CN100567456C - A kind of fire retardant and preparation method thereof - Google Patents
A kind of fire retardant and preparation method thereof Download PDFInfo
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- CN100567456C CN100567456C CNB2007101222432A CN200710122243A CN100567456C CN 100567456 C CN100567456 C CN 100567456C CN B2007101222432 A CNB2007101222432 A CN B2007101222432A CN 200710122243 A CN200710122243 A CN 200710122243A CN 100567456 C CN100567456 C CN 100567456C
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Abstract
The invention discloses a kind of fire retardant and preparation method thereof, this fire retardant comprises following raw materials in weight portion: phosphoric acid: 0.5-1.3; Urea: 0.3-0.6; Catalyzer: 0.002-0.004.Fire retardant of the present invention carries out polyreaction by phosphoric acid and urea and is prepared into liquor or pulvis under the effect of catalyzer.Preparation method's simple and fast of fire retardant of the present invention, low cost of manufacture, easy to use.Fire retardant of the present invention is a kind of aq. type nitrogen phosphorus inorganic combustion inhibitor, the effect with potion economic benefits and social benefits, and not only flame retardant effect is remarkable, and has the effect of the formaldehyde of significantly dissolving.More than 50%, smoke suppressing is good, and the flue gas that produces is nontoxic by the flame-retardant plywood oxygen index of fire retardant of the present invention preparation.The environmental-protecting performance of fire retardant can be stabilized in E
0Level (≤0.5mg/L).
Description
Technical field
The present invention relates to a kind of fire retardant material and preparation method thereof, particularly a kind of flame retarded formulations that is used for timber and preparation method thereof.
Background technology
Timber and wood-based plate are widely used in interior decoration, furniture manufacturing, building construction and the extraneous adornment, and these materials belong to combustible matl, very easily cause fire, and the anti-flaming function that how to improve material has become the problem of whole world extensive concern.
At present, the most popular method that prevents timber and wood-based plate presence of fire is to use fire retardant in these materials, these fire retardants are mostly based on compounds such as phosphorous, nitrogen, boron, aluminium and halogens, inorganic combustion inhibitor owing to have good flame resistance, do not produce toxic gas (except the halogen flame), do not separate out, characteristics such as non-volatile, cheap, wide material sources, security height are used widely.
For example, (author: Li Yanyun etc.) disclose a kind of phosphorus-nitrogen is inorganic combustion inhibitor to the article of delivering on " fine chemistry industry " 2000 the 2nd phases " Wood fire retardant treatment process research ", and it mainly is the fire resistant fluid that is made into by a certain percentage by Dyhard RU 100, formaldehyde, urea, primary ammonium phosphate.This inorganic combustion inhibitor mainly uses with solution morphology, as by timber is flooded, obtains flame retardant effect.Phosphorus-nitrogen flame retardant has fire-retardant synergy, reduces decomposition temperature, increases the generation of charcoal, effects such as the generation of minimizing inflammable gas and reduction heat.Because phosphorus-nitrogen flame retardant more and more comes into one's own it to the friendly of environment, but this fire retardant has formaldehyde to exist, and formaldehyde is carcinogenic substance, therefore easily environment is produced and pollutes.
Open day be to disclose a kind of wood fire retardant and preparation method thereof in July 10, publication number in 1996 Chinese patent application that is CN1126234A, this fire retardant is mixed by urea, phosphoric acid, borax, formaldehyde etc., can add in the urea-formaldehyde resin adhesive at this fire retardant of wood-based plate preparation process and plays fire retardation; Open day be to disclose a kind of fire-proof flame-retarded agent in April 5, publication number in 2000 Chinese patent application that is CN1249325A, this fire retardant is mixed by urea, phosphoric acid, borax, boric acid etc., is applicable to the fire-retardant of inflammable substance such as cotton, chemical fibre, paper, timber.Though disclosed fire retardant has the simple low cost and other advantages of manufacture method in the above-mentioned document, it contains toxic substances such as boron class, formaldehyde, is unfavorable for environmental protection.
Open day be to disclose a kind of phosphor nitrogen composite combustion inhibitor in July 26, publication number in 2006 Chinese patent application that is CN1807552A, this fire retardant carries out adding behind the chemical reaction neutralizing agent such as ammonia by urea and phosphoric acid again and carries out neutralization reaction and make, be applicable to the fire-retardant of inflammable substance such as textiles and timber-work, the preparation method of this fire retardant is simpler relatively, safety and environmental protection.
Summary of the invention
The purpose of this invention is to provide a kind of possessing of timber fire retardant of formaldehyde effect and preparation method thereof of dissolving that is used for, this fire retardant is colourless, do not have and smell, and itself is nontoxic, have smoke suppressing, and preparation cost is low.
For realizing the object of the invention, the invention provides a kind of fire retardant, comprise following weight part proportioning raw material:
Phosphoric acid (concentration is 85%) 0.5-1.3
Urea 0.3-0.6
Catalyzer 0.002-0.004
It is formulated that wherein catalyzer adopts following raw materials in weight portion: tin chloride 0.8-1.2; Copper sulfate 1.5-2.5; Sodium-chlor 0.8-1.2; Iron(ic) chloride 0.8-1.2; Tai-Ace S 150 0.8-1.2; Boric acid 0.8-1.2; Zinc chloride 1.5-2.5.
Particularly, the weight part proportioning of fire retardant raw material is selected:
Phosphoric acid (concentration is 85%) 0.7-1.1
Urea 0.35-0.45
Catalyzer 0.0025-0.0035
Particularly, comprise also in the raw material of fire retardant of the present invention that weight part is the softening water of 0.7-1.8, the preferred 0.9-1.6 of softening water weight part.
For realizing the object of the invention, the invention provides a kind of preparation method of fire retardant, comprise making phosphoric acid and urea under the effect of catalyzer, carry out polyreaction.
Particularly, described reaction comprises following step in sequence:
1) in reactor, adds phosphoric acid, stir heating simultaneously, make temperature rise to 50-60 ℃;
2) add urea, the mixture of phosphoric acid and urea is stirred, make material distribute, be heated evenly;
When 3) temperature rises to 90-120 ℃, in reactor, add catalyzer, continue heating;
4) make temperature rise to 130-140 ℃ after, stop the heating;
5) make reactant be cooled to 60-80 ℃, in reactor, add softening water, stir.
Wherein, the temperature of softening water is 40-60 ℃.
Particularly, the preparation method of fire retardant of the present invention comprises following step in sequence:
1) in reactor, adds phosphoric acid, stir heating simultaneously, make temperature rise to 50-60 ℃;
2) add urea, the mixture of phosphoric acid and urea is stirred, make material distribute, be heated evenly;
When 3) temperature rises to 90-120 ℃, in reactor, add catalyzer, continue heating;
4) make temperature rise to 130-150 ℃ after, when the reactant volume increases to 2-2.5 times of original volume, stop heating;
5) product in the reactor is poured out, treated behind its cooling curing it to be ground into powdery.
Particularly, in above-mentioned steps 4) in the reactant volume stop described heating when increasing to original 2-2.5 times.
Particularly, in above-mentioned steps 3) in temperature rise to 110-120 ℃, described stirring velocity is controlled at 50-70 rev/min.
Fire retardant of the present invention is a kind of aq. type nitrogen phosphorus inorganic combustion inhibitor, its advantage applies in the following areas:
1) fire retardant of the present invention has the effect of potion economic benefits and social benefits, not only flame retardant effect is remarkable, and has an effect of the formaldehyde of significantly dissolving, by evidence at aspects such as wood-based plate, textiles, paper, the flame retardant properties of fire retardant of the present invention is fine, and the flame-retardant plywood oxygen index of the preparation of using is more than 50%.Environmental-protecting performance can be stabilized in the E0 level (≤0.5mg/L).
2) main raw material of preparation fire retardant of the present invention all belongs to the nontoxicity industrial chemicals, produce and use in all can toxigenicity and harm humans health and environment, compliance with environmental protection requirements.
3) smoke suppressing of fire retardant of the present invention is good, and the flue gas that produces is nontoxic, and with the medium density fibre board (MDF) of its preparation, its smoke density grade SDR only is 24 after testing, and that stipulates in the GB GB/T8627 is lower than 75 index.
4) fire retardant of the present invention colourless, do not have and to smell, with the article of its processing, can not change or hide the original decorative colour of article, texture, can not produce any peculiar smell, so the situation of article grade can not occur reducing.
5) fire retardant pulvis of the present invention is water-soluble very good, under normal temperature condition, its dissolving can be obtained concentration up to 40% solution.
6) preparation method of fire retardant of the present invention is simple, so the cost of finished product is low.The liquid flame retardant manufacturing cost of the present invention of 1 ton of solid content 50 ± 2%: industrial chemicals is 2150 yuan, and other manufacturing costs such as water, electricity, vapour, depreciation of equipment, overheads, wage for workmen are 450 yuan, add up to 2600 yuan/ton; The price of pulvis then is 5200 yuan/ton, and well below the price of existing domestic and international fire retardant, cost is respectively the 1/2-1/3 of existing domestic fire retardant, the 1/10-1/20 of external fire retardant.
Embodiment
Below in conjunction with specific embodiment the present invention is done detailed description.
Embodiment 1
1) carrying out raw material by following weight proportion gets the raw materials ready:
Softening water (hardness is lower than 8 degree) 1.3kg
Phosphoric acid (concentration is 85%) 1.0kg
Urea (content 99%) 0.5kg
Catalyzer: 0.0035kg
Wherein, catalyzer is the pistac pulvis that prepare voluntarily Beijing Forestry University's Materials science and technical college environmental protection flame retardant technique center, raw material comprises tin chloride 1 weight part, copper sulfate 2 weight parts, sodium-chlor 1 weight part, iron(ic) chloride 1 weight part, Tai-Ace S 150 1 weight part, boric acid 1 weight part, zinc chloride 2 weight parts, and it is ground evenly back mixing.
2) in the reactor of being furnished with agitator, thermometer and prolong, add the phosphoric acid in the reaction raw materials, stir heating simultaneously, stirring velocity is controlled to be 50 rev/mins, makes temperature rise to 60 ℃;
3) in reactor, add whole urea, simultaneously the mixture of phosphoric acid and urea is proceeded to stir, make material distribute, be heated evenly;
When 4) making temperature rise to 120 ℃, slowly evenly add catalyzer in reactor, mixture is reacted, reaction mass becomes light green;
5) after the continuation heating makes temperature reach 135 ℃, observing response phenomenon in the time of heating, along with temperature raises, light green liquid becomes the oyster white dope gradually, foam sharply increases, rate of rise in temperature is obviously accelerated, the volume of material expands rapidly, and prolong has a large amount of gases to discharge, and the volume of question response still internal reaction thing stops heating when increasing to the twice of original volume, continue to stir, material in reactor relies on the heat release of self at vigorous reaction, and temperature continues to rise, and question response tends to be steady, when temperature begins to descend, show that reaction finishes;
6) be cooled to 70 ℃, the adding temperature is 50 ℃ a softening water in reactor, stirs;
7) it is standby to pour products therefrom into containers store.
The technical indicator of product:
Outward appearance: transparent liquid
Solid content (%) 48
PH value 5.8
Viscosity (being coated with-4 glasss) (25 ℃, S) 10.94
Proportion (g/cm
3) 1.26
Time limit (year) 2 is arranged
Embodiment 2
1) carrying out raw material by following weight proportion gets the raw materials ready:
Softening water 1.8kg
Phosphoric acid (concentration is 85%) 1.3kg
Urea (content 99%) 0.54kg
Catalyzer: 0.0038kg
Catalyzer is identical with catalyzer among the embodiment 1.
2) in the reactor of being furnished with agitator, thermometer and prolong, add the phosphoric acid in the reaction raw materials, stir heating simultaneously, stirring velocity is controlled to be 50 rev/mins, makes temperature rise to 50 ℃;
3) in reactor, add urea, simultaneously the mixture of phosphoric acid and urea is proceeded to stir, make material distribute, be heated evenly;
4) continue to heat when making temperature rise to 115 ℃, in reactor, slowly evenly add catalyzer, mixture is reacted;
5) after the continuation heating makes temperature reach 135 ℃, observing response phenomenon when continuing heating, along with temperature raises, light green liquid becomes the oyster white dope gradually, foam sharply increases, rate of rise in temperature is obviously accelerated, the volume of material expands rapidly, and prolong has a large amount of gases to discharge, and the volume of question response still internal reaction thing stops heating when increasing to the twice of original volume, continue to stir, material in reactor relies on the heat release of self at vigorous reaction, and temperature continues to rise, and question response tends to be steady then that temperature no longer rises, when temperature begins to descend, show that reaction finishes;
6) be cooled to 80 ℃, the adding temperature is 60 ℃ a softening water in reactor, stirs.
7) it is standby to pour products therefrom into containers store.
The technical indicator of product:
Outward appearance: transparent liquid
Solid content (%): 45
PH value: 5.2
Viscosity (being coated with-4 glasss) (25 ℃, S) 10.85
Proportion (g/cm
3) 1.2
Time limit (year) is arranged: 2
Embodiment 3
1) carrying out raw material by following weight proportion gets the raw materials ready:
Softening water 1kg
Phosphoric acid (concentration is 85%) 0.65kg
Urea (content 99%) 0.38kg
Catalyzer: 0.0028kg
Wherein, catalyzer is the pistac pulvis that prepare voluntarily Beijing Forestry University's Materials science and technical college environmental protection flame retardant technique center, raw material comprises tin chloride 0.8 weight part, copper sulfate 2.5 weight parts, sodium-chlor 1.2 weight parts, iron(ic) chloride 0.8 weight part, Tai-Ace S 150 0.8 weight part, boric acid 0.8 weight part, zinc chloride 1.5 weight parts, and it is ground evenly back mixing.
2) in the reactor of being furnished with stirrer, temperature and pressure indicating meter and prolong, add the phosphoric acid in the reaction raw materials, stir heating simultaneously, the control stirring velocity is 70 rev/mins, makes temperature rise to 60 ℃;
3) in reactor, add urea, the mixture of phosphoric acid and urea is proceeded to stir, make material distribute, be heated evenly;
4) continue to heat when making temperature rise to 110 ℃, in reactor, slowly evenly add catalyzer, mixture is reacted;
5) after the continuation heating makes temperature reach 130 ℃, observing response phenomenon when continuing heating, along with temperature raises, light green liquid becomes the oyster white dope gradually, foam sharply increases, and rate of rise in temperature is obviously accelerated, and the volume of material expands rapidly, prolong has a large amount of gases to discharge, be mainly ammonia and water vapour, water absorbs, and the volume of question response still internal reaction thing stops heating when increasing to the twice of original volume, continue to stir, material in reactor relies on the heat release of self at vigorous reaction, and temperature continues to rise, and question response tends to be steady then that temperature no longer rises, when temperature begins to descend, show that reaction finishes;
6) be cooled to 80 ℃, the adding temperature is 60 ℃ a softening water in reactor, stirs;
7) it is standby to pour products therefrom into containers store.
The technical indicator of product:
Outward appearance: transparent liquid
Solid content (%): 46
PH value: 5.6
Viscosity (being coated with-4 glasss) (25 ℃, S) 11.2
Proportion (g/cm
3) 1.25
Time limit (year) is arranged: 2
Embodiment 4
1) carrying out raw material by following weight proportion gets the raw materials ready:
Softening water 0.70kg
Phosphoric acid (concentration is 85%) 0.5kg
Urea (content 99%) 0.32kg
Catalyzer: 0.0025kg
Catalyzer wherein is with embodiment 3.
2) in the reactor of being furnished with stirrer, temperature and pressure indicating meter and prolong, add the phosphoric acid in the reaction raw materials, stir heating simultaneously, the control stirring velocity is 70 rev/mins, makes temperature rise to 60 ℃;
3) in reactor, add urea, continue heating;
When 4) making temperature rise to 110 ℃, in reactor, slowly evenly add catalyzer, mixture is reacted;
5) after the continuation heating makes temperature reach 130 ℃, observing response phenomenon when continuing heating, along with temperature raises, light green liquid becomes the oyster white dope gradually, foam sharply increases, and rate of rise in temperature is obviously accelerated, and the volume of material expands rapidly, prolong has a large amount of gases to discharge, be mainly ammonia and water vapour, water absorbs, and the volume of question response still internal reaction thing stops heating when increasing to the twice of original volume, continue to stir, material in reactor relies on the heat release of self at vigorous reaction, and temperature continues to rise, and question response tends to be steady then that temperature no longer rises, when temperature begins to descend, show that reaction finishes;
6) be cooled to 80 ℃, the adding temperature is 60 ℃ a softening water in reactor, stirs;
7) it is standby to pour products therefrom into containers store.
The technical indicator of product:
Outward appearance: transparent liquid
Solid content (%): 49
PH value: 6.0
Viscosity (being coated with-4 glasss) (25 ℃, S) 11.5
Proportion (g/cm
3) 1.28
Time limit (year) is arranged: 2
Embodiment 5
1) carrying out raw material by following weight proportion gets the raw materials ready:
Phosphoric acid (concentration is 85%) 0.75kg
Urea (content 99%) 0.4kg
Catalyzer: 0.003kg
Wherein, catalyzer is the pistac pulvis that prepare voluntarily Beijing Forestry University's Materials science and technical college environmental protection flame retardant technique center, raw material comprises tin chloride 1.2 weight parts, copper sulfate 1.5 weight parts, sodium-chlor 0.8 weight part, iron(ic) chloride 1.2 weight parts, Tai-Ace S 150 1.2 weight parts, boric acid 1.2 weight parts, zinc chloride 2.5 weight parts, and it is ground evenly back mixing.
2) in the reactor of being furnished with stirrer, temperature and pressure indicating meter and prolong, add the phosphoric acid in the reaction raw materials, stir heating simultaneously, the control stirring velocity is 70 rev/mins, makes temperature rise to 60 ℃;
3) in reactor, add urea, continue heating;
When 4) making temperature rise to 110 ℃, in reactor, slowly evenly add catalyzer, mixture is reacted;
5) after the continuation heating makes temperature reach 130 ℃, observing response phenomenon in the time of heating, along with temperature raises, light green liquid becomes the oyster white dope gradually, foam sharply increases, and rate of rise in temperature is obviously accelerated, and the volume of material expands rapidly, prolong has a large amount of gases to discharge, be mainly ammonia and water vapour, water absorbs, and the volume of question response still internal reaction thing stops heating when increasing to the twice of original volume, continue to stir, material in reactor relies on the heat release of self at vigorous reaction, and temperature continues to rise, and question response tends to be steady then that temperature no longer rises, when temperature begins to descend, show that reaction finishes;
6) the oyster white dope in the reactor being poured out, be placed in the ventilating kitchen, was cooling curing after 30-60 minute, pulverized with pulverizer then and can obtain powdered fire retardant product.
7) products therefrom being put into plastic bag sealing stores for future use.
The technical indicator of product:
Outward appearance: white powder
Solid content (%): 100
Proportion (g/cm
3) 2.3
Time limit (year) is arranged: 5
Embodiment 6
1) carrying out raw material by following weight proportion gets the raw materials ready:
Phosphoric acid (concentration is 85%) 1.1kg
Urea (content 99%) 0.52kg
Catalyzer: 0.004kg
Catalyzer wherein is with embodiment 5.
2) in the reactor of being furnished with stirrer, temperature and pressure indicating meter and prolong, add the phosphoric acid in the reaction raw materials, stir heating simultaneously, the control stirring velocity is 70 rev/mins, makes temperature rise to 60 ℃;
3) in reactor, add urea, continue heating;
When 4) making temperature rise to 115 ℃, in reactor, slowly evenly add catalyzer, mixture is reacted;
5) after the continuation heating makes temperature reach 130 ℃, observing response phenomenon when continuing heating, along with temperature raises, light green liquid becomes the oyster white dope gradually, foam sharply increases, and rate of rise in temperature is obviously accelerated, and the volume of material expands rapidly, prolong has a large amount of gases to discharge, be mainly ammonia and water vapour, water absorbs, and the volume of question response still internal reaction thing stops heating when increasing to the twice of original volume, continue to stir, material in reactor relies on the heat release of self at vigorous reaction, and temperature continues to rise, and question response tends to be steady then that temperature no longer rises, when temperature begins to descend, show that reaction finishes;
6) immediately the oyster white dope in the reactor being poured out, products therefrom is placed in the ventilating kitchen, was cooling curing after 30-60 minute, pulverized with pulverizer then and can obtain the powdered fire retardant.
7) products therefrom being put into plastic bag sealing stores for future use.
The technical indicator of product:
Outward appearance: white powder
Solid content (%): 100%
Proportion (g/cm
3) 2.2
Time limit (year) is arranged: 5
Experimental example 1
Adopt the product preparation glued board of embodiment of the invention 1-4 respectively.
1, experiment material
Veneer: board using poplar board, thickness 1.4-1.5mm, water ratio 7%-9%, breadth 450 * 450mm;
Urea-formaldehyde resin adhesive: take from Beijing Tai Er chemical company, model WG-2115 glued board glue, the performance index of product are as follows:
Solid content (%) 60.9
PH value 7.5
Viscosity (being coated with-4 glasss) (20 ℃, S) 59s
Curing speed (s) 47
Free formaldehyde content (%) 0.36
Storage period (my god) 28
2, concrete experimental procedure:
1) fire retardant with embodiment of the invention 1-4 flooded the place 30 minutes to veneer;
2) using the removal moisture drying case, is under 80 ℃ the veneer of handling to be carried out drying treatment at drying temperature, and its final water ratio is reached 6～8%;
3) impregnation: 15% the flour that adds urea glue weight in urea glue mixes, and 1% the ammonium chloride that adds urea glue weight again stirs and gets final product.
4) veneer that drying is crossed carries out gluing, and the Amount of spread of every veneer is the two-sided 340g/m that is coated with
2
5) to being colded pressing successively by the sheet material of five layers of veneer assembly, making the finished product glued board after hot pressing, cooling and the cutting edge, the pressure of wherein colding pressing is 1～1.2MPa, and the time of colding pressing is 30min; Hot pressing pressure is 1.2MPa, and hot pressing temperature is 100 ℃, and hot pressing time is 55s/mm.
3. plywood character detects
By GB/T17657-1999 " Test methods of evaluating the properties of woodbased panels and surface decorated woodbased panels " the glued board product for preparing is carried out Performance Detection, detected result sees Table 1.
Measure the oxygen index index of the glued board product of preparation with reference to GB/T2406-93 " plastics flammability test method oxygen index method ", detected result sees Table 1.The oxygen index of the B1 level of GB50222-95 " code for fire prevention design of interior decoration of buildings " regulation is 〉=48%.
Detect according to the II class plate of stipulating in the Japanese JAS standard, concrete grammar: the glued board product was soaked 3 hours in 70 ± 3 ℃ hot water, in 60 ± 3 ℃ baking oven, dried by the fire 3 hours again, then detect its glue-line situation, meet relevant dipping stripping performance in the JAS standard, detected result sees Table 1.
Reference examples 1
Adopt the WG-2115 glued board to prepare glued board in contrast with glue, except that flooding without fire retardant of the present invention, other preparation processes are identical with experimental example 1.Detected result sees Table 1.
Reference examples 2
Adopt commercial a kind of nitrogen-phosphorus be aq. type fire retardant (ammonium polyphosphate flame retardant that Shanghai Xinhua fire retardant head factory is purchased, the polymerization degree is less than 20) in contrast, except that with this fire retardant veneer being carried out the dip treating, other preparation processes are identical with experimental example 1.Detected result sees Table 1.
Table 1
Experimental result in the table 1 shows, fire retardant of the present invention not only flame retardant effect is remarkable, and effect: with the glued board of fire retardant dip treating of the present invention with the formaldehyde of significantly dissolving, its flame-retardant plywood oxygen index is more than 60%, the oxygen index (〉=48%) that meets the B1 level of GB50222-95 " code for fire prevention design of interior decoration of buildings " regulation, and burst size of methanal≤0.14mg/L, make the environmental-protecting performance of glued board can be stabilized in the E0 level (≤0.5mg/L).Detected result illustrates that also fire retardant of the present invention is little to the physical and mechanical property influence of glued board, and its performance index meet the glued board national standard.
Smoke suppressing detects
According to GB/T 8627-1999 " material of construction burning or the smoke density experimental technique that decomposes " veneer that step 2 obtains of experimental example 1 is carried out smoke density and detect, regulation smoke density grade SDR≤75 are qualified in this GB.Detected result sees Table 2
Table 2
Sample dimensions is 25.4 ± 0.1mm * 25.4 ± 0.1mm, and the SDR majority of flame-retardant plywood is far smaller than the regulation of GB (SDR≤75) in 40～45 scope, therefore shows that fire retardant of the present invention has good smoke suppressing.
Experimental example 2
Adopt the product preparation shaving board of embodiment of the invention 5-6 respectively.
The shaving board raw material adopts Aspen wood shavings, and the wood shavings water ratio is 2-4%; Two kinds of glue that urea-formaldehyde resin adhesive provides for Furen Wood Industry Co., Ltd., Fujian, product performance index is as follows respectively:
Urea-formaldehyde resin adhesive 1: the mol ratio of formaldehyde/urea (F/U) is 1.5, and solid content is 50%, pH value 7.85, viscosity (being coated with-4 glasss) 48s
Urea-formaldehyde resin adhesive 2: formaldehyde/urea (F/U) mol ratio is 1.7, and solid content is 57%, pH value 7.98, viscosity (being coated with-4 glasss) 61s
By the following prepared breadth shaving board that is 310 * 370 * 12mm:
Hot pressing temperature is 170 ℃, and hot pressing time is 20s/mm, and the hot pressing top pressure is 4.9MPa, and resin added is 10% of a wood shavings weight, and the applied amount of powdery combustion inhibitor is 15% of a wood shavings weight.
The concrete technical process of shaving board is: with wood shavings dry to water ratio be 2-4%, be applied for the urea glue of wood shavings weight 10%, then spray powdery combustion inhibitor into wood shavings weight 15%, will be through mat formation moulding and be hot pressed into plate of the wood shavings that fire retardant was handled, cool off afterwards, detect the performance of shaving board.
By GB/T17657-1999 " wood-based plate and face artificial board physicochemical property experimental technique " detection method the shaving board product of producing is carried out Performance Detection, detected result sees Table 3.
Reference examples 3
Adopt shaving board that above-mentioned urea-formaldehyde resin prepares identical breadth in contrast, except not adding fire retardant of the present invention, all the other are all identical with experimental example 2.The detected result of the shaving board that makes is as shown in table 3.
Table 3
Experimental result shows, fire retardant of the present invention not only has significant flame retardant effect, and burst size of methanal effect highly significant in the reduction shaving board, when add-on be wood shavings weight 15% the time, oxygen index reaches more than 52%, and the burst size of methanal reduction reaches more than 96%, make the flame retardant rating of shaving board reach the B1 level, and the environmental protection grade of shaving board reaches the E0 level.Detected result illustrates that also fire retardant of the present invention is little to the physical and mechanical property influence of shaving board, and its performance index meet the shaving board national standard.
Cost analysis
Fire retardant applied amount of the present invention is pressed 15% of wood shavings weight and is calculated, and every cubic metre of shaving board probably needs pulvis fire retardant 90kg, and the fire retardant cost is by 5200 yuan of/ton calculating, and then every cubic metre of shaving board cost improves about 468 yuan.
On the one hand, use for reference the foreign market experience, the cost of fire retardant of the present invention is domestic existing 1/2-1/3 with the based flame retardant cost, be external existing 1/10-1/20, therefore compare the fire-resistant-chipboard for preparing with existing fire retardant and significantly reduce with the expense of the fire-resistant-chipboard of fire retardant preparation of the present invention with the based flame retardant cost.
On the other hand, shaving board with fire retardant production of the present invention is that overall flame is handled, be different from the general shaving board that only carries out the surface fireproof processing fully, not only can reach fire-retardant purpose, but also have the effect of eliminating formaldehyde, therefore not need to take other way to eliminate formaldehyde, therefore save because of eliminating operation and the cost that formaldehyde increased in addition, only that is to say with fire-retardant required cost, just can reach fire-retardant and two purposes of environmental protection, obviously is not only to economize operation but also save cost.
Claims (9)
1, a kind of fire retardant is characterized in that comprising following raw materials in weight portion:
Phosphoric acid 0.5-1.3
Urea 0.3-0.6
Catalyzer 0.002-0.004
Wherein, described concentration of phosphoric acid is 85%; Described catalyzer comprises following materials of weight proportions: tin chloride 0.8-1.2, copper sulfate 1.5-2.5, sodium-chlor 0.8-1.2, iron(ic) chloride 0.8-1.2, Tai-Ace S 150 0.8-1.2, boric acid 0.8-1.2, zinc chloride 1.5-2.5.
2, fire retardant as claimed in claim 1 is characterized in that the weight part proportioning of described fire retardant raw material is selected:
Phosphoric acid 0.7-1.1
Urea 0.35-0.45
Catalyzer 0.0025-0.0035.
3, fire retardant as claimed in claim 1 or 2 is characterized in that also comprising that following weight part is the softening water of 0.7-1.8.
4, a kind of preparation method of fire retardant as claimed in claim 1 or 2 is characterized in that making phosphoric acid and urea to carry out polyreaction under the effect of catalyzer.
5, preparation method as claimed in claim 4 is characterized in that described reaction comprises following step in sequence:
1) in reactor, adds phosphoric acid, stir heating simultaneously, make temperature rise to 50-60 ℃;
2) add urea, the mixture of phosphoric acid and urea is stirred, make material distribute, be heated evenly;
When 3) temperature rises to 90-120 ℃, in reactor, add catalyzer, continue heating, stir;
4) make temperature rise to 130-140 ℃ after, stop the heating;
5) product in the reactor is poured out, treated behind its cooling curing it to be ground into powdery.
6, preparation method as claimed in claim 4 is characterized in that described reaction comprises following step in sequence:
1) in reactor, adds phosphoric acid, stir heating simultaneously, make temperature rise to 50-60 ℃;
2) add urea, the mixture of phosphoric acid and urea is stirred, make material distribute, be heated evenly;
When 3) temperature rises to 90-120 ℃, in reactor, add catalyzer, continue heating, stir;
4) make temperature rise to 130-140 ℃ after, stop the heating;
5) make reactant be cooled to 60-80 ℃, adding weight part in reactor is the softening water of 0.7-1.8, stirs.
7,, it is characterized in that reactant volume in the described step 4) stops described heating when increasing to 2-2.5 times of original volume as claim 5 or 6 described preparation methods.
8, preparation method as claimed in claim 6 is characterized in that: the temperature of described softening water is 40-60 ℃.
9, as claim 5 or 6 described preparation methods, it is characterized in that: the temperature in the described step 3) is selected 110-120 ℃, and described stirring velocity is controlled at 50-70 rev/min.
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|---|---|---|---|---|
| CN101913180A (en) * | 2010-07-28 | 2010-12-15 | 山东省产品质量监督检验研究院 | Method for manufacturing indoor environmentally-friendly flame retardant blockboard |
| CN102490220A (en) * | 2011-12-20 | 2012-06-13 | 徐州盛和木业有限公司 | Preparation method of antiflaming mothproof natural veneer overlay decorative board |
| CN102775995A (en) * | 2012-07-18 | 2012-11-14 | 苏州萃智新技术开发有限公司 | Neutral flame retardant liquid |
| CN102807875A (en) * | 2012-07-18 | 2012-12-05 | 苏州萃智新技术开发有限公司 | Corrosion resistant and fire retardant liquid |
| CN102775997A (en) * | 2012-07-18 | 2012-11-14 | 苏州萃智新技术开发有限公司 | Environment-friendly inflaming-retarding liquid |
| CN102775996A (en) * | 2012-07-18 | 2012-11-14 | 苏州萃智新技术开发有限公司 | High-permeability inflaming retarding liquid |
| CN102975252B (en) * | 2012-11-22 | 2015-06-24 | 北京林业大学 | Wood treatment agent and preparation method thereof |
| CN102975246B (en) * | 2012-11-22 | 2015-06-24 | 北京林业大学 | Wood treatment agent and preparation method thereof |
| CN102975250B (en) * | 2012-11-22 | 2015-06-03 | 北京林业大学 | Wood modifier and preparation method thereof |
| CN102975251B (en) * | 2012-11-22 | 2015-06-03 | 北京林业大学 | Flame retardant for wood as well as preparation method and applications of flame retardant for wood |
| CN102975253B (en) * | 2012-11-22 | 2015-06-03 | 北京林业大学 | Wood fire retardant, preparation method and applications thereof |
| CN104210002B (en) * | 2014-07-25 | 2016-04-13 | 北京林业大学 | A kind of composite flame-retardant agent, preparation method and its usage |
-
2007
- 2007-09-24 CN CNB2007101222432A patent/CN100567456C/en not_active Expired - Fee Related
Non-Patent Citations (4)
| Title |
|---|
| BL-环保阻燃剂. 李光沛，余丽萍，刘毅.精细与专用化学品，第14卷第18期. 2006 |
| BL-环保阻燃剂. 李光沛，余丽萍，刘毅.精细与专用化学品，第14卷第18期. 2006 * |
| 环保阻燃胶的开发. 李光沛，蔡静蕊，王旭等.林产工业，第29卷第3期. 2002 |
| 环保阻燃胶的开发. 李光沛，蔡静蕊，王旭等.林产工业，第29卷第3期. 2002 * |
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