CN102071032A - Amino resin-containing flame retardant and preparation method thereof - Google Patents
Amino resin-containing flame retardant and preparation method thereof Download PDFInfo
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Abstract
The invention discloses an amino resin-containing flame retardant and a preparation method thereof. The flame retardant comprises a phosphorus-nitrogen series flame retardant, an inorganic flame retardant and amino resin, wherein the phosphorus-nitrogen series flame retardant is covered by the inorganic flame retardant; the inorganic flame retardant is covered by the amino resin; and the weight percentage ratio of the phosphorus-nitrogen series flame retardant to the inorganic flame retardant to the amino resin is 100:(1-100):(1-30). The flame retardant is applied to the flame retarding process of a plant fiber board, the physical and chemical properties, the processability and the service performance of the plant fiber board cannot be damaged, and the combustion smoke concentration and the toxicity of flame-retardant wooden materials in a fire disaster can be reduced.
Description
Technical field
The present invention relates to flame retardant area, especially relate to a kind of fire retardant that contains aminoresin and preparation method thereof.
Background technology
The Ministry of Public Security and the Ministry of Construction have issued and implemented " code for fire prevention design of interior decoration of buildings " in 1992, State Administration for Quality Supervision and Inspection and Quarantine has issued GB 8624-2006 " material of construction and the classification of goods combustionproperty " in 2006, GB/T 20284-2006 " the monomer combustion tests of material of construction or goods ", GB/T20285-2006 " classification of material producing smoke toxicity risk " and GB20286-2006 five compulsory standards such as " public place fire-retardant product and assembly combustionproperty require and sign ", to architectural decorative and fitting materials, the flame retardant properties of furniture has been done concrete regulation, and the material combustion performance that requires to be applied to public building and high-rise civil building is not less than the C level of GB8624-2006 or the B1 level of GB8624-1997.
Vegetable fiberboard is to be framework material with the vegetable fibre, adds tackiness agent and water-resisting agent, drying, mat formation, operations such as hot pressing, sanding make.With its good physical and mechanical property and processing characteristics, be widely used in production, floor production, boats and ships and the vehicle interior decoration of building decoration and fitment, furniture production, wooden door, vegetable fiberboard is identical with other wood materials, have higher combustion heat value, lower catching fire temperature and very fast flame propagation velocity, belong to combustible material.
In order to reduce the fire hazard of vegetable fiberboard, adopt phosphorus-compound nitrogen series that it is carried out fire-retardant finish usually.Phosphorus-the compound nitrogen series flame retardant properties is good, wide material sources, cheap, but with the subject matter of phosphorus-compound nitrogen series production fire-retardant plant fiber plate is: compare with the general fibre plate of same specification, mechanical property reduces by 15～45%; Water absorbability and thickness swelling rate increase, and can't satisfy processing and service requirements; Under the high temperature, phosphorus-compound nitrogen series impels timber composition dehydration carbonization to become charcoal non activated, causes the concentration of carbon monoxide in the smog to increase, and the hazardness of smog in the fire is increased.
In order to remedy above-mentioned defective, patent CN03116283.5 adopts melamine-formaldehyde resin that ammonium polyphosphate is coated processing, patent CN200810057901.9 adopts amino aminoresin that ammonium polyphosphate is carried out modification and handles, can reduce the water-absorbent of ammonium polyphosphate, but can not change the chemical reaction process of fire retardant and timber under the high temperature, the combustion product gases harm of fire-retardant wood-based materials increases.
Inorganic combustion inhibitor aluminium hydroxide, magnesium hydroxide can reduce the flue gas toxity of macromolecular material, but usually per 100 parts of macromolecular materials need add 40～60 parts aluminium hydroxide and/or magnesium hydroxide and just can work.The adding of a large amount of inorganic materials, grievous injury the processing characteristics and the use properties of vegetable fiberboard.
Therefore, need a kind of physical and mechanical property, flame retardant properties and flue gas toxity that does not damage vegetable fiberboard of development to meet fire retardant of relevant criterion and preparation method thereof.
Summary of the invention
The technical problem to be solved in the present invention provides a kind of fire retardant that contains aminoresin; This fire retardant uses in the fire-retardant process of vegetable fiberboard, can not damage physical and chemical performance, processing characteristics and the use properties of vegetable fiberboard, reduces the combustion product gases concentration and the toxicity of fire-retardant wood-based materials under the fire.
Another technical problem that the present invention will solve provides a kind of preparation method who contains the fire retardant of aminoresin.
For solving above-mentioned first technical problem, a kind of fire retardant that contains aminoresin of the present invention, it comprises phosphorus-nitrogen flame retardant, inorganic combustion inhibitor and aminoresin; Described phosphorus-nitrogen flame retardant coats inorganic combustion inhibitor outward, and described inorganic combustion inhibitor coats aminoresin outward; The weight percent of described phosphorus-nitrogen flame retardant, inorganic combustion inhibitor and aminoresin is 100:1～100:1～30.
Further, the weight percent of described phosphorus-nitrogen flame retardant, inorganic combustion inhibitor and aminoresin is 100:5～20:3～15.
Further, described phosphorus-nitrogen flame retardant is that primary ammonium phosphate, Secondary ammonium phosphate, triammonium phosphate, ammonium polyphosphate, phosphoguanidine, phosphoric acid are narrowed a kind of, two or more mixture in basic urea, phosphoric acid ester, melamine phosphate, the melamine pyrophosphate.
Further, described inorganic combustion inhibitor is a kind of, two or more the mixture in aluminium hydroxide, magnesium hydroxide, the zinc hydroxide.
Further, described aminoresin is a kind of, two or more the mixture in urea-formaldehyde resin, cyanurotriamide modified urea resin, melamine resin, the terpolycyantoamino-formaldehyde resin.
For solving above-mentioned second technical problem, a kind of preparation method who contains the fire retardant of aminoresin of the present invention comprises the steps:
When 1) stirring phosphorus-nitrogen flame retardant joined and be made into suspension in the solvent;
2) add the aqueous solution of Tai-Ace S 150 and/or aluminum nitrate and/or magnesium chloride and/or sal epsom and/or zinc sulfate and/or zinc chloride and/or zinc nitrate in the suspension, under 25 ℃～100 ℃ condition, kept 5 minutes～120 minutes, get mixture A;
3) in mixture A, add ammoniacal liquor and/or aqueous sodium hydroxide solution, under 25 ℃～100 ℃ condition, kept 5 minutes～120 minutes, get mixture B;
4) in mixture B, add aminoresin, use phosphoric acid to regulate pH most 5.0 ± 0.5, under 25 ℃～100 ℃ condition, kept 30 minutes～120 minutes, filter or extraction or rotary evaporation or vacuum-evaporation or spraying drying, to remove partial solvent, make the paste fire retardant, or remove whole solvents and make powdery combustion inhibitor;
Wherein, the Tai-Ace S 150 that adds in per 100 gram phosphorus-nitrogen flame retardants and/or the total mole number of aluminum nitrate and/or magnesium chloride and/or sal epsom and/or zinc sulfate and/or zinc chloride and/or zinc nitrate are 0.0064 mole～1.71 moles, are preferably 0.032 mole～0.342 mole; The mol ratio of Tai-Ace S 150 and/or aluminum nitrate and/or magnesium chloride and/or sal epsom and/or zinc sulfate and/or zinc chloride and/or zinc nitrate and ammoniacal liquor and/or sodium hydroxide is 1:0.001～1:8.0, is preferably 1:0.06～1:2.1.
Further, described phosphorus-nitrogen flame retardant is that primary ammonium phosphate, Secondary ammonium phosphate, triammonium phosphate, ammonium polyphosphate, phosphoguanidine, phosphoric acid are narrowed a kind of, two or more mixture in basic urea, phosphoric acid ester, melamine phosphate, the melamine pyrophosphate.
Further, described inorganic combustion inhibitor is a kind of, two or more the mixture in aluminium hydroxide, magnesium hydroxide, the zinc hydroxide.
Further, described aminoresin is a kind of, two or more the mixture in urea-formaldehyde resin, cyanurotriamide modified urea resin, melamine resin, the terpolycyantoamino-formaldehyde resin.
Further, described solvent comprises polarity commonly used or non-polar solvents such as water, ethanol, toluene, dimethylbenzene.
Further, a kind of preparation method who contains the fire retardant of aminoresin of the present invention comprises the steps:
1) Tai-Ace S 150 and/or aluminum nitrate and/or magnesium chloride and/or sal epsom and/or zinc sulfate and/or zinc chloride and/or zinc nitrate are made into saturated aqueous solution; Add 100 gram phosphorus-nitrogen combustion inhibitors when stirring, under 25 ℃～100 ℃ condition, kept 5 minutes～120 minutes, get mixture C;
2) in mixture C, add ammoniacal liquor and/or aqueous sodium hydroxide solution, under 25 ℃～100 ℃ condition, kept 5 minutes～120 minutes, get mixture D;
3) in mixture D, add 0.01 gram～5 gram aminoresin again, use phosphoric acid to regulate pH most 5.0 ± 0.5, under 25 ℃～100 ℃ condition, kept 30 minutes～120 minutes, filter or extraction or rotary evaporation or vacuum-evaporation or spraying drying, make the paste fire retardant to remove partial solvent, or remove whole solvents and make powdery combustion inhibitor;
Wherein, the Tai-Ace S 150 that adds in per 100 gram phosphorus-nitrogen combustion inhibitors and/or the total mole number of aluminum nitrate and/or magnesium chloride and/or sal epsom and/or zinc sulfate and/or zinc chloride and/or zinc nitrate are 0.0064 mole～1.71 moles, are preferably 0.032 mole～0.342 mole; The mol ratio of Tai-Ace S 150 and/or aluminum nitrate and/or magnesium chloride and/or sal epsom and/or zinc sulfate and/or zinc chloride and/or zinc nitrate and ammoniacal liquor and/or sodium hydroxide is 1:0.001～1:8.0, is preferably 1:0.06～1:2.1.
Further, described phosphorus-nitrogen flame retardant is that primary ammonium phosphate, Secondary ammonium phosphate, triammonium phosphate, ammonium polyphosphate, phosphoguanidine, phosphoric acid are narrowed a kind of, two or more mixture in basic urea, phosphoric acid ester, melamine phosphate, the melamine pyrophosphate.
Further, described inorganic combustion inhibitor is a kind of, two or more the mixture in aluminium hydroxide, magnesium hydroxide, the zinc hydroxide.
Further, described aminoresin is a kind of, two or more the mixture in urea-formaldehyde resin, cyanurotriamide modified urea resin, melamine resin, the terpolycyantoamino-formaldehyde resin.
Further, described solvent comprises polarity commonly used or non-polar solvents such as water, ethanol, toluene, dimethylbenzene.
The preparation method of above-mentioned fire retardant is not a preparation fire retardant unique method of the present invention, but the preferred method of preparation fire retardant of the present invention.
The fire retardant that makes by aforesaid method, surface deposition inorganic combustion inhibitor at phosphorus-nitrogen combustion inhibitor, close the hydrophilic group-NH4 of phosphorus-nitrogen combustion inhibitor, reduce the water absorbability and the solubleness of phosphorus-nitrogen combustion inhibitor significantly, can reduce of the influence of phosphorus-nitrogen combustion inhibitor the flame retardant fibre board physical and mechanical property; When running into fire, phosphorus-nitrogen combustion inhibitor decomposes is ammonia, water, tetra-sodium etc., and this reaction is thermo-negative reaction, has reduced the temperature of fire-retardant plant fiber plate heat affected zone, makes sheet material pyrolysis and combustion reaction interest for delinquency; The ammonia G﹠W has diluted the concentration of combustion zone inflammable gas, combustion chain reaction capable of blocking; The inorganic combustion inhibitor thermal endothermic decomposition discharges water outlet, becomes oxide compound, and this reaction is thermo-negative reaction, has reduced the temperature of fire-retardant plant fiber plate heat affected zone, makes sheet material pyrolysis and combustion reaction interest for delinquency; Under the aluminium that exists in inorganic combustion inhibitor and/or the catalysis of metals such as magnesium and/or zinc, tetra-sodium impels Mierocrystalline cellulose and hemicellulose dehydration carbonization to become charcoal non activated, reduces the thermal discharge and the heat release speed of combustion of wood significantly, and combustion chain reaction is interrupted; Aluminum oxide that generates after inorganic combustion inhibitor decomposes and/or magnesium oxide and/or zinc oxide have changed the dehydration carbonization process of Mierocrystalline cellulose and hemicellulose, and the output of carbon monoxide is significantly reduced; The pore texture of aluminum oxide and/or magnesium oxide and/or zinc oxide, can active adsorption the cigarette that produces of burning, reduce the smoke toxicity of goods when fire.
Fire retardant of the present invention has following beneficial effect:Fire retardant of the present invention is applied in the fire-retardant process of vegetable fiberboard, can not damage physical and chemical performance, processing characteristics and the use properties of vegetable fiberboard, can reduce the combustion product gases concentration and the toxicity of fire-retardant wood-based materials under the fire.
Description of drawings
Below in conjunction with accompanying drawing the specific embodiment of the present invention is described in further detail.
Fig. 1 is a fire retardant structural representation of the present invention.
Embodiment
Embodiment 1
A kind of preparation method who contains the fire retardant of aminoresin comprises the steps:
Be made into suspension with being added to the water in the melamine pyrophosphate when 1) stirring;
2) in suspension, add aluminum sulfate aqueous solution, kept 120 minutes down, get mixture A at 25 ℃;
3) in mixture A, add ammonia soln, kept 5 minutes down, get mixture B at 25 ℃;
4) in mixture B, add terpolycyantoamino-formaldehyde resin, regulate pH most 5.0 ± 0.5, kept 30 minutes, filter, make the paste fire retardant at 25 ℃～30 ℃ with phosphoric acid;
Wherein, the Tai-Ace S 150 mole number that adds in per 100 gram melamine pyrophosphates is 0.0064 mole; The mol ratio of Tai-Ace S 150 and ammoniacal liquor is 1:0.001; The weight ratio of melamine pyrophosphate and aminoresin is: 100:6.
Embodiment 2
A kind of preparation method who contains the fire retardant of aminoresin comprises the steps:
When 1) stirring melamine phosphate joined and be made into suspension in the ethanol;
2) in suspension, add magnesium chloride brine, kept 5 minutes down, get mixture A at 95 ℃;
3) in mixture A, add aqueous sodium hydroxide solution, kept 5 minutes down, get mixture B at 95 ℃;
4) add terpolycyantoamino-formaldehyde resin in mixture B, regulate pH most 5.0 ± 0.5 with phosphoric acid, kept 30 minutes at 100 ℃, rotary evaporation is made the powdery combustion inhibitor product to remove whole solvents;
Wherein, the mole number of the magnesium chloride that adds in per 100 gram melamine phosphates is 1.71 moles; The mol ratio of magnesium chloride and sodium hydroxide is 1:8.0; The weight ratio of melamine phosphate and aminoresin is: 100:8.
Embodiment 3
A kind of preparation method who contains the fire retardant of aminoresin comprises the steps:
When 1) stirring phosphoric acid being narrowed basic urea joins and is made into suspension in the toluene;
2) in suspension, add zinc sulfate solution, kept 60 minutes down, get mixture A at 50 ℃;
3) in mixture A, add ammonia soln, kept 60 minutes down, get mixture B at 50 ℃;
4) add cyanurotriamide modified urea resin in mixture B, regulate pH most 5.0 ± 0.5 with phosphoric acid, kept 60 minutes at 95 ℃, vacuum-evaporation is made paste fire retardant of the present invention to remove partial solvent;
Wherein, per 100 gram phosphoric acid mole number of narrowing the zinc sulfate that adds in the basic urea is 0.032 mole; The mol ratio of zinc sulfate ammoniacal liquor is 1:0.06; The weight ratio that phosphoric acid is narrowed basic urea and aminoresin is: 100:4.
Embodiment 4
A kind of preparation method who contains the fire retardant of aminoresin comprises the steps:
1) aluminum nitrate is made into saturated aqueous solution; Add 100 gram phosphoric acid ester in the time of stirring, kept 120 minutes down, get mixture C at 45 ℃;
2) in mixture C, add ammonia soln, kept 120 minutes down, get mixture D at 25 ℃;
3) add melamine resin again in mixture D, regulate pH most 5.0 ± 0.5 with phosphoric acid, kept 120 minutes at 75 ℃, spraying drying is made powdery combustion inhibitor to remove whole solvents;
Wherein, the mole number of the aluminum nitrate that adds in per 100 gram phosphoric acid ester is 0.01 mole; The mol ratio of aluminum nitrate and ammoniacal liquor is 1:0.01.
Embodiment 5
A kind of preparation method who contains the fire retardant of aminoresin comprises the steps:
1) sal epsom is made into saturated aqueous solution; Add 100 gram phosphoguanidines in the time of stirring, kept 5 minutes down, get mixture C at 95 ℃;
2) in mixture C, add aqueous sodium hydroxide solution, kept 5 minutes down, get mixture D at 95 ℃;
3) in mixture D, add urea-formaldehyde resin again, regulate pH most 5.0 ± 0.5, kept 30 minutes, filter,, make the paste fire retardant to remove partial solvent at 95 ℃ with phosphoric acid;
Wherein, the mole number of the sal epsom that adds in per 100 gram phosphoguanidines is 1.71 moles; The mol ratio of sal epsom and sodium hydroxide is 1:7.0.
Embodiment 6
A kind of preparation method who contains the fire retardant of aminoresin comprises the steps:
1) zinc sulfate is made into saturated aqueous solution; Add 100 gram ammonium polyphosphates in the time of stirring, kept 60 minutes down, get mixture C at 50 ℃;
2) in mixture C, add ammonia soln, kept 60 minutes down, get mixture D at 50 ℃;
3) add urea-formaldehyde resin again in mixture D, regulate pH most 5.0 ± 0.5 with phosphoric acid, kept 30 minutes at 95 ℃, extraction is made the paste fire retardant to remove partial solvent;
Wherein, the mole number of the zinc sulfate that adds in per 100 gram ammonium polyphosphates is 0.08 mole; The mol ratio of zinc sulfate and/or zinc chloride and/or zinc nitrate and ammoniacal liquor is 1:2.
Embodiment 7
A kind of preparation method who contains the fire retardant of aminoresin comprises the steps:
In reactor, add 50 gram water, be warming up to 80 ℃, add 0.05 mole anhydrous slufuric acid aluminium in the time of stirring, be cooled to behind Tai-Ace S 150 dissolving the becoming transparent liquid 20 ℃ ± 2 ℃ standby, hereinafter to be referred as A1 liquid;
Add 100 gram dehydrated alcohols in reactor, add 40 gram primary ammonium phosphates, 60 gram Secondary ammonium phosphates in the time of stirring, keeping temperature is 20 ℃ ± 2 ℃, continues to stir 15 minutes; About 15 minutes, add A1 liquid when stirring, continue to stir 45 minutes; Adding content is 25% ammoniacal liquor 33.6 grams, continues to stir 30 minutes, is warming up to 80 ℃ ± 2 ℃, kept 60 minutes, and added 12 gram melamine resins, regulate pH most 5.0 ± 0.5 with phosphoric acid, kept 120 minutes at 75 ℃, obtain fire retardant emulsion 210 grams, hereinafter to be referred as fire retardant Z1; Fire retardant emulsion Z1 is filtered, water is fully cleaned,, be ground into 300 purpose powder, obtain fire retardant Z6 120 ℃～130 ℃ dryings 2 hours; All comprise phosphorus-compound nitrogen series 100 grams among fire retardant Z1, the Z6, aluminium hydroxide 7.8 grams, aminoresin 6 grams.
Embodiment 8
A kind of preparation method who contains the fire retardant of aminoresin comprises the steps:
In reactor, add 50 gram water, be warming up to 80 ℃, add 0.1 mole magnesium sulfate heptahydrate in the time of stirring, be cooled to behind sal epsom dissolving the becoming transparent liquid 50 ℃ ± 2 ℃ standby, hereinafter to be referred as A2 liquid;
Add 100 gram dehydrated alcohols in reactor, add 100 gram phosphoric acid in the time of stirring and narrow basic urea, keeping temperature is 25 ℃, continues to stir 15 minutes; About 15 minutes, add A2 liquid when stirring, continue to stir 45 minutes; Adding content is 25% ammoniacal liquor 28 grams, continues to stir 30 minutes, is warming up to 80 ℃ ± 2 ℃, kept 60 minutes, and added 15 gram urea-formaldehyde resins, regulate pH most 5.0 ± 0.5 with phosphoric acid, kept 120 minutes at 85 ℃, obtain fire retardant emulsion 210 grams, hereinafter to be referred as fire retardant Z2; Fire retardant emulsion Z2 is filtered, water is fully cleaned,, be ground into 300 purpose powder, obtain fire retardant Z7 120 ℃～130 ℃ dryings 2 hours; All comprise phosphorus-compound nitrogen series 100 grams among fire retardant Z2, the Z7, magnesium hydroxide 5.8 grams, aminoresin 7.5 grams.
Embodiment 9
A kind of preparation method who contains the fire retardant of aminoresin comprises the steps:
In reactor, add 50 gram water, be warming up to 80 ℃, add 0.1 mole Zinc Sulphate Heptahydrate in the time of stirring, be cooled to behind zinc sulfate dissolving the becoming transparent liquid 50 ℃ ± 2 ℃ standby, hereinafter to be referred as A3 liquid;
Add 100 gram dehydrated alcohols in reactor, add 50 gram phosphoric acid in the time of stirring and narrow basic urea, 50 gram Secondary ammonium phosphates, keeping temperature is 20 ℃ ± 2 ℃, continues to stir 15 minutes; About 15 minutes, add A3 liquid when stirring, continue to stir 45 minutes; Adding content is 25% ammoniacal liquor 28 grams, continues to stir 30 minutes, is warming up to 80 ℃ ± 2 ℃, kept 60 minutes, and added melamine resin 13 grams, regulate pH most 5.0 ± 0.5 with phosphoric acid, kept 30 minutes at 95 ℃, obtain fire retardant emulsion 215 grams, hereinafter to be referred as fire retardant Z3; Fire retardant emulsion Z3 is filtered, water is fully cleaned,, be ground into 300 purpose powder, obtain fire retardant Z8 120 ℃～130 ℃ dryings 2 hours; All comprise phosphorus-compound nitrogen series 100 grams among fire retardant Z3, the Z8, zinc hydroxide 9.9 grams, aminoresin 6.5 grams.
Embodiment 10
A kind of preparation method who contains the fire retardant of aminoresin comprises the steps:
In reactor, add 50 gram water, be warming up to 25 ℃, add 0.05 mole of anhydrous slufuric acid aluminium in the time of stirring, Tai-Ace S 150 dissolving becoming transparent liquid; Add 50 gram phosphoric acid when stirring and narrow basic urea, 50 gram ammonium polyphosphates, keeping temperature is 25 ℃ ± 2 ℃, continues to stir 45 minutes; Adding content is 25% ammoniacal liquor 56 grams, continues to stir 30 minutes; Add melamine resin 20 grams, regulate pH most 5.0 ± 0.5, kept 90 minutes, obtain fire retardant emulsion 230 grams, hereinafter to be referred as fire retardant Z4 at 75 ℃ with phosphoric acid; Fire retardant emulsion Z4 is filtered, water is fully cleaned,, be ground into 300 purpose powder, obtain fire retardant Z9 120 ℃～130 ℃ dryings 2 hours; All comprise phosphorus-compound nitrogen series 100 grams among fire retardant Z4, the Z9, aluminium hydroxide 7.8 grams, aminoresin 10 grams.
Embodiment 11
A kind of preparation method who contains the fire retardant of aminoresin, comprise the steps: in reactor, to add 50 gram water, be warming up to 50 ℃, add 0.05 mole of anhydrous slufuric acid aluminium and 0.05 mole of magnesium sulfate heptahydrate in the time of stirring, Tai-Ace S 150 and sal epsom dissolving becoming transparent liquid; Add 50 gram melamine phosphates, 50 gram ammonium polyphosphates when stirring, keeping temperature is 25 ℃ ± 2 ℃, continues to stir 45 minutes; Adding content is 25% ammoniacal liquor 56 grams, continues to stir 30 minutes; Add urea-formaldehyde resin 30 grams, regulate pH most 5.0 ± 0.5, kept 50 minutes, obtain fire retardant emulsion 245 grams, hereinafter to be referred as fire retardant Z5 at 100 ℃ with phosphoric acid; Fire retardant emulsion Z5 is filtered, water is fully cleaned,, be ground into 300 purpose powder, obtain fire retardant Z10 120 ℃～130 ℃ dryings 2 hours; All comprise phosphorus-compound nitrogen series 100 grams among fire retardant Z5, the Z10, aluminium hydroxide 7.8 grams, magnesium hydroxide 2.9 grams, aminoresin 15 grams.
Obviously, the above embodiment of the present invention only is for example of the present invention clearly is described, and is not to be qualification to embodiments of the present invention.For those of ordinary skill in the field, can also make other changes in different forms on the basis of the above description.Here can't give exhaustive to all embodiments.Everyly belong to the row that conspicuous variation that technical scheme of the present invention extends out or change still are in protection scope of the present invention.
Claims (10)
1. fire retardant that contains aminoresin, it is characterized in that: it comprises phosphorus-nitrogen flame retardant, inorganic combustion inhibitor and aminoresin; Described phosphorus-nitrogen flame retardant coats inorganic combustion inhibitor outward, and described inorganic combustion inhibitor coats aminoresin outward; The weight percent of described phosphorus-nitrogen flame retardant, inorganic combustion inhibitor and aminoresin is 100:1～100:1～30.
2. a kind of fire retardant that contains aminoresin according to claim 1 is characterized in that: the weight percent of described phosphorus-nitrogen flame retardant, inorganic combustion inhibitor and aminoresin is 100:5～20:3～15.
3. a kind of fire retardant that contains aminoresin according to claim 1 and 2 is characterized in that: described phosphorus-nitrogen flame retardant is that primary ammonium phosphate, Secondary ammonium phosphate, triammonium phosphate, ammonium polyphosphate, phosphoguanidine, phosphoric acid are narrowed a kind of, two or more mixture in basic urea, phosphoric acid ester, melamine phosphate, the melamine pyrophosphate.
4. a kind of fire retardant that contains aminoresin according to claim 1 and 2 is characterized in that: described inorganic combustion inhibitor is a kind of, two or more the mixture in aluminium hydroxide, magnesium hydroxide, the zinc hydroxide.
5. a kind of fire retardant that contains aminoresin according to claim 1 and 2 is characterized in that: described aminoresin is a kind of, two or more the mixture in urea-formaldehyde resin, cyanurotriamide modified urea resin, melamine resin, the terpolycyantoamino-formaldehyde resin.
6. as a kind of preparation method who contains the fire retardant of aminoresin as described in the claim 1-5, it is characterized in that, comprise the steps:
When 1) stirring phosphorus-nitrogen flame retardant joined and be made into suspension in the solvent;
2) add the aqueous solution of Tai-Ace S 150 and/or aluminum nitrate and/or magnesium chloride and/or sal epsom and/or zinc sulfate and/or zinc chloride and/or zinc nitrate in the suspension, under 25 ℃～100 ℃ condition, kept 5 minutes～120 minutes, get mixture A;
3) in mixture A, add ammoniacal liquor and/or aqueous sodium hydroxide solution, under 25 ℃～100 ℃ condition, kept 5 minutes～120 minutes, get mixture B;
4) in mixture B, add aminoresin, use phosphoric acid to regulate pH most 5.0 ± 0.5, under 25 ℃～100 ℃ condition, kept 30 minutes～120 minutes; Filter or extraction or rotary evaporation or vacuum-evaporation or spraying drying, to remove partial solvent, make the paste fire retardant, or remove whole solvents and make powdery combustion inhibitor;
Wherein, the Tai-Ace S 150 that adds in per 100 gram phosphorus-nitrogen flame retardants and/or the total mole number of aluminum nitrate and/or magnesium chloride and/or sal epsom and/or zinc sulfate and/or zinc chloride and/or zinc nitrate are 0.0064 mole～1.71 moles; The mol ratio of Tai-Ace S 150 and/or aluminum nitrate and/or magnesium chloride and/or sal epsom and/or zinc sulfate and/or zinc chloride and/or zinc nitrate and ammoniacal liquor and/or sodium hydroxide is 1:0.001～1:8.0.
7. a kind of preparation method who contains the fire retardant of aminoresin according to claim 6 is characterized in that: the Tai-Ace S 150 that adds in per 100 gram phosphorus-nitrogen flame retardants and/or the total mole number of aluminum nitrate and/or magnesium chloride and/or sal epsom and/or zinc sulfate and/or zinc chloride and/or zinc nitrate are 0.032～0.342 mole; The mol ratio of Tai-Ace S 150 and/or aluminum nitrate and/or magnesium chloride and/or sal epsom and/or zinc sulfate and/or zinc chloride and/or zinc nitrate and ammoniacal liquor and/or sodium hydroxide is 0.06～2.1.
8. a kind of preparation method who contains the fire retardant of aminoresin according to claim 6 is characterized in that: described solvent is water, ethanol, toluene or dimethylbenzene.
9. as the described a kind of preparation method who contains the fire retardant of aminoresin of claim 1-5, it is characterized in that, comprise the steps:
1) Tai-Ace S 150 and/or aluminum nitrate and/or magnesium chloride and/or sal epsom and/or zinc sulfate and/or zinc chloride and/or zinc nitrate are made into saturated aqueous solution; Add 100 gram phosphorus-nitrogen combustion inhibitors when stirring, under 25 ℃～100 ℃ condition, kept 5 minutes～120 minutes, get mixture C;
2) in mixture C, add ammoniacal liquor and/or aqueous sodium hydroxide solution, under 25～100 ℃ condition, kept 5 minutes～120 minutes, get mixture D;
3) add 1 gram～30 gram aminoresin in the mixture D again, use phosphoric acid to regulate pH most 5.0 ± 0.5, under 25 ℃～100 ℃ condition, kept 30 minutes～120 minutes; Filter or extraction or rotary evaporation or vacuum-evaporation or spraying drying, make the paste fire retardant to remove partial solvent, or remove whole solvents and make powdery combustion inhibitor;
Wherein, the Tai-Ace S 150 that adds in per 100 gram phosphorus-nitrogen combustion inhibitors and/or the total mole number of aluminum nitrate and/or magnesium chloride and/or sal epsom and/or zinc sulfate and/or zinc chloride and/or zinc nitrate are 0.0064 mole～1.71 moles; The mol ratio of Tai-Ace S 150 and/or aluminum nitrate and/or magnesium chloride and/or sal epsom and/or zinc sulfate and/or zinc chloride and/or zinc nitrate and ammoniacal liquor and/or sodium hydroxide is 1:0.001～1:8.0.
10. a kind of preparation method who contains the fire retardant of aminoresin according to claim 9 is characterized in that: the Tai-Ace S 150 that adds in per 100 gram phosphorus-nitrogen combustion inhibitors and/or the total mole number of aluminum nitrate and/or magnesium chloride and/or sal epsom and/or zinc sulfate and/or zinc chloride and/or zinc nitrate are 0.032 mole～0.342 mole; The mol ratio of Tai-Ace S 150 and/or aluminum nitrate and/or magnesium chloride and/or sal epsom and/or zinc sulfate and/or zinc chloride and/or zinc nitrate and ammoniacal liquor and/or sodium hydroxide is 1:0.06～1:2.1.
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Cited By (8)
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| CN102321487A (en) * | 2011-06-24 | 2012-01-18 | 苏州科技学院 | Nano composite intumescent flame retardant and preparation method thereof |
| WO2013066908A1 (en) | 2011-10-31 | 2013-05-10 | Lubrizol Advanced Materials, Inc. | Non-halogen flame retardant as coatings for fibrous filter media |
| WO2014193754A1 (en) | 2013-05-28 | 2014-12-04 | Lubrizol Advanced Materials, Inc. | Non-halogen flame retardant polymers |
| CN104312092A (en) * | 2014-10-15 | 2015-01-28 | 东莞市若茂环保建材有限公司 | Nitrogen-phosphorus compounded expansive type halogen-free flame retardant as well as application thereof in wood-plastic composite material |
| US9290639B2 (en) | 2011-10-31 | 2016-03-22 | Lubrizol Advanced Materials, Inc. | Non-halogen flame retardant polymers |
| CN105437352A (en) * | 2014-09-12 | 2016-03-30 | 北京盛大华源科技有限公司 | Fireproof medium-density fiber board and preparation method thereof |
| CN107759956A (en) * | 2017-11-08 | 2018-03-06 | 蚌埠市华鼎机械科技有限公司 | A kind of preparation method of acid corrosion-resistant battery case |
| CN115819696A (en) * | 2022-10-26 | 2023-03-21 | 福州大学 | Low-free-formaldehyde melamine formaldehyde resin with antibacterial property and preparation method thereof |
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| CN101045779A (en) * | 2007-04-19 | 2007-10-03 | 四川大学 | Preparation method of melamine resin double coated Deca-BDE |
| CN101880408A (en) * | 2010-06-25 | 2010-11-10 | 北京盛大华源科技有限公司 | Flame retardant and preparation method thereof |
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| CN101045779A (en) * | 2007-04-19 | 2007-10-03 | 四川大学 | Preparation method of melamine resin double coated Deca-BDE |
| CN101880408A (en) * | 2010-06-25 | 2010-11-10 | 北京盛大华源科技有限公司 | Flame retardant and preparation method thereof |
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102321487A (en) * | 2011-06-24 | 2012-01-18 | 苏州科技学院 | Nano composite intumescent flame retardant and preparation method thereof |
| WO2013066908A1 (en) | 2011-10-31 | 2013-05-10 | Lubrizol Advanced Materials, Inc. | Non-halogen flame retardant as coatings for fibrous filter media |
| US9290639B2 (en) | 2011-10-31 | 2016-03-22 | Lubrizol Advanced Materials, Inc. | Non-halogen flame retardant polymers |
| US9783687B2 (en) | 2011-10-31 | 2017-10-10 | Lubrizol Advanced Materials, Inc. | Non-halogen flame retardant as coatings for fibrous filter media |
| WO2014193754A1 (en) | 2013-05-28 | 2014-12-04 | Lubrizol Advanced Materials, Inc. | Non-halogen flame retardant polymers |
| CN105437352A (en) * | 2014-09-12 | 2016-03-30 | 北京盛大华源科技有限公司 | Fireproof medium-density fiber board and preparation method thereof |
| CN105437352B (en) * | 2014-09-12 | 2017-12-15 | 北京盛大华源科技有限公司 | One kind fire prevention medium density fibre board (MDF) and preparation method thereof |
| CN104312092A (en) * | 2014-10-15 | 2015-01-28 | 东莞市若茂环保建材有限公司 | Nitrogen-phosphorus compounded expansive type halogen-free flame retardant as well as application thereof in wood-plastic composite material |
| CN104312092B (en) * | 2014-10-15 | 2016-08-24 | 东莞市若茂环保建材有限公司 | A kind of nitrogen phosphorus compounds expanding halide-free fire-retardant and the application at wood plastic composite thereof |
| CN107759956A (en) * | 2017-11-08 | 2018-03-06 | 蚌埠市华鼎机械科技有限公司 | A kind of preparation method of acid corrosion-resistant battery case |
| CN115819696A (en) * | 2022-10-26 | 2023-03-21 | 福州大学 | Low-free-formaldehyde melamine formaldehyde resin with antibacterial property and preparation method thereof |
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