CN115948070A - Bio-based interior wall intumescent fire-retardant coating and preparation method thereof - Google Patents
Bio-based interior wall intumescent fire-retardant coating and preparation method thereof Download PDFInfo
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Abstract
The application provides a bio-based interior wall intumescent fire-retardant coating, which comprises the following raw materials in parts by weight: 20-50 parts of bio-based intumescent flame retardant, 10-30 parts of bio-based filler, 8-15 parts of pigment, 20-50 parts of resin, 0.1-1 part of antibacterial agent, 0.5-1.8 parts of film-forming aid, 0.5-1.5 parts of freeze-thaw resistant aid, 0.6-1.2 parts of dispersing agent and 0.1-0.3 part of defoaming agent. The invention uses renewable substances such as biological substances, biological extracts and the like as raw materials, reduces the use of non-renewable resources, reduces carbon emission, reduces the pollution of chemical production and protects the environment. Compared with the conventional intumescent fire-retardant coating, the intumescent fire-retardant coating has good hydrophobicity and storage stability. The coating can be used for civil interior walls, has good decoration and fire resistance, adopts a bio-based material without harmful substances, is green and healthy, can continuously and effectively adsorb and degrade formaldehyde, and improves the fire resistance limit of a wall surface base material.
Description
Technical Field
The application belongs to the technical field of fireproof coatings, and relates to a bio-based interior wall intumescent fireproof coating and a preparation method thereof.
Background
With the progress of society, the national economy is continuously improved, the building is high-rise, and the possibility of fire of the building is increased when a large amount of novel materials are introduced and used in the building. The fire occurrence frequency of the modern society is high, and causes of building fire occurrence and expansion are not only related to damage of fire-fighting facilities, untimely fire suppression at the initial stage and the like, but also have a very close relationship with used building materials.
When the temperature of prestressed reinforcement concrete (common building material) reaches 200 ℃, the yield point begins to drop, and when the temperature is 300 ℃, the prestress almost completely disappears; at 300 ℃, the strength of the concrete begins to decline, the strength at 500 ℃ is reduced by about half, and the strength at 800 ℃ is almost lost. In a building fire, the floor slabs are broken and collapsed within about 0.5h, and meanwhile, a large amount of toxic gas is generated when oil paint or emulsion paint for interior decoration is burnt; statistically, more than 80% of the victims in a fire are killed by inhalation of too much toxic gas and smoke. The fire resistance limit of the wall surface can be increased by using an aqueous fire retardant coating.
The expansion type fireproof coating on the market consists of an acid source (ammonium polyphosphate), a gas source (melamine and urea) and a carbon source (pentaerythritol, dextrin, starch and sucrose). At high temperature, a honeycomb carbonized layer is quickly formed, the heat insulation, smoke suppression and fire spread retarding effects are good, and meanwhile, no dense smoke or harmful gas is generated, so that the flame retardant is an environment-friendly flame retardant. However, ammonium polyphosphate contains a large amount of hydrophilic groups, so that the ammonium polyphosphate has strong water solubility and hydrolyzability, and has strong chelation with some metal ions, so that the water resistance, scrubbing resistance and storage property are poor.
The chemical synthesis method of the existing common intumescent flame retardant raw materials (ammonium polyphosphate, pentaerythritol and melamine) consumes a large amount of non-renewable energy sources such as coal, petroleum and the like; meanwhile, harmful gas and greenhouse gas emissions are generated.
Disclosure of Invention
In order to solve the problems, the invention aims to prepare a bio-based interior wall intumescent fire-retardant coating by using biological substances, biological extracts and bio-based synthetic and modified substances as materials, and has the advantages of environmental protection, energy conservation and emission reduction; meanwhile, the use of non-renewable energy sources is reduced, and the sustainable development of the coating industry is facilitated.
The invention provides a bio-based interior wall intumescent fire-retardant coating which comprises the following raw materials in parts by weight:
20-50 parts of bio-based intumescent flame retardant, 10-30 parts of bio-based filler, 8-15 parts of pigment, 20-50 parts of resin, 0.1-1 part of antibacterial agent, 0.5-1.8 parts of film-forming assistant, 0.5-1.5 parts of freeze-thaw resisting assistant, 0.6-1.2 parts of dispersing agent and 0.1-0.3 part of defoaming agent.
Further, the synthesis method of the bio-based intumescent flame retardant comprises the following steps:
(1) Premixing 20-80 parts of phytate and 10-50 parts of natural nitrogen-containing macromolecules in ultrasonic waves for 30min to obtain a mixture 1;
(2) Slowly adding the mixture 1 into a calcium hydroxide aqueous solution at normal temperature, and stirring at the speed of 10-20r/s for 2-3h to obtain a reaction solution 1;
(3) Slowly adding 20-60 parts of polyhydroxy-containing bio-based carrier into the reaction liquid 1, introducing nitrogen, and stirring at the speed of 20-50r/s for 4-5h to obtain a reaction liquid 2;
(4) Filtering out the precipitate in the reaction solution 2, washing with ammonia water in an ultrasonic cleaner, centrifuging, and filtering for 2-3 times;
(5) And putting the cleaned precipitate into a clean beaker, putting the beaker into a 60 ℃ oven for drying for 2-3h, and then crushing, grinding and sieving the dried product to obtain the bio-based intumescent flame retardant.
Further, the bio-based filler is 2000-mesh shell powder.
Further, the pigment is one or more of rutile type titanium dioxide, anatase type titanium dioxide and nano titanium dioxide.
Further, the resin is one or more of phenylpropionic acid emulsion, VAE emulsion, silicone-acrylic emulsion and vinyl acetate-acrylic emulsion.
Further, the antibacterial agent is marine organism extract, such as one or more of chitosan micropowder, chitin, hinokitiol, and graminum.
Further, the film forming auxiliary agent is one or more of alcohol ester dodeca, alcohol ester hexadecane and propylene glycol.
Further, the antifreeze additive is glycol.
Further, the dispersant is an ammonium salt dispersant. The ammonium salt dispersant has better dispersibility on the flame retardant, and the ammonium ions and the flame retardant have synergistic effect.
Further, the defoaming agent is one or more of organic silicon and mineral oil.
A preparation method of a bio-based interior wall intumescent fire retardant coating comprises the following steps:
adding 0.6-1.2 parts of dispersing agent, 0.1-0.3 part of defoaming agent and 0.1-1 part of bactericide into water, and stirring for 1-3min to prepare dispersion liquid;
slowly adding 8-15 parts of pigment, 10-30 parts of bio-based filler and 20-50 parts of bio-based flame retardant into the dispersion liquid, dispersing for 3-5min at 500-900 rpm, and stirring for 20-30 min at 1200-1900 rpm, so as to prepare dispersed slurry;
adjusting the rotating speed to 800-1000 rpm, adding 0.5-1.8 parts of film-forming assistant, 0.5-1.5 parts of freeze-thaw resisting assistant and 20-50 parts of resin into the dispersion slurry, and stirring for 5-10min to obtain the bio-based interior wall intumescent fire-retardant coating.
The invention has the beneficial effects that: the invention uses renewable substances such as biological substances, biological extracts and the like as raw materials, reduces the use of non-renewable resources, reduces carbon emission, reduces the pollution of chemical production and protects the environment.
Compared with the conventional intumescent fire-retardant coating, the intumescent fire-retardant coating has good hydrophobicity and storage stability. At present, the used expansion flame retardant is short-chain ammonium polyphosphate which has poor stability, is easy to chelate with other metal ions and release ammonia gas, and is easy to dissolve in water and hydrolyze.
The coating can be used for civil interior walls, has good decoration and fire resistance, adopts a biological base material, has no harmful substances, is green and healthy, can continuously and effectively adsorb and degrade formaldehyde, and improves the fire resistance limit of the base material (wall surface).
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are required to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and that those skilled in the art can also obtain other related drawings based on the drawings without inventive efforts.
Fig. 1 is a schematic diagram of the expansion principle of the bio-based inner wall in the present application.
Detailed Description
The following detailed description properly refers to the accompanying drawings and specifically discloses an embodiment of the bio-based interior wall intumescent fire retardant coating and the preparation method thereof. But a detailed description thereof will be omitted. For example, detailed descriptions of well-known matters and repetitive descriptions of actually the same structures may be omitted. This is to avoid unnecessarily obscuring the following description, and to facilitate understanding by those skilled in the art. The drawings and the following description are provided for those skilled in the art to fully understand the present application, and are not intended to limit the subject matter recited in the claims.
The "ranges" disclosed herein are defined in terms of lower limits and upper limits, with a given range being defined by a selection of one lower limit and one upper limit that define the boundaries of the particular range. Ranges defined in this manner may or may not include the stated limits and may be arbitrarily combined, i.e., any lower limit may be combined with any upper limit to form a range. For example, if ranges of 60-120 and 80-110 are listed for a particular parameter, it is understood that ranges of 60-110 and 80-120 are also contemplated. Furthermore, if the minimum range values 1 and 2 are listed, and if the maximum range values 3,4, and 5 are listed, the following ranges are all contemplated: 1-3, 1-4, 1-5, 2-3, 2-4 and 2-5. In this application, unless otherwise stated, the numerical range "a-b" represents a shorthand representation of any combination of real numbers between a and b, where a and b are both real numbers. For example, a numerical range of "0 to 5" indicates that all real numbers between "0 to 5" have been listed herein, and "0 to 5" is only a shorthand representation of the combination of these numbers. In addition, when a parameter is an integer of 2 or more, it is equivalent to disclose that the parameter is, for example, an integer of 2, 3,4, 5, 6, 7, 8, 9, 10, 11, 12, or the like.
All embodiments and alternative embodiments of the present application may be combined with each other to form new solutions, if not specifically stated.
All technical and optional features of the present application may be combined with each other to form new solutions, if not otherwise specified.
All steps of the present application may be performed sequentially or randomly, preferably sequentially, if not specifically stated. For example, the method comprises steps (a) and (b), meaning that the method may comprise steps (a) and (b) performed sequentially, and may also comprise steps (b) and (a) performed sequentially. For example, reference to the process further comprising step (c) means that step (c) may be added to the process in any order, for example, the process may comprise steps (a), (b) and (c), may also comprise steps (a), (c) and (b), may also comprise steps (c), (a) and (b), etc.
The terms "comprises" and "comprising" as used herein mean either open or closed unless otherwise specified. For example, the terms "comprising" and "comprises" may mean that additional components not listed may also be included or included, or that only listed components may be included or included.
In this application, the term "or" is inclusive, unless otherwise specified. For example, the phrase "a or B" means "a, B, or both a and B. More specifically, either of the following conditions satisfies the condition "a or B": a is true (or present) and B is false (or not present); a is false (or not present) and B is true (or present); or both a and B are true (or present).
In one embodiment of the present application, the present application provides a method for preparing a bio-based interior wall intumescent fire retardant coating, comprising the following steps:
adding 0.6-1.2 parts of dispersant, 0.1-0.3 part of defoamer and 0.1-1 part of bactericide into water, and stirring for 1-3min to prepare dispersion liquid;
slowly adding 8-15 parts of pigment, 10-30 parts of bio-based filler and 20-50 parts of bio-based flame retardant into the dispersion liquid, dispersing for 3-5min at 500-900 rpm, and stirring for 20-30 min at 1200-1900 rpm, so as to prepare dispersed slurry;
adjusting the rotating speed to 800-1000 rpm, adding 0.5-1.8 parts of film-forming aid, 0.5-1.5 parts of freeze-thaw resistant aid and 20-50 parts of resin into the dispersion slurry, and stirring for 5-10min to obtain the bio-based interior wall intumescent fire retardant coating.
The reaction mechanism is as follows:
1. mechanism of fire protection
When the bio-based flame retardant is heated, strong acid can be decomposed, the strong acid reacts with hydroxyl on carbon chains in the polymer to generate dehydration reaction, and meanwhile, inert gases such as nitrogen, ammonia, carbon dioxide and the like can be decomposed to form a honeycomb-shaped carbonization layer, so that the fire spread is prevented.
(1) Principle of expansion (fig. 1):
(2) Equation of reaction principle
2. Mechanism of formaldehyde degradation
The shell powder has a strong adsorption effect and can adsorb free formaldehyde in the air on a wall surface; a large amount of amino groups in the flame retardant can react with free formaldehyde in the air to generate Schiff base, so that the reaction equation for effectively degrading formaldehyde is as follows:
-NH 2 +HCHO→-N＝CH 2 +H 2 O
examples
Hereinafter, examples of the present application will be described. The following description of the embodiments is merely exemplary in nature and is in no way intended to limit the present disclosure. The examples, where specific techniques or conditions are not indicated, are to be construed according to the techniques or conditions described in the literature in the art or according to the product specifications. The reagents or instruments used are conventional products which are commercially available, and are not indicated by manufacturers.
Example one
(1) 0.5 part of ammonium salt dispersant, 0.2 part of organic silicon defoamer and 0.4 part of chitin/chitosan are added into 10 parts of water and stirred for 3min to prepare dispersion liquid.
(2) And then slowly adding 15 parts of rutile titanium dioxide, 30 parts of shell powder and 20 parts of bio-based flame retardant into the dispersion liquid, dispersing for 3min at 500rpm, adjusting the rotating speed to 1500rpm, and stirring for 30min to prepare dispersed slurry.
(3) Adjusting the rotating speed to 800rpm, adding 0.9 part of alcohol ester twelve, 0.8 part of ethylene glycol and 22 parts of VAE emulsion into the dispersion slurry, and stirring for 5min to obtain the bio-based interior wall intumescent fire-retardant coating.
Example two
(4) 0.5 part of ammonium salt dispersant, 0.2 part of organic silicon defoamer and 0.4 part of chitin/chitosan are added into 10 parts of water and stirred for 3min to prepare dispersion liquid.
(5) And slowly adding 15 parts of rutile titanium dioxide, 20 parts of shell powder and 30 parts of bio-based flame retardant into the dispersion liquid, dispersing for 3min at 500rpm, adjusting the rotating speed to 1500rpm, and stirring for 30min to prepare dispersed slurry.
(6) Adjusting the rotating speed to 800rpm, adding 0.9 part of alcohol ester twelve, 0.8 part of ethylene glycol and 22 parts of VAE emulsion into the dispersion slurry, and stirring for 5min to obtain the bio-based interior wall intumescent fire-retardant coating.
EXAMPLE III
(7) 0.5 part of ammonium salt dispersant, 0.2 part of organic silicon defoamer and 0.4 part of chitin/chitosan are added into 10 parts of water and stirred for 3min to prepare dispersion liquid.
(8) And slowly adding 13 parts of rutile titanium dioxide, 12 parts of shell powder and 40 parts of bio-based flame retardant into the dispersion liquid, dispersing for 3min at 500rpm, adjusting the rotating speed to 1500rpm, and stirring for 30min to prepare dispersed slurry.
(9) Adjusting the rotating speed to 800rpm, adding 0.9 part of dodecyl alcohol ester, 0.8 part of ethylene glycol and 22 parts of VAE emulsion into the dispersion slurry, and stirring for 5min to obtain the bio-based interior wall intumescent fire retardant coating.
Example four
(10) 0.5 part of ammonium salt dispersant, 0.2 part of organic silicon defoamer and 0.4 part of chitin/chitosan are added into 10 parts of water and stirred for 3min to prepare dispersion liquid.
(11) And slowly adding 10 parts of rutile titanium dioxide, 5 parts of shell powder and 50 parts of bio-based flame retardant into the dispersion liquid, dispersing for 3min at 500rpm, adjusting the rotating speed to 1500rpm, and stirring for 30min to prepare dispersed slurry.
(12) Adjusting the rotating speed to 800rpm, adding 0.9 part of alcohol ester twelve, 0.8 part of ethylene glycol and 22 parts of VAE emulsion into the dispersion slurry, and stirring for 5min to obtain the bio-based interior wall intumescent fire-retardant coating.
EXAMPLE five
(13) Adding 0.5 part of ammonium salt dispersant, 0.2 part of organic silicon defoamer and 0.4 part of chitin/chitosan into 15 parts of VAE emulsion, and stirring for 3min to prepare dispersion.
(14) Then 15 parts of rutile titanium dioxide and 50 parts of bio-based flame retardant are slowly added into the dispersion liquid, dispersed for 3min at 500rpm, stirred for 30min at the rotation speed of 1500rpm, and prepared into dispersion slurry.
(15) Adjusting the rotating speed to 800rpm, adding 1.8 parts of alcohol ester twelve, 0.5 part of glycol and 16.4 parts of VAE emulsion into the dispersion slurry, and stirring for 5min to obtain the bio-based interior wall intumescent fire-retardant coating.
Further, the performance test of the bio-based interior wall intumescent fire retardant coatings prepared in examples 1-5
Description of the experiment: the blank group is the common inner wall latex paint on the market. And (3) testing the fire resistance: examples 1-5 were uniformly painted twice on the surface of a simulated wall substrate using a pressurized cement of dimensions 50cm x 0.5cm, with a wet film thickness of 200 μm each time, and cured 7d after drying for fire resistance testing. Selecting diesel oil with higher combustion heat value as a fire source, timing from ignition, recording back surface temperature until the temperature of the back plate reaches 300 ℃ (the limit temperature of the cement plate and the temperature of the rapid reduction of the yield point of the reinforcing steel bar) as end point temperature, and recording the time as the duration of fire resistance as t. The expansion ratio is calculated by the ratio h2/h1 of the thickness h2 of the carbon layer after combustion to the thickness h1 of the coating before expansion. The scrubbing resistance and contrast ratio test method adopts GB/T9756-2018; the formaldehyde purification rate and formaldehyde purification durability are tested by a JC/T1074-2008 test method.
| Item | Blank group | Example one | Example two | Example three | Example four | Example five |
| Contrast ratio | 0.95 | 0.95 | 0.93 | 0.93 | 0.91 | 0.93 |
| Scrub resistant | 9999 | 9999 | 8500 | 5000 | 5000 | 4200 |
| Fire resistance | 1 minute | 25min | 28min | 32min | 48min | 55min |
| Purification rate of formaldehyde | Is free of | 76.6％ | 79.1％ | 85.6％ | 89.1.1％ | 88.3％ |
| Durability of Formaldehyde purification | Is free of | 60.6％ | 66.5％ | 69.2％ | 73.1％ | 78.8％ |
| Expansion ratio | Does not expand | 35 times of | 41 times of | 45 times of | 73 times that of the traditional Chinese medicine | 80 times of |
As can be seen from the table above, the invention has better fireproof function, formaldehyde degradation function and decorative effect, and the functions can be adjusted according to the requirements.
A single variable method is adopted for comparison experiments, other components and weight are unchanged, and different dispersant types are used for comparing fire resistance and expansibility.
The data show that the ammonium salt dispersant has better dispersibility on the flame retardant, and the ammonium ions and the flame retardant have synergistic effect.
The crystallinity of the common interior wall latex paint in the paint is serious, so that the storage stability is poor; the plant-based flame retardant is environment-friendly and healthy, low in water solubility and free of crystallinity, and ensures the effects of high fineness, excellent paint film, excellent fullness and the like of the interior wall coating. The modified flame retardant has a nano level, has a good nano size effect, and can ensure the fullness of a paint film and color retention after being applied to an inner wall paint.
The present application is not limited to the above embodiments. The above embodiments are merely examples, and embodiments having substantially the same configuration as the technical idea and exhibiting the same operation and effect within the technical scope of the present application are all included in the technical scope of the present application. In addition, various modifications that can be conceived by those skilled in the art are applied to the embodiments and other embodiments are also included in the scope of the present application, in which some of the constituent elements in the embodiments are combined and constructed, without departing from the scope of the present application.
Claims (10)
1. The bio-based interior wall intumescent fire-retardant coating is characterized by comprising the following raw materials in parts by weight:
20-50 parts of bio-based intumescent flame retardant, 10-30 parts of bio-based filler, 8-15 parts of pigment, 20-50 parts of resin, 0.1-1 part of bactericide, 0.5-1.8 parts of film-forming assistant, 0.5-1.5 parts of freeze-thaw resisting assistant, 0.6-1.2 parts of dispersing agent and 0.1-0.3 part of defoaming agent.
2. The intumescent fire retardant coating for inner wall of bio-based as claimed in claim 1, characterized in that said bio-based filler is shell powder.
3. The intumescent fire retardant coating for interior walls of claim 1, wherein said pigment is one of rutile type titanium dioxide, anatase type titanium dioxide and nano titanium dioxide.
4. The intumescent fire retardant coating for interior walls of claim 1, wherein said resin is one of styrene-acrylic emulsion, VAE emulsion, silicone-acrylic emulsion and vinyl acetate-acrylic emulsion.
5. The intumescent fire retardant coating for interior walls of claim 1, wherein said antibacterial agent is marine organism extract.
6. The intumescent fire retardant coating for interior walls of claim 1, wherein said film forming agent is one of ester twelve alcohol, ester sixteen alcohol and propylene glycol.
7. The intumescent fire retardant coating for inner wall of bio-based as claimed in claim 1, wherein said anti-freeze auxiliary is ethylene glycol.
8. The intumescent fire retardant coating for interior walls of claim 1, wherein said dispersant is ammonium salt dispersant.
9. The intumescent fire retardant coating for interior walls of claim 1, wherein said defoamer is silicone, mineral oil.
10. A method for preparing an intumescent anticorrosion coating according to any one of claims 1 to 9, characterized in that: the method comprises the following steps:
adding 0.6-1.2 parts of dispersing agent, 0.1-0.3 part of defoaming agent and 0.1-1 part of bactericide into water, and stirring for 1-3min to prepare dispersion liquid;
slowly adding 8-15 parts of pigment, 10-30 parts of bio-based filler and 20-50 parts of bio-based flame retardant into the dispersion liquid, dispersing for 3-5min at 500-900 rpm, and stirring for 20-30 min at 1200-1900 rpm, so as to prepare dispersed slurry;
adjusting the rotating speed to 800-1000 rpm, adding 0.5-1.8 parts of film-forming aid, 0.5-1.5 parts of freeze-thaw resistant aid and 20-50 parts of resin into the dispersion slurry, and stirring for 5-10min to obtain the bio-based interior wall intumescent fire retardant coating.
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