CN110128692B - Flame-retardant B1-grade polyurethane wood-like door and preparation method thereof - Google Patents

Flame-retardant B1-grade polyurethane wood-like door and preparation method thereof Download PDF

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CN110128692B
CN110128692B CN201910360364.3A CN201910360364A CN110128692B CN 110128692 B CN110128692 B CN 110128692B CN 201910360364 A CN201910360364 A CN 201910360364A CN 110128692 B CN110128692 B CN 110128692B
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polyether polyol
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王林生
黄海军
刘洋宏
曹开东
余伟
陈亭
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Chongqing Odeon Industry Co.,Ltd.
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Chongqing Oudian Industrial Co ltd
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    • C08G65/02—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring
    • C08G65/26—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds
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    • C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
    • C08J9/06—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent
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    • C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
    • C08J9/12—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a physical blowing agent
    • C08J9/14—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a physical blowing agent organic
    • C08J9/143—Halogen containing compounds
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    • C08J2203/00—Foams characterized by the expanding agent
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Abstract

The invention provides a flame-retardant B1-grade polyurethane wood-like door and a preparation method thereof, wherein the wood-like door comprises a polyurethane base material and paint sprayed on the polyurethane base material, the polyurethane base material is prepared by reacting a component A and a component B, and the mass ratio of the component A to the component B is 1: 1.2-1.8; the component A comprises polyether polyol, a surfactant, a foaming agent, a flame retardant and a catalyst; the component B is isocyanate and/or modified isocyanate. The invention has the characteristics of smooth surface, compact surface, few microscopic pinhole defects and fine and smooth foam holes, greatly facilitates the post-treatment polishing and repairing procedures, and has the characteristics of good flame retardance and no solid filler, and is convenient for rapid molding of equipment.

Description

Flame-retardant B1-grade polyurethane wood-like door and preparation method thereof
Technical Field
The invention relates to the technical field of polyurethane materials, in particular to a flame-retardant B1-grade polyurethane wood-like door and a preparation method thereof.
Background
The Polyurethane (PU) wood-like material is a medium-high density microporous material developed in the middle of 70 s of 20 th century, and its density is greater than 150Kg/m3The wood-like composite material has the advantages of high rigidity and mechanical strength, simple forming process, high production efficiency, changeable shapes of molded products and the like, and can be used as various medium-high grade wood-like products instead of wood. The Polyurethane (PU) wood-like material is made up by using polyurethane combined polyether and polymeric polyisocyanate through the processes of mixing, stirring, pouring mould, closing mould, foaming, curing and forming, demoulding and trimmingThe rigid polyurethane foam of the process is also commonly called polyurethane rigid foam. The plastic-strip wood is also researched more in China, is applied to high-grade export furniture and decoration engineering, and also has more wood-plastic composite materials, and the plastic-strip wood is used for solving the contradiction between higher and higher requirements on the quantity and quality of wood and over-exploitation and use of forest resources. Polyurethane rigid foam plastics are currently more applied to filling core materials of composite doors.
The patent "CN 2881039Y a wood-like polyurethane door" discloses a wood-like polyurethane door with natural wood grain-like grains on the surface not falling off.
The patent CN102758582B A wood-like polyurethane door and a preparation method thereof disclose a wood-like polyurethane door which is moisture-proof, does not absorb water, has small expansion coefficient, is not warped or bent after long-term use, is not easy to crack, has good consistency of manufactured products, is not mildewed, is not damaged by worms, has flame retardant property reaching B1 grade, and has excellent processing properties of sawing, nailing, planing and the like. The patent uses a door body in which a plurality of layers of plate bodies which have a supporting function and are spliced together are integrally formed, and discloses a preparation method of a wood-like polyurethane door.
The flame retardant property of the existing wood-like polyurethane wood-like door is obtained by a solid filler mode, and the problems that the realization of a casting molding process of a polyurethane foaming machine is unfavorable, the appearance defect that more fine pinholes exist on the surface of a product prepared by molding, and the complicated post-treatment, polishing and repairing are needed exist.
Disclosure of Invention
The invention provides a flame-retardant B1-grade polyurethane wood-like door and a preparation method thereof, aiming at solving the problems that the conventional wood-like polyurethane wood-like door is realized by a casting molding process of an unfavorable polyurethane foaming machine, the appearance defect that more fine pinholes exist on the surface of a product prepared by molding, and the more complicated post-treatment, polishing and repairing are needed.
The flame-retardant B1-grade polyurethane wood-like door comprises a polyurethane base material and paint sprayed on the polyurethane base material, wherein the polyurethane base material is prepared by reacting a component A and a component B, and the mass ratio of the component A to the component B is 1: 1.2-1.8; the above-mentionedThe component A comprises polyether polyol, a surfactant, a foaming agent, a flame retardant and a catalyst; the component B is isocyanate and/or modified isocyanate; wherein the polyether polyol at least comprises polyether polyol Ia and flame-retardant polyether polyol Ib; the surfactant comprises a siloxane surfactant and/or a fluorine-containing surfactant; the foaming agent is low-boiling point alkane, fluorocarbon, dichloromethane, n-pentane, isopentane, cyclopentane and CO2One or more of (a); the flame retardant is one or more of halogenated phosphate, modified melamine liquid compound, halogen/antimony/nitrogen-containing flame retardant and the like; the catalyst comprises at least one trimerization catalyst and a catalyst and/or a gel catalyst, and the mass part ratio of polyether polyol, surfactant, foaming agent, flame retardant and catalyst in the component A is as follows: 100: 0.5-5: 0.1-10: 5-30: 0.3-3.
Further, the isocyanate index R of the polyurethane wood-like door is 1.2-2.0;
the isocyanate index R can be calculated by the following formula:
Figure BDA0002046670540000021
wherein: b1NCO％，B2NCO％﹒﹒﹒,BpNCO％The mass percentage of NCO of corresponding isocyanate or modified isocyanate in the component B is respectively;
mB1，mB2…，mBprespectively the mass of corresponding isocyanate or modified isocyanate in the component B;
mH2Ois the mass of water;
mnwhere n is a, b, c …, mass of the corresponding polyether polyol, fnTo correspond to the average functionality of the polyether polyol,
Figure BDA0002046670540000022
of corresponding polyether polyolsA number average molecular weight;
mvis the mass of the catalyst, fvCorresponding to the number of isocyanate-reactive hydrogen atoms per molecule of catalyst,
Figure BDA0002046670540000023
is the number average molecular weight of the corresponding catalyst.
Furthermore, the isocyanate index R of the polyurethane wood-like door is 1.4-1.8.
Further, the polyether polyol Ia is prepared by polymerizing propylene oxide and/or ethylene oxide by taking a polyol and/or a polyamine mixture as an initiator, has the average functionality of 4-6 and the number average molecular weight of 500-1000; the flame-retardant polyether polyol Ib is prepared by performing ring-opening polymerization reaction on a flame-retardant group compound containing phosphorus and/or chlorine and/or antimony and an initiator or a polyether polyol mixture under the protection of inert gas, slowly heating to 180 ℃ and keeping for 2 hours, so that the flame-retardant polyether polyol containing multiple flame-retardant groups containing phosphorus and/or chlorine and/or antimony can be prepared, the average functionality is 1-6, the molecular weight is 300-1000, and the halogen content is more than or equal to 10%.
Further, the polyether polyol Ia takes propylene oxide as a polymerization monomer, and is formed by end-capping polymerization of the propylene oxide, the average functionality is 5, and the number-average molecular weight is 600-800; the average functionality of the flame-retardant polyether polyol Ib is 3, the molecular weight is 400-600, and the halogen content is not less than 15%.
Further, the surfactant is an organosiloxane copolymer surfactant.
Further, the foaming agent is a water and environment-friendly HFC-365 compound with zero ODP value, and the mass ratio of HFC-365 to water is 5: 95.
further, the flame retardant is one or more of halogenated phosphate ester which is liquid at the temperature of-20-200 ℃, melamine which is liquid at the temperature of-20-200 ℃ and nitrogen-containing heterocyclic derivatives thereof.
The invention also comprises a preparation method of the polyurethane wood-like door, which comprises the following steps:
a) s1, accurately weighing the polyether polyol, the surfactant, the foaming agent, the flame retardant and the catalyst according to the proportion, and uniformly mixing to form a component A;
s2, controlling the A component and the B component at-20-50 ℃, uniformly mixing the A component and the B component through a polyurethane high-pressure foaming machine with the set parameter A/B injection pressure of 11.0-11.5/10.0-10.5MPa respectively, injecting the mixture into a mold, and injecting the mixture into the mold under the mold locking pressure of 5.5-9.5 kilogram force/cm2Keeping for 30-60min, carrying out foaming and curing reaction, and demoulding to obtain the polyurethane base material with compact appearance and clear smooth lines; the free foam density of the polyurethane rigid foam of the polyurethane substrate is 150-300Kg/m3The overall density of the polyurethane substrate is 450-750Kg/m3；
S3, and after the polyurethane base material prepared in the step S2 is subjected to surface cleaning, polishing and paint spraying, the flame-retardant B1-grade polyurethane wood-like door is obtained.
Further, the mixing temperature of the component A and the component B in the step S2 is 20-30 ℃, and the free foam density of the polyurethane rigid foam of the polyurethane base material is 200-240Kg/m3The bulk density is 550-650Kg/m3。
As a preferred embodiment of the present invention, the polyether polyol of the present invention comprises the following components:
the starter of the polyether polyol la comprises one or more of ethylene glycol, propylene glycol, diethylene glycol, dipropylene glycol, tripropylene glycol, diethylene glycol, dipropylene glycol, glycerol, trimethylolpropane, pentaerythritol, sorbitol, sucrose, alkylene oxide adducts of polyhydroxyalkanes, preferably one or more mixtures of sorbitol and pentaerythritol or glycerol or trimethylolpropane.
The flame-retardant polyether polyol Ib is prepared from phosphate chloride or phosphorus chloride (PCl)3) Or the mixture of chloropropene or phosphorus and/or antimony containing compound and initiator or polyether polyol is ring-opening polymerized under the protection of inert gas to obtain the flame-retarding polyether polyol with several flame-retarding radicals including phosphorus, chlorine, antimony, etc. and the flame-retarding polyether polyol containing phosphorus and antimony is preferably reacted with isocyanate to form hard foamed polyurethane material with one layer of surface energy generated during fireThe dense carbonization zone can effectively prevent the flame from further burning inwards, and the halogen polyether can decompose halogenated hydrocarbon gas at high temperature to isolate oxygen in the outside air, thereby achieving the purpose of good flame retardance.
The polyether polyol ic is prepared by taking polyol and/or polyamine as an initiator, taking propylene oxide as a polymerization monomer and performing end-capping polymerization on the propylene oxide, wherein the polyether polyol ic has the average functionality of 3-6, preferably 4-5, and the number average molecular weight of 200-1000, preferably 300-500, and the initiator comprises one or more of glycerol, triethanolamine, pentaerythritol, diethylene glycol, sorbitol and sucrose, preferably one or more of pentaerythritol, diethylene glycol, sorbitol and sucrose; wherein the polyether polyol is preferably prepared by jointly starting from diamine and sorbitol;
the polyether polyol id is prepared by taking polyamine and/or polyol as an initiator, taking propylene oxide as a polymerization monomer and performing end-capping polymerization on the propylene oxide, wherein the average functionality is 2-4, preferably 3, and the number-average molecular weight is 300-200, preferably 400-1000; the initiator comprises one or more of glycerol, trimethylolpropane, triethanolamine, pentaerythritol, diethylenetriamine and sorbitol, preferably one or more of glycerol, trimethylolpropane and triethanolamine.
The functionality of the polyether polyol only calculates the functional groups of hydroxyl and amino which can participate in the polyurethane reaction.
The isocyanates useful in the B component of the present invention are aliphatic, cycloaliphatic, araliphatic, aromatic isocyanates or combinations thereof. Preferably, the mass fraction of NCO groups in the isocyanate and/or modified isocyanate of said B-component according to the present invention is from 25 to 35%, preferably from 30 to 33%, calculated on the mass of isocyanate and/or modified isocyanate. The isocyanate in the component B is diphenylmethane diisocyanate and/or polymethylene polyphenyl isocyanate, preferably diphenylmethane diisocyanate, and the diphenylmethane diisocyanate comprises one or more of 2,4 ' -diphenylmethane diisocyanate, 2 ' -diphenylmethane diisocyanate and 4,4 ' -diphenylmethane diisocyanate; the modified isocyanates include polyisocyanates containing one or more of urethane groups, allophanate groups, urea groups, biuret groups, carbodiimide groups and uretonimine groups. They may be used alone or in any desired mixture with one another. Examples of such B components include, but are not limited to, one or more of PM-200, PM-300, W8215, W8212, Huntsman's sup5005, 5888 and BASF's M20A, M20S in Van der Waals Chemicals.
Blowing agents of the present invention include, but are not limited to, low boiling alkanes, fluorocarbons, water, methylene chloride, n-pentane, isopentane, cyclopentane, CO2For example, water and hydrofluorocarbons are preferably used in combination. The foaming agent takes water as a chemical auxiliary foaming agent, the initial reaction releases heat, the subsequent high-boiling-point physical foaming agent is promoted to volatilize, and the environment-friendly HFC-365 with zero ODP value is selected to compound non-flammable HFC with the content of 5 percent, so that the flammability defect of directly using HF-C365 is overcome.
The flame retardant comprises one or more of halogenated phosphate, modified melamine liquid compound, halogen/antimony/nitrogen-containing flame retardant and the like; preferably one or more of halogenated phosphate ester which is liquid at-20-200 ℃, melamine which is liquid at-20-200 ℃ and nitrogen heterocyclic ring derivative thereof; examples of halophosphate esters of the present invention include, but are not limited to, one or more of tris (2-chloropropyl) phosphate (TCPP), tris (2-chloroethyl) phosphate (TCEP), tris (2, 3-dichloropropyl) phosphate (TDCP), tetrakis (2-chloroethyl) diethylene ether diphosphate, tetrakis (2-chloroethyl) ethylene diphosphate, and tetrakis (2-chloroethyl) -2, 2-dichloromethyl-1, 3-propylene diphosphate. Other examples of IV) flame retardants that can be used in the present invention include, but are not limited to, FR-130, FR-212, FR-1830, FR-68, and the like, all in Wanhua chemistry.
The catalyst of the present invention comprises at least one trimerisation catalyst and one catalyst of the catalytic type and/or one catalyst of the gel type.
In general, the types of catalysts are mainly distinguished by their catalytic tendency, including three types, namely catalysis of trimeric condensation of isocyanate groups to form polyheterocyclic polyisocyanates, and catalysis of blowing reactions and catalysis of gelling reactions. The catalyst that catalyzes the foaming reaction is often referred to as a catalytic catalyst or a foaming catalyst, and the catalyst that catalyzes the gel is often referred to as a gel catalyst. The catalysts commonly used at present have the functions of foaming and gel catalysis at the same time, but have different degrees of catalysis tendency.
The trimerization catalyst of the present invention comprises nitrogen group element compound, organic metal compound and the like as trimerization catalyst of aliphatic and aromatic isocyanate, such as formate of 2-hydroxy-N, N, N-trimethyl-1-propylamine, N, N' -tris (dimethylaminopropyl) -hexahydrotriazine, 2,4, 6-tris (dimethylaminomethyl) phenol are commonly used tertiary amine trimerization catalyst.
The catalyst for hair growth according to the present invention comprises a catalyst for hair growth which may or may not contain an oxygen atom, and examples thereof include one or more of bis (dimethylaminoethyl) ether (a1), N-Dimethylethanolamine (DMEA), N-dimethylcyclohexylamine, pentamethyldiethylenetriamine, N-dimethylisopropylpropylenediamine, triethylamine, tributylamine, N-dimethylaminopropylamine, dimethylethanolamine, N ' -tetramethylethylenediamine, N ' -trimethyl-N ' -hydroxyethylbisaminoethyl ether. Other examples of commercially available catalyst include KC121 of Wanhua chemistry, and the like. Examples of the gel-type catalyst according to the present invention include, but are not limited to, gel-type amine catalysts, amidines, organometallic compounds, or combinations thereof. Examples of the gel-type amine catalyst include, but are not limited to, triethylenediamine (a33), N-dimethyl-N ', N' -bis (2-hydroxypropyl) -1, 3-propanediamine, and the like. Examples of the amidines include, but are not limited to, 1, 8-diazabicyclo [5.4.0] undec-7-ene and 2, 3-dimethyl-3, 4,5, 6-tetrahydropyrimidine, and salts thereof. The organometallic compound may include organotin compounds such as dibutyltin dilaurate, stannous octoate, dibutyltin diacetate, dioctyltin diacetate, dibutyltin maleate, and the like. Bismuth salts of organic carboxylic acids may also be selected. Other suitable gel-type catalysts are, for example, 2,4, 6-tris (dimethylaminomethyl) phenol. Other commercially available gel-type catalysts also include KC-100, KC101, etc. of Wanhua chemistry.
The trimerization catalyst of the present invention is preferably formate of 2-hydroxy-N, N, N-trimethyl-1-propylamine (TMR-2), 2,4, 6-tris (dimethylaminomethyl) phenol (DMP-30).
The catalyst is preferably one or more of bis (dimethylaminoethyl) ether, N, N-dimethylethanolamine, N, N-dimethylcyclohexylamine, pentamethyldiethylenetriamine, N, N-dimethylisopropylpropylenediamine, N, N, N '-trimethyl-N' -hydroxyethyl bisaminoethyl ether and KC121 of Wanhua chemical company; the gel-type catalyst is preferably one or more of 2,4, 6-tris (dimethylaminomethyl) phenol, triethylenediamine, dibutyltin dilaurate, stannous octoate, dibutyltin diacetate, KC-100 and KC101 from Vawa chemical company.
The preferable mass parts of the polyether polyol, the surfactant, the foaming agent, the flame retardant and the catalyst in the component A are as follows: 100: 1-1.5: 1.1-5.5: 10-15: 0.3-0.8.
According to the invention, a sorbitol initiator propylene oxide polymerization and end-capped polyether polyol, a phosphorus/antimony/chlorine-containing flame-retardant group reaction type flame-retardant polyether polyol, a compound foaming agent are selected for synergistic foaming, and a PIR system is catalyzed to form a synergistic flame-retardant effect, so that the prepared polyurethane hard wood-like door semi-finished product has the characteristics of smooth surface, compact surface, few microscopic pinhole defects and fine and smooth pores, is greatly convenient for post-treatment polishing and repairing processes, has good flame retardance and does not contain solid filler, and is convenient for equipment rapid molding, the tensile strength is 8-20MPa, the bending strength is 20-40MPa, the flame-retardant performance test standard is GB/T8624 and 2014B1 grade, and the oxygen index is not less than 32.
The polyurethane rigid foam can also be applied to products with higher requirements on strength, appearance and flame retardance, such as polyurethane wood-like doors, windows, furniture and the like.
Drawings
FIG. 1 is a partially enlarged photograph of example 1 of a flame retardant B1 grade polyurethane wood-like door of the present invention.
FIG. 2 is a partially enlarged photograph of example 2 of a flame retardant B1 grade polyurethane wood-like door of the present invention.
FIG. 3 is a partially enlarged photograph of example 3 of a flame retardant B1 grade polyurethane wood-like door of the present invention.
FIG. 4 is a partially enlarged photograph of example 4 of a flame retardant B1 grade polyurethane wood-like door of the present invention.
FIG. 5 is a partially enlarged photograph of example 5 of a flame retardant B1 grade polyurethane wood-like door of the present invention.
FIG. 6 is a partially enlarged photograph of example 6 of a flame retardant B1 grade polyurethane wood-like door of the present invention.
FIG. 7 is a partially enlarged photograph of example 7 of a flame retardant B1 grade polyurethane wood-like door of the present invention.
FIG. 8 is a partially enlarged photograph of example 8 of a flame retardant B1 grade polyurethane wood-like door of the present invention.
FIG. 9 is a partially enlarged photograph of example 9 of a flame retardant B1 grade polyurethane wood-like door of the present invention.
FIG. 10 is a partially enlarged photograph of example 10 of a flame retardant B1 grade polyurethane wood-like door of the present invention.
FIG. 11 is a partially enlarged photograph of example 11 of a flame retardant B1 grade polyurethane wood-like door of the present invention.
FIG. 12 is a partially enlarged photograph of example 12 of a flame retardant B1 grade polyurethane wood-like door of the present invention.
FIG. 13 is an enlarged, partial photographic view of example 13 of a flame retardant B1 grade polyurethane wood-like door of the present invention.
FIG. 14 is an enlarged partial photograph of example 14 of a flame retardant B1 grade polyurethane wood-like door of the present invention.
FIG. 15 is an enlarged partial photographic view of example 15 of a flame retardant B1 grade polyurethane wood-like door of the present invention.
FIG. 16 is an enlarged partial photograph of example 16 of a flame retardant B1 grade polyurethane wood-like door of the present invention.
FIG. 17 is a partially enlarged photograph of comparative example 1 of a polyurethane wood-like door which is a commercial product.
FIG. 18 is a partially enlarged photograph of comparative example 2 of a polyurethane wood-like door which is a commercial product.
FIG. 19 is a partially enlarged photograph of comparative example 4 of a polyurethane wood-like door which is a commercial product.
FIG. 20 is a comparison graph of actual effects of patent CN102758582 and the product of the patent.
The flame-retardant B1-grade polyurethane wood-like door of the invention is further described with reference to the accompanying drawings and specific examples.
Detailed Description
The chemical names, structural formulae or chemical substances limited by technical parameters well known to those skilled in the art referred to in the components throughout the present invention represent effective components acting on the reaction system of the present invention, and also represent all or main components of the components, and in addition, a small amount of impurities or solvents and the like are included, which are common in the art, and do not affect the implementation of the reaction system and technical scheme of the present invention. The matters not described in the present invention, such as impurities in the components, small amounts of solvents, preparation methods, etc., can be explained and illustrated by those well known to those skilled in the art.
The preparation of the polyether polyol of the present invention is more clearly illustrated by a method for synthesizing polyether polyol which is commonly used in the art, but the preparation of the polyether polyol of the present invention is not limited thereto.
The polyether polyol synthesis method briefly describes that: according to the relative molecular mass theory of the target product, the mass of an initiator (such as glycerol, trimethylolpropane, pentaerythritol, sorbitol and the like), a catalyst (such as KOH) and a polymerization monomer propylene oxide are calculated, the dosage of the catalyst is 0.1-1.0 percent of the total dosage, and a step-by-step feeding method is adopted. Firstly putting an initiator and a catalyst into a reaction kettle, vacuumizing, introducing nitrogen for three times for replacement, firstly adding 40% of the total amount of a polymerization monomer according to the required propylene oxide feeding quality, heating the reaction kettle to 85-120 ℃, keeping the pressure in the kettle at 0.1-0.8MPa, stopping feeding when the temperature in the kettle exceeds 120 ℃, continuing feeding when the temperature is in a proper range, adding 30% after reacting for 1h, adding 30% after 1h, adding phosphoric acid for neutralizing KOH after the pressure in the kettle is reduced to negative pressure, performing vacuum dehydration after water washing to obtain colorless transparent viscous liquid, and testing the hydroxyl value and the relative molecular mass to verify as a target product;
the synthesis method of the flame-retardant polyether polyol is briefly described as follows: putting 558g of glycerol and 114g of antimony chloride into a dry reaction kettle, gradually dropwise adding 71g of phosphorus oxychloride at 70-80 ℃, heating to 80-90 ℃ after dropwise adding, keeping the temperature for reaction for 1h, removing a byproduct hydrogen chloride gas generated in the reaction through reduced pressure distillation, dropwise adding 1295g of epichlorohydrin into the system for ring-opening polymerization, controlling the reaction temperature to be 110-120 ℃, keeping the reaction for 2h, removing small molecules through reduced pressure distillation, washing with water, and performing vacuum-pumping dehydration treatment to obtain the light yellow transparent chlorine/phosphorus/antimony-containing flame-retardant polyether polyol.
The starting materials used in the examples according to the invention and in the comparative examples are described below:
polyether polyol Ia 1: taking a mixture of sorbitol and diethylene glycol with a molar ratio of 7:3 as an initiator, carrying out ring-opening polymerization on propylene oxide, and capping the propylene oxide to obtain a product with a number average molecular weight of 700;
polyether polyol Ia 2: taking a mixture of sorbitol and diethylene glycol with a molar ratio of 8:2 as an initiator, carrying out ring-opening polymerization on propylene oxide, and capping the propylene oxide to obtain a product with a number average molecular weight of 750;
polyether polyol Ia 3: taking a mixture of sucrose and diethylene glycol with a molar ratio of 3.7:6.3 as an initiator, carrying out ring-opening polymerization on propylene oxide, and capping the propylene oxide with a number average molecular weight of 550;
polyether polyol lb 1: glycerol and antimony trichloride initiator are gradually added to react with phosphorus oxychloride, and after the byproduct is removed, epichlorohydrin is used for ring-opening polymerization to obtain reactive flame-retardant polyether polyol containing three flame-retardant elements, namely 3-5% of phosphorus, 30-40% of chlorine and 10-15% of antimony;
polyether polyol lb 2: mixing dipropylene glycol and phosphate, gradually carrying out addition reaction on phosphorus oxychloride, removing by-products, and carrying out ring-opening polymerization on epichlorohydrin to obtain reactive flame-retardant polyether polyol containing 6-9% of phosphorus and 30-40% of chlorine flame-retardant elements;
polyether polyol ic 1: sorbitol and toluenediamine mixture initiator, propylene oxide ring-opening polymerization, functionality of 4, number average molecular weight of 300;
polyether polyol ic 2: diethylene triamine is used as an initiator, propylene oxide is subjected to ring opening polymerization, and the number average molecular weight is 450;
polyether polyol id 1: TMN400, Tianjin Tripetro-chemical Co
Polyether polyol id 2: TMN700, Tianjin Tripetro-chemical Co
Surfactant IIa: b8870, Woods winning and creating Co
Surfactant IIb: s6930, Beijing Yintaider science and technology Ltd
Foaming agent: HFC-365mfc/227, 93/7 German Suwei
Flame retardant IIIa: tetrakis (2-chloroethyl) diethylene ether diphosphate;
flame retardant IIIb: FR-130, Wanhua chemical product;
catalyst IVa: formate of 2-hydroxy-N, N, N-trimethyl-1-propylamine
Catalyst IVb: WANALYST KC100 Wanhua chemical products.
Catalyst IVc: n, N-dimethyl-N ', N' -bis (2-hydroxypropyl) -1, 3-propanediamine.
Catalyst IVd: 2,4, 6-tris (dimethylaminomethyl) phenol
Catalyst IVe: WANALYST KC101, Wanhua chemical products.
And B component:
M20A, product of BASF, having an NCO content of 32.0% by weight and an average functionality of from 2.5 to 2.7;
w8215, a Wanhua chemical product, having an NCO content of 32.5% by weight and an average functionality of 2.6-2.7;
in examples 1 to 16, polyether polyol, a compound foaming agent, a surfactant, a catalyst and a flame retardant are added into a charging basket with a stirrer according to the formula shown in table 1 and uniformly mixed to form a material A, the material A, B is controlled at 20 to 30 ℃, the A/B injection pressure of a polyurethane high-pressure foaming machine is set to be 11.0 to 11.5/10.0 to 10.5MPa respectively, the material is opened or closed and poured into a mold, the mold is opened after 30 to 60 minutes of pressure maintaining, a polyurethane wood-like door semi-finished product is obtained, and the polyurethane wood-like door product is obtained after post-treatment.
Table 1 examples formulations (contents of components are in parts by mass)
Figure BDA0002046670540000101
Figure BDA0002046670540000111
Figure BDA0002046670540000112
Figure BDA0002046670540000121
Note: the starting time is as follows: the A component and the B component are started to be timed by high-pressure machine injection, and the time until the mixture starts to expand or grow is called as the initiation time, also called as the cream time;
the debonding time is as follows: the A/B double-component is injected by a high-pressure machine to start timing, the surface of the foam body is pressed by a PE film, the PE film has no bonding effect with the surface of the foam body, the PE film can be freely separated, and the used time is the debonding time.
TABLE 2 comparative example formulation (the content of the components is in parts by mass)
Figure BDA0002046670540000122
Figure BDA0002046670540000131
Note: "-" indicates that the sample foam was sticky and no detackification time could be obtained.
TABLE 3 polyurethane foam Properties
Figure BDA0002046670540000132
Figure BDA0002046670540000141
Through the comparison and inspection results, the flame-retardant B1-grade polyurethane wood-like door disclosed by the invention has a good flame-retardant effect, and the indexes such as the surface flatness, the free bubble density, the tensile strength, the bending strength, the oxygen index and the like of a polyurethane substrate are greatly superior to those of similar products, so that the door has the characteristics of smooth surface, compact surface, few microscopic pinhole defects and fine and smooth pores, is greatly convenient for post-treatment polishing and repairing processes, and has good flame retardance. The invention does not contain solid filler, is convenient for quick molding of equipment, has simple process, and can be applied to products with higher requirements on strength, appearance and flame retardance, such as polyurethane wood-like doors, windows, furniture and the like.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements, etc. made by those skilled in the art within the spirit and principle of the present invention should be included in the scope of the present invention.

Claims (3)

1. The flame-retardant B1-grade polyurethane wood-like door comprises a polyurethane base material and paint sprayed on the polyurethane base material, wherein the polyurethane base material is prepared by reacting a component A and a component B, and the component A comprises the following substances in parts by mass:
Figure FDA0003436096700000011
the component B comprises the following substances in parts by mass:
W8215 120
M20A 20
Sup5005 20；
wherein polyether polyol Ia 1: taking a mixture of sorbitol and diethylene glycol with a molar ratio of 7:3 as an initiator, carrying out ring-opening polymerization on propylene oxide, and capping the propylene oxide to obtain a product with a number average molecular weight of 700;
polyether polyol Ia 3: taking a mixture of sucrose and diethylene glycol with a molar ratio of 3.7:6.3 as an initiator, carrying out ring-opening polymerization on propylene oxide, and capping the propylene oxide with a number average molecular weight of 550;
polyether polyol lb 1: glycerol and antimony trichloride initiator are gradually added to react with phosphorus oxychloride, and after the byproduct is removed, epichlorohydrin is used for ring-opening polymerization to obtain reactive flame-retardant polyether polyol containing three flame-retardant elements, namely 3-5% of phosphorus, 30-40% of chlorine and 10-15% of antimony;
polyether polyol ic 1: sorbitol and toluenediamine mixture initiator, propylene oxide ring-opening polymerization, functionality of 4, number average molecular weight of 300;
polyether polyol id 1: TMN 400;
surfactant B8870;
foaming agent: HFC-365mfc/227, 93/7;
flame retardant IIIa: tetrakis (2-chloroethyl) diethylene ether diphosphate;
flame retardant IIIb: FR-130;
catalyst IVa: formate of 2-hydroxy-N, N-trimethyl-1-propylamine;
catalyst IVb: WANALYST KC100, respectively;
catalyst IVd: 2,4, 6-tris (dimethylaminomethyl) phenol;
and B component:
M20A, NCO content 32.0% by weight, average functionality 2.5-2.7;
w8215, NCO content 32.5 wt%, average functionality 2.6-2.7;
isocyanate index 1.65;
the isocyanate index R can be calculated by the following formula:
Figure FDA0003436096700000021
wherein: b1NCO％，B2NCO％﹒﹒﹒,BpNCO％Of NCO's of the corresponding isocyanates or modified isocyanates, respectively, of component BMass percentage content;
mB1，mB2…，mBprespectively the mass of corresponding isocyanate or modified isocyanate in the component B;
mH2Ois the mass of water;
mnwhere n is a, b, c …, mass of the corresponding polyether polyol, fnTo correspond to the average functionality of the polyether polyol,
Figure FDA0003436096700000022
is the number average molecular weight of the corresponding polyether polyol;
mvis the mass of the catalyst, fvCorresponding to the number of isocyanate-reactive hydrogen atoms per molecule of catalyst,
Figure FDA0003436096700000023
is the number average molecular weight of the corresponding catalyst.
2. The method for preparing the flame-retardant B1-grade polyurethane wood-like door according to claim 1, wherein the method comprises the following steps:
s1, accurately weighing the polyether polyol, the surfactant, the foaming agent, the flame retardant and the catalyst according to the proportion, and uniformly mixing to form a component A;
s2, controlling the A component and the B component at-20-50 ℃, uniformly mixing the A component and the B component through a polyurethane high-pressure foaming machine with the set parameter A/B injection pressure of 11.0-11.5/10.0-10.5MPa respectively, injecting the mixture into a mold, and injecting the mixture into the mold under the mold locking pressure of 5.5-9.5 kilogram force/cm2Keeping for 30-60min, carrying out foaming and curing reaction, and demoulding to obtain the polyurethane base material with compact appearance and clear smooth lines; the free foam density of the polyurethane rigid foam of the polyurethane substrate is 150-300Kg/m3The overall density of the polyurethane substrate is 450-750Kg/m3；
S3, and after the polyurethane base material prepared in the step S2 is subjected to surface cleaning, polishing and paint spraying, the flame-retardant B1-grade polyurethane wood-like door is obtained.
3. The method for preparing the flame-retardant B1-grade polyurethane wood-like door as claimed in claim 2, wherein the mixing temperature of the component A and the component B in the step S2 is 20-30 ℃, and the free foam density of the rigid polyurethane foam of the polyurethane substrate is 200-240Kg/m3The bulk density is 550-650Kg/m3。
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CN102758582A (en) * 2012-07-19 2012-10-31 黄吉力 Wood-like polyurethane door and preparation method thereof
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CN103183806A (en) * 2013-04-17 2013-07-03 北京东方雨虹防水技术股份有限公司 High-flame-retardant hard polyurethane foam material and preparation method thereof
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CN101503504A (en) * 2008-12-01 2009-08-12 无锡双象化学工业有限公司 Preparation of polyurethane rigid foam wood-like material
CN102758582A (en) * 2012-07-19 2012-10-31 黄吉力 Wood-like polyurethane door and preparation method thereof
CN103073986A (en) * 2012-12-19 2013-05-01 烟台万华聚氨酯股份有限公司 Advanced flame-retardant polyurethane spray foam material and preparation method thereof
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