CN103722600B - A kind of Wood modifier and preparation method thereof - Google Patents
A kind of Wood modifier and preparation method thereof Download PDFInfo
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- CN103722600B CN103722600B CN201310714204.7A CN201310714204A CN103722600B CN 103722600 B CN103722600 B CN 103722600B CN 201310714204 A CN201310714204 A CN 201310714204A CN 103722600 B CN103722600 B CN 103722600B
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Abstract
The present invention relates to a kind of fire-retarding of wood modifier, comprise by weight following composition: 20～200 parts of phosphoric acid; 20～100 parts, urea; 0.1～1.0 part of catalyst; 5～20 parts of tetrakis hydroxymetyl phosphonium sulfurics; 2～15 parts of aluminium triphosphates; 0.1～2.5 part of aerosol-OT salt; 40～200 parts, water. Wood fire retardant provided by the invention not only flame retardant effect is remarkable, and has good dimensionally stable function. Process timber rate of body weight gain in the time of 20% left and right, oxygen index (OI) can reach more than 50%, and dimensional stability ASE can reach more than 35%. Wood fire retardant preparation method provided by the invention is simple, and cost is lower, is applicable to promoting the use of.
Description
Technical field
The present invention relates to a kind of Wood modifier and preparation method thereof, and in treating of woodApplication, belongs to Wooden modifying fire proofing field.
Background technology
Timber and goods thereof are widely used in interior decoration, Furniture manufacture, building construction and outerDuring portion decorates, these materials belong to combustible material, utmost point fire hazardous, and expand with wet and contract with dry,Dimensional stability is poor, and the anti-flammability and the dimensional stability that how to improve material have become full generationThe problem of boundary's extensive concern.
At present, the most popular method that prevents timber and goods breaking out of fire thereof is at these materialsMiddle use fire retardant, these fire retardants are mostly based on changes such as phosphorous, nitrogen, boron, aluminium and halogensCompound, inorganic combustion inhibitor is owing to having good flame resistance, not producing toxic gas (halogen resistanceExcept combustion agent), do not separate out, non-volatile, cheap, wide material sources, the high spy of securityPut and be used widely.
Phosphorus-nitrogenated flame retardant has fire-retardant synergy, reduces decomposition temperature, increases the life of charcoalBecome, reduce the generation of imflammable gas and reduce the effects such as heat.
For example, article " the hexamethyl phosphinylidyne of delivering on the 7th phase of " forest product industry " nineteen ninety-fiveThe research of triamine wood fire retardant " a kind of HMPA fire retardant of using is disclosed to woodMaterial carries out impregnation process, obtains flame retardant effect. It within open day, is on April 5th, 2000, openNumber a kind of fire-proof flame-retarded agent is disclosed, this resistance in the Chinese patent application of CN1249325ACombustion agent is mixed by urea, phosphoric acid, borax, boric acid etc., be applicable to cotton, chemical fibre,The combustibles such as paper, timber fire-retardant. Open day is on July 26th, 2006, publication numberA kind of phosphor nitrogen composite combustion inhibitor is disclosed in the Chinese patent application for CN1807552A, shouldFire retardant is to be undertaken adding after chemical reaction nertralizer to carry out as ammoniacal liquor by urea and phosphoric acid againNeutralization reaction is made, and is applicable to the fire-retardant of the combustibles such as textile and timber-work, this resistanceThe preparation method of combustion agent is relatively simple, safety and environmental protection.
Although to have manufacture method simple for disclosed fire retardant in above-mentioned document, cost is low, resistanceThe advantages such as combustion property is good, and smoke suppressing effect is good, but its permeability, resistance leachability are poor, to woodThe dimensional stability of material is not contributed.
Summary of the invention
Be difficult to be uniformly distributed in timber for overcoming existing wood fire retardant poor permeability, and effectThe technological deficiency such as single, the invention provides a kind of fire-retarding of wood modifier of Multifunction.
To achieve these goals, the present invention adopts following technical scheme:
A kind of fire-retarding of wood modifier, comprises following composition by weight:
Described catalyst consists of the following composition by weight: 0.8～1.2 part of stannic chloride; Sulfuric acid1.5～2.5 parts of copper; 0.8～1.2 part, sodium chloride; 0.8～1.2 part, iron chloride; Aluminum sulfate 0.8～1.2Part; 0.8～1.2 part of boric acid; 1.5～2.5 parts of zinc chloride.
When fire-retarding of wood modifier provided by the invention acts on timber, can ooze by Quick uniformIn timber, (polymerization under catalyst action of phosphoric acid and urea is produced to improve flame-retardant composition thoroughlyThing) retention in timber. When the drying of wood, between the groups such as flame-retardant composition and timber hydroxylThere is cross-linking reaction, thereby the stability of timber and resistance leachability are also improved significantly.
Preferably, described flame-proof modifier by weight, comprises following composition:
Described phosphoric acid is that mass percent concentration is 80～90% phosphate aqueous solution.
Most preferably, described flame-proof modifier by weight, comprises following composition:
The present invention also provides the preparation method of described fire-retarding of wood modifier, comprises following stepRapid:
(1) in reactor, add phosphoric acid, stir and heat;
(2) in the time of temperature rise to 50～60 DEG C, in described reactor, add urea, stirMix evenly;
(3) continue heating,, in described reactor, add when the temperature rise to 90～120 DEG CEnter catalyst,, stop heating when the temperature rise to 130～140 DEG C;
(4) question response still is cooled to 60～80 DEG C naturally, adds water, stirs;
(5), when question response still is cooled to 20～30 DEG C, add tetrakis hydroxymetyl phosphonium sulfuric, trimerizationAluminum phosphate and aerosol-OT salt, stir and obtain fire-retarding of wood modifier.
Wherein, each component of described catalyst can be mixed with any order of addition in advanceClose, be then added into as a whole in described reactor.
In above-mentioned preparation process, the rotating speed of described stirring is 50～70 revs/min.
In described step (3), behind temperature rise to 130～140 DEG C, in described reactorReactant volume increases to 2～3 times of original volume.
The present invention also provides the use of above-mentioned fire-retarding of wood modifier as timber size stabilizing agentOn the way.
The present invention, by adjusting existing fire retardant formula, adds the tetra methylol sulfuric acid of appropriate ratioPhosphorus, aluminium triphosphate, aerosol-OT salt, gained fire-retarding of wood modifier not onlyCan have good flame retardant effect, dimensional stability, the reduction that can also obviously improve timber are run offRate, reduces burst size of methanal, has multiple combination functions.
Technical solution of the present invention tool has the following advantages:
(1) not only flame retardant effect is remarkable for wood fire retardant provided by the invention, and hasGood dimensionally stable function. Process timber rate of body weight gain in the time of 20% left and right, oxygen index (OI) can reachTo more than 50%, dimensional stability ASE can reach more than 35%.
(2) fire retardant provided by the invention has formaldehyde elimination function, for people such as glued boardsMake plate processing, can effectively improve wood-based plate environmental protection characteristic, process glued board rate of body weight gain 10%When the left and right, E2Level plywood environmental-protecting performance can be stabilized in E0Level (≤0.5mg/L).
(3) wood fire retardant preparation method provided by the invention is simple, and cost is lower, 1 tonThe liquid flame retardant manufacturing cost of the present invention of solids content 40% left and right is about 3800 yuan/ton,Well below the price of existing domestic and international wood fire retardant.
Detailed description of the invention
Following examples are used for illustrating the present invention, but are not used for limiting the scope of the invention.
Embodiment 1
1, carry out material preparation by following weight proportion:
Wherein, catalyst is Beijing Forestry University's material science and technical college's environmental protection flame retardant skillThe pistac pulvis that prepare voluntarily at art center, preparation process is as follows: by weight by chlorination1.0 parts, tin, 2.0 parts, copper sulphate, 0.9 part, sodium chloride, 1.1 parts, iron chloride, aluminum sulfate 0.8After part, 1.2 parts of boric acid and 1.8 parts of grindings of zinc chloride, mix and get final product.
2, preparation process is as follows:
1), being furnished with in the reactor of agitator, thermometer and condenser pipe, add phosphoric acid moltenLiquid, stirs heating simultaneously;
2), treat temperature rise until approximately 60 DEG C in reactor, add urea, simultaneously to phosphoric acidProceed to stir with the mixture of urea, make material distribute, be heated evenly;
3), until temperature rise during to 110-115 DEG C, in reactor lentamente, add equablyEnter catalyst mixture is reacted, now reaction mass becomes light green color; Continue heating,Observing response phenomenon simultaneously, along with temperature raises, it is sticky that light green color liquid becomes milky graduallyThick thing, foam sharply increases, and rate of rise in temperature is obviously accelerated, and the volume of material is swollen rapidlySwollen, condenser pipe has a large amount of gas to discharge, and when question response temperature in the kettle reaches 135 DEG C, stops addingHeat; Now the volume of reactant is increased to the twice left and right of original volume, continues to stir, anti-Answer material in still to rely on the heat release of self to continue vigorous reaction, temperature continues to rise, question responseTend to be steady, when temperature starts to decline, show to react complete;
4), described reactor is cooled to 60～80 DEG C naturally, add water, stir;
5), reactor is while being cooled to 20～30 DEG C, adds tetrakis hydroxymetyl phosphonium sulfuric, trimerization phosphorusAcid aluminium and aerosol-OT salt, stir and obtain fire-retarding of wood modifier.
Embodiment 2
1, carry out material preparation by following weight proportion:
Wherein, catalyst is Beijing Forestry University's material science and technical college's environmental protection flame retardant skillThe pistac pulvis that prepare voluntarily at art center, preparation process is as follows: by weight by chlorination0.9 part, tin, 1.6 parts, copper sulphate, 1.0 parts, sodium chloride, 1.0 parts, iron chloride, aluminum sulfate 1.2After part, 1.1 parts of boric acid and 2.0 parts of grindings of zinc chloride, mix and get final product.
2, preparation process is as follows:
1), being furnished with in the reactor of agitator, thermometer and condenser pipe, add phosphoric acid,Stir heating simultaneously;
2), treat temperature rise until 50 DEG C, in reactor, add urea, simultaneously to phosphoric acidProceed to stir with the mixture of urea, make material distribute, be heated evenly;
3), continue heating while making temperature rise to 110-115 DEG C, in reactor lentamente,Add equably catalyst that mixture is reacted; Continue heating, observing response is existing simultaneouslyResemble, along with temperature raises, light green color liquid becomes milky dope gradually, and foam sharplyIncrease, rate of rise in temperature is obviously accelerated, and the volume of material expands rapidly, and condenser pipe has greatlyAmount gas is discharged, and question response still temperature reaches 130 DEG C of left and right and stops heating, now reactantVolume is increased to 2.5 times of left and right of original volume, continues to stir, and material in reactor relies on certainlyThe heat release of body continues vigorous reaction, and temperature continues to rise, and question response tends to be steady temperature notRise again, when temperature starts to decline, show to react complete;
4), described reactor is cooled to 60～80 DEG C, add water, stir;
5), reactor is while being cooled to 20～30 DEG C, adds tetrakis hydroxymetyl phosphonium sulfuric, trimerization phosphorusAcid aluminium and aerosol-OT salt, stir and get final product.
Embodiment 3
1, carry out material preparation by following weight proportion:
Wherein, catalyst is with embodiment 1; Preparation process is with embodiment 1.
Embodiment 4
1, carry out material preparation by following weight proportion:
Wherein, catalyst is with embodiment 2; Preparation process is with embodiment 2
Experimental example 1
Adopt respectively the flame retardant products of embodiment of the present invention 1-4 to prepare glued board.
1, experiment material:
Veneer: board using poplar board, thickness 1.4-1.5mm, moisture content 8% left and right, breadth410×410mm；
Adhesive: commercially available modified urea-formaldehyde resin adhesive (cyanurotriamide modified, consumption and urineThe mol ratio of urea formaldehyde consumption is 1.1), the performance indications of product are as follows:
2, specific experiment step:
1) fire retardant of embodiment of the present invention 1-4 is made into the aqueous solution that solid content is 10wt%,Respectively veneer is carried out to impregnation process 30 minutes;
2) using moisture eliminating drying box, is at 80 DEG C, the veneer of processing to be carried out at baking temperatureDry processing, reaches 6～8% its final moisture content;
3) impregnation: in adhesive, add by weight 15% flour, 1% ammonium chloride,Stir;
4) veneer is carried out to gluing, glue-spread is two-sided painting 280g/m2；
5) to being colded pressing successively by the sheet material of five layers of veneer assembly, hot pressing, cooling and cutting edge.The pressure of wherein colding pressing is 1-1.2MPa, and the time of colding pressing is 30min; Hot pressing pressure is1.0-1.2MPa, hot pressing temperature is 120 DEG C, hot pressing time is 60s/mm.
3, plywood character detects
Press GB/T17657-1999 " test methods of evaluating the properties of wood-based panels and surface decorated wood-based panels "Plywood product to preparation carries out Performance Detection, and testing result is in table 1.
Measure preparation with reference to GB/T2406-93 " Plastics Combustion test method oxygen index method "The oxygen index (OI) index of plywood product. GB50222-95 " building interior Decoration Design fire preventionSpecification " oxygen index (OI) of B1 level of regulation is >=48%.
Detect concrete grammar: by glue according to the II class plate specifying in Japanese JAS standardPlywood product soaks 3 hours in the hot water of 70 ± 3 DEG C, then dries 3 in the baking oven of 60 ± 3 DEG CHour, then detect its glue-line situation, meet relevant dipping stripping performance in JAS standard.
According to GB/T8627-1999 " construction material burning or the smoke density test method of decomposing "Carry out smoke density detection, smoke density grade SDR≤75 are qualified.
Reference examples 1
Except not adopting fire retardant dipping of the present invention, other step is identical with experimental example 1,Prepare same glued board in contrast.
Reference examples 2
Adopting commercial nitrogen-phosphorus is aqua type fire retardant (CASNo.:68333-79-9, ShanghaiXinhua's fire retardant head factory, the degree of polymerization is less than 20) replace wood fire retardant of the present invention to soakStain (solid content concentration, dip time etc. are all identical with experimental example 1), other step also with realityTest example 1 identical, prepare same glued board in contrast.
Reference examples 3
Except not adding aerosol-OT salt, other step is same as Example 4.The result of experimental example and reference examples is as shown in table 1:
Table 1 plywood character test result
Result in table 1 shows, fire retardant of the present invention not only flame retardant effect is remarkable, and toolThere is obvious formaldehyde eradicating efficacy. With the glued board of fire retardant impregnation process of the present invention, its resistanceCombustion glued board oxygen index (OI) is more than 58%, and burst size of methanal can be stabilized in E0Level (≤0.5mg/L),Be better than existing flame retardant products.
Experimental example 2
The impregnation process time is become to 10 minutes, and baking temperature becomes 60 DEG C, and whole moisture content is6-12%, other step is identical with experimental example 1, and test implementation example 1-4, reference examples 1 are glued togetherThe performance of plate, result is as shown in table 2:
Table 2 plywood character test result
Result in table 2 shows, fire retardant of the present invention not only flame retardant effect is remarkable, and oozesSpeed can change wood performance soon, at short notice thoroughly. Have obvious formaldehyde eliminate withSmoke suppressing effect. Process glued board with fire retardant of the present invention, glued board oxygen index (OI) more than 55%,Burst size of methanal can be stabilized in E0Level (≤0.5mg/L), and demonstrate good smoke suppressing.
Experimental example 3
Adopt respectively the flame retardant products of embodiment of the present invention 1-4 to process cotton wood.
Poplar: the age of tree 10 years, sapwood, size (radially × tangential × axially) 30 × 30 × 5mm;
Press following PROCESS FOR TREATMENT poplar test specimen:
It is the water-soluble of 10wt% that the fire retardant of embodiment of the present invention 1-4 is made into respectively to solid contentLiquid.
Poplar test specimen is used benzene and alcohol mixeding liquid (2:1) extracting 12 hours before use, putsEnter in 105 DEG C of air dry ovens 12 hours, the weight that weighs over dry test specimen is also measured its size.
Test specimen is put in the beaker that fills above-mentioned preparation, pushes down test specimen with stone. By beakerPut into vacuum tank, under vacuum 0.02MPa normal temperature state, keep 0.5 hour; Return toNormal pressure, keeps 24 hours. Take out test specimen, surface is wiped only; Put into 105 DEG C of forced air dryingsCase 12 hours, measures its weight and size.
The test specimen of processing is put into the beaker that fills clear water, ensured that the water surface covers test specimen.Beaker is put into the dry case of vacuum, and vacuum 0.02MPa, keeps 0.5 hour, and normal pressure keeps24 hours, measure its weight and size. Again test specimen is put into 105 DEG C of air dry ovens 12Hour, weigh the weight of over dry test specimen and measure its size.
Reference examples 4
The fire retardant that adopts reference examples 2, is made into the aqueous solution that solid content is 10wt%, to poplarWood is processed, and step is identical with experimental example 3.
Reference examples 5
Except not adding aerosol-OT salt, other step is same as Example 4,And be made into the aqueous solution that solid content is 10wt%, poplar is processed.
The result of embodiment 1-4 and reference examples 3,4 is as shown in table 3:
Table 3 test specimen the performance test results
Result in table 3 shows, the timber that adopts fire retardant processing of the present invention rate of body weight gain,Dimensional stability, turnover rate aspect are in general obviously better than existing reference examples, have shownDimensionally stable effect, and there is good resistance leachability. As can be seen here tetrakis hydroxymetyl phosphonium sulfuric,Adding of aluminium triphosphate, aerosol-OT salt, can promote fire retardant and woodReaction between material, thus the permeability of raising fire retardant strengthens dimensional stability, reduces streamMistake rate.
The result of experimental example 1-3 and reference examples 1-3 shows: fire retardant provided by the invention not onlyFlame retardant effect ideal but also have obvious dimensionally stable effect is a kind of novel, manyThe flame retardant products of function.
Although, above with a general description of the specific embodiments the present invention has been done in detailMost description, but on basis of the present invention, can make some modifications or improvements it, this is to thisThose skilled in the art are apparent. Therefore, on the basis of not departing from spirit of the present inventionUpper these modifications or improvements, all belong to the scope of protection of present invention.
Claims (6)
1. a fire-retarding of wood modifier, is characterized in that, comprises by weight following composition:
Described phosphoric acid is that mass percent concentration is 80～90% phosphate aqueous solution.
2. fire-retarding of wood modifier according to claim 1, is characterized in that described catalysisAgent consists of the following composition by weight: 0.8～1.2 part of stannic chloride; 1.5～2.5 parts, copper sulphate;0.8～1.2 part, sodium chloride; 0.8～1.2 part, iron chloride; 0.8～1.2 part, aluminum sulfate; Boric acid 0.8～1.2 part; 1.5～2.5 parts of zinc chloride.
3. the preparation method of fire-retarding of wood modifier described in claim 1 or 2, its feature existsIn, comprise the following steps:
(1) in reactor, add phosphoric acid, stir and heat;
(2) in the time of temperature rise to 50～60 DEG C, in described reactor, add urea, stirMix evenly;
(3) continue heating,, in described reactor, add when the temperature rise to 90～120 DEG CEnter catalyst,, stop heating when the temperature rise to 130～140 DEG C;
(4) question response still is cooled to 60～80 DEG C naturally, adds water, stirs;
(5) question response still continues, after cooling uniform temperature, to add tetrakis hydroxymetyl phosphonium sulfuric, threePoly aluminium phosphate and aerosol-OT salt, stir and obtain fire-retarding of wood modifier.
4. preparation method according to claim 3, is characterized in that, in step (5)In, when described reactor is cooled to 20～30 DEG C, add tetrakis hydroxymetyl phosphonium sulfuric, tripolyphosphateAluminium and aerosol-OT salt.
5. preparation method according to claim 3, is characterized in that, described stirringRotating speed is 50～70 revs/min.
6. the arbitrary described fire-retarding of wood modifier of claim 1-2 is as timber size stabilizing agentPurposes.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102334751A (en) * | 2010-07-28 | 2012-02-01 | 南通烟滤嘴有限责任公司 | Paper-core filter rod for cigarettes and manufacturing method thereof |
| CN102773894A (en) * | 2012-07-06 | 2012-11-14 | 苏州萃智新技术开发有限公司 | Environment-friendly flame-retardant liquid for flame retarding of wood and preparation method for environment-friendly flame-retardant liquid |
| CN102975246A (en) * | 2012-11-22 | 2013-03-20 | 北京林业大学 | Wood treatment agent and preparation method thereof |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102334751A (en) * | 2010-07-28 | 2012-02-01 | 南通烟滤嘴有限责任公司 | Paper-core filter rod for cigarettes and manufacturing method thereof |
| CN102773894A (en) * | 2012-07-06 | 2012-11-14 | 苏州萃智新技术开发有限公司 | Environment-friendly flame-retardant liquid for flame retarding of wood and preparation method for environment-friendly flame-retardant liquid |
| CN102975246A (en) * | 2012-11-22 | 2013-03-20 | 北京林业大学 | Wood treatment agent and preparation method thereof |
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