JP6284657B2 - Water-soluble flameproofing agent composition for wood and flameproofing method - Google Patents

Description

  The present invention relates to a water-soluble flameproofing agent composition for wood and a flameproofing treatment method. More specifically, the present invention relates to a general wood and a water-based paint applied to the treated wood surface only by a spray or a brush. Easy to penetrate, can suppress flame propagation, has excellent carbonization area, afterflame time and afterglow time, has no white color / peeling / dirt of water-based paint color, and is flameproof at normal temperature and pressure, The present invention relates to a water-soluble flameproofing agent composition for wood and a flameproofing treatment method that can provide a flameproofing effect for a long time without using other auxiliary agents.

  It is almost impossible from the technical and economic point of view to flameproof the woods, fibers and plastics used in our lives, and the necessity is actually very low. For this reason, it is a normal case that only an object that is recognized as necessary from the fire prevention side is prescribed to be flameproofed.

  Looking at the cases in Europe, the United States, and Japan, in addition to building interior materials, the interior materials of various transport vehicles such as vehicles and aircraft, combustible parts of various electrical and electronic products, In South Korea, plywood, fiberboard, carpets, curtains, etc., which are interior materials for special places such as high-rise buildings, theatres, hotels, hospitals, automobiles, etc. It is regulated by the Fire Service Act as a flameproof treatment target.

  Looking at the above flameproofing objects by material; it can be roughly divided into three types, such as woods, fibers, plastics, etc. Varies greatly depending on the material.

  Among these, wood is a natural material widely used in the manufacture of architecture, furniture, furniture, etc., and due to the characteristics of the material, it has the disadvantage that it is very vulnerable to degradation by fire, microorganisms or various insects, but it is water-based. When the paint is applied to the wood surface, it protects the wood and maintains its aesthetic appearance. It is advantageous in that it can be protected from various wind damages without being damaged by various microorganisms and insects.

  For the reason described above, it is almost impossible to apply and treat the flame retardant by spray method on the wood surface to which the water-based paint is applied in this way (from the technical and economic viewpoints, It is rarely done (because the necessity is very few in reality).

  On the other hand, there are a physical processing method and a chemical processing method as a flameproofing method for wood, but the chemical processing method is mainly used for the reason of the flameproofing effect and economical reasons. The chemical treatment method refers to treating a flameproof object with a chemical having an excellent flameproofing effect, and such chemical is called a flameproofing agent composition.

  In addition, wood-related flame retardant compositions are mainly used with halogen-based flame retardants, phosphorus-based flame retardants and inorganic flame retardants coated on the surface, and existing flame retardant compositions. Provides flame retardancy by forming a flame retardant coating on the surface of wood, and the flame retardant composition absorbs very little by the coated body when the flame retardant coating is formed. Since the speed is very slow, there is a problem of reduced work efficiency.

  However, in the case of timber structures, as mentioned above, considering that most of their life ends due to fire or biological degradation, it is possible to carry out treatments such as antiseptic and insectproofing together with flameproofing on wood. The life and performance of various structures made of wood can be dramatically improved.

  In the case of general timber buildings, the moisture content of 13 to 15% is maintained, but the moisture content changes depending on the climate and natural environment, and in rainy weather or in areas where fog frequently occurs, It can be seen that the moisture content of wood is high.

  This is an important factor when the water content of wood is high and the water-based flameproofing agent decreases the adhesion ability of the wood surface and the penetration into the wood. That is, it becomes an important factor that brings about a decrease in flameproof performance.

  Flameproofing methods for flameproofing objects include: spraying or direct coating surface treatment, metal plate or other non-combustible material on the wood surface, flameproofing agent composition or flameproofing coating on the wood surface ( and the impregnation method in which the flameproofing agent composition penetrates into the wood.

  Among the impregnation methods, the pressurization method is a method in which the flameproofing agent composition is infiltrated using vacuum and pressure, and the flameproofing agent composition can penetrate into the inside of the tree, so it is very effective. Since this method requires an autoclave, it can be applied only to the processing of small timber, and wooden buildings and large timber are difficult to process.

  In addition, the impregnation method by the non-pressurization method is not different from the spray coating method in terms of effectiveness, and can be applied only to the treatment of small timber, just like the above-mentioned pressurization method. After all, surface treatment methods in which the flame retardant composition is sprayed or painted onto the wood surface are the most practical and economical.

  In addition, as conventional general wood flameproofing agents, water-soluble inorganic salts, that is, phosphates such as ammonium phosphate and sodium phosphate, sulfates such as ammonium sulfate and sodium sulfate, borax or boric acid are used. Has been.

  These water-soluble inorganic salts are relatively excellent in flameproofing effect. However, when these chemicals are applied to wooden buildings, after drying, sparkling crystalline powder and thin white powder are formed on the wood surface. The white powder phenomenon may occur, or it may react with calcium carbonate in the water-based paint component for a long period of time to change to an insoluble and infusible salt such as calcium sulfate or calcium phosphate. As a result, the flameproofness was lowered.

  Hereinafter, the prior art and the like are as follows when the patent documents are emphasized.

  As a flame retardant used for impregnation of non-woven fabric, silk fabric, wood or paper in Patent Document 1, specifically, it has excellent fire resistance function, and unlike the flame retardant using oily raw material, the environment is less harmful. There has been disclosed a water-soluble inorganic flame retardant which does not induce pollution and has a strength increased by impregnating a non-woven fabric or the like with a flame retardant, and exhibits cold resistance, stability, water resistance and elasticity.

  Patent Document 2 contains an improved flame retardant containing guanylurea phosphate [(H2N-C (NH) -NH-C (O) -NH2) .H3PO4] (GUP) and boric acid, and these flame retardants Materials including improved wood and composite wood products and improved flame retardants are disclosed.

  In Patent Document 3, the flame retardant composition is 85 to 99% by weight of an aqueous magnesium ammonium phosphate solution, 0.1 to 5.0% by weight of a silane adhesive, 0.1 to 5.0% by weight of boric acid, borax. A water-soluble flame retardant composition and a flame retardant treatment method comprising 0.1 to 10.0% by weight and 0.1 to 10.0% by weight of ammonium phosphate are disclosed.

  Patent Document 4 is composed of guanidine phosphate, formalin, penetration enhancer, wood preservative, anticorrosive, silane coupling agent, and distilled water, and has excellent flameproofing, antiseptic and insecticidal effects, discoloration, peeling and Disclosed is a flameproofing agent composition for preserving wooden cultural properties that can prevent generation of dirt and can be expected to have an excellent antiseptic effect, and a method for producing the same.

  In Patent Document 5, there is no white flower, exfoliation, dirt, and harmfulness to the flameproofing liquid with excellent carbonization area afterflame time and afterglow time and 13 kinds of reddish blue, and it is applied to wood such as wooden cultural assets. Thus, there has been disclosed a silicone-phosphorus wood tanning flameproofing agent that can suppress the spread of flame to the maximum even if a fire occurs in wood.

  Patent Document 6 describes that flame propagation can be suppressed by applying or spraying to wood, rice straw, Korean paper, clothing, etc., and it has excellent carbonization area, afterflame time, and residual dust time. Room temperature curable presence / absence organic binder flame retardant that is not harmful to white flower, exfoliation, dirt, etc., improves flame retardance on the surface and inside / outside of the porous structure and at the same time prevents deterioration of the structure A composition is disclosed.

  Further, Patent Document 7 discloses a step of placing wood in an aqueous solution of sodium silicate (Na2SiO3) as a main agent and subjecting it to a pressure treatment; a step of placing wood in an aqueous solution of sodium silicate and performing a pressure treatment; A step in which wood is placed in an aqueous solution of boric acid (H 3 BO 3), ammonium hydrogen phosphate II ((NH 4) 2 HPO 4), or ammonium borate (NH 4 BO 3), which is an auxiliary agent; A method of applying a pressure treatment by putting wood in an aqueous solution of an agent; a method of treating a wood with flame retardancy, which imparts flame retardancy to the wood in a step of drying after the auxiliary treatment is completed is disclosed.

  However, the flame retardant treatment method for wood has an advantage that it can maintain the flameproof performance for a long period of time, but it is a method that requires a decompression condition. is there.

  In other words, it is a method of improving the flameproofing performance by forming a salt in the wood cells by flameproofing the wood divided into the main agent treatment and the auxiliary agent treatment. Although there is an advantage that it can be maintained, it is a method that requires a decompression condition, which is also possible only in the treatment of small wood, and has the disadvantage that the treatment process is complicated.

  In addition, Patent Document 8 discloses a flameproofing pigment coating method in which an acrylic resin and a pigment solvent are blended with a flameproofing agent and an acrylic resin that are applied by mixing a flameproofing agent in an amount of about 25% to 30% of the total weight. Patent Document 9 discloses a flameproof fabric to which flameproofing is imparted by a flameproofing method using a pretreatment liquid containing pullulan and a flameproofing agent.

Korean Published Patent No. 2003-0076806 Specification Korean Published Patent No. 2004-0028724 Specification Korean Open Patent No. 2008-0113651 Specification Korean registered patent No.0917665 specification Korean Registered Patent No. 1286967 Specification Korean Published Patent No. 2013-0024864 Specification Korean Published Patent No. 2013-0112102 Specification Japanese Published Patent No. 08-001077 Specification Japanese Published Patent No. 22-106377

  The conventional method for flameproofing, insecticidal and antiseptic treatment of wood structures is a method of impregnating a chemical having flameproofing performance first after impregnating the chemical having flameproofing performance and then impregnating the chemical having a component having insecticidal and antiseptic performance. Or, conversely, it has been treated by a method of impregnating a drug having insect repellent and antiseptic performance first and then impregnating and drying a chemical having flame repellent performance after drying.

  However, these methods have at least two impregnation processes and two or more drying processes, and have disadvantages such as spending a lot of processing time and cost. There is a problem that the appearance is deteriorated due to occurrence of white flower phenomenon, dirt phenomenon, gloss phenomenon, and peeling phenomenon.

  Therefore, the present invention provides flameproofing performance, antiseptic and insecticidal effects without applying white powder or white flower phenomenon by applying simple spray coating at normal temperature without decompression and pressurization on wood treated with water-based paint as well as general wood surfaces. A water-soluble flameproofing agent composition for wood that can be applied simultaneously is provided, and a method for flameproofing using the water-soluble flameproofing agent composition for wood is provided.

  The invention also provides a flameproofing agent composition having excellent carbonization area afterflame time and residual dust time and an aqueous paint so that the spread of flame can be suppressed by applying the aqueous paint to the treated wood surface. Provided is a method for flameproofing using an excellent water-soluble flameproofing agent composition for wood that is free from white flower, exfoliation, dirt and harm.

  The present invention for solving the above-mentioned problems is as follows: 60 g of ammonium phosphate is added to 300 g of distilled water (base water) and stirred for 30 minutes, 40 g of urea is added and stirred for 30 minutes, and then 40 g of phosphoric acid is added. After slowly charging and stirring for 1 hour, 60 g of silicon hydrate is added and stirred at 50 ° C. or lower for 1 hour to produce.

In addition, using this, impurities are removed from the object to be treated. When the temperature is less than 10 ° C. and when the humidity is 70% or more, avoid the flameproof treatment, and the distance during the spray operation is maintained at a distance of 40 cm or more. The spray pressure is suitably 80 to 120 kg / cm ² , and the amount of treatment at one time is 0.35 kg / m ² , and after 24 to 48 hours of drying at room temperature, the same method is used again for a total of 2 times. Flame treatment is provided to provide the convenience of the flameproof treatment method.

  In addition, after infiltrating into the wood by a non-pressure impregnation method without a decompression treatment step, after spray flameproofing treatment only with the main agent, it is naturally dried at room temperature for 24 to 48 hours without any other auxiliary treatment, Provided is a processing method characterized in that large wooden buildings and large timbers exhibit sufficient performance by spray coating and at the same time can reduce work time.

  This will be described below based on the invention described in the claims.

  According to the first aspect of the present invention; 60 g of ammonium phosphate is added to 300 g of distilled water (base water) and stirred for 30 minutes, and 40 g of urea is added thereto and stirred for 30 minutes, and then 40 g of phosphoric acid is added. Is slowly added and stirred for 1 hour, and then 60 g of silicon hydrate is added, and the mixture is stirred for 1 hour at 50 ° C. or less to produce.

According to the invention described in claim 2, when the water-soluble flameproofing agent composition for wood described in claim 1 is used to perform a flameproofing treatment on an object to be treated (wood coated with a water-based paint), Avoid spraying at temperatures below 10 ° C and humidity of 70% or higher, and maintain a distance of 40 cm or more from the object to be processed, with a spray pressure of 80 to 120 kg / cm ² and a throughput of 0.35 kg / m ² for primary spray application. A step of drying at a normal temperature for 24 to 48 hours after the completion of the primary spray coating; and a step of performing a secondary spray coating on the dried processing object under the same conditions and method as the primary spray. And

  According to the invention described in claim 3, the composition contains an Si content of 0.1 to 1.5 wt%, an N content of 0.5 to 3.5 wt%, and a P content of 0.8 to 2.5 wt%. It is characterized by comprising a flameproofing agent composition.

  According to a fourth aspect of the present invention, the present invention is characterized by a flameproof treatment method in which a wood flameproofing step is performed so as to penetrate into the wood by a non-pressure impregnation method without a decompression treatment step.

  According to the invention described in claim 5, in the flame-proofing method for wood, after applying a spray and a brush to wood coated with general wood and water-based paint and passing through a drying process, flameproof performance and white flower, It is characterized by a flameproof treatment method that does not cause dirt, gloss, or waterborne paint peeling.

  According to the invention described in claim 6, in claim 1, after the flameproofing agent composition described in claim 1 is flameproofed with a spray and a brush, the room temperature is obtained without any other auxiliary treatment. It is characterized by being naturally dried for 24 to 48 hours.

  According to the invention described in claim 7, since large wooden buildings and large timbers are difficult to be processed by the pressure method, spray coating provides sufficient flameproofing performance and at the same time shortens the working time. To do.

  In the present invention, an alkyl [alkyl] or alkoxy [alkoxy] group of a silicone compound has a forming reaction to a hydroxy functional silicone by a phosphorus compound, and the functional silicone and the phosphorus compound By forming an electrostatic bond and bonding with silicone having a lower surface tension, surface treatment properties and dispersibility can be improved, and it is possible to impart excellent flameproofness by penetrating into the wood only by spray coating.

  Further, in the present invention, due to the low surface energy of silicone, transition occurs on the surface when heated by a fire source, pyrolyzing at a higher temperature to form a SiO2 protective layer, and phosphorus is char (carbonized layer, hereinafter referred to as char) By protecting the char where the silicone is formed, the heat transfer from the fire source and additional combustion are prevented by synergistic effects with each other, and the thermal decomposition of the wood is delayed, and excellent flameproof performance is expected it can.

  In addition, the present invention can treat a flameproofing agent composition by simple spray coating on a wood surface treated with a water-based paint, in particular, it can be easily penetrated during the treatment, and there is no change in the hue of the water-based paint. Since it can be expected to have the advantage of not producing dirt and luster and the effect of flameproofing, antiseptic and insecticidal, it can shorten working time, greatly reduce human resources and costs, and can expect considerable economic benefits.

  In addition, the present invention provides a simple and quick method of natural drying for 24 to 48 hours at room temperature without any other auxiliary treatment after the flameproof treatment by the spray method (surface coated with water-based paint). In comparison with the existing work where the flameproofing agent is hardly treated by the spray method on the top, it is possible to expect benefits and effects that can simultaneously reduce the work time and provide an economic effect.

  Further, the present invention can be expected to have the same effect as the case of wood to which the water-based paint is applied even when applied to general wood that has not been treated with the water-based paint.

The flowchart which showed roughly the process of the flame-proof processing method by this invention Photograph showing carbonization (Char) formation according to the present invention Photo of the result of XRD analysis to confirm the crystal structure of char formed on a wood specimen after carbonization test by applying a silicone-phosphate flame retardant to the wood specimen. Photograph showing surface energy of water-soluble flame retardant composition for wood Photo showing surface energy of flame retardant composition for wood Photograph showing before / after processing of general wood and wood coated with water-based paint Photograph showing one use example of the present invention

  The present invention comprises a flameproofing agent as a reaction product utilizing various functional groups of silicon hydrate, a silicone compound having a flameproofing effect and a flameproofing phosphorus compound, and a water-based paint is treated. When applied to a wood surface, a water-soluble flame retardant composition for wood that can be easily penetrated into the interior of the wood just by spray coating, and a spray-proof coating using the water-soluble flame retardant composition for wood described above. The present invention is characterized by providing a flameproof treatment method that can easily handle large wooden buildings, wood, and the like with a flame treatment method, and that can save work time and work time.

  The process of flameproofing using the wood-based water flameproofing agent is as follows.

Impurities are removed from the object to be treated, and when the temperature is less than 10 ° C. and when the humidity is 70% or more, avoid the flameproof treatment, maintain a distance of 40 cm or more when spraying the flameproofing agent composition, and the spray pressure is 80-120 kg / cm < ² > is suitable, and the amount of treatment at one time is 0.35 kg / m < ² >. After drying at room temperature for 24 to 48 hours, flameproofing treatment is again performed twice in total by the same method.

  Further, the flameproofing agent containing a Si content of 0.1 to 1.5 wt%, an N content of 0.5 to 3.5 wt%, and a P content of 0.8 to 2.5 wt% in the flameproofing liquid composition By forming an electrostatic bond between a functional silicone and a phosphorus compound, a white silicone compound phosphorus flame retardant composition and cellulose, hemicellolose and lignin are crosslinked by forming a composition. Provided is a flameproofing agent composition that forms a firmer carbonized film by improving performance.

  The silicone-phosphorus flame retardant based on the structure of the silicone-phosphorus flame retardant simultaneously exhibits the performance of the organic phosphate flame retardant composition and the properties of the inorganic silicone flame retardant composition, The organic phosphate flame retardant mechanism is that the organic phosphate flame retardant composition primarily forms phosphoric acid by thermal decomposition, and such phosphoric acid forms pyrophosphate and water through a condensation reaction. Let

  In the flameproofing agent composition containing phosphorus, the reaction mainly occurs in the condensed phase, and phosphoric acid extracts water in the condensed phase from the thermal decomposition of the substrate to form char.

(Chemical formula 1)
Char formation example

  The water produced by the reaction has an effect of diluting the oxidized gas phase that assists ignition, and in the case of phosphoric acid and pyrophosphate produced at this time, it can catalyze the dehydration reaction of the terminal alcohol group.

  It promotes the dehydration reaction of the terminal alcohol groups contained in cellulose, hemicellolose and lignin, which are the main main components of wood, to generate water again, and at the same time generate a carbon-carbon double bond. This double bond forms a char layer by cross-linking at high temperature to separate and protect the surface of the adherend from the flame, thereby suppressing new radical generation related to ignition, volatilization of plastics, oxygen diffusion Suppression, heat dissipation from flame, and formation of a flameproof layer can be provided (see FIG. 1).

  FIG. 2 shows the result of XRD analysis to confirm the crystal structure of char formed on a wood specimen after applying a silicone-phosphate flame retardant to the wood specimen and performing a carbonization test. However, the synthesized silicone-phosphate flame retardant showed a peak indicating a form of an amorphous structure with 2θ of 25.

  Table 1 shows the results of analyzing XRF in order to apply a silicone-phosphate flame retardant to the wood specimen and confirm the components of char formed on the wood specimen after the carbonization test. As shown in Table 1, the P ratio was the highest at 65.41%, and it was found that Si was 29.30%, K was 5.01%, and S was 0.28%. As a result of XRF analysis of the char component generated by foaming, the presence of Si and P was confirmed.

(Table 1)

  As mentioned above, silicone compounds can maximize the flameproofing effect by phosphate char formation, as seen in the hydroxy group bond of wood cellulose, treat the water-based paint to protect the wood, aesthetics It has the advantage that it can be protected from various wind damages without being damaged by various microorganisms and insects.

  In addition to the flameproofing property of phosphorus when bonded to silicone compounds, the bondability with silicone with lower surface tension can improve the processability and dispersibility of the surface that can be easily treated with spray (and brush). Thus, the flameproofing agent composition penetrates into the water-based paint layer of wood treated with the water-based paint, and is absorbed from the surface of the wood to the depth, and exhibits a flameproof effect when in contact with a fire source. (Figs. 4 and 5)

  Hereinafter, specific embodiments of the present invention will be described in detail through test result values and the like.

[Example 1]
Based on 300 g of distilled water (base water) in a 500 ml three-necked round bottom flask equipped with a stirrer, thermometer, condenser, and 60 g of ammonium phosphate, and stirred for 30 minutes.
After 40 g of urea was added and stirred for 30 minutes,
After slowly adding 40 g of phosphoric acid and stirring for 1 hour, 60 g of silicon hydrate was added and stirred at 50 ° C. or lower for 1 hour to produce a flameproofing agent composition.

  In addition, the flameproofing agent composition as described above was subjected to a flameproofing treatment by a spray method at room temperature, avoiding the flameproofing treatment when the temperature was less than 10 ° C. and when the humidity was 70% or more.

This will be described more specifically.
First, an object to be treated for flameproofing treatment (wood coated with water-based paint) removes impurities, avoids flameproofing treatment when the temperature is less than 10 ° C. and humidity is 70% or more, and spray pressure 80 applied to the processing object with ~120kg / cm ^2.

At this time, the distance from the object to be processed is maintained at a distance of 40 cm or more, the amount of treatment is 0.35 kg / m ² , and primary spray coating is performed.

  When the primary spray application is completed, the film is dried at room temperature for 24 to 48 hours and sufficiently cured, and then subjected to secondary spray application under the same conditions and method as the primary spray, and subjected to a flameproof treatment twice in total.

  The test results when the moisture content of the fireproofed wood test piece is 15% are as follows.

[Hazardous substances and basic physical property tests]
1) Content of VOCs 10 mL of a flame retardant composition was placed in a head space vial, heated at 90 ° C. for 30 minutes, and air generated in the head space was injected into the GC / MS for measurement. The concentrations of the measured quantitative substance and the unknown substance such as toluene were combined and calculated by the VOC content.
-Device name: Headspace sampler (Perkin-elmer, USA),
Tarac GC / DSQMS (ThermoFinnigan, USA)

2) Formaldehyde emission amount Flame retardant composition was applied to both sides of test piece (70mm x 150mm, 8 sheets) and placed in a desiccator containing 300ml of distilled water, maintained at 23 ° C for 24 hours and contained in distilled water The formed formaldehyde was developed and measured with a UV absorptiometer (UV-1650PC, SHIMADZU).

3) Heavy metal content (Pb, Cd, Hg, Cr6 +)
Acetone is added to the flameproofing agent composition, and the solid content is separated by centrifugation. The solid sample is dried by adding hydrochloric acid and stirring at 30 ° C. for 15 minutes, and the liquid sample is all dried by adding nitric acid. Then, each solution was filled to 50 ml with distilled water, and each solution was analyzed using ICP, AAS, and UV absorptiometer.

4) Hydrogen ion concentration (pH)
The flame retardant composition was measured with a pH meter.

5) The specific gravity specific gravity bottle was filled with the flameproofing agent composition, and the measurement was performed using the difference in weight between the front and back.

The values of this test result are as shown in Table 2 below.
(Table 2)
Presence / absence of hazardous substances and basic physical property test results

[Weather resistance test]
1) Accelerated weather resistance test conditions After the test piece coated with the flameproofing agent composition was dried for 7 days or more, it was placed in an accelerated weather resistance tester and tested under the following conditions.
-Equipment name: accelerated weathering tester UV2000 (ATLAS, USA),
Color difference meter I-7 (McBath, UK)
Test cycle: UV 50 ° C., 4 h → condensation 40 ° C., 4 h
-Cycle repetition: 25 times, total 200 hours-Irradiance: 0.63 W / m2
-Lamp type: UV-A 340 nm

2) Measurement item-appearance: A comparison between before and after the accelerated weathering test was conducted, and whiteness, peeling, dirt, and gloss phenomenon were judged with the naked eye of the tester to confirm the presence or absence of abnormality.
-Comparison color difference: The color difference value is obtained by measuring the chromaticity before and after the test using a color difference meter on the test piece coated with the flame retardant composition and the blank test piece not coated with the flame retardant composition. The difference between the color difference value of the test piece coated with the flameproofing agent composition and the color difference value of the blank test piece not coated with the flameproofing agent composition is less than 3.0 for each test piece, and the average for each aqueous paint color Was less than 1.5.

The values of this test result are as shown in Table 3 below.
(Table 3)
Weather resistance test results

[Flameproof test]
1) Test conditions for flameproof evaluation-Device name: Flameproof tester (FL-45MC, SUGA test instrument)
-Flame length: 65mm
-Heating time: 2 minutes

2) Measurement items and criteria-Afterflame time: The time from when the flame of the burner is removed until the flame burns off and within 10 seconds-Residual time: After removing the burner flame, the flame is not raised Time until burning stops, within 30 seconds-Carbonized area: Area of the carbonized portion of the test piece (wood) after the test, 50 cm ² .
(Measuring equipment: PLANIX EX (TAMAYA technologies Inc., JAPAN))
-Carbonization length: The length of the carbonized part of the test piece (wood) after the test, 20 cm.

The test result values are shown in Table 4 below.
(Table 4)
Flameproof test results

[Residuality test]
1) Test conditions for evaluation of residual property-weather resistance test: A test piece coated with a flameproofing agent composition is placed in an accelerated weather resistance tester, and an accelerated weather resistance test is performed under the following conditions.
-Flameproof test: A flameproof test is performed on the test piece subjected to the accelerated weathering test.
-Device name: Accelerated weathering tester UV2000 (ATLAS, USA)
Test cycle: UV 50 ° C., 4 h → condensation 40 ° C., 4 h
-Cycle repetition: 25 times, total 200 hours-Irradiance: 0.63 W / m ²
-Lamp type: UV-A 340 nm
-Device name: Flame retardant tester (FL-45MC, SUGA test instrument)
-Flame length: 65mm
-Heating time: 2 minutes

2) Measurement items and criteria-Afterflame time: The time from when the flame of the burner is removed until the flame burns off and within 10 seconds-Residual time: After removing the burner flame, the flame is not raised Time until burning stops, within 30 seconds-Carbonized area: Area of the carbonized portion of the test piece (wood) after the test, 55 cm ²
(Measuring equipment: PLANIX EX (TAMAYA technologies Inc., JAPAN))
-Carbonization length: the length of the carbonized part of the test piece (wood) after the test, 25 cm

The values of this test result are as shown in Table 5 below.
(Table 5)
Persistence test results

[Hygroscopic and drying test]
A test piece to which the flameproofing agent composition is applied and a blank test piece to which the flameproofing agent composition is not applied are respectively placed in a thermo-hygrostat and tested under the following conditions.

1) Constant temperature and humidity test conditions-device name: constant temperature and humidity chamber WK-340 (WEISS, German), color difference meter I-7 (McBath, UK)
Test cycle: (50 ± 2) ° C., (95 ± 3)% R.D. H. , 4h
→ (20 ± 2) ℃, 1h
→ (60 ± 2) ℃, 8h
→ (20 ± 2) ℃, 1h
-Cycle repetition: 10 times, total 140 hours

2) Measurement item-appearance: Comparison between before and after the accelerated weathering test, and the presence of abnormality was confirmed by judging the whiteness, peeling, and dirt phenomenon with the naked eye of the tester.
-Comparison color difference: The color difference value was calculated | required by measuring the chromaticity before and behind a test piece which apply | coated the flameproofing agent composition, and the blank test piece which has not applied the flameproofing agent composition using a color difference meter.
-The difference between the color difference value of the test piece coated with the flameproofing agent composition and the color difference value of the blank test piece not coated with the flameproofing agent composition is less than 3.0 for each test piece, It was less than 1.5.

The values of the test results are as shown in Table 6 below.
(Table 6)
Moisture absorption and drying test results

[Nonwoven fabric test]
-Marked at a distance of 25 mm and 10 mm from one end in the length direction of the test piece.
-A flame was applied to one end of the specimen for 30 seconds, the time from when the flame passed the 25 mm marking display to the arrival at the 100 mm marking line was measured, and the velocity was calculated.

<Evaluation criteria>
When a test piece having a thickness of 3.0 mm or more has a burning rate of 40 mm / min or less, a test piece having a thickness of less than 3.0 mm has a burning rate of 75 mm / min or less, HD grade was given.

The values of this test result are as shown in Table 7 below.
(Table 7)
Nonwoven test results

The following are the results of the quasi-incombustibility test for antiseptic, insecticidal, antifungal, and wood in Example 1.
(Table 8)
Antiseptic performance test

<Semi-incombustible test results>
(Table 9-1)
1. Sample name: Flame-proof wood

(Table 9-2)
2. Test results

  As shown in the above test results, it is judged that there are some effects of antiseptic and mildewproofing, and in the case of a quasi-incombustible test, the test piece itself is a flammable substance, which is insufficient as a test piece in the quasi-incombustible test. It is judged that the performance of the flame retardant material is sufficient.

[Example 2]
A test piece was manufactured by the same flameproofing method using the same flameproofing agent composition as in Example 1, and tested by the same test method as in Example 1.

  However, the test results when the moisture content of the wood (test piece) is 30% are as follows.

(Table 10)
Weather resistance test results

(Table 11)
Flameproof test results

(Table 12)
Persistence test results

(Table 13)
Moisture absorption and drying test results

[Example 3]
A test piece was manufactured by the same flameproofing method using the same flameproofing agent composition as in Example 1, and tested by the same test method as in Example 1.

However, the test results when the moisture content of the wood (test piece) is 50% are as follows.
(Table 14)
Weather resistance test results

(Table 15)
Flameproof test results

(Table 16)
Persistence test results

(Table 17)
Moisture absorption and drying test results

[Example 4]
A test piece was manufactured by the same flameproofing method using the same flameproofing agent composition as in Example 1, and tested by the same test method as in Example 1.

However, the test results when the moisture content of the wood (test piece) is 70% are as follows.
(Table 18)
Weather resistance test results

(Table 19)
Flameproof test results

(Table 20)
Persistence test results

(Table 21)
Moisture absorption and drying test results

[Experiment and experimental results]
Table 22 below shows the results of the flame retardant composition for a wooden building produced by polymerizing silicone and a phosphorus compound produced as described above, based on the test standards for flame retardant composition.
(Table 22)

  In general, in the case of timber buildings, the moisture content is maintained at 13 to 15%, and the moisture content changes according to the climate and natural environment. It can be seen that the moisture content of the wood is relatively high.

Therefore, the present invention compares the flameproof performance during the flameproofing treatment according to the moisture content of the wood, and the result shows that the flameproof performance is lowered when the moisture content of the wood is 70% or more.

Claims (3)

60 g of ammonium phosphate was added to 300 g of distilled water and stirred for 30 minutes. After 40 g of urea was added and stirred for 30 minutes, 40 g of phosphoric acid was slowly added and stirred for 1 hour. A water-soluble flame retardant composition for wood, which is produced by adding 60 g of a product and stirring the mixture at 50 ° C. or lower for 1 hour. Using the water-soluble flameproofing agent composition for wood according to claim 1, when subjecting a treatment object (wood coated with a water-based paint) to flameproofing,
Avoid spraying when the temperature is less than 10 ° C or when the humidity is 70% or higher, and maintain a distance of 40 cm or more from the object to be processed, and a primary spray at a spray pressure of 80 to 120 kg / cm ² and a processing amount of 0.35 kg / m ² A step of applying, after completion of the primary spray application, a step of drying at room temperature for 24 to 48 hours; and a step of applying a secondary spray to the dried processing object under the same conditions and method as the primary spray. A method for flameproofing a water-soluble flameproofing agent composition for wood. After using the water-soluble flame retardant composition for wood according to claim 1 and performing a flameproof treatment with a spray and a brush, it is naturally dried at room temperature for 24 to 48 hours without any other auxiliary treatment. A method for flameproofing a water-soluble flameproofing agent composition for wood.

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