiment of the present invention has a limited oxygen index as high as 35 or more, and simultaneously has a burning smoke density of less than 10%, and as the burning smoke density rapidly decreases, the smoke amount is significantly reduced compared with the technical solutions in examples 2 to 12, and the flame retardant wallpaper has a better smoke abatement effect. Meanwhile, the addition of the modified montmorillonite component, the combined application of the 2, 5-furandicarboxylic acid di (trans-2 hexene) ester liquid plasticizer and the cyclotriphosphazene flame retardant II and the proportion thereof have important influences on the limiting oxygen index and the smoke abatement effect of the wallpaper, have important protection effects on the wallpaper substrate, and maintain higher mechanical property, excellent flame retardant property and smoke abatement effect.
Experimental example 3: and (3) detecting the sound insulation and noise reduction performance:
the flame retardant wallpaper of examples 1-12 was dressed in a narrow space of 1m × 1m × 1m, and a sound source (60dB) with the same power was placed in the space, and decibel number test was performed outside the space, and the decibel number measured outside the space without the wallpaper was used as a control, and the statistical analysis results are shown in fig. 4. As can be seen from the graph of fig. 4, the noise of the flame-retardant wallpaper in example 1 is reduced by more than 50% compared with the space without the wallpaper, which shows that the flame-retardant wallpaper of the present invention has excellent sound insulation and noise reduction performance.
Conventional techniques in the above embodiments are known to those skilled in the art, and therefore, will not be described in detail herein.
While the above detailed description has shown, described, and pointed out novel features as applied to various embodiments, it will be understood that various omissions, substitutions, and changes in the form and details of the device or method illustrated may be made without departing from the spirit of the disclosure. In addition, the various features and methods described above may be used independently of one another, or may be combined in various ways. All possible combinations and sub-combinations are intended to fall within the scope of the present disclosure. Many of the embodiments described above include similar components, and thus, these similar components are interchangeable in different embodiments. While the invention has been disclosed in the context of certain embodiments and examples, it will be understood by those skilled in the art that the invention extends beyond the specifically disclosed embodiments to other alternative embodiments and/or uses and obvious modifications and equivalents thereof. Accordingly, the invention is not intended to be limited by the specific disclosure of preferred embodiments herein.
Claims (10)
1. The preparation method of the flame-retardant wallpaper is characterized by comprising the following steps: mixing alginate fibers, coffee carbon fibers and whole wood pulp for pulping, making and drying to obtain a wallpaper base layer, and dipping the wallpaper base layer by using a flame retardant I and drying to obtain a flame-retardant base layer; and mixing the PVC resin and the 2, 5-furandicarboxylic acid di (trans-2 hexene) ester liquid plasticizer uniformly to obtain a PVC premix, mixing the PVC premix and the cyclotriphosphazene flame retardant II uniformly to obtain a PVC paste, coating the PVC paste on the surface of the flame-retardant base layer, and solidifying and forming to obtain the flame-retardant PVC paste.
2. The method of claim 1, wherein: the method specifically comprises the following steps:
1) mixing and pulping alginate fibers, coffee carbon fibers and whole wood pulp, brooming the fibers as much as possible, controlling the concentration of slurry to be 25-40 wt%, controlling the beating degree of the slurry to be 23-31 DEG SR, adding a dispersing agent, mixing and stirring for 35-40 min, and then making and drying the slurry to obtain a wallpaper base layer;
2) soaking the wallpaper base layer in the step 1) in a flame retardant I, performing ultrasonic dipping treatment and drying to obtain a flame retardant base layer;
3) uniformly mixing the PVC resin and a2, 5-furandicarboxylic acid di (trans-2 hexene) ester liquid plasticizer according to the weight ratio of 10-50: 1 to obtain a PVC premix;
4) uniformly mixing the PVC premix and the cyclotriphosphazene flame retardant II to obtain a PVC paste;
5) and (3) coating the PVC paste on the surface of the flame-retardant base layer in the step 2) through 60-mesh screen printing, drying at the temperature of 150-200 ℃ for 30-150 s, and solidifying and forming to obtain the flame-retardant PVC paste.
3. The method according to claim 1 or 2, characterized in that: the weight ratio of the alginate fibers, the coffee carbon fibers and the whole wood pulp in the step 1) is 15-30: 5-10: 100.
4. The method according to claim 1 or 2, characterized in that: step 1) the basis weight of the wallpaper base material is 195-210 g/m2。
5. The method according to any one of claims 1 to 4, wherein: step 2) the flame retardant I comprises the following components in parts by weight: 3.5 to 5.5 parts of formaldehyde, 0.2 to 0.3 part of dicyandiamide, 0.3 to 0.4 part of guanidine salt, 10 to 15 parts of phosphate and 12 to 17 parts of modified montmorillonite.
6. The method of claim 5, wherein: the flame retardant I is prepared according to the following method:
1) adjusting the pH value of formaldehyde to 8.5-9.6 by using alkali liquor, and heating to 65-70 ℃;
2) dissolving formaldehyde and guanidine salt in a phosphate aqueous solution, and carrying out heat preservation reaction for 120-150 min;
3) then adding dicyandiamide and modified montmorillonite, and reacting at 65-70 ℃;
4) and after the guanidine salt and the dicyandiamide are dissolved, continuously reacting for 120-240 min to obtain the product.
7. The method according to any one of claims 1 to 4, wherein: the 2, 5-furan dicarboxylic acid di (trans-2 hexene) ester liquid plasticizer of the step 3) is prepared by the following steps:
1) slowly dripping excessive thionyl chloride into 2, 5-furandicarboxylic acid, carrying out reflux reaction at 40-50 ℃ for at least 5 hours, cooling to room temperature, and carrying out reduced pressure distillation to obtain white solid 2, 5-furandicarboxylic dichloride;
2) under ice bath, slowly dripping triethylamine into a dichloromethane solution containing trans-2-hexenol and 2, 5-furandicarboxyl dichloride, stirring for 45-60 min, removing the ice bath, slowly heating to room temperature, and reacting for at least 24 h;
3) and after the reaction is finished, washing the obtained product by using 1.2-1.5 mol/L hydrochloric acid, 3.0-5.0% sodium bicarbonate water solution and saturated sodium chloride water solution in sequence, and removing dichloromethane to obtain the compound.
8. The method according to any one of claims 1 to 4, wherein: the cyclotriphosphazene flame retardant II in the step 3) is prepared by the following steps:
1) slowly dripping a tetrahydrofuran solution of hexachlorocyclotriphosphazene into the tetrahydrofuran solution containing p-hydroxybenzaldehyde and triethylamine, performing reflux reaction, adding water, spirally distilling out a solid, filtering, drying and recrystallizing with ethyl acetate to obtain hexa-p-formyl phenoxycyclotriphosphazene;
2) carrying out reflux reaction on six pairs of aldehyde phenoxy cyclotriphosphazene, aniline and 1,4 dioxane for at least 24 h; then adding water to evaporate solids by rotary evaporation, filtering and drying to obtain hexa- (p-N-phenylmethyliminophenoxy) cyclotriphosphazene;
3) adding hexa- (p-N-phenylmethyliminophenoxy) cyclotriphosphazene and DOPO into a large amount of 1,4 dioxane according to the mass ratio of 1:7, carrying out reflux reaction for at least 24h, concentrating, pouring into a proper amount of ethanol, precipitating a large amount of white solid, carrying out ultrasonic treatment and washing for multiple times, and carrying out vacuum drying to obtain the cyclotriphosphazene flame retardant II.
9. The method according to any one of claims 1 to 8, wherein: in the step 4), the weight ratio of the 2, 5-furandicarboxylic acid di (trans-2 hexene) ester liquid plasticizer to the cyclotriphosphazene flame retardant II is 3.5-4.0: 1.
10. The flame-retardant wallpaper is characterized in that: prepared by the method of any one of claims 1 to 9.
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