CN115030335A - Composite insulation board for building external wall and preparation method thereof - Google Patents

Composite insulation board for building external wall and preparation method thereof Download PDF

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Publication number
CN115030335A
CN115030335A CN202210799367.9A CN202210799367A CN115030335A CN 115030335 A CN115030335 A CN 115030335A CN 202210799367 A CN202210799367 A CN 202210799367A CN 115030335 A CN115030335 A CN 115030335A
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polyol
triazine
insulation board
preparation
parts
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CN115030335B (en
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沈长涛
张会敏
渠涛
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Xuzhou Jingxin New Material Co ltd
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Xuzhou Jingxin New Material Co ltd
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    • E—FIXED CONSTRUCTIONS
    • E04—BUILDING
    • E04B—GENERAL BUILDING CONSTRUCTIONS; WALLS, e.g. PARTITIONS; ROOFS; FLOORS; CEILINGS; INSULATION OR OTHER PROTECTION OF BUILDINGS
    • E04B1/00—Constructions in general; Structures which are not restricted either to walls, e.g. partitions, or floors or ceilings or roofs
    • E04B1/62—Insulation or other protection; Elements or use of specified material therefor
    • E04B1/74—Heat, sound or noise insulation, absorption, or reflection; Other building methods affording favourable thermal or acoustical conditions, e.g. accumulating of heat within walls
    • E04B1/76—Heat, sound or noise insulation, absorption, or reflection; Other building methods affording favourable thermal or acoustical conditions, e.g. accumulating of heat within walls specifically with respect to heat only
    • E04B1/78—Heat insulating elements
    • E04B1/80—Heat insulating elements slab-shaped
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/40—High-molecular-weight compounds
    • C08G18/4009—Two or more macromolecular compounds not provided for in one single group of groups C08G18/42 - C08G18/64
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/40—High-molecular-weight compounds
    • C08G18/48—Polyethers
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/40—High-molecular-weight compounds
    • C08G18/64—Macromolecular compounds not provided for by groups C08G18/42 - C08G18/63
    • C08G18/6415—Macromolecular compounds not provided for by groups C08G18/42 - C08G18/63 having nitrogen
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/70—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
    • C08G18/72—Polyisocyanates or polyisothiocyanates
    • C08G18/74—Polyisocyanates or polyisothiocyanates cyclic
    • C08G18/76—Polyisocyanates or polyisothiocyanates cyclic aromatic
    • C08G18/7657—Polyisocyanates or polyisothiocyanates cyclic aromatic containing two or more aromatic rings
    • C08G18/7664—Polyisocyanates or polyisothiocyanates cyclic aromatic containing two or more aromatic rings containing alkylene polyphenyl groups
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G2101/00—Manufacture of cellular products
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G2110/00—Foam properties
    • C08G2110/0083—Foam properties prepared using water as the sole blowing agent
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02B—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO BUILDINGS, e.g. HOUSING, HOUSE APPLIANCES OR RELATED END-USER APPLICATIONS
    • Y02B30/00—Energy efficient heating, ventilation or air conditioning [HVAC]
    • Y02B30/90—Passive houses; Double facade technology

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Organic Chemistry (AREA)
  • Polymers & Plastics (AREA)
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  • Chemical Kinetics & Catalysis (AREA)
  • Architecture (AREA)
  • Physics & Mathematics (AREA)
  • Engineering & Computer Science (AREA)
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  • Civil Engineering (AREA)
  • Electromagnetism (AREA)
  • Acoustics & Sound (AREA)
  • Polyurethanes Or Polyureas (AREA)

Abstract

The invention discloses a composite insulation board for a building outer wall and a preparation method thereof, the scheme takes glass fiber gridding cloth as a bottom layer, polyurethane foam forms a polyurethane insulation layer, a surface layer adopts a cement mortar layer, a cement fiber board or a calcium silicate board, and a bottom layer-polyurethane insulation layer-surface layer composite structure forms the insulation board.

Description

Composite insulation board for building external wall and preparation method thereof
Technical Field
The invention relates to the technical field of insulation boards, in particular to a composite insulation board for a building outer wall and a preparation method thereof.
Background
The outer wall insulation board is compounded by polymer mortar, glass fiber gridding cloth, flame-retardant molded polystyrene foam boards or extruded sheets and other materials, can meet the energy-saving requirement of current house buildings, improves the insulation level of the outer walls of industrial and civil buildings, is also a preferred material for energy-saving reconstruction of the existing buildings, is used in the fields of high-rise outer walls, indoor markets, industrial equipment and the like, and has the advantages of low manufacturing cost, good effect, corrosion resistance, no pollution and the like.
The polyurethane foaming layer is also a commonly used insulation board material in the market, but the flame retardant property of the polyurethane foaming layer is poor, a flame retardant is generally added into polyurethane conventionally, the mechanical property and the thermal insulation property of the polyurethane foaming layer are affected by the addition of the flame retardant, and the polyurethane foaming layer is inconvenient to use in practice.
Based on the above situation, the application discloses a composite insulation board for a building outer wall and a preparation method thereof, so as to solve the technical problem.
Disclosure of Invention
The invention aims to provide a composite insulation board for a building outer wall and a preparation method thereof, and aims to solve the problems in the background technology.
In order to solve the technical problems, the invention provides the following technical scheme:
a composite insulation board for building exterior walls and a preparation method thereof comprise the following steps:
(1) uniformly stirring trimethylolpropane, triazine polyol and N, N-dimethylformamide under a nitrogen environment, adding isophorone diisocyanate, and reacting at 80-85 ℃ for 50-60min to obtain a material A;
adding mixed solution of isophorone diisocyanate and N, N-dimethylformamide into the material A, stirring and reacting for 40-50min, adding mixed solution of trimethylolpropane and N, N-dimethylformamide, continuing to react for 1-1.5h, then adding mixed solution of triazine polyol and N, N-dimethylformamide, reacting for 40-50min, collecting a product after the reaction is finished, and evaporating a solvent to obtain flame-retardant polyol;
(2) mixing flame-retardant polyol, polyether polyol, a foam stabilizer, a catalyst and deionized water, stirring and mixing for 10-20min under an oil bath at 40-45 ℃, adding polymethylene polyphenyl polyisocyanate, and continuously stirring for 6-10s to obtain a polyurethane foaming liquid;
paving a plurality of layers of glass fiber mats in a mold, injecting polyurethane foaming liquid into the mold, foaming and curing, curing at 70-80 ℃, and demolding to obtain a polyurethane heat-insulating layer;
(3) taking the bottom layer, the polyurethane heat-insulation board and the surface layer, gluing and compounding the surface layer, the polyurethane heat-insulation layer and the bottom layer from top to bottom to obtain a matrix, cutting and trimming the matrix, coating a fluorocarbon coating on the surface of one side of the matrix, which is close to the surface layer, and drying to obtain the composite heat-insulation board.
According to an optimized scheme, in the step (2), the raw materials of each component comprise: 30-40 parts of flame-retardant polyol, 60-70 parts of polyether polyol, 6-8 parts of foam stabilizer, 1-2 parts of catalyst, 1-2 parts of deionized water and 120 parts of polymethylene polyphenyl polyisocyanate 110-.
According to an optimized scheme, in the step (3), the bottom layer is made of glass fiber gridding cloth, and the surface layer is made of any one of a cement mortar layer, a cement fiberboard and a calcium silicate board.
In an optimized scheme, in the step (1), the preparation steps of the triazine polyol are as follows: uniformly mixing 1,3, 5-s-triazine triol and diethylenetriamine, heating to 120-130 ℃, adding ethanolamine, continuing to heat to 200-210 ℃, stirring for 20-30min, adding a 5A molecular sieve, carrying out heat preservation reaction for 4-5h, carrying out reduced pressure distillation after the reaction is finished, and collecting a product to obtain the triazine polyol.
According to an optimized scheme, the molar ratio of the 1,3, 5-s-triazine triol to the diethylenetriamine to the ethanolamine is 1: 1: 4; the dosage of the 5A molecular sieve is 20-25 wt% of 1,3, 5-s-triazine triol.
According to an optimized scheme, in the step (1), when the material A is prepared, the use amounts of the components are as follows: the molar ratio of the total amount of the isophorone diisocyanate, the trimethylolpropane and the triazine polyol is 1: 2; the molar ratio of the trimethylolpropane to the triazine polyol is 1: 1.
according to an optimized scheme, in the step (1), when the flame-retardant polyol is prepared, the following components are used: the molar ratio of the material A to the isophorone diisocyanate to the trimethylolpropane to the triazine polyol is 1: 5: 1: 1.
according to an optimized scheme, the composite insulation board is prepared by the preparation method of the composite insulation board for the building outer wall.
Compared with the prior art, the invention has the following beneficial effects: the invention discloses a composite insulation board for a building outer wall and a preparation method thereof.
According to the scheme, when polyurethane is foamed, polyether polyol, flame-retardant polyol with a flame-retardant function and polymethylene polyphenyl polyisocyanate are introduced to react to form polyurethane foaming liquid, then the glass fiber mat is used as a reinforcing material and placed in a mold, the polyurethane foaming liquid is injected, and the polyurethane insulating layer covering the glass fiber mat is formed through foaming and curing; the introduction of the flame-retardant polyol can improve the flame retardant property of the polyurethane, and the component participates in the reaction as a polyol component, so that other flame retardant components are not required to be added in the system, the problem of poor compatibility between other flame retardants and the polyurethane is avoided, and the mechanical property of the polyurethane is ensured.
On the basis, the design scheme of the flame-retardant polyol is as follows:
(1) firstly, mixing trimethylolpropane and triazine polyol, and carrying out graft reaction on the mixture and isophorone diisocyanate to form a material A, wherein the molar ratio of the total amount of the isophorone diisocyanate, the trimethylolpropane and the triazine polyol is controlled to be 1: 2, under the proportion, two isocyanate groups of isophorone diisocyanate can be in graft reaction with a component containing hydroxyl in a system to form an intermediate (material A) containing a flame-retardant triazine ring; then the material A is subjected to hyperbranched reaction, the material A is taken to react with isophorone diisocyanate, then trimethylolpropane and triazine polyol are introduced to carry out branching so as to form polyol with a hyperbranched structure, and the polyol with the hyperbranched structure can participate in the reaction of a polyurethane system, so that the crosslinking degree of the polyurethane system is improved, and the mechanical property of the polyurethane is improved; meanwhile, due to the existence of the flame-retardant triazine ring in the triazine polyol, the mechanical property and the flame retardant property of the polyurethane heat-insulating layer can be improved.
(2) According to the scheme, 1,3, 5-s-triazine triol reacts with diethylenetriamine and ethanolamine, on one hand, hydroxyl is introduced to form polyol to participate in the reaction, on the other hand, amino is introduced, and the amino can also participate in the reaction in a subsequent polyurethane system; meanwhile, due to the existence of the triazine polyol, the addition sequence of materials is limited in the process of branching reaction, and the addition sequence is as follows: the preparation method comprises the steps of adding trimethylolpropane firstly and introducing triazine polyol, and aims to utilize amino groups contained in the triazine polyol to enable enough amino groups to participate in a polyurethane system reaction, wherein the amino groups can react with isocyanate groups in the system to generate urea bonds, so that a micro-pore structure of the polyurethane is improved, and meanwhile, the mechanical property of the polyurethane can be improved.
As a more optimized scheme, in actual processing, after a material A is prepared, the glass fiber felt is placed in a KH-550 silane coupling agent, and then placed in a mixed solution of isophorone diisocyanate and the material A for grafting and dipping, so that the surface of the glass fiber felt contains a structure similar to that of flame-retardant polyol, and hydroxyl is introduced to improve the compatibility between the glass fiber felt and polyurethane foaming liquid, and further improve the overall mechanical property of a polyurethane heat-insulating layer.
The invention discloses a composite insulation board for a building outer wall and a preparation method thereof, wherein the proportion of components in each level is appropriate, the process design is simple, the prepared composite insulation board is suitable for the field of building outer wall insulation, the flame retardant property is better, the mechanical property is ensured while the insulation property is considered, and the composite insulation board has higher practicability.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In the present example, 1,3, 5-s-triazine triol, ethanolamine, and triethylene diamine were all obtained from Shanghai Allandin chemical Co., Ltd; diethylenetriamine and 5A molecular sieves are purchased from national medicine group chemical reagent company Limited and from national medicine group chemical reagent company Limited; trimethylolpropane and N, N-dimethylformamide are purchased from Dukolon reagent; isophorone diisocyanate is available from sigma-aldrich sigma aldrich (shanghai) trade, ltd; the polyether polyol is 4110, the hydroxyl value is 480-520 mg/g, and the polyether polyol is purchased from internationalization; the foam stabilizer is AK-8805 which is purchased from Nanjing Demei Shiwo; the organic bismuth catalyst is
Figure BDA0003733429070000041
Purchased from the united states leaders; polymethylene polyphenyl polyisocyanate is PM-200 and is purchased from Wanhua chemistry; the glass fiber felt is 400g/m 2 Purchased from owens koreaning. The glass fiber mesh cloth, the calcium silicate plate and the fluorocarbon coating are all conventional commercial products, and can be adjusted according to actual purchase requirements.
Example 1:
a composite heat-insulation board for building external walls and a preparation method thereof comprise the following steps:
(1) uniformly mixing 1,3, 5-s-triazine triol and diethylenetriamine, heating to 120 ℃, adding ethanolamine, continuously heating to 200 ℃, stirring for 30min, adding a 5A molecular sieve, reacting for 4h under heat preservation, distilling under reduced pressure after the reaction is finished, and collecting a product to obtain the triazine polyol. The mol ratio of the 1,3, 5-s-triazine triol to the diethylenetriamine to the ethanolamine is 1: 1: 4; the dosage of the 5A molecular sieve is 25 wt% of 1,3, 5-s-triazine triol.
Uniformly stirring trimethylolpropane, triazine polyol and N, N-dimethylformamide under a nitrogen environment, adding isophorone diisocyanate, and reacting at 80 ℃ for 60min to obtain a material A; the molar ratio of the total amount of the isophorone diisocyanate, the trimethylolpropane and the triazine polyol is 1: 2; the molar ratio of the trimethylolpropane to the triazine polyol is 1: 1.
adding mixed solution of isophorone diisocyanate and N, N-dimethylformamide into the material A, stirring at 85 ℃ for reacting for 40min, adding mixed solution of trimethylolpropane and N, N-dimethylformamide, keeping the temperature for continuing reacting for 1h, then adding mixed solution of triazine polyol and N, N-dimethylformamide, keeping the temperature for reacting for 40min, collecting a product after the reaction is finished, and evaporating a solvent to obtain flame-retardant polyol; the molar ratio of the material A to the isophorone diisocyanate to the trimethylolpropane to the triazine polyol is 1: 5: 1: 1.
(2) mixing 30 parts by weight of flame-retardant polyol, 70 parts by weight of polyether polyol, 6 parts by weight of foam stabilizer, 1 part by weight of catalyst and 1 part by weight of deionized water, stirring and mixing for 20min at 40 ℃ in an oil bath, adding 110 parts by weight of polymethylene polyphenyl polyisocyanate, and continuously stirring for 8s to obtain a polyurethane foaming liquid; the catalyst is an organic bismuth catalyst and triethylene diamine, and the mass ratio is 1: 1, compounding.
Paving a plurality of layers of glass fiber mats in a mold, injecting polyurethane foaming liquid into the mold, foaming and curing, curing at 70 ℃, and demolding to obtain a polyurethane heat-insulating layer; the glass fiber mat is 10 wt% of the polyurethane foaming liquid.
(3) Taking the bottom layer, the polyurethane heat-insulation board and the surface layer, gluing and compounding the surface layer, the polyurethane heat-insulation layer and the bottom layer from top to bottom to obtain a matrix, cutting and trimming the matrix, coating a fluorocarbon coating on the surface of one side of the matrix, which is close to the surface layer, and drying to obtain the composite heat-insulation board. The bottom layer is glass fiber mesh cloth, and the surface layer is a calcium silicate board.
Example 2:
a composite heat-insulation board for building external walls and a preparation method thereof comprise the following steps:
(1) uniformly mixing 1,3, 5-s-triazine triol and diethylenetriamine, heating to 125 ℃, adding ethanolamine, continuously heating to 205 ℃, stirring for 25min, adding a 5A molecular sieve, reacting for 4.5h under heat preservation, distilling under reduced pressure after the reaction is finished, and collecting a product to obtain the triazine polyol. The mol ratio of the 1,3, 5-s-triazine triol to the diethylenetriamine to the ethanolamine is 1: 1: 4; the dosage of the 5A molecular sieve is 25 wt% of 1,3, 5-s-triazine triol.
Taking trimethylolpropane, triazine polyol and N, N-dimethylformamide, uniformly stirring in a nitrogen environment, adding isophorone diisocyanate, and reacting at 85 ℃ for 55min to obtain a material A; the molar ratio of the total amount of the isophorone diisocyanate, the trimethylolpropane and the triazine polyol is 1: 2; the molar ratio of the trimethylolpropane to the triazine polyol is 1: 1.
adding mixed solution of isophorone diisocyanate and N, N-dimethylformamide into the material A, stirring at 85 ℃ for reacting for 45min, adding mixed solution of trimethylolpropane and N, N-dimethylformamide, keeping the temperature for continuing reacting for 1.2h, then adding mixed solution of triazine polyol and N, N-dimethylformamide, keeping the temperature for reacting for 45min, collecting a product after the reaction is finished, and evaporating a solvent to obtain flame-retardant polyol; the molar ratio of the material A to the isophorone diisocyanate to the trimethylolpropane to the triazine polyol is 1: 5: 1: 1.
(2) mixing 35 parts by weight of flame-retardant polyol, 65 parts by weight of polyether polyol, 7 parts by weight of foam stabilizer, 1.5 parts by weight of catalyst and 1.5 parts by weight of deionized water, stirring and mixing for 15min under the condition of oil bath at 45 ℃, adding 115 parts by weight of polymethylene polyphenyl polyisocyanate, and continuously stirring for 8s to obtain polyurethane foaming liquid; the catalyst is an organic bismuth catalyst and triethylene diamine, and the mass ratio is 1: 1, compounding.
Paving a plurality of layers of glass fiber mats in a mold, injecting polyurethane foaming liquid into the mold, foaming and curing, curing at 70 ℃, and demolding to obtain a polyurethane heat-insulating layer; the glass fiber mat is 10 wt% of the polyurethane foaming liquid.
(3) Taking the bottom layer, the polyurethane heat-insulation layer and the surface layer, gluing and compounding the surface layer, the polyurethane heat-insulation layer and the bottom layer in sequence from top to bottom to obtain a matrix, cutting and trimming the matrix, coating a fluorocarbon coating on the surface of one side of the matrix, which is close to the surface layer, and drying to obtain the composite heat-insulation board. The bottom layer is glass fiber mesh cloth, and the surface layer is a calcium silicate board.
Example 3:
a composite heat-insulation board for building external walls and a preparation method thereof comprise the following steps:
(1) uniformly mixing 1,3, 5-s-triazine triol and diethylenetriamine, heating to 130 ℃, adding ethanolamine, continuously heating to 210 ℃, stirring for 20min, adding a 5A molecular sieve, reacting for 5h under heat preservation, distilling under reduced pressure after the reaction is finished, and collecting a product to obtain the triazine polyol. The mol ratio of the 1,3, 5-s-triazine triol to the diethylenetriamine to the ethanolamine is 1: 1: 4; the dosage of the 5A molecular sieve is 25 wt% of 1,3, 5-s-triazine triol.
Uniformly stirring trimethylolpropane, triazine polyol and N, N-dimethylformamide in a nitrogen environment, adding isophorone diisocyanate, and reacting at 85 ℃ for 50min to obtain a material A; the molar ratio of the total amount of the isophorone diisocyanate, the trimethylolpropane and the triazine polyol is 1: 2; the molar ratio of the trimethylolpropane to the triazine polyol is 1: 1.
adding mixed solution of isophorone diisocyanate and N, N-dimethylformamide into the material A, stirring at 85 ℃ for reaction for 50min, adding mixed solution of trimethylolpropane and N, N-dimethylformamide, keeping the temperature for continuous reaction for 1.5h, then adding mixed solution of triazine polyol and N, N-dimethylformamide, keeping the temperature for reaction for 50min, collecting a product after the reaction is finished, and evaporating a solvent to obtain flame-retardant polyol; the molar ratio of the material A to isophorone diisocyanate to trimethylolpropane to triazine polyol is 1: 5: 1: 1.
(2) mixing 40 parts by weight of flame-retardant polyol, 60 parts by weight of polyether polyol, 8 parts by weight of foam stabilizer, 2 parts by weight of catalyst and 2 parts by weight of deionized water, stirring and mixing for 10min at 45 ℃ in an oil bath, adding 120 parts by weight of polymethylene polyphenyl polyisocyanate, and continuously stirring for 8s to obtain polyurethane foaming liquid; the catalyst is an organic bismuth catalyst and triethylene diamine, and the mass ratio is 1: 1, compounding.
Paving a plurality of layers of glass fiber mats in a mold, injecting polyurethane foaming liquid into the mold, foaming and curing, curing at 70 ℃, and demolding to obtain a polyurethane heat-insulating layer; the glass fiber mat is 10 wt% of the polyurethane foaming liquid.
(3) Taking the bottom layer, the polyurethane heat-insulation board and the surface layer, gluing and compounding the surface layer, the polyurethane heat-insulation layer and the bottom layer from top to bottom to obtain a matrix, cutting and trimming the matrix, coating a fluorocarbon coating on the surface of one side of the matrix, which is close to the surface layer, and drying to obtain the composite heat-insulation board. The bottom layer is glass fiber gridding cloth, and the surface layer is a calcium silicate board.
Example 4:
a composite heat-insulation board for building external walls and a preparation method thereof comprise the following steps:
(1) uniformly mixing 1,3, 5-s-triazine triol and diethylenetriamine, heating to 130 ℃, adding ethanolamine, continuously heating to 210 ℃, stirring for 20min, adding a 5A molecular sieve, reacting for 5h under heat preservation, distilling under reduced pressure after the reaction is finished, and collecting a product to obtain the triazine polyol. The mol ratio of the 1,3, 5-s-triazine triol to the diethylenetriamine to the ethanolamine is 1: 1: 4; the dosage of the 5A molecular sieve is 25 wt% of 1,3, 5-s-triazine triol.
Uniformly stirring trimethylolpropane, triazine polyol and N, N-dimethylformamide in a nitrogen environment, adding isophorone diisocyanate, and reacting at 85 ℃ for 50min to obtain a material A; the molar ratio of the total amount of the isophorone diisocyanate, the trimethylolpropane and the triazine polyol is 1: 2; the molar ratio of the trimethylolpropane to the triazine polyol is 1: 1.
adding mixed solution of isophorone diisocyanate and N, N-dimethylformamide into the material A, stirring at 85 ℃ for reaction for 50min, adding mixed solution of trimethylolpropane and N, N-dimethylformamide, keeping the temperature for continuous reaction for 1.5h, then adding mixed solution of triazine polyol and N, N-dimethylformamide, keeping the temperature for reaction for 50min, collecting a product after the reaction is finished, and evaporating a solvent to obtain flame-retardant polyol; the molar ratio of the material A to isophorone diisocyanate to trimethylolpropane to triazine polyol is 1: 5: 1: 1.
(2) mixing 40 parts by weight of flame-retardant polyol, 60 parts by weight of polyether polyol, 8 parts by weight of foam stabilizer, 2 parts by weight of catalyst and 2 parts by weight of deionized water, stirring and mixing for 10min at 45 ℃ in an oil bath, adding 120 parts by weight of polymethylene polyphenyl polyisocyanate, and continuously stirring for 8s to obtain polyurethane foaming liquid; the catalyst is an organic bismuth catalyst and triethylene diamine, and the mass ratio is 1: 1, compounding.
The method comprises the following steps of pretreating the glass fiber felt: soaking a glass fiber felt in a mixed solution of a KH-550 silane coupling agent, ethanol and deionized water for 10min, soaking the glass fiber felt in a mixed solution of isophorone diisocyanate and toluene at 85 ℃ for 20min, adding the material A, continuing to soak for 20min, and drying to obtain the pretreated glass fiber felt.
Paving a plurality of layers of glass fiber mats in a mold, injecting polyurethane foaming liquid into the mold, foaming and curing, curing at 70 ℃, and demolding to obtain a polyurethane heat-insulating layer; the glass fiber mat is 10 wt% of the polyurethane foaming liquid.
(3) Taking the bottom layer, the polyurethane heat-insulation board and the surface layer, gluing and compounding the surface layer, the polyurethane heat-insulation layer and the bottom layer from top to bottom to obtain a matrix, cutting and trimming the matrix, coating a fluorocarbon coating on the surface of one side of the matrix, which is close to the surface layer, and drying to obtain the composite heat-insulation board. The bottom layer is glass fiber mesh cloth, and the surface layer is a calcium silicate board.
Comparative example 1: comparative example 1 a control was carried out on the basis of example 3, in comparative example 1 no flame-retardant polyol was introduced, and the remaining process steps were unchanged.
A composite heat-insulation board for building external walls and a preparation method thereof comprise the following steps:
(1) mixing 100 parts of polyether polyol, 8 parts of foam stabilizer, 2 parts of catalyst and 2 parts of deionized water by weight, stirring and mixing for 10min under the condition of oil bath at 45 ℃, adding 120 parts of polymethylene polyphenyl polyisocyanate, and continuously stirring for 8s to obtain polyurethane foaming liquid; the catalyst is an organic bismuth catalyst and triethylene diamine, and the mass ratio is 1: 1, compounding.
Paving a plurality of layers of glass fiber mats in a mold, injecting polyurethane foaming liquid into the mold, foaming and curing, curing at 70 ℃, and demolding to obtain a polyurethane heat-insulating layer; the glass fiber mat accounts for 10 wt% of the polyurethane foaming liquid.
(2) Taking the bottom layer, the polyurethane heat-insulation board and the surface layer, gluing and compounding the surface layer, the polyurethane heat-insulation layer and the bottom layer from top to bottom to obtain a matrix, cutting and trimming the matrix, coating a fluorocarbon coating on the surface of one side of the matrix, which is close to the surface layer, and drying to obtain the composite heat-insulation board. The bottom layer is glass fiber mesh cloth, and the surface layer is a calcium silicate board.
Comparative example 2: comparative example 2 a control was carried out on the basis of example 3, comparative example 2 without the triazine polyol being introduced and the remaining process steps being unchanged.
A composite insulation board for building exterior walls and a preparation method thereof comprise the following steps:
(1) uniformly stirring trimethylolpropane and N, N-dimethylformamide under a nitrogen environment, adding isophorone diisocyanate, and reacting for 50min at 85 ℃ to obtain a material A; the molar ratio of the isophorone diisocyanate to the trimethylolpropane is 1: 2.
adding a mixed solution of isophorone diisocyanate and N, N-dimethylformamide into the material A, stirring at 85 ℃ for reacting for 50min, adding a mixed solution of trimethylolpropane and N, N-dimethylformamide, keeping the temperature, continuing to react for 1.5h, collecting a product after the reaction is finished, and evaporating a solvent to obtain flame-retardant polyol; the molar ratio of the material A to the isophorone diisocyanate to the trimethylolpropane is 1: 5: 2.
(2) mixing 40 parts by weight of flame-retardant polyol, 60 parts by weight of polyether polyol, 8 parts by weight of foam stabilizer, 2 parts by weight of catalyst and 2 parts by weight of deionized water, stirring and mixing for 10min at 45 ℃ in an oil bath, adding 120 parts by weight of polymethylene polyphenyl polyisocyanate, and continuously stirring for 8s to obtain polyurethane foaming liquid; the catalyst is an organic bismuth catalyst and triethylene diamine, and the mass ratio is 1: 1, compounding.
Paving a plurality of layers of glass fiber mats in a mold, injecting polyurethane foaming liquid into the mold, foaming and curing, curing at 70 ℃, and demolding to obtain a polyurethane heat-insulating layer; the glass fiber mat is 10 wt% of the polyurethane foaming liquid.
(3) Taking the bottom layer, the polyurethane heat-insulation board and the surface layer, gluing and compounding the surface layer, the polyurethane heat-insulation layer and the bottom layer from top to bottom to obtain a matrix, cutting and trimming the matrix, coating a fluorocarbon coating on the surface of one side of the matrix, which is close to the surface layer, and drying to obtain the composite heat-insulation board. The bottom layer is glass fiber gridding cloth, and the surface layer is a calcium silicate board.
Comparative example 3: comparative example 3 a control was carried out on the basis of example 3, in comparative example 3 no diethylenetriamine was introduced and the remaining process steps were unchanged.
A composite heat-insulation board for building external walls and a preparation method thereof comprise the following steps:
(1) adding ethanolamine into 1,3, 5-s-triazine triol, continuously heating to 210 ℃, stirring for 20min, adding a 5A molecular sieve, reacting for 5h under heat preservation, distilling under reduced pressure after the reaction is finished, and collecting a product to obtain the triazine polyol. The mol ratio of the 1,3, 5-s-triazine triol to the ethanolamine is 1: 4; the dosage of the 5A molecular sieve is 25 wt% of 1,3, 5-s-triazine triol.
Uniformly stirring trimethylolpropane, triazine polyol and N, N-dimethylformamide in a nitrogen environment, adding isophorone diisocyanate, and reacting at 85 ℃ for 50min to obtain a material A; the molar ratio of the total amount of the isophorone diisocyanate, the trimethylolpropane and the triazine polyol is 1: 2; the molar ratio of the trimethylolpropane to the triazine polyol is 1: 1.
adding mixed solution of isophorone diisocyanate and N, N-dimethylformamide into the material A, stirring at 85 ℃ for reaction for 50min, adding mixed solution of trimethylolpropane and N, N-dimethylformamide, keeping the temperature for continuous reaction for 1.5h, then adding mixed solution of triazine polyol and N, N-dimethylformamide, keeping the temperature for reaction for 50min, collecting a product after the reaction is finished, and evaporating a solvent to obtain flame-retardant polyol; the molar ratio of the material A to the isophorone diisocyanate to the trimethylolpropane to the triazine polyol is 1: 5: 1: 1.
(2) mixing 40 parts by weight of flame-retardant polyol, 60 parts by weight of polyether polyol, 8 parts by weight of foam stabilizer, 2 parts by weight of catalyst and 2 parts by weight of deionized water, stirring and mixing for 10min at 45 ℃ in an oil bath, adding 120 parts by weight of polymethylene polyphenyl polyisocyanate, and continuously stirring for 8s to obtain polyurethane foaming liquid; the catalyst is an organic bismuth catalyst and triethylene diamine, and the mass ratio is 1: 1, compounding.
Paving a plurality of layers of glass fiber mats in a mold, injecting polyurethane foaming liquid into the mold, foaming and curing, curing at 70 ℃, and demolding to obtain a polyurethane heat-insulating layer; the glass fiber mat is 10 wt% of the polyurethane foaming liquid.
(3) Taking the bottom layer, the polyurethane heat-insulation layer and the surface layer, gluing and compounding the surface layer, the polyurethane heat-insulation layer and the bottom layer in sequence from top to bottom to obtain a matrix, cutting and trimming the matrix, coating a fluorocarbon coating on the surface of one side of the matrix, which is close to the surface layer, and drying to obtain the composite heat-insulation board. The bottom layer is glass fiber mesh cloth, and the surface layer is a calcium silicate board.
Comparative example 4: comparative example 4 a control was carried out on the basis of example 3, in comparative example 4 no hyperbranched was carried out, and the remaining process steps were unchanged.
A composite insulation board for building exterior walls and a preparation method thereof comprise the following steps:
(1) uniformly mixing 1,3, 5-s-triazine triol and diethylenetriamine, heating to 130 ℃, adding ethanolamine, continuously heating to 210 ℃, stirring for 20min, adding a 5A molecular sieve, reacting for 5h under heat preservation, distilling under reduced pressure after the reaction is finished, and collecting a product to obtain the triazine polyol. The mol ratio of the 1,3, 5-s-triazine triol to the diethylenetriamine to the ethanolamine is 1: 1: 4; the dosage of the 5A molecular sieve is 25 wt% of 1,3, 5-s-triazine triol.
(2) Mixing 40 parts by weight of triazine polyol, 60 parts by weight of polyether polyol, 8 parts by weight of foam stabilizer, 2 parts by weight of catalyst and 2 parts by weight of deionized water, stirring and mixing for 10min at the temperature of 45 ℃ in an oil bath, adding 120 parts by weight of polymethylene polyphenyl polyisocyanate, and continuously stirring for 8s to obtain polyurethane foaming liquid; the catalyst is an organic bismuth catalyst and triethylene diamine, and the mass ratio of the organic bismuth catalyst to the triethylene diamine is 1: 1, compounding.
Paving a plurality of layers of glass fiber mats in a mold, injecting polyurethane foaming liquid into the mold, foaming and curing, curing at 70 ℃, and demolding to obtain a polyurethane heat-insulating layer; the glass fiber mat is 10 wt% of the polyurethane foaming liquid.
(3) Taking the bottom layer, the polyurethane heat-insulation board and the surface layer, gluing and compounding the surface layer, the polyurethane heat-insulation layer and the bottom layer from top to bottom to obtain a matrix, cutting and trimming the matrix, coating a fluorocarbon coating on the surface of one side of the matrix, which is close to the surface layer, and drying to obtain the composite heat-insulation board. The bottom layer is glass fiber gridding cloth, and the surface layer is a calcium silicate board.
Comparative example 5: comparative example 5a control was made on the basis of example 3, comparative example 5 does not limit the order of addition of trimethylolpropane and triazine polyol during branching, and the remaining process steps are unchanged.
A composite heat-insulation board for building external walls and a preparation method thereof comprise the following steps:
(1) uniformly mixing 1,3, 5-s-triazine triol and diethylenetriamine, heating to 130 ℃, adding ethanolamine, continuously heating to 210 ℃, stirring for 20min, adding a 5A molecular sieve, reacting for 5h under heat preservation, distilling under reduced pressure after the reaction is finished, and collecting a product to obtain the triazine polyol. The mol ratio of the 1,3, 5-s-triazine triol to the diethylenetriamine to the ethanolamine is 1: 1: 4; the dosage of the 5A molecular sieve is 25 wt% of 1,3, 5-s-triazine triol.
Uniformly stirring trimethylolpropane, triazine polyol and N, N-dimethylformamide in a nitrogen environment, adding isophorone diisocyanate, and reacting at 85 ℃ for 50min to obtain a material A; the molar ratio of the total amount of the isophorone diisocyanate, the trimethylolpropane and the triazine polyol is 1: 2; the molar ratio of the trimethylolpropane to the triazine polyol is 1: 1.
adding mixed solution of isophorone diisocyanate and N, N-dimethylformamide into the material A, stirring at 85 ℃ for reacting for 50min, adding mixed solution of trimethylolpropane, triazine polyol and N, N-dimethylformamide, keeping the temperature, continuing to react for 2.5h, collecting a product after the reaction is finished, and evaporating the solvent to obtain flame-retardant polyol; the molar ratio of the material A to the isophorone diisocyanate to the trimethylolpropane to the triazine polyol is 1: 5: 1: 1.
(2) mixing 40 parts by weight of flame-retardant polyol, 60 parts by weight of polyether polyol, 8 parts by weight of foam stabilizer, 2 parts by weight of catalyst and 2 parts by weight of deionized water, stirring and mixing for 10min at 45 ℃ in an oil bath, adding 120 parts by weight of polymethylene polyphenyl polyisocyanate, and continuously stirring for 8s to obtain polyurethane foaming liquid; the catalyst is an organic bismuth catalyst and triethylene diamine, and the mass ratio of the organic bismuth catalyst to the triethylene diamine is 1: 1, compounding.
Paving a plurality of layers of glass fiber mats in a mold, injecting polyurethane foaming liquid into the mold, foaming and curing, curing at 70 ℃, and demolding to obtain a polyurethane heat-insulating layer; the glass fiber mat is 10 wt% of the polyurethane foaming liquid.
(3) Taking the bottom layer, the polyurethane heat-insulation board and the surface layer, gluing and compounding the surface layer, the polyurethane heat-insulation layer and the bottom layer from top to bottom to obtain a matrix, cutting and trimming the matrix, coating a fluorocarbon coating on the surface of one side of the matrix, which is close to the surface layer, and drying to obtain the composite heat-insulation board. The bottom layer is glass fiber mesh cloth, and the surface layer is a calcium silicate board.
Detection experiment:
the heat-insulating board is prepared according to the preparation methods disclosed in the embodiments 1 to 4 and the comparative examples 1 to 5, the fluorocarbon coating is not coated during the test, and the performance of the obtained polyurethane heat-insulating layer is detected, wherein the specific detection method comprises the following steps:
1. according to GB/T8813-2008 "determination of compression Property of rigid foam", the detection temperature is 25 ℃, the load is 100N, the sample is a circular piece with a diameter of 50mm and a thickness of 50mm, the compression speed is 5mm/min, and the sample is compressed to 85% of the thickness during compression.
2. The tensile strength of the rigid foam is detected according to GB/T9641-1988 method for testing the tensile property of the rigid foam, the tensile speed is 5mm/min at 25 ℃, and the sample is a square sheet with the side length of 25mm and the thickness is 6.5 mm. The thermal conductivity is measured according to the standard disclosed in ASTM C518-2004 at a temperature of 25 ℃.
3. And detecting the limit oxygen index of the polyurethane heat-insulating layer and recording data.
Figure BDA0003733429070000121
And (4) conclusion: the invention discloses a composite insulation board for a building outer wall and a preparation method thereof, wherein the proportion of components in each level is appropriate, the process design is simple, the prepared composite insulation board is suitable for the field of insulation of the building outer wall, the flame retardant property is better, the mechanical property is ensured while the insulation property is considered, and the composite insulation board has higher practicability.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (8)

1. A preparation method of a composite insulation board for a building outer wall is characterized by comprising the following steps: the method comprises the following steps:
(1) uniformly stirring trimethylolpropane, triazine polyol and N, N-dimethylformamide under a nitrogen environment, adding isophorone diisocyanate, and reacting at 80-85 ℃ for 50-60min to obtain a material A;
adding mixed solution of isophorone diisocyanate and N, N-dimethylformamide into the material A, stirring and reacting for 40-50min, adding mixed solution of trimethylolpropane and N, N-dimethylformamide, continuing to react for 1-1.5h, then adding mixed solution of triazine polyol and N, N-dimethylformamide, reacting for 40-50min, collecting a product after the reaction is finished, and evaporating a solvent to obtain flame-retardant polyol;
(2) mixing flame-retardant polyol, polyether polyol, a foam stabilizer, a catalyst and deionized water, stirring and mixing for 10-20min under an oil bath at 40-45 ℃, adding polymethylene polyphenyl polyisocyanate, and continuously stirring for 6-10s to obtain a polyurethane foaming liquid;
paving a plurality of layers of glass fiber mats in a mold, injecting polyurethane foaming liquid into the mold, foaming and curing, curing at 70-80 ℃, and demolding to obtain a polyurethane heat-insulating layer;
(3) taking the bottom layer, the polyurethane heat-insulation board and the surface layer, gluing and compounding the surface layer, the polyurethane heat-insulation layer and the bottom layer from top to bottom to obtain a matrix, cutting and trimming the matrix, coating a fluorocarbon coating on the surface of one side of the matrix, which is close to the surface layer, and drying to obtain the composite heat-insulation board.
2. The preparation method of the composite insulation board for the building outer wall according to claim 1, characterized by comprising the following steps: in the step (2), the raw materials of each component comprise: 30-40 parts of flame-retardant polyol, 60-70 parts of polyether polyol, 6-8 parts of foam stabilizer, 1-2 parts of catalyst, 1-2 parts of deionized water and 120 parts of polymethylene polyphenyl polyisocyanate 110-.
3. The preparation method of the composite insulation board for the building outer wall according to claim 1, characterized by comprising the following steps: in the step (3), the bottom layer is glass fiber gridding cloth, and the surface layer is any one of a cement mortar layer, a cement fiber board and a calcium silicate board.
4. The preparation method of the composite insulation board for the building outer wall according to claim 1, characterized by comprising the following steps: in the step (1), the preparation steps of the triazine polyol are as follows: uniformly mixing 1,3, 5-s-triazine triol and diethylenetriamine, heating to 130 ℃ for heating to 120-.
5. The preparation method of the composite insulation board for the building outer wall according to claim 4, characterized by comprising the following steps: the mol ratio of the 1,3, 5-s-triazine triol to the diethylenetriamine to the ethanolamine is 1: 1: 4; the dosage of the 5A molecular sieve is 20-25 wt% of 1,3, 5-s-triazine triol.
6. The preparation method of the composite insulation board for the building outer wall according to claim 1, characterized by comprising the following steps: in the step (1), when the material A is prepared, the dosage of each component is as follows: the molar ratio of the total amount of the isophorone diisocyanate, the trimethylolpropane and the triazine polyol is 1: 2; the molar ratio of the trimethylolpropane to the triazine polyol is 1: 1.
7. the preparation method of the composite insulation board for the exterior wall of the building according to claim 1, characterized by comprising the following steps: in the step (1), when the flame-retardant polyol is prepared, the following components are used: the molar ratio of the material A to the isophorone diisocyanate to the trimethylolpropane to the triazine polyol is 1: 5: 1: 1.
8. the composite insulation board prepared by the preparation method of the composite insulation board for the building external wall according to any one of claims 1 to 7.
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