CN115305039A - Full-water foaming type damping fireproof adhesive and application thereof - Google Patents

Full-water foaming type damping fireproof adhesive and application thereof Download PDF

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Publication number
CN115305039A
CN115305039A CN202210925418.8A CN202210925418A CN115305039A CN 115305039 A CN115305039 A CN 115305039A CN 202210925418 A CN202210925418 A CN 202210925418A CN 115305039 A CN115305039 A CN 115305039A
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source
parts
weight
fire
retardant
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CN115305039B (en
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张武军
王书传
邬宵宵
陈鸿栅
何镕海
王诗榕
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XINHE NEW MATERIAL CO Ltd
Xinhe New Material Suzhou Co ltd
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XINHE NEW MATERIAL CO Ltd
Xinhe New Material Suzhou Co ltd
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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J175/00—Adhesives based on polyureas or polyurethanes; Adhesives based on derivatives of such polymers
    • C09J175/02—Polyureas
    • 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
    • C08G18/08—Processes
    • C08G18/10—Prepolymer processes involving reaction of isocyanates or isothiocyanates with compounds having active hydrogen in a first reaction step
    • 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
    • C08G18/42—Polycondensates having carboxylic or carbonic ester groups in the main chain
    • C08G18/4266—Polycondensates having carboxylic or carbonic ester groups in the main chain prepared from hydroxycarboxylic acids and/or lactones
    • C08G18/4269—Lactones
    • C08G18/4277—Caprolactone and/or substituted caprolactone
    • 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
    • C08G18/52—Polythioethers
    • 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
    • C08G18/65—Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
    • C08G18/66—Compounds of groups C08G18/42, C08G18/48, or C08G18/52
    • C08G18/6633—Compounds of group C08G18/42
    • C08G18/6637—Compounds of group C08G18/42 with compounds of group C08G18/32 or polyamines of C08G18/38
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    • 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
    • C08G18/65—Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
    • C08G18/66—Compounds of groups C08G18/42, C08G18/48, or C08G18/52
    • C08G18/6633—Compounds of group C08G18/42
    • C08G18/6637—Compounds of group C08G18/42 with compounds of group C08G18/32 or polyamines of C08G18/38
    • C08G18/6648—Compounds of group C08G18/42 with compounds of group C08G18/32 or polyamines of C08G18/38 with compounds of group C08G18/3225 or C08G18/3271 and/or polyamines of C08G18/38
    • C08G18/6651—Compounds of group C08G18/42 with compounds of group C08G18/32 or polyamines of C08G18/38 with compounds of group C08G18/3225 or C08G18/3271 and/or polyamines of C08G18/38 with compounds of group C08G18/3225 or polyamines of C08G18/38
    • 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
    • C08G18/65—Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
    • C08G18/66—Compounds of groups C08G18/42, C08G18/48, or C08G18/52
    • C08G18/6666—Compounds of group C08G18/48 or C08G18/52
    • C08G18/667—Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38
    • 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
    • C08G18/7614—Polyisocyanates or polyisothiocyanates cyclic aromatic containing only one aromatic ring
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    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02—Non-macromolecular additives
    • C09J11/04—Non-macromolecular additives inorganic
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02—Non-macromolecular additives
    • C09J11/06—Non-macromolecular additives organic
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
    • H01M50/10—Primary casings; Jackets or wrappings
    • H01M50/116—Primary casings; Jackets or wrappings characterised by the material
    • H01M50/124—Primary casings; Jackets or wrappings characterised by the material having a layered structure
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
    • H01M50/10—Primary casings; Jackets or wrappings
    • H01M50/14—Primary casings; Jackets or wrappings for protecting against damage caused by external factors
    • H01M50/141—Primary casings; Jackets or wrappings for protecting against damage caused by external factors for protecting against humidity
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
    • H01M50/10—Primary casings; Jackets or wrappings
    • H01M50/14—Primary casings; Jackets or wrappings for protecting against damage caused by external factors
    • H01M50/143—Fireproof; Explosion-proof
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/32—Phosphorus-containing compounds
    • C08K2003/321—Phosphates
    • C08K2003/322—Ammonium phosphate
    • C08K2003/323—Ammonium polyphosphate
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/38—Boron-containing compounds
    • C08K2003/387—Borates

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  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Fireproofing Substances (AREA)

Abstract

The invention discloses a full-water foaming type damping fireproof adhesive and application thereof. The raw materials of the all-water foaming type damping fire-proof adhesive comprise matrix resin, a trinity fire retardant, water and the like. The three-in-one flame retardant is formed by reacting at least three of a C source, an N source, a P source, a B source and a Si source. The matrix resin includes a polyurea resin. The fireproof glue does not contain a physical foaming agent harmful to the atmosphere, can be coated on the surface of a new energy battery pack or the surface and/or the interior of a new energy vehicle body to form a flame-retardant heat-insulation protection structure, has damping, shock-absorbing and sound-insulating functions in a normal environment, can provide a more comfortable passenger environment, can form a carbon layer with fireproof, heat-insulation and other functions due to thermal expansion under a fire condition, and can effectively guarantee the safety of vehicle passengers.

Description

Full-water foaming type damping fireproof adhesive and application thereof
Technical Field
The invention relates to the field of damping fireproof glue, in particular to full-water foaming type damping fireproof glue containing a trinity flame retardant, a preparation method of the full-water foaming type damping fireproof glue and application of the full-water foaming type damping fireproof glue to the surfaces of new energy battery packs and new energy vehicles.
Background
In recent years, the new energy vehicle industry has been rapidly developed, and the safety problem of the new energy battery pack has been receiving more and more attention. Generally, a lithium ion battery pack is used in a new energy automobile, and is prone to fire hazard when being squeezed by external force and thermally out of control. These fires may spread throughout the vehicle, placing the driver and passengers at risk. The electric automobile ignition accident caused by the thermal runaway of the battery pack indicates that the safety guarantee of passengers can be provided only by effectively protecting the battery unit, the battery pack and the automobile. However, the existing fire-proof schemes for new energy batteries and new energy vehicles have some defects, such as unsatisfactory fire-retardant performance, high cost, large occupied space, single function and the like. Therefore, how to develop a fireproof material with low cost, strong flame retardant property, small occupied space and multiple functions has become a difficult problem to be solved in the field.
Disclosure of Invention
The invention mainly aims to provide a full-water foaming type damping fireproof adhesive and application thereof, so as to overcome the defects of the prior art.
In order to achieve the purpose, the technical scheme adopted by the invention comprises the following steps:
one aspect of the invention provides a full-water foaming type damping fireproof adhesive which comprises the following raw materials in parts by weight: 50-70 parts of matrix resin, 20-30 parts of trinity flame retardant and 1-3 parts of water;
wherein the triune flame retardant is formed by the reaction of at least three of a C source, an N source, a P source, a B source, and a Si source.
In one embodiment, the method of preparing the trinomial flame retardant comprises: uniformly mixing 0-40 parts by weight of C source, 0-40 parts by weight of N source, 0-40 parts by weight of P source, 0-40 parts by weight of B source and 0-40 parts by weight of Si source at room temperature, wherein the using amount of at least three of the C source, the N source, the P source, the B source and the Si source is more than 0, and then kneading and reacting for 2-4h at 120-150 ℃.
Illustratively, the triune flame retardant is formed by reacting 20-40 parts by weight of a C source, 20-40 parts by weight of an N source and 30-40 parts by weight of a P source.
Illustratively, the triune flame retardant is formed by reacting 20-40 parts by weight of a B source, 20-40 parts by weight of an N source, and 30-40 parts by weight of a Si source.
Illustratively, the three-in-one flame retardant is formed by reacting 20 to 40 parts by weight of a C source, 20 to 40 parts by weight of an N source and 20 to 40 parts by weight of a B source.
Illustratively, the trinomial flame retardant is formed by reacting 20-40 parts by weight of an N source, 30-40 parts by weight of a P source and 20-40 parts by weight of an Si source.
The carbon residue rate of the two trinity flame retardants formed by the participation of the Si source is better than that of the other two trinity flame retardants without the participation of the Si source.
The above trinity flame retardant composed of different sources shows no significant difference in fire-retardant performance.
The C source, the N source, the P source, the B source, the Si source and the like react to form the trinity flame retardant, so that the respective flame-retardant and heat-insulating properties of the trinity flame retardant can be comprehensively exerted, the molecular weight of the trinity flame retardant is increased, the compatibility with a film-forming high-molecular substance is also greatly improved, the expansion flame-retardant and synergetic performance is better when the trinity flame retardant is fired, the pore diameter of a carbon layer is uniform and compact, and the fireproof and heat-insulating properties are better than those of the trinity flame retardant; and the attenuation rate of the fireproof performance is lower after the environmental aging.
In one embodiment, the C source includes any one or a combination of more of pentaerythritol, dipentaerythritol, neopentyl glycol, trimethylolpropane, and is not limited thereto.
In one embodiment, the N source includes any one or combination of melamine, dicyandiamide, ammonium polyphosphate, ammonium pentaborate, and is not limited thereto.
In one embodiment, the P source includes phosphorus pentoxide, phosphorus trioxide, ammonium polyphosphate, hydroxylated phosphate, and is not limited thereto.
In one embodiment, the Si source includes a combination of any one or more of ethyl silicate and its polymer, 3-aminopropyltriethoxysilane, (aminoethyl) aminopropyltrimethoxysilane, gamma-glycidoxypropyltrimethoxysilane, gamma-isocyanatopropyltriethoxysilane, 3- (acryloxy) propyltrimethoxysilane, without limitation.
In one embodiment, the B source includes any one or combination of boric acid, ammonium pentaborate, boron trioxide, borax pentahydrate, and is not limited thereto.
In one embodiment, the matrix resin comprises a polyurea resin formed primarily from the reaction of an isocyanate and an amine in a molar ratio of 3 to 6: 4 to 7.
In one embodiment, the amine includes any one or combination of diethyltoluenediamine, dimethylthiotoluenediamine, 4,4' -methylene-bis (3-chloro-2,6-diethylaniline), polyaspartic acid esters, and is not limited thereto.
In one embodiment, the isocyanate includes, but is not limited to, TDI-polythiol prepolymer or TDI-PCL prepolymer, wherein the weight average molecular weight of the polythiol or PCL is 1500-2000, and the NCO content of the TDI-polythiol prepolymer or TDI-PCL prepolymer is 6-10wt%.
In one embodiment, the method of preparing the isocyanate comprises: adding 1-1.5 parts by weight of polythiol or PCL into a reaction kettle, heating to 80-85 ℃ in protective atmosphere, adding 3-4 parts by weight of TDI, reacting for 2-3 h, adding a chain extender to adjust the content of NCO, reacting for 30min, cooling and discharging to obtain the isocyanate.
Further, the chain extender includes N, N' -diethyl-1,3-propanediamine (deppa), and is not limited thereto.
In one embodiment, the raw material of the all-water foaming type damping fire-proof glue comprises an A component and a B component; the component A comprises amine, a three-in-one flame retardant, water, reinforcing fibers which can be added or not added, and fillers which can be added or not added; the component B comprises isocyanate.
In one embodiment, the raw material of the fire-proof glue further comprises 1-3 parts by weight of reinforcing fiber and 10-15 parts by weight of filler.
Further, the reinforcing fiber includes at least one of a mineral fiber and a carbon fiber, and is not limited thereto.
Further, the filler includes any one or a combination of more of talc powder, quartz powder, titanium white, expandable graphite, and is not limited thereto.
Another aspect of the invention provides the use of the all-water foaming type damping fire-proof adhesive, for example, the use in the preparation of a new energy battery pack or a protective structure of a new energy vehicle. Specifically, the all-water foaming damping fireproof adhesive can be coated on a substrate to form a protective structure. The protective structure can be a protective layer on the surface of a new energy battery pack, a protective layer on the surface of an instrument panel, a decorative part and the like in the new energy vehicle,other protective structures are also possible, which have multiple functions, for example, CO formed by the reaction of water and isocyanate in the said all-water-blown damping fire-protection adhesive 2 The foaming agent enables the colloid to expand to form a pore damping structure, has a damping, shock-absorbing and sound-insulating function under a normal environment, provides a more comfortable passenger environment, and under a fire condition, the colloid continues to expand by heating to form a carbon-containing layer protection structure with a fireproof and heat-insulating function, so that the personal safety of vehicle passengers can be effectively protected.
Compared with the prior art, the all-water foaming type damping fireproof adhesive provided by the invention adopts polyurea resin as matrix resin, is added with the trinity flame retardant and water, and utilizes CO formed by the reaction of water and isocyanate 2 The foaming agent expands colloid to form a pore damping structure, so that the foaming agent is safe and environment-friendly, has damping, shock-absorbing and sound-insulating functions in normal environment, utilizes the characteristics that a trinity flame retardant has better resin component compatibility and better thermal expansion flame-retardant cooperativity and the like than an expansion flame-retardant system such as ammonium polyphosphate-pentaerythritol-melamine and the like, can enable the colloid to continue to expand under the condition of fire to form a carbon layer for fire prevention and heat insulation, avoids the phenomenon of nonuniform pores of the carbon layer, avoids the defects that the expansion flame-retardant system such as ammonium polyphosphate-pentaerythritol-melamine is easy to absorb moisture and cannot resist water and the like, has low attenuation rate of environmental aging fire-proof performance, and can more effectively protect the safety of vehicle occupants.
Particularly, the invention adopts the TDI-polythiol prepolymer and the TDI-PCL prepolymer to form the polyurea resin, compared with hydroxyl polyalcohol-PAPI type foaming polyurethane and the like, the polyurea resin has better fireproof and flame retardant performance, excellent strength and damping performance of a damp and hot circulating material, can fully meet the external burning requirement of a battery pack of GB38031-2020 and the like, and can greatly prolong or inhibit or even prevent the spread of fire under the condition of thermal runaway of the battery pack and provide more abundant rescue time.
Detailed Description
The following examples are provided to further understand the present invention, not to limit the scope of the present invention, but to provide the best mode, not to limit the content and the protection scope of the present invention, and any product similar or similar to the present invention, which is obtained by combining the present invention with other prior art features, falls within the protection scope of the present invention.
The examples do not show the specific experimental steps or conditions, and can be performed according to the conventional experimental steps described in the literature in the field. The reagents or instruments used are conventional reagent products which are commercially available, and manufacturers are not indicated.
Exemplary, the raw materials used in the following examples are as follows: the reinforced fiber is a product of Lapinus company, has the model number of MS610, and is amino silane surface treatment mineral fiber; the titanium white is a product of brocade titanium company, the model is CR506, and is silicon-aluminum and titanium white prepared by a special organic surface treatment chlorination method; the expandable graphite is an 80-mesh product of Qingdao Jin Tao graphite Co.
Embodiment 1 this example provides an all-water foaming type damping fire-proof adhesive, which comprises the following raw materials:
the component A is formed by uniformly mixing 80g of dimethylthiotoluenediamine, 90g of C-N-P-containing trinity flame retardant, 9g of reinforcing fiber, 45g of filler and 6g of water at a high speed and then filling;
and a B component comprising 70g of TDI-polythiol prepolymer.
During construction, the component A and the component B are mixed to obtain the full-water foaming type damping fire-proof adhesive.
The raw materials of the C-N-P-containing trinity flame retardant comprise dipentaerythritol, ammonium polyphosphate and melamine, and the specific preparation method comprises the following steps:
uniformly mixing 10 parts (by weight if not specifically stated below) of dipentaerythritol, 20 parts of ammonium polyphosphate and 10 parts of melamine in a mixer at 25 ℃, kneading the mixed materials on a steel kneader at 125 ℃ for 2 hours, and crushing and sieving to obtain the C-N-P-containing trinity flame retardant.
The preparation method of the TDI-polythiol prepolymer comprises the following steps: adding 100g of polythiol (Mw = 1500) into a reaction kettle, introducing nitrogen for protection, heating to 80 ℃, reacting for 2 hours after dropping 300g of TDI, adding DEPDA to adjust the NCO content to about 6wt% required, reacting for 30 minutes, cooling and discharging to obtain the TDI-polythiol prepolymer.
Comparative example 1 the raw materials of the all-water foaming type damping fire-proof adhesive provided by the comparative example are basically the same as those of the example 1, and the differences are that: a mixture (the total weight is 90 g) of dipentaerythritol, ammonium polyphosphate and melamine with the mass ratio of 1: 2: 1 replaces the C-N-P containing trinity flame retardant.
Comparative example 2 this comparative example provides a foamed fire-retardant adhesive which is substantially the same as example 1, except that: 150g of hydroxyl polyol-PAPI type foaming polyurethane replaces dimethylthiotoluenediamine in the component A, and the component B is omitted.
Embodiment 2 this example provides a full water foaming type damping fire-proof glue, and its raw materials include:
the component A is formed by uniformly mixing 80g of dimethylthiotoluenediamine, 40g of C-N-B-containing trinity flame retardant, 4g of reinforcing fiber, 20g of filler and 6g of water at a high speed and then filling;
and a component B comprising 60g of TDI-PCL prepolymer.
During construction, the component A and the component B are mixed to obtain the full-water foaming type damping fire-proof adhesive.
The raw materials of the C-N-B trinity flame retardant comprise trimethylolpropane, ammonium pentaborate and dicyandiamide, and the specific preparation method comprises the following steps:
uniformly mixing 10 parts of trimethylolpropane, 20 parts of ammonium pentaborate and 10 parts of dicyandiamide at 25 ℃ in a mixer; and kneading the mixed materials on a steel kneading machine at 150 ℃ for 3h, and crushing and sieving to obtain the C-N-B trinity flame retardant.
The preparation method of the TDI-PCL prepolymer comprises the following steps: adding 150g of PCL (Mw = 2000) into a reaction kettle, introducing nitrogen for protection, heating to 80 ℃, dropwise adding 300g of TDI, reacting for 2h, adding DEPDA to adjust the NCO content to about 8wt% as required, reacting for 30min, cooling and discharging to obtain the TDI-PCL prepolymer.
Comparative example 3 the raw materials of the all-water foaming type damping fire-proof adhesive provided by the comparative example are basically the same as those of the example 2, and the differences are that: a mixture of trimethylolpropane, ammonium pentaborate and dicyandiamide (total weight is 90 g) in a mass ratio of 1: 2: 1 is used to replace the C-N-B trinity flame retardant.
Embodiment 3 this example provides a full water foaming type damping fire-proof adhesive, its raw materials include:
the component A is formed by uniformly mixing 70g of polyaspartic acid ester, 50g of N-P-Si-containing trinity flame retardant, 2g of reinforcing fiber, 20g of filler and 2g of water at a high speed and then filling;
and a component B comprising 50g of TDI-PCL prepolymer.
During construction, the component A and the component B are mixed to obtain the full-water foaming type damping fire-proof adhesive.
The raw materials of the N-P-Si-containing trinity flame retardant comprise gamma-glycidyl ether oxypropyl trimethoxy silane, ammonium polyphosphate and melamine, and the specific preparation method comprises the following steps:
uniformly mixing 10 parts of ammonium polyphosphate, 5 parts of melamine and 3 parts of gamma-glycidyl ether oxypropyl trimethoxy silane at 25 ℃ in a mixer; and kneading the mixed materials on a steel kneader at 120 ℃ for 4 hours, and crushing and sieving to obtain the N-P-Si containing trinity flame retardant.
The preparation method of TDI-PCL prepolymer was the same as that of example 2.
Comparative example 4 the raw materials of the all-water foamed damping fire-proof adhesive provided by the comparative example are basically the same as those of the example 3, and the differences are that: the mixture (total weight is 90 g) of ammonium polyphosphate, melamine and gamma-glycidoxypropyltrimethoxysilane in the mass ratio of 10: 5: 3 replaces the trinity flame retardant containing N-P-Si.
Embodiment 4 this example provides an all water foaming type damping fire-proof adhesive, and its raw materials include:
the component A is formed by uniformly mixing 80g of 4,4' -methylene-bis (3-chloro-2,6-diethylaniline), 90g of B-N-Si-containing trinity flame retardant, 9g of reinforcing fiber, 45g of filler and 6g of water at a high speed and then filling;
and a component B, which comprises 70g of TDI-PCL prepolymer.
During construction, the component A and the component B are mixed to obtain the full-water foaming type damping fire-proof adhesive.
The raw materials of the B-N-Si-containing trinity flame retardant comprise boric acid, (aminoethyl) aminopropyltrimethoxysilane and melamine, and the specific preparation method comprises the following steps:
uniformly mixing 10 parts of boric acid, 5 parts of melamine and 3 parts of (aminoethyl) aminopropyltrimethoxysilane in a mixer at room temperature; and kneading the mixed materials on a steel kneader at 140 ℃ for 2 hours, and crushing and sieving to obtain the B-N-Si containing trinity flame retardant.
The preparation method of the TDI-PCL prepolymer comprises the following steps: adding 100g of PCL (Mw = 2000) into a reaction kettle, introducing nitrogen for protection, heating to 85 ℃, dropwise adding 400g of TDI, reacting for 2h, adding DEPDA to adjust the NCO content to be about 10wt% as required, reacting for 30min, cooling and discharging to obtain the TDI-PCL prepolymer.
Comparative example 5 the raw materials of the all-water foamed damping fire-proof adhesive provided by the comparative example are basically the same as those of example 4, and the differences are that: the mixture of boric acid, (aminoethyl) aminopropyltrimethoxysilane and melamine (total weight is 90 g) with the mass ratio of 10: 5: 3 replaces the B-N-Si containing triune flame retardant.
The fire-retardant adhesive obtained in examples 1 to 4 of the present invention and the fire-retardant adhesive obtained in comparative examples 1 to 5 were subjected to fire-retardant property and damping property tests, and the test results are shown in table 1. The fire resistance test is carried out according to GB38031-2020, the damping performance test is carried out according to GB/T18258, the high and low temperature resistant cycle alternation test is carried out according to Q/CR546.3, the water resistance test is carried out according to GB/T1733-1993, the adhesion test is carried out according to GB/T5210-2006, and the carbon residue content is measured according to GB17144 petroleum product carbon residue measurement method (micro method).
TABLE 1 test results of performance of fire-retardant adhesive of examples 1-4 and comparative examples 1-5
Figure BDA0003780015830000071
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications therefrom are within the scope of the invention.

Claims (10)

1. The all-water foaming type damping fireproof adhesive is characterized by comprising the following components in parts by weight: 50-70 parts of matrix resin, 20-30 parts of trinity flame retardant and 1-3 parts of water;
wherein the tri-integral flame retardant is formed by reacting at least three of a C source, an N source, a P source, a B source and a Si source.
2. The all-water foaming damping fire-proof adhesive according to claim 1, wherein the preparation method of the trinity fire retardant comprises the following steps: uniformly mixing 0-40 parts by weight of C source, 0-40 parts by weight of N source, 0-40 parts by weight of P source, 0-40 parts by weight of B source and 0-40 parts by weight of Si source at room temperature, wherein the using amount of at least three of the C source, the N source, the P source, the B source and the Si source is more than 0, and then kneading and reacting for 2-4h at 120-150 ℃.
3. The all-water foaming damping fire-retardant adhesive according to claim 1 or 2, wherein the triune fire-retardant is formed by the reaction of 20 to 40 parts by weight of a C source, 20 to 40 parts by weight of an N source and 30 to 40 parts by weight of a P source; or the three-in-one flame retardant is formed by the reaction of 20 to 40 parts by weight of a B source, 20 to 40 parts by weight of an N source and 30 to 40 parts by weight of a Si source; or the three-in-one flame retardant is formed by the reaction of 20 to 40 parts by weight of a C source, 20 to 40 parts by weight of an N source and 20 to 40 parts by weight of a B source; or the three-in-one flame retardant is formed by the reaction of 20 to 40 parts by weight of an N source, 30 to 40 parts by weight of a P source and 20 to 40 parts by weight of an Si source.
4. The all-water foaming damping fire-retardant adhesive of claim 1 or 2, wherein the C source comprises any one or combination of pentaerythritol, dipentaerythritol, neopentyl glycol, trimethylolpropane;
and/or the N source comprises any one or more of melamine, dicyandiamide, ammonium polyphosphate and ammonium pentaborate;
and/or the P source comprises phosphorus pentoxide, phosphorus trioxide, ammonium polyphosphate and hydroxylated phosphate;
and/or the Si source comprises the combination of any one or more of ethyl silicate and polymers thereof, 3-aminopropyl triethoxysilane, (aminoethyl) aminopropyl trimethoxysilane, gamma-glycidoxypropyl trimethoxysilane, gamma-isocyanopropyltriethoxysilane and 3- (acryloyloxy) propyltrimethoxysilane;
and/or the B source comprises any one or more of boric acid, ammonium pentaborate, boron trioxide and borax pentahydrate.
5. The all-water foamable damping fire-retardant adhesive according to claim 1, wherein the matrix resin comprises a polyurea resin formed mainly by reacting isocyanate and amine in a molar ratio of 3 to 6: 4 to 7.
6. The all-water intumescent damping fire gum of claim 5, wherein the amine comprises any one or combination of diethyltoluenediamine, dimethylthiotoluenediamine, 4,4' -methylene-bis (3-chloro-2,6-diethylaniline), polyaspartic acid ester;
and/or the isocyanate comprises TDI-polythiol prepolymer or TDI-PCL prepolymer, wherein the weight average molecular weight of polythiol or PCL is 1500-2000, and the NCO content of the TDI-polythiol prepolymer or TDI-PCL prepolymer is 6-10wt%.
7. The all-water foaming type damping fire-proof adhesive according to claim 6, wherein the preparation method of the isocyanate comprises the following steps: adding 1-1.5 parts by weight of polythiol or PCL into a reaction kettle, heating to 80-85 ℃ in a protective atmosphere, adding 3-4 parts by weight of TDI, reacting for 2-3 h, adding a chain extender to adjust NCO content, reacting for 30min, and then cooling and discharging to obtain the isocyanate;
wherein the chain extender comprises N, N' -diethyl-1,3-propanediamine.
8. The all-water foaming damping fire-proof adhesive according to claim 1, wherein the raw materials of the fire-proof adhesive further comprise 1-3 parts by weight of reinforcing fibers and 10-15 parts by weight of fillers;
the reinforcing fibers comprise at least one of mineral fibers and carbon fibers; the filler comprises any one or combination of more of talcum powder, quartz powder, titanium dioxide and expandable graphite.
9. The all-water foaming type fire-retardant damping glue according to any one of claims 5 to 7, wherein the raw materials of the all-water foaming type fire-retardant damping glue comprise an A component and a B component; the component A comprises amine, a three-in-one flame retardant, water, reinforcing fibers which can be added or not added, and fillers which can be added or not added; the component B comprises isocyanate.
10. Use of the all-water foaming damping fire-retardant adhesive according to any one of claims 1 to 9 in the preparation of a new energy battery pack or a protective structure of a new energy vehicle.
CN202210925418.8A 2022-08-03 2022-08-03 All-water foaming type damping fireproof adhesive and application thereof Active CN115305039B (en)

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