CN112430378A - Fireproof composition and preparation method and application thereof - Google Patents
Fireproof composition and preparation method and application thereof Download PDFInfo
- Publication number
- CN112430378A CN112430378A CN202011285995.2A CN202011285995A CN112430378A CN 112430378 A CN112430378 A CN 112430378A CN 202011285995 A CN202011285995 A CN 202011285995A CN 112430378 A CN112430378 A CN 112430378A
- Authority
- CN
- China
- Prior art keywords
- parts
- mass
- fireproof
- composition
- preparation
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L61/00—Compositions of condensation polymers of aldehydes or ketones; Compositions of derivatives of such polymers
- C08L61/34—Condensation polymers of aldehydes or ketones with monomers covered by at least two of the groups C08L61/04, C08L61/18 and C08L61/20
-
- 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
- C08G14/00—Condensation polymers of aldehydes or ketones with two or more other monomers covered by at least two of the groups C08G8/00 - C08G12/00
- C08G14/02—Condensation polymers of aldehydes or ketones with two or more other monomers covered by at least two of the groups C08G8/00 - C08G12/00 of aldehydes
- C08G14/04—Condensation polymers of aldehydes or ketones with two or more other monomers covered by at least two of the groups C08G8/00 - C08G12/00 of aldehydes with phenols
- C08G14/12—Chemically modified polycondensates
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/22—After-treatment of expandable particles; Forming foamed products
- C08J9/224—Surface treatment
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/22—After-treatment of expandable particles; Forming foamed products
- C08J9/228—Forming foamed products
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2325/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring; Derivatives of such polymers
- C08J2325/02—Homopolymers or copolymers of hydrocarbons
- C08J2325/04—Homopolymers or copolymers of styrene
- C08J2325/06—Polystyrene
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2461/00—Characterised by the use of condensation polymers of aldehydes or ketones; Derivatives of such polymers
- C08J2461/34—Condensation polymers of aldehydes or ketones with monomers covered by at least two of the groups C08J2461/04, C08J2461/18, and C08J2461/20
-
- 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
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2217—Oxides; Hydroxides of metals of magnesium
- C08K2003/2224—Magnesium hydroxide
-
- 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
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2296—Oxides; Hydroxides of metals of zinc
-
- 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
- C08K2003/382—Boron-containing compounds and nitrogen
- C08K2003/385—Binary compounds of nitrogen with boron
-
- 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
-
- 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
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- General Chemical & Material Sciences (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Fireproofing Substances (AREA)
Abstract
The invention relates to the field of materials, in particular to a fireproof composition and a preparation method and application thereof. The invention provides a fireproof composition which is a liquid dispersion system comprising the following components in parts by mass: 18-35 parts of modified phenolic resin, 0.5-1.2 parts of polyurethane, 0.5-1.2 parts of fluorinated polyurethane, and 5-13 parts of heat-conducting filler and flame retardant. The surface of the fireproof composition film prepared by the invention reaches a super-hydrophobic state, the porosity of the film is increased, the moisture transmission rate of the microporous film is increased, and the evaporation and release of moisture are accelerated, so that the air permeability of the fireproof composition film is improved, the fireproof composition material can easily transmit heat through air flow, the self-cooling function in a high-temperature environment is realized, and the energy consumption is effectively saved; and the fireproof composition has a self-cooling function, maintains good flame retardant property, and can reach the requirement of B1 level.
Description
Technical Field
The invention relates to the field of materials, in particular to a fireproof composition and a preparation method and application thereof.
Background
At present, 15% of the global power consumption comes from a cooling system, which causes a great energy crisis, so that people have conducted a great deal of research on how to reduce the energy consumption in the aspect of cooling, and develop some materials capable of realizing self-cooling so as to relieve the energy consumption pressure.
Materials with fireproof performance are widely applied in daily life, however, the existing fireproof materials do not have the function of self-cooling, and after the fireproof materials are used for decoration, the fireproof materials can bring great burden to an electric power system at high temperature in summer.
Disclosure of Invention
Therefore, there is a need for a fireproof composition with self-cooling function and better flame retardancy, and a preparation method and an application thereof.
In one aspect of the invention, a fire-retardant composition is provided, which is a liquid dispersion system comprising the following components in parts by mass:
in one embodiment, the modified phenolic resin is prepared from the following components in parts by mass:
the preparation method comprises the following steps: adding the phenol into a reaction container, adding part of the formaldehyde, the dicyandiamide and part of the catalyst at the rotating speed of 800-1000 r/min, heating to 65-75 ℃ within 30min, and keeping the temperature for 10-20 min;
heating to 80-100 ℃ within 40min, preserving heat for 15-25 min, then cooling to 60-65 ℃, and then adding the rest of formaldehyde, the rest of catalyst and the water;
heating to 80-100 ℃ within 20min, and maintaining the viscosity at 3000-5000 mpa-s;
adding the 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide and the ether solvent, heating to 110-130 ℃, preserving the heat for 1.5-2.5 h, and then cooling to room temperature.
In one embodiment, the catalyst is Ba (OH)2·8H2O, NaOH; the preparation components of the modified phenolic resin also comprise 2-10 parts by mass of aqueous hydrogen peroxide, wherein the mass fraction of the aqueous hydrogen peroxide is 10-14%; in the preparation process, the aqueous hydrogen peroxide solution and the ether solvent are added together; the preparation components of the modified phenolic resin also comprise 5-15 parts by mass of methanol aqueous solution, wherein the mass fraction of the methanol aqueous solution is 9-12%; in the preparation process, the methanol aqueous solution and the dicyandiamide are added together.
In one embodiment, the main component of the nanoscale heat-conducting filler is at least one of boron nitride, zinc oxide and vitrified micro bubbles; the flame retardant is at least one of graphite, magnesium hydroxide, red phosphorus, triphenyl phosphate, zinc borate and ammonium polyphosphate; the flame retardant is 10-21 parts by mass.
In one embodiment, the halogen-free; the emulsion also comprises 4-12 parts by mass of emulsion, wherein the emulsion is at least one of styrene-acrylic emulsion and pure acrylic emulsion.
In one embodiment, the pH of the fire-retardant composition is 8-9.
According to the invention, a certain mass part of modified phenolic resin, polyurethane, fluorinated polyurethane, heat-conducting filler and flame retardant are mixed, so that the surface roughness of the prepared fireproof composition film is increased, a super-hydrophobic state is achieved, the contact area with water drops is reduced, the porosity of the film is increased, the moisture transmission rate of a microporous film is increased, the evaporation and release of moisture are accelerated, the air permeability is improved, the fireproof composition material can easily transmit heat through air flow, the self-cooling function in a high-temperature environment is realized, and the energy consumption is effectively saved; and the fireproof composition has a self-cooling function, maintains good flame retardant property, and can reach the requirement of B1 level.
In another aspect of the invention, a TPS board is provided, which comprises expandable polystyrene beads and a fire-retardant component coated on the surfaces of the expandable polystyrene beads;
the fireproof component is obtained by drying the fireproof composition.
The invention also provides a preparation method of the TPS plate, which comprises the following steps:
pre-foaming polystyrene beads, coating and wrapping the fireproof composition, adding a curing agent, and uniformly stirring to obtain a mixture;
and drying and forming the mixture.
In one embodiment, the polystyrene beads are used in an amount of 20 to 40 parts by mass, the fireproof composition is used in an amount of 180 to 200 parts by mass, and the curing agent is used in an amount of 2 to 10 parts by mass.
In one embodiment, 5-9 parts by mass of Ca (OH) are added after the mixture is obtained2Aqueous solution of said Ca (OH)2The mass fraction of the aqueous solution is 1-3%.
Detailed Description
In order that the invention may be more fully understood, reference will now be made to the accompanying examples. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Furthermore, the terms "first", "second" and "first" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include at least one such feature. In the description of the invention, "a plurality" means at least two, e.g., two, three, etc., unless explicitly specified otherwise. In the description of the present invention, "a plurality" means at least one, e.g., one, two, etc., unless specifically limited otherwise.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
The invention provides a fireproof composition which is a liquid dispersion system comprising the following components in parts by mass:
preferably, the fire-retardant composition is a liquid dispersion comprising, in parts by mass:
further preferably, the fire-retardant composition is a liquid dispersion comprising, in parts by mass:
within the preset mass part range, certain modified phenolic resin, polyurethane, fluorinated polyurethane, heat-conducting filler and flame retardant are mixed, so that the surface roughness of the prepared fireproof composition film is increased, a super-hydrophobic state is achieved, the contact area with water drops is reduced, the porosity of the film is increased, the moisture transmission rate of a microporous film is increased, the evaporation and release of moisture are accelerated, the air permeability of the fireproof composition film is improved, the fireproof composition material can easily transmit heat through air flow, the self-cooling function in a high-temperature environment is realized, and the energy consumption is effectively saved; and the fireproof composition has a self-cooling function, maintains good flame retardant property, has an oxygen index LOI of over 32 percent, and meets the requirement of a fireproof flame retardant B1 grade.
In one specific example, the modified phenolic resin is prepared from the following components in parts by mass:
preferably, the modified phenolic resin is prepared from the following components in parts by mass:
further preferably, the modified phenolic resin is prepared from the following components in parts by mass:
the preparation method comprises the following steps: adding phenol into a reaction container, adding part of formaldehyde, dicyandiamide and part of catalyst at the rotating speed of 800 r/min-1000 r/min, then heating to 65-75 ℃ within 30min, and preserving heat for 10-20 min;
heating to 80-100 ℃ within 40min, preserving heat for 15-25 min, then cooling to 60-65 ℃, and then adding the rest of formaldehyde, the rest of catalyst and water;
heating to 80-100 ℃ within 20min, and maintaining the viscosity at 3000-5000 mpa-s;
adding 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide and ether solvent, heating to 110-130 ℃, keeping the temperature for 1.5-2.5 h, and cooling to room temperature.
In a preset mass part range, formaldehyde, phenol and dicyandiamide can react to generate dicyandiamide phenolic resin, and 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO) and carbon-nitrogen triple bond in the dicyandiamide phenolic resin generate addition reaction through P-H bond of the DOPO and the dicyandiamide phenolic resin to realize modification of the dicyandiamide phenolic resin; DOPO is easy to generate oxidation pyrolysis reaction in the air to generate oxyacid of phosphorus, and the oxyacid is solidified on the surface of the resin to isolate oxygen and promote the dehydration and carbonization of the solidified resin to form a carbonized layer, so that the flame retardant property of the phenolic resin can be effectively improved; in addition, through modification, the content of phosphorus and nitrogen in the system is improved, the heat release rate of the system is further reduced, and the flame retardant property of the material is also improved to a certain extent.
In one specific example, the catalyst in the modified phenolic resin is Ba (OH)2·8H2O, NaOH. Reasonable catalyst type and dosage can enable the catalytic action to be moderate, the reaction is easy to control, the probability of free phenol being oxidized into quinone is reduced, the material is not easy to discolor, the absorbance of the resin liquid is maintained in a lower range, and the resin liquid can be applied to light color decoration scenes.
In a specific example, the preparation components of the modified phenolic resin further comprise 2-10 parts by mass of aqueous hydrogen peroxide, and the mass fraction of the aqueous hydrogen peroxide is 10-14%; in the preparation process, the aqueous hydrogen peroxide solution and the ether solvent are added together. The hydrogen peroxide has a bleaching effect, can decompose colored quinone groups to lighten the color of the phenolic resin, and the reaction product is mainly water, so that the environmental pollution can not be caused, and meanwhile, the performance of the material such as wet strength and the like can not be adversely affected within a reasonable dosage range.
In a specific example, the preparation components of the modified phenolic resin further comprise 5-15 parts by mass of a methanol aqueous solution, wherein the mass fraction of the methanol aqueous solution is 9-12%; in the preparation process, methanol aqueous solution and dicyandiamide are added together. The addition of a certain mass portion of methanol to the modified phenolic resin can maintain the curing reaction rate at a reasonable level, so that the composition is easier to store and transport and can be conveniently applied to the production of subsequent downstream products.
In one specific example, the nanoscale thermally conductive filler is at least one of boron nitride, zinc oxide, and vitrified micro bubbles. The compounding of the heat-conducting filler, the polyurethane and the fluorinated polyurethane can increase the surface roughness Ra value of the film after the film is formed by the material, the film is converted into a super-hydrophobic state, the contact area with water drops is reduced, the porosity of the film is increased, the moisture transmission rate of the microporous film is increased, the evaporation and release of moisture are accelerated, the air permeability is improved, the fireproof composition material can easily transmit heat through air flow, the self-cooling function in a high-temperature environment is realized, and the energy consumption is effectively saved.
In a specific example, the flame retardant is at least one of graphite, magnesium hydroxide, red phosphorus, triphenyl phosphate, zinc borate, and ammonium polyphosphate. The flame retardant is used, so that the flame retardant property of the material can be further improved.
In a specific example, the amount of the flame retardant is 10 to 21 parts by mass.
In a specific example, the liquid crystal display further comprises 1-6 parts by mass of acyl halide, wherein the acyl halide is at least one of acetyl chloride, benzoyl chloride and oxalic acid chloride. The acyl halide can perform esterification reaction with phenolic hydroxyl to protect the phenolic hydroxyl, so that the phenomenon that free phenolic hydroxyl is oxidized into quinone or other structures to cause material discoloration is avoided, and the application of the material in light-colored decorative scenes is limited. To prevent the discoloration of phenolic resin, the traditional method is to prevent oxidation by brushing an isolation layer outside, so that the subsequent construction is complex, the oxidation layer can be brushed repeatedly, and the heat dissipation effect of the material can be influenced. By adding acyl halide, phenolic hydroxyl is protected, and the material can be modified radically, so that the material is not easy to discolor even if the material is used for a long time or washed by a large amount of rainwater.
In a specific example, the emulsion further comprises 4-12 parts by mass of emulsion, wherein the emulsion is at least one of styrene-acrylic emulsion and pure acrylic emulsion. The emulsion can promote the film forming process of the composition, help the material film forming to have higher porosity and moisture transmission rate, further improve the air permeability of the material, enable the material to better transfer heat and realize the self-cooling function.
In one specific example, the pH of the fire-protecting composition is 8 to 9. The pH value of the fireproof composition is maintained in the range, so that the phenolic hydroxyl in the material is not easy to dissociate and is oxidized into quinone under the condition that the physical properties are not influenced, and the material is not easy to discolor after being used for a long time.
According to the invention, a certain mass part of modified phenolic resin, polyurethane, fluorinated polyurethane, heat-conducting filler and flame retardant are mixed, so that the surface roughness of the prepared fireproof composition film is increased, a super-hydrophobic state is achieved, the contact area with water drops is reduced, the porosity of the film is increased, the moisture transmission rate of a microporous film is increased, the evaporation and release of moisture are accelerated, the air permeability is improved, the fireproof composition material can easily transmit heat through air flow, the self-cooling function in a high-temperature environment is realized, and the energy consumption is effectively saved; and the fireproof composition has a self-cooling function, maintains good flame retardant property, has an oxygen index LOI of over 32 percent, and meets the requirement of a fireproof flame retardant B1 grade.
The invention also provides a TPS plate which comprises the expandable polystyrene beads and a fireproof component coated on the surfaces of the expandable polystyrene beads;
the fireproof component is obtained by drying the fireproof composition.
The invention also provides a preparation method of the TPS plate, which comprises the following steps:
pre-foaming polystyrene beads, coating and wrapping the fireproof composition, adding a curing agent, and uniformly stirring to obtain a mixture;
and drying the mixture, screening particles, forming, aging, and cutting according to requirements after aging to obtain the TPS plate finished product.
In a specific example, the curing agent is at least one of benzenesulfonic acid, phenolsulfonic acid, sodium petroleum sulfonate and phosphoric acid.
In one specific example, the polystyrene beads are used in an amount of 20 to 40 parts by mass, the fire-retardant composition is used in an amount of 180 to 200 parts by mass, and the curing agent is used in an amount of 2 to 10 parts by mass.
In a specific example, 5 to 9 parts by mass of Ca (OH) is added after the mixture is obtained2Aqueous solution, Ca (OH)2The mass fraction of the aqueous solution is 1-3%. A certain amount of Ca (OH)2The aqueous solution can neutralize the excessive acid in the curing agent, reduce the generation of free phenolic hydroxyl, and further prevent the material from being easily subjected to oxidation reaction to cause color change.
The present invention will be described in further detail with reference to specific examples and comparative examples. It is understood that the following examples are more specific to the apparatus and materials used, and in other embodiments, are not limited thereto.
Examples of fire-retardant compositions, comparative examples:
TABLE 1
TABLE 2
| Comparative example | 1 | 2 | 3 | 4 | 5 |
| Modified phenolic resin | 20 | 20 | 20 | 20 | 20 |
| Polyurethane | 0.4 | 1.5 | 0.4 | 0.5 | 0.5 |
| Fluorinated polyurethanes | 0.4 | 1.5 | 1.5 | 0.5 | 0.5 |
| Boron nitride | 4 | 13.5 | 4 | 4 | 13.5 |
| Graphite (II) | 0.1 | 0.1 | 0.1 | 0.1 | 0.1 |
| Magnesium hydroxide | 10 | 10 | 10 | 10 | 10 |
Characterization test:
preparation of TPS plates:
taking 30 parts by mass of polystyrene beads for pre-foaming, coating and wrapping the fireproof compositions shown in the examples in table 1 and the comparative examples in table 2, adding 6 parts by mass of curing agent, and uniformly stirring to obtain a mixture; the mixture was oven dried, granulated, formed, then aged and cut to yield the finished TPS boards as listed in table 3.
TABLE 3
As can be seen from Table 3, the flame retardant property of the embodiment of the invention is good, the oxygen index LOI can reach more than 32%, and the requirement of the B1-grade fireproof material on the flame retardant property is met; physical properties such as tensile strength and bending strength are also better represented; the moisture transmission rate of the microfilm is correspondingly improved along with the increase of the roughness and the porosity of the board surface, which shows that the improvement of the roughness and the porosity of the board surface in a certain range is beneficial to the evaporation and the release of water and the self-cooling effect of the material is improved; in comparative examples 1, 3 and 4, the use amount of polyurethane, fluorinated polyurethane or boron nitride is small or the collocation is unbalanced, so that the plate surface roughness and the porosity of the material are too low, the moisture transmission rate and the heat conductivity coefficient of the microfilm are too low, and the self-cooling performance of the material is influenced; in comparative examples 2 and 5, the use amount of polyurethane, fluorinated polyurethane or boron nitride is too large or the collocation is unbalanced, so that the volume water absorption of the material is greatly increased, and the storage and transportation of the material are not facilitated; meanwhile, the flame retardant property of the material is negatively influenced, the oxygen index LOI in the comparative example is lower than 30%, the requirement of B1-grade flame retardant property cannot be met, the material can be combusted to a certain extent, and the material has great potential safety hazard when being used for flame retardance.
Modified phenolic resin examples, comparative examples and characterization tests:
TABLE 4
TABLE 5
| Comparative example | 6 | 7 | 8 | 9 |
| Formaldehyde (I) | 32 | 32 | 32 | 32 |
| Phenol and its preparation | 24 | 24 | 24 | 24 |
| Water (W) | 10 | 10 | 10 | 10 |
| Dicyandiamide | 6 | 16 | 7 | 7 |
| DOPO | 3 | 3 | 6 | 16 |
| Ethylene glycol methyl ether | 5 | 5 | 5 | 5 |
| Ba(OH)2·8H2O | 4 | 4 | 4 | 4 |
TABLE 6
As can be seen from Table 6, the modified phenolic resins prepared in examples 6-10 have balanced properties, and the properties such as viscosity, solid content, activity time, water solubility ratio and wet strength can reach better levels, and meanwhile, the flame retardant property is greatly improved, and the LOI value of the oxygen index can reach more than 32%, so that the flame retardant property required by B1 level is realized. In comparative examples 6 and 8, the dosage of dicyandiamide and DOPO is less, which directly causes the flame retardant property of the modified phenolic resin to be reduced to below B1 level; in comparative examples 7 and 9, the use of dicyandiamide and DOPO in a larger amount affects the activity time and the water solubility of the phenolic resin.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (10)
1. The fireproof composition is characterized by comprising the following components in parts by mass:
2. the fireproof composition according to claim 1, wherein the modified phenolic resin is prepared from the following components in parts by mass:
the preparation method comprises the following steps: adding the phenol into a reaction container, adding part of the formaldehyde, the dicyandiamide and part of the catalyst at the rotating speed of 800-1000 r/min, heating to 65-75 ℃ within 30min, and keeping the temperature for 10-20 min;
heating to 80-100 ℃ within 40min, preserving heat for 15-25 min, then cooling to 60-65 ℃, and then adding the rest of formaldehyde, the rest of catalyst and the water;
heating to 80-100 ℃ within 20min, and maintaining the viscosity at 3000-5000 mpa-s;
adding the 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide and the ether solvent, heating to 110-130 ℃, preserving the heat for 1.5-2.5 h, and then cooling to room temperature.
3. A fire-retardant composition according to claim 2, wherein said catalyst is ba (oh)2·8H2O, NaOH; the preparation components of the modified phenolic resin also comprise 2-10 parts by mass of aqueous hydrogen peroxide, wherein the mass fraction of the aqueous hydrogen peroxide is 10-14%; in the preparation process, the aqueous hydrogen peroxide solution and the ether solvent are added together; the preparation components of the modified phenolic resin also comprise 5-15 parts by mass of methanol aqueous solution, wherein the mass fraction of the methanol aqueous solution is 9-12%; in the preparation process, the methanol aqueous solution and the dicyandiamide are added together.
4. The fireproofing composition of claim 1, wherein the nanoscale thermally conductive filler comprises at least one of boron nitride, zinc oxide, and vitrified micro bubbles as a main component; the flame retardant is at least one of graphite, magnesium hydroxide, red phosphorus, triphenyl phosphate, zinc borate and ammonium polyphosphate; the flame retardant is 10-21 parts by mass.
5. The fireproofing composition of claim 1, further comprising 1 to 6 parts by mass of an acyl halide, wherein the acyl halide is at least one of acetyl chloride, benzoyl chloride, and oxalic acid chloride; the emulsion also comprises 4-12 parts by mass of emulsion, wherein the emulsion is at least one of styrene-acrylic emulsion and pure acrylic emulsion.
6. A fire-retardant composition as claimed in any one of claims 1 to 5, wherein the pH of the fire-retardant composition is in the range of from 8 to 9.
7. A TPS board comprising expandable polystyrene beads and a fire retardant component coating the surface of the expandable polystyrene beads;
the fireproof component is obtained by drying the fireproof composition of any one of claims 1 to 6.
8. A preparation method of a TPS plate is characterized by comprising the following steps:
pre-foaming polystyrene beads, coating and wrapping the fireproof composition according to any one of claims 1 to 6, adding a curing agent, and uniformly stirring to obtain a mixture;
and drying and forming the mixture.
9. The preparation method of claim 8, wherein the polystyrene beads are used in an amount of 20 to 40 parts by mass, the fire-retardant composition is used in an amount of 180 to 200 parts by mass, and the curing agent is used in an amount of 2 to 10 parts by mass.
10. The method according to claim 9, wherein 5 to 9 parts by mass of Ca (OH) is added after the mixture is obtained2Aqueous solution of said Ca (OH)2The mass fraction of the aqueous solution is 1-3%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011285995.2A CN112430378A (en) | 2020-11-17 | 2020-11-17 | Fireproof composition and preparation method and application thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011285995.2A CN112430378A (en) | 2020-11-17 | 2020-11-17 | Fireproof composition and preparation method and application thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN112430378A true CN112430378A (en) | 2021-03-02 |
Family
ID=74700776
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202011285995.2A Pending CN112430378A (en) | 2020-11-17 | 2020-11-17 | Fireproof composition and preparation method and application thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112430378A (en) |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104004281A (en) * | 2014-05-29 | 2014-08-27 | 哈尔滨工业大学空间钢结构幕墙有限公司 | Building thermosetting composite resin foamed insulation board and preparation method thereof |
| CN104072939A (en) * | 2014-06-20 | 2014-10-01 | 山东圣泉化工股份有限公司 | Modified polystyrene board and preparation method thereof |
| US20150284638A1 (en) * | 2011-10-31 | 2015-10-08 | Asia Cuanon Technology (Shanghai) Co., Ltd. | Fireproof composition and fireproof thermal insulation board |
| CN109504228A (en) * | 2018-11-12 | 2019-03-22 | 青岛海诺中天科技股份有限公司 | A kind of fireproof heated board and preparation method thereof |
| CN111004412A (en) * | 2019-12-20 | 2020-04-14 | 亚士创能科技(上海)股份有限公司 | Fireproof heat-insulation composition, fireproof heat-insulation composite board and preparation method thereof |
| CN111040323A (en) * | 2019-11-21 | 2020-04-21 | 天津科技大学 | A-2-grade fireproof TPS (thermoplastic polystyrene) heat-insulation board and preparation method thereof |
-
2020
- 2020-11-17 CN CN202011285995.2A patent/CN112430378A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20150284638A1 (en) * | 2011-10-31 | 2015-10-08 | Asia Cuanon Technology (Shanghai) Co., Ltd. | Fireproof composition and fireproof thermal insulation board |
| CN104004281A (en) * | 2014-05-29 | 2014-08-27 | 哈尔滨工业大学空间钢结构幕墙有限公司 | Building thermosetting composite resin foamed insulation board and preparation method thereof |
| CN104072939A (en) * | 2014-06-20 | 2014-10-01 | 山东圣泉化工股份有限公司 | Modified polystyrene board and preparation method thereof |
| CN109504228A (en) * | 2018-11-12 | 2019-03-22 | 青岛海诺中天科技股份有限公司 | A kind of fireproof heated board and preparation method thereof |
| CN111040323A (en) * | 2019-11-21 | 2020-04-21 | 天津科技大学 | A-2-grade fireproof TPS (thermoplastic polystyrene) heat-insulation board and preparation method thereof |
| CN111004412A (en) * | 2019-12-20 | 2020-04-14 | 亚士创能科技(上海)股份有限公司 | Fireproof heat-insulation composition, fireproof heat-insulation composite board and preparation method thereof |
Non-Patent Citations (3)
| Title |
|---|
| 周文英等: "《聚合物基导热复合材料》", 30 June 2017, 国防工业出版社 * |
| 李珠: "《玻化微珠保温材料的系列研究与"城市窑洞"式绿色建筑》", 31 December 2011, 北京邮电大学出版社 * |
| 钱之荣等: "《耐火材料实用手册》", 30 September 1992, 冶金工业出版社 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102977402B (en) | Preparation method of coated halogen-free flame-retardant foamable polystyrene | |
| CN106414573A (en) | Phenol resin foam body and method for producing same | |
| WO2011085531A1 (en) | Flame retardant polymeric foam material and manufacturing method thereof | |
| CA1100695A (en) | Non-punking non-corrosive phenolic foam | |
| CN101724254A (en) | Efficient halogen-free anti-inflaming polyurethane hard foam and preparation method thereof | |
| CN104292492A (en) | Preparation method of polystyrene foam board | |
| KR20110126484A (en) | Highly flame-retardant expanded polystyrene molded product using multi-layer coated expanded polystyrene particle | |
| CN105111676A (en) | Preparation method and application of light-weight high-strength plate made of phenolic aldehyde foam composites | |
| CN107629186A (en) | A kind of preparation method of resistance combustion polyurethane foam | |
| CN102516785A (en) | Core-shell urea formaldehyde modified lignin intumescent flame-retardant charring agent and preparation method thereof | |
| KR101431484B1 (en) | Frame retardant coating method for polystyrene foam beads | |
| CN105348726A (en) | Method for manufacturing pressure-proof, warping-resistant, hydrophobic, flame-resistant and thermal-insulated foam material | |
| CN112661925B (en) | Flame-retardant polyurethane foaming thermal insulation material for thermal insulation sandwich board and preparation method thereof | |
| CN110804203A (en) | Halogen-free flame retardant expandable polystyrene particles and preparation method thereof | |
| CN110358141A (en) | A kind of preparation method of fire retardant high molecular material | |
| CN109867942A (en) | A kind of preparation method and products thereof of fire-retardant fretting map polyphenylene oxide composite material | |
| CN112430378A (en) | Fireproof composition and preparation method and application thereof | |
| KR101489583B1 (en) | Non-Flammable composite for expanded polystyrene foam and manufacturing method thereof | |
| CN116769369A (en) | Intumescent fire-retardant coating and preparation method thereof | |
| RU2714917C1 (en) | Composition for fire-resistant foamed polyurethane | |
| CN115010401B (en) | Environment-friendly heat-preservation wallboard and preparation method thereof | |
| CN107117925A (en) | High-flame-retardant heat-insulating material | |
| CN101157780A (en) | Flame-resistant vinyl benzene polymer foam plastic | |
| CN105968670A (en) | Flame-retardant polyvinyl alcohol foam material | |
| KR101565281B1 (en) | Insulating Material Compositions for Having Inorganic Foam Material, Process for preparing Insulating Materials and Insulating Materials Prepared Therefrom |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20210302 |