CN118146687A - Emergency fireproof heat-insulating coating and preparation method thereof - Google Patents
Emergency fireproof heat-insulating coating and preparation method thereof Download PDFInfo
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- 238000000576 coating method Methods 0.000 title claims abstract description 114
- 239000011248 coating agent Substances 0.000 title claims abstract description 107
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 239000004964 aerogel Substances 0.000 claims abstract description 69
- 239000001913 cellulose Substances 0.000 claims abstract description 64
- 229920002678 cellulose Polymers 0.000 claims abstract description 64
- 239000003822 epoxy resin Substances 0.000 claims abstract description 29
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 29
- -1 polyethylene terephthalate Polymers 0.000 claims abstract description 28
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 26
- 238000000034 method Methods 0.000 claims abstract description 26
- 239000004925 Acrylic resin Substances 0.000 claims abstract description 25
- 229920000178 Acrylic resin Polymers 0.000 claims abstract description 25
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 25
- 238000010438 heat treatment Methods 0.000 claims abstract description 22
- 229920000139 polyethylene terephthalate Polymers 0.000 claims abstract description 22
- 239000005020 polyethylene terephthalate Substances 0.000 claims abstract description 22
- GUCYFKSBFREPBC-UHFFFAOYSA-N [phenyl-(2,4,6-trimethylbenzoyl)phosphoryl]-(2,4,6-trimethylphenyl)methanone Chemical compound CC1=CC(C)=CC(C)=C1C(=O)P(=O)(C=1C=CC=CC=1)C(=O)C1=C(C)C=C(C)C=C1C GUCYFKSBFREPBC-UHFFFAOYSA-N 0.000 claims abstract description 21
- 229920005610 lignin Polymers 0.000 claims abstract description 21
- 238000002156 mixing Methods 0.000 claims abstract description 18
- 238000003756 stirring Methods 0.000 claims abstract description 18
- 230000004048 modification Effects 0.000 claims abstract description 16
- 238000012986 modification Methods 0.000 claims abstract description 16
- 238000005470 impregnation Methods 0.000 claims abstract description 9
- 239000000203 mixture Substances 0.000 claims abstract description 7
- 239000002585 base Substances 0.000 claims description 35
- 238000009413 insulation Methods 0.000 claims description 24
- 239000003513 alkali Substances 0.000 claims description 17
- 230000008569 process Effects 0.000 claims description 13
- 239000003795 chemical substances by application Substances 0.000 claims description 8
- 239000004615 ingredient Substances 0.000 claims description 8
- 239000002270 dispersing agent Substances 0.000 claims description 3
- 239000003242 anti bacterial agent Substances 0.000 claims description 2
- 238000007598 dipping method Methods 0.000 claims description 2
- 230000001678 irradiating effect Effects 0.000 claims description 2
- 239000000843 powder Substances 0.000 claims description 2
- 239000003755 preservative agent Substances 0.000 claims description 2
- 238000009210 therapy by ultrasound Methods 0.000 claims description 2
- 230000009970 fire resistant effect Effects 0.000 claims 1
- 239000002994 raw material Substances 0.000 abstract description 4
- 238000012512 characterization method Methods 0.000 description 44
- 239000000243 solution Substances 0.000 description 25
- 230000000694 effects Effects 0.000 description 21
- 230000001680 brushing effect Effects 0.000 description 12
- 239000003973 paint Substances 0.000 description 12
- 239000007788 liquid Substances 0.000 description 10
- 238000001514 detection method Methods 0.000 description 8
- 229920002125 Sokalan® Polymers 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- 239000013530 defoamer Substances 0.000 description 6
- PMYUVOOOQDGQNW-UHFFFAOYSA-N hexasodium;trioxido(trioxidosilyloxy)silane Chemical compound [Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[O-][Si]([O-])([O-])O[Si]([O-])([O-])[O-] PMYUVOOOQDGQNW-UHFFFAOYSA-N 0.000 description 6
- 229920001296 polysiloxane Polymers 0.000 description 6
- 239000007864 aqueous solution Substances 0.000 description 5
- 230000007547 defect Effects 0.000 description 5
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 4
- 239000003063 flame retardant Substances 0.000 description 4
- 230000005484 gravity Effects 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
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- 238000006555 catalytic reaction Methods 0.000 description 2
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- 238000012827 research and development Methods 0.000 description 2
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- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 1
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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
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D133/00—Coating compositions based on 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 only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Coating compositions based on derivatives of such polymers
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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
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/18—Fireproof paints including high temperature resistant paints
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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
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/63—Additives non-macromolecular organic
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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
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/65—Additives macromolecular
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Abstract
The invention belongs to the field of coatings, and particularly relates to an emergency fireproof heat-insulating coating and a preparation method thereof. The method comprises the following steps: 1) Proportioning raw materials; 2) Performing modification treatment on the cellulose aerogel: adding the cellulose aerogel into lignin solution for low-pressure ultrasonic impregnation treatment, and then adding epoxy resin and then heating to obtain modified cellulose aerogel; 3) And (3) preparing a base solution: adding polyethylene terephthalate into water-based acrylic resin, stirring and uniformly mixing, slowly adding phenyl bis (2, 4, 6-trimethylbenzoyl) phosphine oxide, and carrying out ultraviolet irradiation under the condition of heating and constant temperature until the mixture is colloidal to obtain a base solution; 4) And (3) uniformly mixing and stirring the modified cellulose aerogel, the auxiliary agent and the base solution to obtain the emergency fireproof heat-insulating coating. The heat-insulating coating has good uniformity after being cured, and has certain emergency fireproof capability.
Description
Technical Field
The invention belongs to the field of coatings, and particularly relates to an emergency fireproof heat-insulating coating and a preparation method thereof.
Background
Thermal insulation coatings are a common and commonly used special building or equipment coating that is primarily used to insulate heat, to avoid overcooling or overheating of the building and/or equipment interior, and to maintain a constant temperature to some extent, to reduce the energy consumed to control the building and/or equipment heat.
However, most of the existing heat-insulating coatings are organic coating systems, and inorganic system coatings have better use effects and performances than organic system coatings, but have higher cost, so that most of the heat-insulating coatings are still developed and used mainly by organic coating systems. However, the organic coating has larger use defects, and particularly when the organic coating is used in partial special environments, the heat-insulating coating needs to have certain special properties besides the conventional heat-insulating property, the ageing resistance and the like. Most common heat-insulating paint used in parts of machine rooms and emergency places, the existing organic system heat-insulating paint has no fireproof performance and even has certain inflammability, so that the heat-insulating paint also needs to be matched with the fireproof paint for use. The compatibility of the two kinds of paint is generally limited, and the paint can be used in a mixed mode or used in sequence to form a composite layer, so that the situation of peeling and the like is easy to occur.
Therefore, an important research and development direction of the current industry is how to effectively improve the emergency fireproof performance of the organic system heat-insulating paint, so that the organic system heat-insulating paint has certain fireproof and flame-retardant capabilities.
Disclosure of Invention
The invention provides an emergency fireproof heat-insulating coating and a preparation method thereof, aiming at solving the problems that the existing organic heat-insulating coating generally does not have fireproof and flame-retardant capabilities, does not have emergency fireproof performance, has poor compatibility with the existing water-based fireproof coating and the like.
The main purpose of the invention is that:
1. The fireproof and flame-retardant performance of the organic heat-insulating coating can be effectively improved;
2. the organic heat-insulating paint can be effectively combined with the water-based fireproof paint.
In order to achieve the above purpose, the present invention adopts the following technical scheme.
A preparation method of an emergency fireproof heat-insulating coating,
The method comprises the following steps:
1) The ingredients are as follows:
6-10 parts of polyethylene terephthalate, 8-12 parts of epoxy resin, 3-5 parts of cellulose aerogel, 1-2 parts of phenyl bis (2, 4, 6-trimethylbenzoyl) phosphine oxide, 1-3 parts of auxiliary agent and 50-60 parts of water-based acrylic resin;
2) Performing modification treatment on the cellulose aerogel:
Adding the cellulose aerogel into lignin solution for low-pressure ultrasonic impregnation treatment, and then adding epoxy resin and then heating to obtain modified cellulose aerogel;
3) And (3) preparing a base solution:
adding polyethylene terephthalate into water-based acrylic resin, stirring and uniformly mixing, slowly adding phenyl bis (2, 4, 6-trimethylbenzoyl) phosphine oxide, and carrying out ultraviolet irradiation under the condition of heating and constant temperature until the mixture is colloidal to obtain a base solution;
4) And (3) uniformly mixing and stirring the modified cellulose aerogel, the auxiliary agent and the base solution to obtain the emergency fireproof heat-insulating coating.
As a preferred alternative to this,
Step 1) and step 2):
the average molecular weight of the epoxy resin is less than or equal to 600;
the cellulose aerogel is powdery aerogel powder with the mesh number of more than or equal to 200 meshes.
As a preferred alternative to this,
And 2) dispersing the lignin solution into water from alkali lignin, wherein the dosage of the alkali lignin is 3-5 g/mL of water.
As a preferred alternative to this,
The low-pressure ultrasonic dipping treatment in the step 2) is carried out under the condition of the pressure of less than or equal to 0.2atm, the ultrasonic treatment is carried out for 15 to 30 minutes, and then the constant temperature treatment is carried out for 50 to 70 minutes under the condition of 50 to 70 ℃ when the heating treatment is carried out.
As a preferred alternative to this,
Step 3) the heating constant temperature is controlled to be 50-60 ℃;
and 3) irradiating the ultraviolet irradiation process by adopting a 10W ultraviolet lamp for 3-5 min.
As a preferred alternative to this,
The auxiliary agents in step 1) and step 3) comprise defoamers and/or leveling agents and/or dispersants and/or preservatives and/or antibacterial agents and/or mildewcides.
An emergency fireproof heat-insulating coating.
The core of the technical scheme of the invention is to change the curing form of the heat-insulating coating and change the heat-insulating coating formed by the heat-insulating coating after encountering high temperature or even open fire.
Common organic coating curing time is slower, particularly aqueous acrylate thermal insulation coating has strong fluidity and longer curing time, so that the coating effect at the vertical face and the like is limited, and a relatively serious problem is caused by the fact that heat insulation filler such as aerogel and vacuum microbeads dispersed in the coating can generate serious uneven distribution, which is caused by slow curing of the coating and slow falling of the heat insulation filler under the action of gravity. Even if a sufficient amount of auxiliary agents such as dispersing agents are added, the defect is difficult to effectively solve, so that the difference of the heat conductivity coefficients of the upper end and the lower end of the vertical face is generated, and the heat insulation performance of the upper end is weakened. The invention is improved in two aspects, on one hand, the polyethylene terephthalate and the phenyl bis (2, 4, 6-trimethylbenzoyl) phosphine oxide are used for realizing a certain degree of liquid cross-linking with the aqueous acrylic resin through pretreatment, the viscosity of the aqueous acrylic resin is increased, the aqueous acrylic resin is converted into a gel state with relatively poor fluidity and surface dry solidification is formed, during the pretreatment, the polyethylene terephthalate and the aqueous acrylic resin can be polymerized in a free radical gradual polymerization mode under the catalysis promotion effect of the phenyl bis (2, 4, 6-trimethylbenzoyl) phosphine oxide, so that the aqueous acrylic resin is converted into a gel state with poor fluidity from a liquid state with high fluidity, but the gel state does not show direct and obvious viscosity, and on the other hand, the cellulose is subjected to modification treatment.
In the modification process, firstly, alkali Lignin (Lignin) and Cellulose Aerogel (CA) are mixed to form alkali Lignin-cellulose aerogel (L-CA), on the basis, the combination of the cellulose aerogel and epoxy resin is realized by cooperation of the alkali Lignin, because if the combination modification is directly carried out on the cellulose aerogel and the epoxy resin, the epoxy resin is easy to infiltrate into the cellulose aerogel in a large amount to cause remarkable reduction of heat insulation performance, the alkali Lignin and the cellulose aerogel can be mutually matched and built to form a secondary structure, particularly, the swelling of the cellulose aerogel in water environment is easy to be promoted, the heat insulation performance of the cellulose aerogel is further strengthened, and then the epoxy resin cannot infiltrate into the inside of the formed alkali Lignin-cellulose aerogel through the characteristic of the alkali Lignin, but a layer of similar shell layer is formed on the outer surface of the alkali Lignin-cellulose aerogel by the epoxy resin, so that the special cellulose aerogel structure with L-CA as a core and the epoxy resin as a shell is constructed, but the formed epoxy resin cannot be of a closed structure, so that the compatibility of the cellulose aerogel and the base liquid needs to be controlled.
Through the cooperation, the dispersibility and stability of the cellulose aerogel in the base liquid can be greatly improved, and the fluidity of the base liquid is changed and the solidification form is changed to a certain extent, so that the heat-insulating coating is more suitable for coating of a vertical surface, and the influence of gravity on the heat-insulating effect of the coating can be greatly reduced.
On the other hand, although polyethylene terephthalate and phenyl bis (2, 4, 6-trimethylbenzoyl) phosphine oxide are introduced in the pretreatment process of the base solution, the pretreatment process is not completely reacted, and after the coating is cured, the coating is subjected to high heat effect or exposed flame effect, the coating can further rapidly react under the heat effect and generate hardening shrinkage, so that the coating breaks to form spontaneous high Wen Tuola under extremely high temperature or exposed flame, the spread of the exposed flame is avoided, and a good fireproof flame-retardant effect is generated, and the defect that the organic thermal insulation coating is easy to ignite under the conventional condition to cause the spread of fire is overcome.
The invention has the beneficial effects that:
The heat-insulating coating can effectively solve the problems that the existing organic heat-insulating coating is slower in curing process, poor in curing film forming effect and the like when being used in a vertical face, effectively improves the uniformity of heat-insulating performance of the heat-insulating coating after curing, has certain emergency fireproof capability, and can generate effective emergency fireproof effect.
Detailed Description
The present invention will be described in further detail with reference to specific examples. Those of ordinary skill in the art will be able to implement the invention based on these descriptions. In addition, the embodiments of the present invention referred to in the following description are typically only some, but not all, embodiments of the present invention. Therefore, all other embodiments, which can be made by one of ordinary skill in the art without undue burden, are intended to be within the scope of the present invention, based on the embodiments of the present invention.
The raw materials used in the examples of the present invention are all commercially available or available to those skilled in the art unless specifically stated otherwise; the methods used in the examples of the present invention are those known to those skilled in the art unless specifically stated otherwise.
The average molecular weight of the commercial epoxy resin used in the embodiment of the invention is 600, the raw material of the cellulose aerogel is purchased from North China nano technology Co., ltd, and the cellulose aerogel is crushed to be more than or equal to 200 meshes, and the raw material of the aqueous acrylic resin is purchased from Jin Run Nanovel materials Co., ltd, with the brand of KRN8210.
Example 1
A method for preparing an emergency fireproof heat-insulating coating, which comprises the following steps:
1) The ingredients are as follows:
8 parts of polyethylene terephthalate, 10 parts of epoxy resin, 4 parts of cellulose aerogel, 1.5 parts of phenyl bis (2, 4, 6-trimethylbenzoyl) phosphine oxide, 2 parts of auxiliary agent and 55 parts of water-based acrylic resin;
the auxiliary agent consists of an acrylic acid polymer leveling agent, a polysiloxane defoamer and sodium disilicate according to the mass ratio of 2:3:5, the proportion of the components is as follows;
2) Performing modification treatment on the cellulose aerogel:
Adding the cellulose aerogel into a sufficient amount (enough to be fully immersed and the same applies below) of alkali lignin aqueous solution with the concentration of 5g/mL, carrying out low-pressure ultrasonic impregnation treatment under the condition of 0.2atm for 30min, then adding epoxy resin, and heating to 60 ℃ for constant temperature treatment for 60min to obtain modified cellulose aerogel;
3) And (3) preparing a base solution:
Adding polyethylene terephthalate into water-based acrylic resin, stirring and uniformly mixing, slowly adding phenyl bis (2, 4, 6-trimethylbenzoyl) phosphine oxide, heating to a constant temperature of 55 ℃, and radiating with 10W ultraviolet for 3min until the mixture is gelatinous to obtain a base solution;
4) And (3) uniformly mixing and stirring the modified cellulose aerogel, the auxiliary agent and the base solution to obtain the emergency fireproof heat-insulating coating.
The emergency fireproof heat-insulating coating prepared in the example is subjected to performance characterization.
The characterization includes the characterization of the curing uniformity and the heat insulation property of the vertical surface coating and the characterization of the fireproof performance.
In the vertical face coating characterization process, the emergency fireproof heat-insulating coating prepared in the embodiment is coated on a wall face (vertical face wall) with the height of 2.5m, the brushing thickness is 3mm, the thickness of an upper end fixing layer and the thickness of a lower end fixing layer of the vertical face wall are detected after 2 hours of brushing, and uniformity is represented by thickness difference. After the emergency fireproof heat-insulating coating is completely solidified to form a heat-insulating layer, the heat conductivity coefficients of the solidified heat-insulating layers at the top end (20 cm at the upper end) and the bottom end (20 cm at the lower end) of the opposite wall are respectively sampled and detected. After the detection is finished, the fireproof performance of the heat-insulating layer formed by curing on the opposite wall is detected, the open flame tip contacts the heat-insulating layer, the contact part of the flame tip is in a round shape with the diameter of about 8cm, the temperature of the flame tip is about 1200 ℃, the contact time is about 30 seconds, and then the damage condition of the heat-insulating layer is observed by removing the flame.
The characterization results are shown in the following table.
From the characterization result, the thermal insulation coating has good elevation coating effect, can effectively relieve the influence of gravity on the thermal insulation coating during elevation coating, effectively keeps the uniformity and the stable performance of the thermal insulation coating coated on an elevation wall, and has good thermal insulation performance at the top end and the bottom end. The fire-proof heat-insulating layer has good emergency fire-proof effect, the heat-insulating layer can not be ignited by open fire to cause combustion and spreading of the heat-insulating layer, fire hazards are generated, on the other hand, the part of the heat-insulating layer, which is directly contacted with the open fire, is directly contracted, broken and separated from the heat-insulating layer, and the broken edge of the heat-insulating layer still keeps good heat-insulating performance after separation.
Example 2
A method for preparing an emergency fireproof heat-insulating coating, which comprises the following steps:
1) The ingredients are as follows:
6 parts of polyethylene terephthalate, 12 parts of epoxy resin, 5 parts of cellulose aerogel, 1 part of phenyl bis (2, 4, 6-trimethylbenzoyl) phosphine oxide, 3 parts of auxiliary agent and 50 parts of water-based acrylic resin;
the auxiliary agent consists of an acrylic acid polymer leveling agent, a polysiloxane defoamer and sodium disilicate according to the mass ratio of 2:3:5, the proportion of the components is as follows;
2) Performing modification treatment on the cellulose aerogel:
Adding the cellulose aerogel into a sufficient amount of alkali lignin aqueous solution with the concentration of 5g/mL, performing low-pressure ultrasonic impregnation treatment under the condition of 0.2atm for 30min, adding epoxy resin, and then heating to 60 ℃ for constant temperature treatment for 60min to obtain modified cellulose aerogel;
3) And (3) preparing a base solution:
Adding polyethylene terephthalate into water-based acrylic resin, stirring and uniformly mixing, slowly adding phenyl bis (2, 4, 6-trimethylbenzoyl) phosphine oxide, heating to a constant temperature of 55 ℃, and radiating with 10W ultraviolet for 3min until the mixture is gelatinous to obtain a base solution;
4) And (3) uniformly mixing and stirring the modified cellulose aerogel, the auxiliary agent and the base solution to obtain the emergency fireproof heat-insulating coating.
The emergency fireproof heat-insulating coating prepared in the example is subjected to performance characterization.
The characterization includes the characterization of the curing uniformity and the heat insulation property of the vertical surface coating and the characterization of the fireproof performance.
In the vertical face coating characterization process, the emergency fireproof heat-insulating coating prepared in the embodiment is coated on a wall face (vertical face wall) with the height of 2.5m, the brushing thickness is 3mm, the thickness of an upper end fixing layer and the thickness of a lower end fixing layer of the vertical face wall are detected after 2 hours of brushing, and uniformity is represented by thickness difference. After the emergency fireproof heat-insulating coating is completely solidified to form a heat-insulating layer, the heat conductivity coefficients of the solidified heat-insulating layers at the top end (20 cm at the upper end) and the bottom end (20 cm at the lower end) of the opposite wall are respectively sampled and detected. After the detection is finished, the fireproof performance of the heat-insulating layer formed by curing on the opposite wall is detected, the open flame tip contacts the heat-insulating layer, the contact part of the flame tip is in a round shape with the diameter of about 8cm, the temperature of the flame tip is about 1200 ℃, the contact time is about 30 seconds, and then the damage condition of the heat-insulating layer is observed by removing the flame.
The characterization results are shown in the following table.
From the characterization results, the heat-insulating paint prepared by the method shows good heat-insulating performance and has good emergency fireproof capability.
Example 3
A method for preparing an emergency fireproof heat-insulating coating, which comprises the following steps:
1) The ingredients are as follows:
10 parts of polyethylene terephthalate, 8 parts of epoxy resin, 3 parts of cellulose aerogel, 2 parts of phenyl bis (2, 4, 6-trimethylbenzoyl) phosphine oxide, 1 part of auxiliary agent and 60 parts of water-based acrylic resin;
the auxiliary agent consists of an acrylic acid polymer leveling agent, a polysiloxane defoamer and sodium disilicate according to the mass ratio of 2:3:5, the proportion of the components is as follows;
2) Performing modification treatment on the cellulose aerogel:
Adding the cellulose aerogel into a sufficient amount of alkali lignin aqueous solution with the concentration of 5g/mL, performing low-pressure ultrasonic impregnation treatment under the condition of 0.2atm for 30min, adding epoxy resin, and then heating to 60 ℃ for constant temperature treatment for 60min to obtain modified cellulose aerogel;
3) And (3) preparing a base solution:
Adding polyethylene terephthalate into water-based acrylic resin, stirring and uniformly mixing, slowly adding phenyl bis (2, 4, 6-trimethylbenzoyl) phosphine oxide, heating to a constant temperature of 55 ℃, and radiating with 10W ultraviolet for 3min until the mixture is gelatinous to obtain a base solution;
4) And (3) uniformly mixing and stirring the modified cellulose aerogel, the auxiliary agent and the base solution to obtain the emergency fireproof heat-insulating coating.
The emergency fireproof heat-insulating coating prepared in the example is subjected to performance characterization.
The characterization includes the characterization of the curing uniformity and the heat insulation property of the vertical surface coating and the characterization of the fireproof performance.
In the vertical face coating characterization process, the emergency fireproof heat-insulating coating prepared in the embodiment is coated on a wall face (vertical face wall) with the height of 2.5m, the brushing thickness is 3mm, the thickness of an upper end fixing layer and the thickness of a lower end fixing layer of the vertical face wall are detected after 2 hours of brushing, and uniformity is represented by thickness difference. After the emergency fireproof heat-insulating coating is completely solidified to form a heat-insulating layer, the heat conductivity coefficients of the solidified heat-insulating layers at the top end (20 cm at the upper end) and the bottom end (20 cm at the lower end) of the opposite wall are respectively sampled and detected. After the detection is finished, the fireproof performance of the heat-insulating layer formed by curing on the opposite wall is detected, the open flame tip contacts the heat-insulating layer, the contact part of the flame tip is in a round shape with the diameter of about 8cm, the temperature of the flame tip is about 1200 ℃, the contact time is about 30 seconds, and then the damage condition of the heat-insulating layer is observed by removing the flame.
The characterization results are shown in the following table.
From the characterization results, the heat-insulating paint prepared by the method shows good heat-insulating performance and has good emergency fireproof capability.
Comparative example 1
A method for preparing an emergency fireproof heat-insulating coating, which comprises the following steps:
1) The ingredients are as follows:
8 parts of polyethylene terephthalate, 10 parts of epoxy resin, 4 parts of cellulose aerogel, 1.5 parts of phenyl bis (2, 4, 6-trimethylbenzoyl) phosphine oxide, 2 parts of auxiliary agent and 55 parts of water-based acrylic resin;
the auxiliary agent consists of an acrylic acid polymer leveling agent, a polysiloxane defoamer and sodium disilicate according to the mass ratio of 2:3:5, the proportion of the components is as follows;
2) Performing modification treatment on the cellulose aerogel:
Adding the cellulose aerogel into a sufficient amount of alkali lignin aqueous solution with the concentration of 5g/mL, performing low-pressure ultrasonic impregnation treatment under the condition of 0.2atm for 30min, adding epoxy resin, and then heating to 60 ℃ for constant temperature treatment for 60min to obtain modified cellulose aerogel;
3) And (3) preparing a base solution:
Adding polyethylene terephthalate into water-based acrylic resin, stirring and uniformly mixing, slowly adding phenyl bis (2, 4, 6-trimethylbenzoyl) phosphine oxide, heating to 55 ℃ and keeping the temperature for 3min to obtain a base solution;
4) And (3) uniformly mixing and stirring the modified cellulose aerogel, the auxiliary agent and the base solution to obtain the emergency fireproof heat-insulating coating.
The emergency fireproof heat-insulating coating prepared in the example is subjected to performance characterization.
The characterization includes the characterization of the curing uniformity and the heat insulation property of the vertical surface coating and the characterization of the fireproof performance.
In the vertical face coating characterization process, the emergency fireproof heat-insulating coating prepared in the embodiment is coated on a wall face (vertical face wall) with the height of 2.5m, the brushing thickness is 3mm, the thickness of an upper end fixing layer and the thickness of a lower end fixing layer of the vertical face wall are detected after 2 hours of brushing, and uniformity is represented by thickness difference. After the emergency fireproof heat-insulating coating is completely solidified to form a heat-insulating layer, the heat conductivity coefficients of the solidified heat-insulating layers at the top end (20 cm at the upper end) and the bottom end (20 cm at the lower end) of the opposite wall are respectively sampled and detected. After the detection is finished, the fireproof performance of the heat-insulating layer formed by curing on the opposite wall is detected, the open flame tip contacts the heat-insulating layer, the contact part of the flame tip is in a round shape with the diameter of about 8cm, the temperature of the flame tip is about 1200 ℃, the contact time is about 30 seconds, and then the damage condition of the heat-insulating layer is observed by removing the flame.
The characterization results are shown in the following table.
From the above characterization results, the base liquid still maintains better fluidity without effective pretreatment, which also results in easy formation of thickness differences during curing and significant increase in difference in thermal conductivity between the top and bottom ends. However, in the aspect of fireproof effect, obvious falling-off phenomenon also occurs. Therefore, even if the vertical surface coating effect of the heat-insulating coating base liquid is improved without effective pretreatment, the vertical surface coating effect is obviously reduced, the heat conductivity coefficient cannot maintain effective uniformity, but the heat-insulating coating base liquid still has good emergency fireproof performance, and can be broken and fall off when encountering open fire so as to avoid the spreading and burning of the heat-insulating layer. The reaction of the actual polyethylene terephthalate, the phenyl bis (2, 4, 6-trimethylbenzoyl) phosphine oxide and the aqueous acrylic resin can be excited by light and heat, the invention adopts a low-power ultraviolet lamp to excite so as to avoid excessive reaction, and the phenyl bis (2, 4, 6-trimethylbenzoyl) phosphine oxide has extremely strong catalytic reaction activity after open fire or extremely high heat excitation, can actually quickly react and shrink, and leads to the breakage of the unreacted parts of the reaction part and the heat-preservation base layer, thereby leading the heat-preservation coating to generate effective emergency fireproof effect.
Comparative example 2
A method for preparing an emergency fireproof heat-insulating coating, which comprises the following steps:
1) The ingredients are as follows:
8 parts of polyethylene terephthalate, 10 parts of epoxy resin, 4 parts of cellulose aerogel, 1.5 parts of phenyl bis (2, 4, 6-trimethylbenzoyl) phosphine oxide, 2 parts of auxiliary agent and 55 parts of water-based acrylic resin;
the auxiliary agent consists of an acrylic acid polymer leveling agent, a polysiloxane defoamer and sodium disilicate according to the mass ratio of 2:3:5, the proportion of the components is as follows;
2) Performing modification treatment on the cellulose aerogel:
adding the cellulose aerogel into enough water, performing low-pressure ultrasonic impregnation treatment for 30min under the condition of 0.2atm, adding epoxy resin, and then heating to 60 ℃ for constant temperature treatment for 60min to obtain modified cellulose aerogel;
3) And (3) preparing a base solution:
Adding polyethylene terephthalate into water-based acrylic resin, stirring and uniformly mixing, slowly adding phenyl bis (2, 4, 6-trimethylbenzoyl) phosphine oxide, heating to a constant temperature of 55 ℃, and radiating with 10W ultraviolet for 3min until the mixture is gelatinous to obtain a base solution;
4) And (3) uniformly mixing and stirring the modified cellulose aerogel, the auxiliary agent and the base solution to obtain the emergency fireproof heat-insulating coating.
The emergency fireproof heat-insulating coating prepared in the example is subjected to performance characterization.
The characterization includes the characterization of the curing uniformity and the heat insulation property of the vertical surface coating and the characterization of the fireproof performance.
In the vertical face coating characterization process, the emergency fireproof heat-insulating coating prepared in the embodiment is coated on a wall face (vertical face wall) with the height of 2.5m, the brushing thickness is 3mm, the thickness of an upper end fixing layer and the thickness of a lower end fixing layer of the vertical face wall are detected after 2 hours of brushing, and uniformity is represented by thickness difference. After the emergency fireproof heat-insulating coating is completely solidified to form a heat-insulating layer, the heat conductivity coefficients of the solidified heat-insulating layers at the top end (20 cm at the upper end) and the bottom end (20 cm at the lower end) of the opposite wall are respectively sampled and detected. After the detection is finished, the fireproof performance of the heat-insulating layer formed by curing on the opposite wall is detected, the open flame tip contacts the heat-insulating layer, the contact part of the flame tip is in a round shape with the diameter of about 8cm, the temperature of the flame tip is about 1200 ℃, the contact time is about 30 seconds, and then the damage condition of the heat-insulating layer is observed by removing the flame.
The characterization results are shown in the following table.
From the characterization result, lignin is not added when the cellulose aerogel is subjected to modification treatment, so that the heat conductivity coefficient of the whole heat insulation coating is increased, the heat insulation performance is weakened, on the other hand, the performance difference of the heat conductivity coefficient at the top end and the heat conductivity coefficient at the bottom end does not accord with the general rule, and thus research and development personnel perform sampling detection and characterization for more times, the characterization result shows that the heat insulation layer formed by curing on the vertical wall has obvious heat conductivity coefficient difference, the detection result shows that the whole appearance is between 0.0703 W.m-1.K-1, the great difference is shown, the trend of being large and small from top to bottom is not influenced by gravity, the irregular distribution is shown, the defect is mainly caused by uneven distribution of the aerogel, and the defect that the heat conductivity coefficient influence of the aerogel is the most obvious factor in the heat insulation coating is caused, and the direct modification treatment of epoxy resin can not be effectively and uniformly dispersed in the heat insulation coating when the aerogel is evenly mixed in a base solution, so that the cellulose aerogel needs to be matched with alkali lignin for modification treatment, and the uniform epoxy resin modification effect is ensured.
Comparative example 3
A method for preparing an emergency fireproof heat-insulating coating, which comprises the following steps:
1) The ingredients are as follows:
8 parts of polyethylene terephthalate, 10 parts of epoxy resin, 4 parts of cellulose aerogel, 2 parts of auxiliary agent and 55 parts of water-based acrylic resin;
the auxiliary agent consists of an acrylic acid polymer leveling agent, a polysiloxane defoamer and sodium disilicate according to the mass ratio of 2:3:5, the proportion of the components is as follows;
2) Performing modification treatment on the cellulose aerogel:
Adding the cellulose aerogel into a sufficient amount of alkali lignin aqueous solution with the concentration of 5g/mL, performing low-pressure ultrasonic impregnation treatment under the condition of 0.2atm for 30min, adding epoxy resin, and then heating to 60 ℃ for constant temperature treatment for 60min to obtain modified cellulose aerogel;
3) And (3) preparing a base solution:
Adding polyethylene terephthalate into water-based acrylic resin, stirring and uniformly mixing, heating to a constant temperature of 55 ℃, and radiating with 10W ultraviolet for 3min to obtain a base solution;
4) And (3) uniformly mixing and stirring the modified cellulose aerogel, the auxiliary agent and the base solution to obtain the emergency fireproof heat-insulating coating.
The emergency fireproof heat-insulating coating prepared in the example is subjected to performance characterization.
The characterization includes the characterization of the curing uniformity and the heat insulation property of the vertical surface coating and the characterization of the fireproof performance.
In the vertical face coating characterization process, the emergency fireproof heat-insulating coating prepared in the embodiment is coated on a wall face (vertical face wall) with the height of 2.5m, the brushing thickness is 3mm, the thickness of an upper end fixing layer and the thickness of a lower end fixing layer of the vertical face wall are detected after 2 hours of brushing, and uniformity is represented by thickness difference. After the emergency fireproof heat-insulating coating is completely solidified to form a heat-insulating layer, the heat conductivity coefficients of the solidified heat-insulating layers at the top end (20 cm at the upper end) and the bottom end (20 cm at the lower end) of the opposite wall are respectively sampled and detected. After the detection is finished, the fireproof performance of the heat-insulating layer formed by curing on the opposite wall is detected, the open flame tip contacts the heat-insulating layer, the contact part of the flame tip is in a round shape with the diameter of about 8cm, the temperature of the flame tip is about 1200 ℃, the contact time is about 30 seconds, and then the damage condition of the heat-insulating layer is observed by removing the flame.
The characterization results are shown in the following table.
From the above characterization results, similar to the results exhibited by comparative example 1, it was demonstrated that this example was not effective in achieving stepwise polymerization of the objective polyethylene terephthalate and the aqueous acrylic resin without using phenyl bis (2, 4, 6-trimethylbenzoyl) phosphine oxide, thereby reducing flowability and achieving the subsequent quick-drying effect. As in examples 1-3 and comparative example 2, the coating was able to form a surface dry film between about 30 and 50 seconds after being applied to a facade wall, thereby restricting the flow of the heat-insulating coating, whereas the heat-insulating coating prepared in comparative example 1 and this example required more than 3 minutes to form a surface dry film, demonstrating that the pretreatment of the base liquid plays a vital role in improving the use effect optimization of the heat-insulating coating on a facade wall. Therefore, it can be seen that, to improve the practical use effect of the heat-insulating coating on the vertical wall and ensure good coating uniformity and performance uniformity, the base liquid needs to be pretreated, and the use of catalytic substances and pretreatment conditions in the pretreatment process can have significant influence on the pretreatment result.
Claims (7)
1. A preparation method of an emergency fireproof heat-insulating coating is characterized in that,
The method comprises the following steps:
1) The ingredients are as follows:
6-10 parts of polyethylene terephthalate, 8-12 parts of epoxy resin, 3-5 parts of cellulose aerogel, 1-2 parts of phenyl bis (2, 4, 6-trimethylbenzoyl) phosphine oxide, 1-3 parts of auxiliary agent and 50-60 parts of water-based acrylic resin;
2) Performing modification treatment on the cellulose aerogel:
Adding the cellulose aerogel into lignin solution for low-pressure ultrasonic impregnation treatment, and then adding epoxy resin and then heating to obtain modified cellulose aerogel;
3) And (3) preparing a base solution:
adding polyethylene terephthalate into water-based acrylic resin, stirring and uniformly mixing, slowly adding phenyl bis (2, 4, 6-trimethylbenzoyl) phosphine oxide, and carrying out ultraviolet irradiation under the condition of heating and constant temperature until the mixture is colloidal to obtain a base solution;
4) And (3) uniformly mixing and stirring the modified cellulose aerogel, the auxiliary agent and the base solution to obtain the emergency fireproof heat-insulating coating.
2. The preparation method of the emergency fireproof heat-insulating coating according to claim 1, which is characterized in that,
Step 1) and step 2):
the average molecular weight of the epoxy resin is less than or equal to 600;
the cellulose aerogel is powdery aerogel powder with the mesh number of more than or equal to 200 meshes.
3. The preparation method of the emergency fireproof heat-insulating coating according to claim 1 or 2, which is characterized in that,
And 2) dispersing the lignin solution into water from alkali lignin, wherein the dosage of the alkali lignin is 3-5 g/mL of water.
4. The preparation method of the emergency fireproof heat-insulating coating according to claim 1, which is characterized in that,
The low-pressure ultrasonic dipping treatment in the step 2) is carried out under the condition of the pressure of less than or equal to 0.2atm, the ultrasonic treatment is carried out for 15 to 30 minutes, and then the constant temperature treatment is carried out for 50 to 70 minutes under the condition of 50 to 70 ℃ when the heating treatment is carried out.
5. The preparation method of the emergency fireproof heat-insulating coating according to claim 1, which is characterized in that,
Step 3) the heating constant temperature is controlled to be 50-60 ℃;
and 3) irradiating the ultraviolet irradiation process by adopting a 10W ultraviolet lamp for 3-5 min.
6. The preparation method of the emergency fireproof heat-insulating coating according to claim 1, which is characterized in that,
The auxiliary agents in step 1) and step 3) comprise defoamers and/or leveling agents and/or dispersants and/or preservatives and/or antibacterial agents and/or mildewcides.
7. An emergency fire-resistant thermal-insulation coating prepared by the method of any one of claims 1 to 6.
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