CN107118682A - A kind of preparation method of phosphatization colloidal sol flame retardant polyurethane powdery paints - Google Patents
A kind of preparation method of phosphatization colloidal sol flame retardant polyurethane powdery paints Download PDFInfo
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- CN107118682A CN107118682A CN201710411383.5A CN201710411383A CN107118682A CN 107118682 A CN107118682 A CN 107118682A CN 201710411383 A CN201710411383 A CN 201710411383A CN 107118682 A CN107118682 A CN 107118682A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
- C09D175/04—Polyurethanes
- C09D175/08—Polyurethanes from polyethers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/08—Processes
- C08G18/10—Prepolymer processes involving reaction of isocyanates or isothiocyanates with compounds having active hydrogen in a first reaction step
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/48—Polyethers
- C08G18/4825—Polyethers containing two hydroxy groups
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/03—Powdery paints
- C09D5/033—Powdery paints characterised by the additives
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/18—Fireproof paints including high temperature resistant paints
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G2150/00—Compositions for coatings
- C08G2150/20—Compositions for powder coatings
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/49—Phosphorus-containing compounds
- C08K5/51—Phosphorus bound to oxygen
- C08K5/52—Phosphorus bound to oxygen only
- C08K5/521—Esters of phosphoric acids, e.g. of H3PO4
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- Polyurethanes Or Polyureas (AREA)
- Organic Insulating Materials (AREA)
Abstract
The invention discloses a kind of preparation method of phosphatization colloidal sol flame retardant polyurethane powdery paints, the phosphatization ester colloidal sol that the present invention is added is in burning, non-flammable gases can be discharged, play the effect of gas phase barrier, zinc stannate can also promote finished product to form stable carbon-coating simultaneously, reach collaboration fireproof effect, the phosphatization ester colloidal sol is by can effectively improve its compatibility with polyurethane after organic-treating, reduction is reunited, improve the stability_intensity of finished product film, the present invention is free of poisonous plasticizer, and Safety and Environmental Protection is good, and combination property is superior.
Description
Technical field
The invention belongs to paint field, and in particular to a kind of preparation method of phosphatization colloidal sol flame retardant polyurethane powdery paints.
Background technology
Polyurethane powder coating is just developing into the main flow of powdery paints, and the ratio shared by powdery paints is increasingly
Greatly, there is excellent weatherability due to polyurethane powder coating, excellent physical and mechanical property and anticorrosive property, film light is rich
Full, wear-resisting, damage resistant, solvent resistant, good leveling property, adhesive force are strong；
Powdery paints is Environmentally friendly coatings, and powdery paints and application have that film performance is excellent, technique is easy, once
Coating saves the energy and resource, reduces environmental pollution, easily realizes the recyclable advantage of automation, powder, one up to higher caliper
Appearance can obtain extensive concern, and polyurethane powder coating coating not only has higher ornamental and excellent physical mechanics property
Can, and have more comprehensive chemical proofing, particularly it is difficult xanthochromia, weatherability and light resistance.Polyurethane powder coating is just
Develop into the main flow of powdery paints, shared ratio is increasing in powdery paints, because polyurethane powder coating has
Excellent weatherability, excellent physical and mechanical property and anticorrosive property, film light is plentiful, wear-resisting, damage resistant, solvent resistant, stream
Levelling is good, adhesive force is strong.It is widely used in the household electrical appliances such as refrigerator, washing machine, air-conditioning and noble furniture, automobile, motorcycle at present
Etc. industry；
But the fire resistance of polyurethane powder coating is not good enough at present, the compatibility of inorganic fire-retarded additive and polyurethane
Difference, causes the stability of film coated surface poor, therefore when fire occurs, film forming matter is often heated prior to dehydration catalyst to be divided
Solution, produces more flammable VOC, influences formation and the structure of layer of charcoal, and then influences the protection to base material
Effect.
The content of the invention
It is inorganic fire-retarded to add it is an object of the invention to which the fire resistance for polyurethane powder coating in the prior art is not good enough
Plus the poor compatibility of agent and polyurethane, causing the problem of stability of film coated surface is poor, there is provided a kind of fire-retardant poly- ammonia of phosphatization colloidal sol
The preparation method of ester powdery paints.
To achieve the above object, the present invention uses following technical scheme：
A kind of preparation method of phosphatization colloidal sol flame retardant polyurethane powdery paints, comprises the following steps：
(1) methenamine, the zirconium oxychloride mixing of 16-20 parts by weight of 0.3-0.5 parts by weight are taken, compound weight is added to
In the deionized water of 80-100 times of amount, rise temperature is 50-68 DEG C, and insulated and stirred 10-20 minutes obtains aqueous dispersions；
(2) zinc acetate, the stannous chloride mixing of 6-8 parts by weight of 5-7 parts by weight are taken, compound weight 170- is added to
In 200 times of deionized water, stir, be sent in 80-85 DEG C of water bath with thermostatic control, add above-mentioned aqueous dispersions, insulation is stirred
Mix 70-100 minutes, 1-2mol/l ammoniacal liquor is added dropwise, regulation pH is 11-12, and insulated and stirred 5-6 hours discharges, and centrifugation will be heavy
Form sediment and wash, dried 1-2 hours at 40-50 DEG C of vacuum, obtain hydroxyl filler；
(3) the castor oil acid calcium of 0.7-2 parts by weight is taken, 30-40 times of its weight, 80-86% ethanol solution is added to
In, stir；
(4) above-mentioned hydroxyl filler is taken, is mixed with the catalyst of 0.8-1 parts by weight, rise temperature is 108-110 DEG C, is added dropwise
It is 50-60 DEG C that temperature is reduced after the POCl3 of 2-3 parts by weight, completion of dropping, and the ethanol for adding above-mentioned castor oil acid calcium is water-soluble
Liquid, insulated and stirred 1-2 hours obtains hydroxyl phosphatization dispersion liquid；
(5) above-mentioned hydroxyl phosphatization dispersion liquid is taken, hydrochloric acid solution that 10-17 parts by weight are added dropwise, that concentration is 10-15%,
Insulated and stirred 2-3 hours at 30-35 DEG C, precipitation is washed in filtering, is dried 1-2 hours at 60-70 DEG C of vacuum, and cooling obtains phosphatization
Ester colloidal sol；
(6) the polypropylene glycol ppg2000 of 106-120 parts by weight is taken, vacuum dehydration 2-3 hours at 108-110 DEG C, reduction
Temperature is to 55-60 DEG C, and insulation is standby, must pre-process polypropylene glycol ppg2000；
(7) above-mentioned phosphatization ester colloidal sol, the triethylamine with 1-2 parts by weight, the mixing of 130-140 parts by weight are taken, temperature is raised
For 55-60 DEG C, insulated and stirred 20-30 minutes adds above-mentioned isocyanate-monomer, pretreatment polypropylene glycol ppg2000, is sent to
In reactor, nitrogen is passed through, the dibutyl tin laurate of 3-4 parts by weight is added, rise temperature is 76-85 DEG C, insulation reaction
4-6 hours, cooling discharging obtained phosphatization base polyurethane prepolymer for use as；
(8) above-mentioned phosphatization base polyurethane prepolymer for use as is taken, is mixed with the trimethylolpropane of 10-13 parts by weight, at 80-90 DEG C
Solidification 10-13 hours, is cooled to normal temperature, wears into fine powder, sieves, obtains the phosphatization colloidal sol flame retardant polyurethane powdery paints.
Described isocyanate-monomer is 2,4 toluene diisocyanate.
Described catalyst is anhydrous Aluminum chloride.
Advantages of the present invention：
The present invention disperses, then with black Lip river using zinc acetate, stannous chloride as raw material in the aqueous solution containing zirconium oxychloride
Tropine is catalyst, is hydrolyzed in the basic conditions, obtains hydroxyl filler, then by the trihydroxy filler by POCl3 at
Reason, disperses in alcohol, obtains hydroxyl phosphatization dispersion liquid, it is blended with hydrochloric acid is esterified afterwards, obtain phosphatization ester colloidal sol, the phosphatization
Ester colloidal sol can discharge non-flammable gases in burning, the effect of gas phase barrier be played, while zinc stannate can also promote into
Product form stable carbon-coating, reach collaboration fireproof effect, the phosphatization ester colloidal sol after organic-treating by can effectively carry
Its high compatibility with polyurethane, reduction is reunited, and improves the stability_intensity of finished product film, the present invention is free of poisonous plasticising
Agent, Safety and Environmental Protection is good, and combination property is superior.
Embodiment
The present invention is described in further detail with reference to embodiment, but the implementation of the present invention is not limited to this,
Without departing from the idea case in the present invention described above, according to ordinary skill knowledge and customary means, various replace is made
Change and change, all should be included within the scope of the invention.
Embodiment 1
A kind of preparation method of phosphatization colloidal sol flame retardant polyurethane powdery paints, comprises the following steps：
(1) methenamine, the zirconium oxychloride mixing of 16 parts by weight of 0.3 parts by weight are taken, 80 times of compound weight is added to
Deionized water in, rise temperature be 50 DEG C, insulated and stirred 20 minutes obtains aqueous dispersions；
(2) zinc acetate, the stannous chloride mixing of 6 parts by weight of 5 parts by weight are taken, going for 200 times of compound weight is added to
In ionized water, stir, in the water bath with thermostatic control for being sent to 85 DEG C, add above-mentioned aqueous dispersions, insulated and stirred 100 minutes, drop
Plus 1mol/l ammoniacal liquor, regulation pH is 12, and insulated and stirred 6 hours discharges, and precipitation is washed in centrifugation, and 1 is dried at 50 DEG C of vacuum
Hour, obtain hydroxyl filler；
(3) the castor oil acid calcium of 0.7 parts by weight is taken, is added in 30 times of its weight, 86% ethanol solution, stirring is equal
It is even；
(4) above-mentioned hydroxyl filler is taken, is mixed with the catalyst of 0.8 parts by weight, rise temperature is 110 DEG C, and 3 parts by weight are added dropwise
POCl3, reduction temperature is 50 DEG C after completion of dropping, adds the ethanol water of above-mentioned castor oil acid calcium, insulated and stirred 1
Hour, obtain hydroxyl phosphatization dispersion liquid；
(5) above-mentioned hydroxyl phosphatization dispersion liquid is taken, hydrochloric acid solution that 10 parts by weight are added dropwise, that concentration is 15%, at 35 DEG C
Precipitation is washed in insulated and stirred 3 hours, filtering, is dried 1-2 hours at 70 DEG C of vacuum, and cooling obtains phosphatization ester colloidal sol；
(6) the polypropylene glycol ppg2000 of 106 parts by weight is taken, vacuum dehydration 3 hours at 110 DEG C, reduction temperature to 60
DEG C, insulation is standby, must pre-process polypropylene glycol ppg2000；
(7) above-mentioned phosphatization ester colloidal sol, the triethylamine with 2 parts by weight, the mixing of 140 parts by weight are taken, rise temperature is 60 DEG C,
Insulated and stirred 20 minutes, adds above-mentioned isocyanate-monomer, pretreatment polypropylene glycol ppg2000, is sent in reactor, is passed through
Nitrogen, adds the dibutyl tin laurate of 3 parts by weight, and rise temperature is 85 DEG C, insulation reaction 4 hours, and cooling discharging obtains phosphorus
Change base polyurethane prepolymer for use as；
(8) above-mentioned phosphatization base polyurethane prepolymer for use as is taken, is mixed with the trimethylolpropane of 13 parts by weight, 10 are solidified at 90 DEG C
Hour, normal temperature is cooled to, fine powder is worn into, sieves, obtains the phosphatization colloidal sol flame retardant polyurethane powdery paints.
Described isocyanate-monomer is 2,4 toluene diisocyanate.
Described catalyst is anhydrous Aluminum chloride.
Embodiment 2
A kind of preparation method of phosphatization colloidal sol flame retardant polyurethane powdery paints, comprises the following steps：
(1) methenamine, the zirconium oxychloride mixing of 20 parts by weight of 0.5 parts by weight are taken, 100 times of compound weight is added to
Deionized water in, rise temperature be 68 DEG C, insulated and stirred 20 minutes obtains aqueous dispersions；
(2) zinc acetate, the stannous chloride mixing of 8 parts by weight of 7 parts by weight are taken, going for 200 times of compound weight is added to
In ionized water, stir, in the water bath with thermostatic control for being sent to 85 DEG C, add above-mentioned aqueous dispersions, insulated and stirred 100 minutes, drop
Plus 2mol/l ammoniacal liquor, regulation pH is 12, and insulated and stirred 6 hours discharges, and precipitation is washed in centrifugation, and 2 are dried at 50 DEG C of vacuum
Hour, obtain hydroxyl filler；
(3) the castor oil acid calcium of 2 parts by weight is taken, is added in 40 times of its weight, 86% ethanol solution, stirring is equal
It is even；
(4) above-mentioned hydroxyl filler is taken, is mixed with the catalyst of 1 parts by weight, rise temperature is 110 DEG C, and 3 parts by weight are added dropwise
It is 60 DEG C that temperature is reduced after POCl3, completion of dropping, adds the ethanol water of above-mentioned castor oil acid calcium, and insulated and stirred 2 is small
When, obtain hydroxyl phosphatization dispersion liquid；
(5) above-mentioned hydroxyl phosphatization dispersion liquid is taken, hydrochloric acid solution that 17 parts by weight are added dropwise, that concentration is 15%, at 35 DEG C
Precipitation is washed in insulated and stirred 3 hours, filtering, is dried 2 hours at 70 DEG C of vacuum, and cooling obtains phosphatization ester colloidal sol；
(6) the polypropylene glycol ppg2000 of 120 parts by weight is taken, vacuum dehydration 3 hours at 110 DEG C, reduction temperature to 60
DEG C, insulation is standby, must pre-process polypropylene glycol ppg2000；
(7) above-mentioned phosphatization ester colloidal sol, the triethylamine with 2 parts by weight, the mixing of 140 parts by weight are taken, rise temperature is 60 DEG C,
Insulated and stirred 30 minutes, adds above-mentioned isocyanate-monomer, pretreatment polypropylene glycol ppg2000, is sent in reactor, is passed through
Nitrogen, adds the dibutyl tin laurate of 4 parts by weight, and rise temperature is 85 DEG C, insulation reaction 6 hours, and cooling discharging obtains phosphorus
Change base polyurethane prepolymer for use as；
(8) above-mentioned phosphatization base polyurethane prepolymer for use as is taken, is mixed with the trimethylolpropane of 13 parts by weight, 13 are solidified at 90 DEG C
Hour, normal temperature is cooled to, fine powder is worn into, sieves, obtains the phosphatization colloidal sol flame retardant polyurethane powdery paints.
Described isocyanate-monomer is 2,4 toluene diisocyanate.
Described catalyst is anhydrous Aluminum chloride.
Embodiment 3
A kind of preparation method of phosphatization colloidal sol flame retardant polyurethane powdery paints, comprises the following steps：
(1) methenamine, the zirconium oxychloride mixing of 16 parts by weight of 0.3 parts by weight are taken, 80 times of compound weight is added to
Deionized water in, rise temperature be 50 DEG C, insulated and stirred 10 minutes obtains aqueous dispersions；
(2) zinc acetate, the stannous chloride mixing of 6 parts by weight of 5 parts by weight are taken, going for 170 times of compound weight is added to
In ionized water, stir, in the water bath with thermostatic control for being sent to 80 DEG C, add above-mentioned aqueous dispersions, insulated and stirred 70 minutes is added dropwise
1mol/l ammoniacal liquor, regulation pH is 11, and insulated and stirred 5 hours discharges, and precipitation is washed in centrifugation, 1 is dried at 40 DEG C of vacuum small
When, obtain hydroxyl filler；
(3) the castor oil acid calcium of 0.7 parts by weight is taken, is added in 30 times of its weight, 80% ethanol solution, stirring is equal
It is even；
(4) above-mentioned hydroxyl filler is taken, is mixed with the catalyst of 0.8 parts by weight, rise temperature is 108 DEG C, and 2 parts by weight are added dropwise
POCl3, reduction temperature is 50 DEG C after completion of dropping, adds the ethanol water of above-mentioned castor oil acid calcium, insulated and stirred 1
Hour, obtain hydroxyl phosphatization dispersion liquid；
(5) above-mentioned hydroxyl phosphatization dispersion liquid is taken, hydrochloric acid solution that 10 parts by weight are added dropwise, that concentration is 10-15%, at 30 DEG C
Precipitation is washed in lower insulated and stirred 2 hours, filtering, is dried 1 hour at 60-70 DEG C of vacuum, and cooling obtains phosphatization ester colloidal sol；
(6) the polypropylene glycol ppg2000 of 106 parts by weight is taken, vacuum dehydration 2 hours at 108 DEG C, reduction temperature to 55
DEG C, insulation is standby, must pre-process polypropylene glycol ppg2000；
(7) above-mentioned phosphatization ester colloidal sol, the triethylamine with 1 parts by weight, the mixing of 130 parts by weight are taken, rise temperature is 55 DEG C,
Insulated and stirred 20 minutes, adds above-mentioned isocyanate-monomer, pretreatment polypropylene glycol ppg2000, is sent in reactor, is passed through
Nitrogen, adds the dibutyl tin laurate of 3 parts by weight, and rise temperature is 76 DEG C, insulation reaction 4 hours, and cooling discharging obtains phosphorus
Change base polyurethane prepolymer for use as；
(8) above-mentioned phosphatization base polyurethane prepolymer for use as is taken, is mixed with the trimethylolpropane of 10 parts by weight, 10 are solidified at 80 DEG C
Hour, normal temperature is cooled to, fine powder is worn into, sieves, obtains the phosphatization colloidal sol flame retardant polyurethane powdery paints.
Described isocyanate-monomer is 2,4 toluene diisocyanate.
Described catalyst is anhydrous Aluminum chloride.
Performance test：
As can be seen that the coating of the present invention has more preferable fire retardant performance.
Claims (3)
1. a kind of preparation method of phosphatization colloidal sol flame retardant polyurethane powdery paints, it is characterised in that comprise the following steps：
(1) methenamine, the zirconium oxychloride mixing of 16-20 parts by weight of 0.3-0.5 parts by weight are taken, compound weight is added to
In 80-100 times of deionized water, rise temperature is 50-68 DEG C, and insulated and stirred 10-20 minutes obtains aqueous dispersions；
(2) zinc acetate, the stannous chloride mixing of 6-8 parts by weight of 5-7 parts by weight are taken, 170-200 times of compound weight is added to
Deionized water in, stir, be sent in 80-85 DEG C of water bath with thermostatic control, add above-mentioned aqueous dispersions, insulated and stirred 70-
100 minutes, 1-2mol/l ammoniacal liquor is added dropwise, regulation pH is 11-12, and insulated and stirred 5-6 hours discharges, and centrifugation will precipitate water
Wash, dried 1-2 hours at 40-50 DEG C of vacuum, obtain hydroxyl filler；
(3) take in the castor oil acid calcium of 0.7-2 parts by weight, ethanol solution that be added to 30-40 times of its weight, 80-86%, stir
Mix uniform；
(4) above-mentioned hydroxyl filler is taken, is mixed with the catalyst of 0.8-1 parts by weight, rise temperature is 108-110 DEG C, 2-3 weights are added dropwise
It is 50-60 DEG C to measure reduction temperature after the POCl3 of part, completion of dropping, adds the ethanol water of above-mentioned castor oil acid calcium, protects
Temperature stirring 1-2 hours, obtains hydroxyl phosphatization dispersion liquid；
(5) above-mentioned hydroxyl phosphatization dispersion liquid is taken, hydrochloric acid solution that 10-17 parts by weight are added dropwise, that concentration is 10-15%, in 30-35
Insulated and stirred 2-3 hours at DEG C, precipitation is washed in filtering, is dried 1-2 hours at 60-70 DEG C of vacuum, and cooling obtains phosphatization ester molten
Glue；
(6) the polypropylene glycol ppg2000 of 106-120 parts by weight is taken, vacuum dehydration 2-3 hours at 108-110 DEG C, temperature is reduced
To 55-60 DEG C, insulation is standby, must pre-process polypropylene glycol ppg2000；
(7) above-mentioned phosphatization ester colloidal sol, the triethylamine with 1-2 parts by weight, the mixing of 130-140 parts by weight are taken, rise temperature is 55-
60 DEG C, insulated and stirred 20-30 minutes adds above-mentioned isocyanate-monomer, pretreatment polypropylene glycol ppg2000, is sent to reaction
In kettle, nitrogen is passed through, the dibutyl tin laurate of 3-4 parts by weight is added, rise temperature is 76-85 DEG C, and insulation reaction 4-6 is small
When, cooling discharging obtains phosphatization base polyurethane prepolymer for use as；
(8) above-mentioned phosphatization base polyurethane prepolymer for use as is taken, is mixed with the trimethylolpropane of 10-13 parts by weight, is solidified at 80-90 DEG C
10-13 hours, normal temperature is cooled to, fine powder is worn into, sieves, obtains the phosphatization colloidal sol flame retardant polyurethane powdery paints.
2. a kind of preparation method of phosphatization colloidal sol flame retardant polyurethane powdery paints according to claim 1, it is characterised in that
Described isocyanate-monomer is 2,4 toluene diisocyanate.
3. a kind of preparation method of phosphatization colloidal sol flame retardant polyurethane powdery paints according to claim 1, it is characterised in that
Described catalyst is anhydrous Aluminum chloride.
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| CN107383310A (en) * | 2017-07-24 | 2017-11-24 | 陈涛 | A kind of preparation method of phosphatization flame retardant polyurethane material |
| CN107880241A (en) * | 2017-11-23 | 2018-04-06 | 清远初曲智能科技有限公司 | A kind of phosphatization colloidal sol flame retardant polyurethane material and preparation method thereof |
| CN108219340A (en) * | 2018-01-03 | 2018-06-29 | 温州市登达化工有限公司 | A kind of soft cross-linked polyurethane materials and preparation method thereof |
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| CN107383310A (en) * | 2017-07-24 | 2017-11-24 | 陈涛 | A kind of preparation method of phosphatization flame retardant polyurethane material |
| CN107880241A (en) * | 2017-11-23 | 2018-04-06 | 清远初曲智能科技有限公司 | A kind of phosphatization colloidal sol flame retardant polyurethane material and preparation method thereof |
| CN108219340A (en) * | 2018-01-03 | 2018-06-29 | 温州市登达化工有限公司 | A kind of soft cross-linked polyurethane materials and preparation method thereof |
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