CN1294236C - Melamine cyanuric acid microcapsule inorganic frame retardant and its preparation method - Google Patents
Melamine cyanuric acid microcapsule inorganic frame retardant and its preparation method Download PDFInfo
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- CN1294236C CN1294236C CNB2004100409908A CN200410040990A CN1294236C CN 1294236 C CN1294236 C CN 1294236C CN B2004100409908 A CNB2004100409908 A CN B2004100409908A CN 200410040990 A CN200410040990 A CN 200410040990A CN 1294236 C CN1294236 C CN 1294236C
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- melamine cyanurate
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Abstract
The present invention relates to a melamine cyanurate microcapsule inorganic flame retardant and a preparation method thereof, which is characterized in that firstly, 10 to 300 portions (by weight) of inorganic flame retarding powder and 100 to 1000 portions (by weight) of water are added into a reaction kettle with a stirrer and a thermometer and dispersed at the temperature of 50 to 130 DEG C; then, 1 to 100 portions (by weight)of flame retarding synergist, 50 to 100 portions (by weight) of melamine and 50 to 200 portions (by weight) of cyanuric acid are added into the reaction kettle and stirred at the temperature of 50 to 150 DEG C so that the components react for 5 minutes to 2 hours; in the reaction process, 100 to 1000 portions (by weight) of water can be complemented, and thus, white emulsion or a thick paste substance of the inorganic flame retardant coated by melamine cyanuric acid is obtained; after the emulsion or the thick paste substance is filtered or centrifugally separated, dried and pulverized, 0.01 to 500 mum of inorganic flame retardant coated by the melamine cyanuric acid is obtained.
Description
One, technical field
The present invention relates to a kind of melamine cyanurate microcapsule inorganic combustion inhibitor and preparation method thereof, belong to the fire retardant preparation field.
Two, background technology
Inorganic combustion inhibitors such as magnesium hydroxide, aluminium hydroxide, phosphoric acid salt, borate, molybdate are to develop environment friendly flame retardant kind rapidly at present, and its consumption accounts for 80% of fire retardant aggregate consumption.Inorganic combustion inhibitor has Halogen, nontoxic, low cigarette, advantage such as inexpensive, is widely used in the polymer materials preparation field.The fire retardant mechanism of different inorganic combustion inhibitors is different, and metal hydroxides class inorganic combustion inhibitor (magnesium hydroxide, aluminium hydroxide) mainly is to discharge combination water by pyrolytic decomposition, plays the cooling fire retardation; Phosphoric acid salt and borate family (as ammonium polyphosphate, zinc borate etc.) then mainly are to form barrier layer at material surface, and the anoxybiotic thermal insulation suppresses burning.
The main drawback of inorganic combustion inhibitor is the surface polarity height, easily moisture absorption conglomeration, interface compatibility is poor when using as polymer flame retardant and between the resin, addition big (generally more than 50wt%), can cause after the filling the mobile variation of polymer processing with the mechanical property deterioration, so surface modification is such Study of Flame Retardant emphasis always.The surface modification of inorganic combustion inhibitor generally adopts coupling agent or tensio-active agent to handle at present, and surface treatment agent commonly used has silane series, titanic acid ester series, hard ester acid and its esters.Can reduce the inorganic combustion inhibitor surface polarity to a certain extent by coupling agent or tensio-active agent processing, the interface binding power between enhancing and the resin matrix increases material mechanical performance, but materials processing flowability and flame retardant properties are not had improvement substantially.
Melamine cyanurate is the triazine ring molecular complex with big plane hydrogen bond network that trimeric cyanamide and cyanuric acid are formed by hydrogen bonded, is a kind of good nitrogen flame retardant and lubricant.Its outward appearance is the white crystals powder with soapy feeling, and is nontoxic, tasteless, is insoluble in water and general organic solvent.It is stable below 300 ℃, and 400 ℃ begin distillation and are decomposed into trimeric cyanamide and cyanuric acid simultaneously.Characteristics such as that melamine cyanurate has is fire-retardant, lubricated, delustring can be used for that plastics are fire-retardant, power lubrication, Coating Matting and makeup and field of printing and dyeing.Melamine cyanurate has the advantage of nontoxic, low cigarette as fire retardant, its preparation is a raw material with trimeric cyanamide and cyanuric acid generally, water is dispersion medium, under 100-120 ℃ of temperature condition, react and make, have from thickening effect in the melamine cyanurate synthetic reaction process, reaction system viscosity continues to rise, and the material state changes no mobile paste into by the soup compound that can flow.
Three, summary of the invention
The objective of the invention is provides a kind of melamine cyanurate microcapsule inorganic combustion inhibitor and preparation method thereof at the deficiencies in the prior art.Be characterized in by realizing being scattered in inorganic combustion inhibitor particle or the coating of the inorganic combustion inhibitor of generation on the spot in the system in the melamine cyanurate building-up process from thickening effect, after resulting paste dehydrates, can be used as fire retardant after the pulverizing and use.
The present inventor finds that inorganic combustion inhibitor frictional coefficient after melamine cyanurate coats reduces, has good lubricity, and its flame-proofed polymer material can keep higher fluidity of molten; Can improve the interface compatibility of inorganic combustion inhibitor and polymer materials with melamine cyanurate as surface coating layer, improve material mechanical performance; Nitrogen flame retardant melamine cyanurate and inorganic combustion inhibitor have complementarity on fire retardant mechanism, give full play to its synergistic effect, and its composite flame retardant system has better flame retardant effect to some polymer materials than single inorganic combustion inhibitor.
The objective of the invention is to realize that by following technical measures wherein said raw material umber is parts by weight except that specified otherwise.
The recipe ingredient of melamine cyanurate microcapsule inorganic combustion inhibitor starting raw material is:
Powders 50-200 part
Trimeric cyanamide 50-100 part
Cyanuric acid 50-200 part
Water 200-2000 part
Retardant synergist 1-100 part
Wherein inorganic combustion inhibitor is at least a of magnesium hydroxide, aluminium hydroxide, ammonium polyphosphate, zinc borate.
Retardant synergist is at least a in phosphoric acid, ammonium sulfate, phospho-wolframic acid, silicotungstic acid, Dyhard RU 100, tetramethylolmethane, the dipentaerythrityl ether.
The preparation method of melamine cyanurate coated inorganic fire retardant:
50～200 parts of powders, water 200-2000 part are added in the reactor of belt stirrer, thermometer, make it to disperse in temperature 50-130 ℃, add retardant synergist 1-100 part, trimeric cyanamide 50-100 part and cyanuric acid 50-200 part successively, in temperature 50-150 ℃ stirring reaction 5 minutes-2 hours, obtain white or light cream or thickness paste; With above-mentioned milk sap or thickness paste after filtration or obtain the melamine cyanurate coated inorganic fire retardant of 0.01-500 μ m after the centrifugation, drying, pulverizing.
The present invention has following advantage:
(1) technology is simple, and is easy to operate.
(2) melamine cyanurate form big plane hydrogen bond network process from the effective coated inorganic fire retardant of thickening effect.
(3) the melamine cyanurate water-intake rate is extremely low, can prevent inorganic combustion inhibitor moisture absorption caking.
(4) melamine cyanurate has excellent lubricating properties, and its coated inorganic fire retardant can reduce latter's frictional coefficient greatly, improves the fluidity of molten of its flame-proofed polymer material, improves its processing characteristics.
(5) melamine cyanurate coated inorganic fire retardant is a kind of novel organic-inorganic composite flame retardants with " nucleocapsid " structure, has complementarity on fire retardant mechanism, gives full play to synergistic effect, can improve the flame retardant properties of single inorganic combustion inhibitor.
(6) melamine cyanurate coated inorganic fire retardant can improve inorganic combustion inhibitor and polymer materials consistency, helps improving the material over-all properties.
Four, embodiment
Below by embodiment the present invention is specifically described.Be necessary to be pointed out that at this following examples only are used for the present invention is further specified; can not be interpreted as limiting the scope of the invention, the person skilled in the art in this field can make some nonessential improvement and adjustment to the present invention according to the invention described above content.
Embodiment:
1. in reactor, retardant synergist Dyhard RU 100 1kg is dissolved in the 200kg water, add magnesium hydrate powder 50kg, stirring makes its homodisperse, again with trimeric cyanamide 50kg and cyanuric acid 50kg, add in the reactor, in 95 ℃ of stirring reactions of temperature 1 hour, the thickness paste that obtains, this paste after filtration, dry, the powder-product that makes average particle size 3 μ m after pulverizing.
2. in reactor, retardant synergist phospho-wolframic acid 30kg is dissolved in the 1000kg water, add ammonium polyphosphate powder 100kg, stirring makes its homodisperse, add trimeric cyanamide 75kg and cyanuric acid 75kg more successively, 110 ℃ of stirring reactions of temperature 30 minutes, obtain the thickness paste, add water 3kg and continue reaction 20 minutes, the gained emulsion makes the powder-product that average particle size is 10 μ m after centrifugation, drying, pulverizing.
3. in reactor, retardant synergist Dyhard RU 100 15kg and tetramethylolmethane 15kg are dissolved in the 1800kg water, add zinc borate power 200kg, stirring makes its homodisperse, the cyanuric acid that adds trimeric cyanamide 100kg and 105kg again, in 100 ℃ of stirring reactions of temperature 10 minutes, obtain white milk sap, this milk sap makes the powder-product that average particle size is 50 μ m after the spraying equipment spraying drying.
4. in reactor, add 400kg water, be warming up to 100 ℃, add 60 kilograms in aluminium hydroxide, stirring makes its homodisperse, add phosphatase 11 kg, silicotungstic acid 1kg, trimeric cyanamide 60kg and cyanuric acid 65kg again and in mixing tank, be pre-mixed, in the middle then immigration reactor, stirring reaction 2 hours, the thickness paste that obtains, this paste after filtration, dry, make the powder-product that average particle size is 150 μ m after pulverizing.
Claims (3)
1. melamine cyanurate microcapsule inorganic combustion inhibitor is characterized in that the recipe ingredient of starting raw material is by weight:
Powders 50-200 part
Trimeric cyanamide 50-100 part
Cyanuric acid 50-200 part
Water 200-2000 part
Retardant synergist 1-100 part
Wherein said melamine cyanurate microcapsule inorganic combustion inhibitor prepares by following method:
Powders and water adding are had in the reactor of agitator, thermometer, make it to disperse in temperature 50-130 ℃, add retardant synergist, trimeric cyanamide and cyanuric acid then, in temperature 50-150 ℃ stirring reaction 5 minutes-2 hours, make white or light cream or thickness paste, after filtration or obtain the melamine cyanurate microcapsule inorganic combustion inhibitor of 0.01-500 μ m after the centrifugation, drying, pulverizing;
Inorganic combustion inhibitor is at least a of magnesium hydroxide, aluminium hydroxide, ammonium polyphosphate, zinc borate.
2. melamine cyanurate microcapsule inorganic combustion inhibitor as claimed in claim 1 is characterized in that retardant synergist is at least a in phosphoric acid, ammonium sulfate, phospho-wolframic acid, silicotungstic acid, Dyhard RU 100, tetramethylolmethane, the dipentaerythrityl ether.
3. the preparation method of melamine cyanurate microcapsule inorganic combustion inhibitor as claimed in claim 1 or 2 is characterized in that:
(1) powders 50～200 weight parts, water 200-2000 weight part are added in the reactor of belt stirrer, thermometer, make it to disperse in temperature 50-130 ℃, add retardant synergist 1-100 weight part, trimeric cyanamide 50-100 weight part and cyanuric acid 50-200 weight part then, in temperature 50-150 ℃ stirring reaction 5 minutes-2 hours, obtain white or light cream or thickness paste;
(2) above-mentioned milk sap or thickness paste after filtration or after the centrifugation, drying, pulverizing, are obtained the melamine cyanurate microcapsule inorganic combustion inhibitor of 0.01-500 μ m.
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2004100409908A CN1294236C (en) | 2004-11-09 | 2004-11-09 | Melamine cyanuric acid microcapsule inorganic frame retardant and its preparation method |
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| CNB2004100409908A CN1294236C (en) | 2004-11-09 | 2004-11-09 | Melamine cyanuric acid microcapsule inorganic frame retardant and its preparation method |
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| CN1632058A CN1632058A (en) | 2005-06-29 |
| CN1294236C true CN1294236C (en) | 2007-01-10 |
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Families Citing this family (13)
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| CN1322044C (en) * | 2005-08-16 | 2007-06-20 | 上海工程技术大学 | Microcapsulized expansion type flame-proof rubber and its preparation method |
| CN101781571B (en) * | 2009-12-18 | 2013-01-09 | 苏州科技学院 | Complex intumescent flame retardant |
| CN101792674B (en) * | 2010-03-19 | 2012-09-12 | 大连理工大学 | Method for preparing nitrogen-phosphorus-magnesium compound fire retardant |
| CN101892020B (en) * | 2010-07-15 | 2012-11-21 | 中国林业科学研究院木材工业研究所 | Flame retardant, preparation method thereof and method for preparing artificial boards from same |
| CN103122101B (en) * | 2013-01-24 | 2015-04-29 | 广东聚石化学股份有限公司 | High glow-wire anti-flaming polypropylene composite and production method of polypropylene composite |
| CN104311500B (en) * | 2014-09-29 | 2016-07-06 | 济南泰星精细化工有限公司 | Sol-gel modified method prepares the method for melamine cyanurate |
| CN104312314A (en) * | 2014-11-19 | 2015-01-28 | 徐妍玲 | Reflexive fireproof paint |
| CN107722356A (en) * | 2017-10-19 | 2018-02-23 | 云南江磷集团股份有限公司 | Melamine cyanurate microencapsulation Red Phosphorus Flame Retardant product and preparation method thereof |
| CN109576808B (en) * | 2018-11-29 | 2021-08-24 | 青岛邦特生态纺织科技有限公司 | Inorganic flame-retardant intelligent temperature-adjusting cellulose fiber and preparation method thereof |
| CN110607066B (en) * | 2019-10-09 | 2021-12-28 | 江苏万纳普新材料科技有限公司 | Special halogen-free flame-retardant synergistic functional master batch for modifying polyformaldehyde and preparation method thereof |
| CN113912909B (en) * | 2021-10-21 | 2023-05-12 | 扬州工业职业技术学院 | Melamine cyanurate/LDH composite flame-retardant material and preparation method thereof |
| CN116082711A (en) * | 2021-11-05 | 2023-05-09 | 甘肃坤远节能环保科技发展有限公司 | Flame retardant formula containing MCA microcapsule silicone rubber foam and preparation method thereof |
| CN113969175A (en) * | 2021-11-23 | 2022-01-25 | 上海聚千新材料发展有限公司 | Production and preparation method of red phosphorus flame-retardant synergist |
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| US4786673A (en) * | 1984-05-21 | 1988-11-22 | Atochem | Flame retarded polyamides |
| JPH11323101A (en) * | 1998-05-11 | 1999-11-26 | Kanegafuchi Chem Ind Co Ltd | Flame-retardant conductive polyester resin composition |
| JP2000160031A (en) * | 1998-12-01 | 2000-06-13 | Chisso Corp | Flame retardant thermoplastic resin composition |
| CN1515615A (en) * | 2003-08-26 | 2004-07-28 | 四川大学 | Molecular composite trimeric cyanamide cyanurate fire retarder and its preparation method and application |
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2004
- 2004-11-09 CN CNB2004100409908A patent/CN1294236C/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4786673A (en) * | 1984-05-21 | 1988-11-22 | Atochem | Flame retarded polyamides |
| JPH11323101A (en) * | 1998-05-11 | 1999-11-26 | Kanegafuchi Chem Ind Co Ltd | Flame-retardant conductive polyester resin composition |
| JP2000160031A (en) * | 1998-12-01 | 2000-06-13 | Chisso Corp | Flame retardant thermoplastic resin composition |
| CN1515615A (en) * | 2003-08-26 | 2004-07-28 | 四川大学 | Molecular composite trimeric cyanamide cyanurate fire retarder and its preparation method and application |
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