CN106883457A - It is a kind of to mould with the preparation method of flame retardant type aluminium pigment - Google Patents
It is a kind of to mould with the preparation method of flame retardant type aluminium pigment Download PDFInfo
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- CN106883457A CN106883457A CN201710077395.9A CN201710077395A CN106883457A CN 106883457 A CN106883457 A CN 106883457A CN 201710077395 A CN201710077395 A CN 201710077395A CN 106883457 A CN106883457 A CN 106883457A
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
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- 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
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/04—Homopolymers or copolymers of ethene
- C08L23/06—Polyethene
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- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/10—Homopolymers or copolymers of propene
- C08L23/12—Polypropene
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- C08L25/00—Compositions of, homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring; Compositions of derivatives of such polymers
- C08L25/02—Homopolymers or copolymers of hydrocarbons
- C08L25/04—Homopolymers or copolymers of styrene
- C08L25/06—Polystyrene
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L27/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers
- C08L27/02—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L27/04—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment containing chlorine atoms
- C08L27/06—Homopolymers or copolymers of vinyl chloride
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- C08L55/00—Compositions of homopolymers or copolymers, obtained by polymerisation reactions only involving carbon-to-carbon unsaturated bonds, not provided for in groups C08L23/00 - C08L53/00
- C08L55/02—ABS [Acrylonitrile-Butadiene-Styrene] polymers
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/08—Metals
- C08K2003/0812—Aluminium
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- C—CHEMISTRY; METALLURGY
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- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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Abstract
The present invention relates to a kind of modeling preparation method of flame retardant type aluminium pigment, surface modification cladding is carried out to aluminium powder by using silicon systems, phosphorus flame retardant two-step method, through mechanical agitation, suction filtration, vacuum drying, obtain the aluminium pigment of Surface coating organic polymer.Aluminium pigment surface prepared by the method carries out the fire-retardant cladding of phosphorus silicon systems, the security that aluminium powder is used in flammable resin can be greatly improved, the addition of phosphorus flame retardant simultaneously, compatibility of the aluminium powder in resin is improve with dispersiveness, contribute to the mechanical property of reinforcement resin, aluminium pigment prepared by the method further widens its application in Plastics Processing Industry, and rational technology, it is easy to operate, be easy to industrialization, be a kind of environment-friendly fire retardant.
Description
Technical field
The present invention relates to a kind of modeling preparation method of flame retardant type aluminium pigment, belong to aluminium pigment preparing technical field.
Background technology
Aluminium pigment is with its " color travel " performance attractive in appearance and its height to visible ray, ultraviolet light and infrared light in recent years
Insulation, radiation-resistant protective value that albedo is played, are well received by consumers, and its consumption rapid development is main
Application field has the every field such as industrial coating, car paint, printing-ink and Plastics Processing Industry.
However, plastics have the shortcomings that as most of macromolecular materials one it is fatal, easy firing and release at high temperature
The heat of amplification quantity, its burning velocity is fast, and difficulty is put out, and thus brings disaster hidden-trouble.It is worth noting that, due to aluminium powder in pigment
Addition can increase the danger of modeling product, its more general dust combustion of burning is rapider, and explosion hazard is big.Therefore exist
Fire retardant is added in plastics fairly common, its flammability can be reduced, slow down burning velocity, contribute to safe handling.But
Aluminium pigment is poor with fire retardant compatibility, is individually dispersed in plastic resin, when resin burns, exposes aerial aluminium powder
Still suffer from potential safety hazard.
At present, when using aluminium pigment, its surface is modified, makes possess flame-retarding characteristic, while improving it in plastics
Dispersed and affine performance in resin, wherein, organic phosphorus compound is conventional additive flame retardant, organic phosphorus compound
With fire-retardant, plasticising dual-use function, halogenation flame retardant can be replaced, be a kind of environment amenable fire retardant.Phosphate is that have
A kind of fire retardant in machine phosphorus compound, the fire retardant aboundresources, while have that steam is forced down, animal migration is small concurrently, good endurance,
Toxicity is low, colourless, odorless, hydrolysis the advantages of, thus phosphate is widely used in makrolon（PC）, acrylonitrile-butadiene-
Styrol copolymer（ABS）, polypropylene（PP）, polyurethane（PU）Deng material.But, most of phosphate flame retardants are liquid,
Poor heat resistance, volatility is big, and the compatibility with polymer is undesirable.Organic silicon fibre retardant is a kind of new and effective, low toxicity, prevents molten
Drop, environment-friendly harmless fire retardant, organic silicon fibre retardant is except with fire resistance, moreover it is possible to improve base material processing characteristics,
Heat resistance etc..Accordingly, as the up-and-coming youngster of fire retardant, obtain developing rapidly still since 21 century, the fire retardant system
Make high cost.And the toxicity of phosphorus fire retardant can be not only reduced using phosphorus-containing organosilicon flame retardant, and it is fire-retardant to reduce silicon
The price of agent, with good cooperative flame retardant effect.
Therefore, it is necessary to provide a kind of phosphoric organic silicon method for coating effective to aluminium powder, form fire-retardant on aluminium powder surface
Property coating film, improve aluminium powder fire resistance and the compatibility with various types of resins, while not destroying the aesthetic effect of aluminium pigment.
The content of the invention
A kind of modeling flame retardant type provided it is an object of the invention to overcome potential safety hazard of the aluminium powder in resin application
The preparation method of aluminium pigment.
The purpose of the present invention can be achieved through the following technical solutions：
It is a kind of to mould with the preparation method of flame retardant type aluminium pigment, it is characterised in that the method is comprised the following steps：
A. 10~100g aluminum pastes are weighed, is by weight 1 by aluminum paste and organic solvent:It is placed in after 3~6 ratio mixing
In container, ultrasonic disperse is carried out 30~60 minutes；
B. the slurries after above-mentioned ultrasound are carried out into water-bath under the conditions of 30~40 DEG C, mechanical agitation 4~8 hours, is 160 with rotating speed
~400 turns/min, then suction filtration, obtains filter cake, by vacuum drying under the conditions of filter cake in an oven 100~120 DEG C；
C. a certain amount of first organic solvent is weighed, is according to weight ratio with the first organic solvent by the aluminium powder after above-mentioned drying
1：The ratio mixing of (5~15), then, under nitrogen protection, to catalyst is added in above-mentioned solvent mixed solution, is adjusted molten
The pH value of agent mixed solution is 8~10；Add silane coupler, the addition of coupling agent be the first organic solvent 0.5%~
5%；Then above-mentioned compound is carried out into mechanical agitation 2~6 hours, reaction temperature is 40~60 DEG C, speed of agitator is 160~400
Turn/min, suction filtration is carried out after stirring；
D. a certain amount of second organic solvent is weighed, is according to weight ratio with the second organic solvent by the aluminium powder after above-mentioned suction filtration
1：The ratio mixing of (5~15), then, under nitrogen protective condition, to adding phosphate, phosphorus in above-mentioned solvent mixed solution
The addition of acid esters is the 0.125%~2.5% of the second organic solvent, then proceeds by 4~8h of mechanical agitation, and speed of agitator is
160~400 turns/min, reaction temperature is controlled at 50~90 DEG C, and suction filtration is carried out after stirring, and filter cake is obtained after suction filtration, then will filter
Cake is placed in vacuum drying in 60 DEG C of baking ovens, obtains modeling flame retardant type aluminium pigment.
Above-mentioned steps（A）Described in organic solvent be in ethyl acetate, n-butyl acetate, tetrahydrofuran, toluene
Plant or two kinds.
Above-mentioned steps（A）Described in aluminum paste be silver dollar type or corn type, particle diameter be 8~100 μm.
Above-mentioned steps（C）Described in the first organic solvent be one or two in methyl alcohol, ethanol, acetone.
Above-mentioned steps（C）Described in catalyst be the one kind in ammoniacal liquor, sodium carbonate.
Above-mentioned steps（C）Described in silane coupler be γ-glycidoxypropyltrime,hoxysilane, phenyl front three
One or more in TMOS, aminomethyl phenyl diethoxy silane, dimethoxydiphenylsilane.
Above-mentioned steps（D）Described in the second organic solvent be one or two in ethanol, toluene, chloroform；
Above-mentioned steps（D）Described in phosphate be tri aromatic ester of phosphic acid, trioctyl phosphate, diethyl phosphite, resorcinol four
One or more in phenyl biphosphonate, bisphenol A tetraphenyl diphosphate etc..
Beneficial effects of the present invention are as follows：
Aluminium pigment surface prepared by the inventive method carries out the fire-retardant modification of phosphorus silicon systems, improves what aluminium pigment was used in plastic resin
Security；Aluminium pigment prepared by the method not only can form the silica diaphragm of obstruct air on its surface, prevent in burning
During the explosive harm of aluminium powder, while under the cooperative flame retardant effect of phosphorus silicon, playing good to the fire-retardant of macromolecular material
Effect, and prepared material remains to keep the aesthetic effect of aluminium pigment；The preparation method rational technology, it is easy to operate, be easy to
Industrialization, it is compatible between the aluminium pigment energy for being coated and resin body, the toughness and impact of resin are improved, it is a kind of environment-friendly
Fire retardant.
Specific embodiment
After now specific embodiment of the invention is described in.
Embodiment 1
A kind of to mould the preparation method for using flame retardant type aluminium pigment, the method is comprised the following steps：
A. 12g aluminum pastes are weighed, aluminum paste are placed in the ethyl acetate organic solvent of 50g, carry out ultrasonic disperse 30 minutes,
The aluminum paste is particle diameter silver dollar matrix shape metallic, and particle diameter is 13 μm；
B. by it is above-mentioned ultrasound after slurries mechanical agitation is carried out under the conditions of 40 DEG C 6 hours, control mixing speed be 180 turns/
Min, then suction filtration, obtains filter cake, by filter cake under the conditions of 100 DEG C vacuum drying；
C. the first organic solvent ethanol of 100g is weighed, by the aluminium powder after above-mentioned drying and the first organic solvent ethanol of 100g
Mixing, then under nitrogen protection, to catalyst ammonia water is added in above-mentioned mixed solvent solution, adjusts the pH value of solvent mixed solution
It is 8, then instills the phenyltrimethoxysila,e mixed solution of the γ of 2g-glycidoxypropyltrime,hoxysilane 1g and 2g,
Then above-mentioned compound is carried out into mechanical agitation 2 hours, reaction temperature is 40 DEG C, speed of agitator is 250 turns/min, is stirred laggard
Row suction filtration；
D. second organic solvents, chloroform of 100g is weighed, the aluminium powder after above-mentioned suction filtration is mixed with the chloroform solvent of 100g, then
Under nitrogen protective condition, then to drip the triphenyl phosphate that speed instills 1g for the speed of 1d/s, mechanical agitation 4h is then proceeded by,
Speed of agitator is 180 turns/min, and reaction temperature is controlled at 75 DEG C, and suction filtration is carried out after reaction, and filter cake is obtained after suction filtration, then will filter
Cake is placed in vacuum drying in 60 DEG C of baking ovens, that is, obtain modeling flame retardant type aluminium pigment.
Sample manufactured in the present embodiment, initial degradation temperature is 220 DEG C, when temperature is reached after 700 DEG C, System forming
The carbon-coating of stabilization, Si-O-Si keys play fine and close cladding, better heat stability on aluminium powder surface.
Embodiment 2
A. 12g aluminum pastes are weighed, aluminum paste are placed in the ethyl acetate organic solvent of 50g, carry out ultrasonic disperse 30 minutes,
The aluminum paste is particle diameter silver dollar matrix shape metallic, and particle diameter is 13 μm；
B. by it is above-mentioned ultrasound after slurries mechanical agitation is carried out under the conditions of 40 DEG C 6 hours, control mixing speed be 180 turns/
Min, then suction filtration, obtains filter cake, by filter cake under the conditions of 100 DEG C vacuum drying；
C. the first organic solvent ethanol and 50g toluene organic solvents of 50g are weighed, by the aluminium powder after above-mentioned drying and the second of 50g
Alcohol and 50g toluene solvants mix, and then under nitrogen protection, to catalyst ammonia water is added in above-mentioned mixed solvent solution, adjust molten
The pH value of agent mixed solution is 8, then aminomethyl phenyl diethoxy silane, the dimethoxydiphenylsilane of 1g, the 1g for instilling 1g
γ-glycidoxypropyltrime,hoxysilane mixed solution, above-mentioned compound is then carried out into mechanical agitation 3 hours, instead
It is 40 DEG C to answer temperature, and speed of agitator is 250 turns/min, and suction filtration is carried out after stirring；
D. second organic solvents, chloroform of 100g is weighed, the aluminium powder after above-mentioned suction filtration is mixed with the toluene organic solvent of 100g,
Then it is under nitrogen protective condition then double for the speed of 1d/s instills 0.5g resorcinols tetraphenyl diphosphate, 0.5g to drip speed
Phenol A tetraphenyl diphosphates, then proceed by mechanical agitation 5h, and speed of agitator is 250 turns/min, and reaction temperature is controlled 60
DEG C, suction filtration is carried out after reaction, filter cake is obtained after suction filtration, filter cake is then placed in vacuum drying in 60 DEG C of baking ovens, that is, obtain modeling and use
Flame retardant type aluminium pigment.
The aluminium powder that modeling flame retardant type aluminium pigment prepared by the present invention is finally coated, organic principle accounts for 10~20%, the pigment
It is widely used in the resins such as polythene PE, polypropylene PP, polyvinylchloride, polystyrene PS, ABS and polycarbonate,
Its injecting products be applied to be related to automobile rub match somebody with somebody, household electrical appliance, electronic apparatus, hardware electrician, decorative building material, toy, commodity
Deng field.
The invention is not limited in above-mentioned implementation method, using raw material same as the previously described embodiments or similar and preparation side
All changes, equivalents and improved preparation method within context of the method fire heap described in it, in guarantor of the invention
Within the scope of shield.
Claims (8)
1. it is a kind of to mould with the preparation method of flame retardant type aluminium pigment, it is characterised in that the method is comprised the following steps：
A. 10~100g aluminum pastes are weighed, is by weight 1 by aluminum paste and organic solvent:It is placed in after 3~6 ratio mixing
In container, ultrasonic disperse is carried out 30~60 minutes；
B. the slurries after above-mentioned ultrasound are carried out into water-bath under the conditions of 30~40 DEG C, mechanical agitation 4~8 hours, is 160 with rotating speed
~400 turns/min, then suction filtration, obtains filter cake, by vacuum drying under the conditions of filter cake in an oven 100~120 DEG C；
C. a certain amount of first organic solvent is weighed, is according to weight ratio with the first organic solvent by the aluminium powder after above-mentioned drying
1：The ratio mixing of (5~15), then, under nitrogen protection, to catalyst is added in above-mentioned solvent mixed solution, is adjusted molten
The pH value of agent mixed solution is 8~10；Add silane coupler, the addition of coupling agent be the first organic solvent 0.5%~
5%；Then above-mentioned compound is carried out into mechanical agitation 2~6 hours, reaction temperature is 40~60 DEG C, speed of agitator is 160~400
Turn/min, suction filtration is carried out after stirring；
D. a certain amount of second organic solvent is weighed, is according to weight ratio with the second organic solvent by the aluminium powder after above-mentioned suction filtration
1：The ratio mixing of (5~15), then, under nitrogen protective condition, to adding phosphate, phosphorus in above-mentioned solvent mixed solution
The addition of acid esters is the 0.125%~2.5% of the second organic solvent, then proceeds by 4~8h of mechanical agitation, and speed of agitator is
160~400 turns/min, reaction temperature is controlled at 50~90 DEG C, and suction filtration is carried out after stirring, and filter cake is obtained after suction filtration, then will filter
Cake is placed in vacuum drying in 60 DEG C of baking ovens, obtains modeling flame retardant type aluminium pigment.
2. the preparation method of flame retardant type aluminium pigment of a kind of modeling according to claim l, it is characterised in that：Above-mentioned steps
（A）Described in organic solvent be one or two in ethyl acetate, n-butyl acetate, tetrahydrofuran, toluene.
3. the preparation method of flame retardant type aluminium pigment of a kind of modeling according to claim l, it is characterised in that：Above-mentioned steps
（A）Described in aluminum paste be silver dollar type or corn type, particle diameter be 8~100 μm.
4. the preparation method of flame retardant type aluminium pigment of a kind of modeling according to claim l, it is characterised in that：Above-mentioned steps
（C）Described in the first organic solvent be one or two in methyl alcohol, ethanol, acetone.
5. the preparation method of flame retardant type aluminium pigment of a kind of modeling according to claim l, it is characterised in that：Above-mentioned steps
（C）Described in catalyst be the one kind in ammoniacal liquor, sodium carbonate.
6. the preparation method of flame retardant type aluminium pigment of a kind of modeling according to claim l, it is characterised in that：Above-mentioned steps
（C）Described in silane coupler be γ-glycidoxypropyltrime,hoxysilane, phenyltrimethoxysila,e, methylbenzene
One or more in base diethoxy silane, dimethoxydiphenylsilane.
7. the preparation method of flame retardant type aluminium pigment of a kind of modeling according to claim l, it is characterised in that：Above-mentioned steps
（D）Described in the second organic solvent be one or two in ethanol, toluene, chloroform.
8. the preparation method of flame retardant type aluminium pigment of a kind of modeling according to claim l, it is characterised in that：Above-mentioned steps
（D）Described in phosphate for tri aromatic ester of phosphic acid, trioctyl phosphate, diethyl phosphite, resorcinol tetraphenyl diphosphate,
One or more in bisphenol A tetraphenyl diphosphate etc..
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710077395.9A CN106883457A (en) | 2017-02-14 | 2017-02-14 | It is a kind of to mould with the preparation method of flame retardant type aluminium pigment |
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| CN201710077395.9A CN106883457A (en) | 2017-02-14 | 2017-02-14 | It is a kind of to mould with the preparation method of flame retardant type aluminium pigment |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112480720A (en) * | 2020-11-26 | 2021-03-12 | 上海颜钛实业有限公司 | Preparation method of aluminum paste pigment and product prepared by preparation method |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101089122A (en) * | 2007-06-15 | 2007-12-19 | 杭州海虹精细化工有限公司 | Surface modified aluminium hydroxide fire retardant and its prepn process |
| US20140227827A1 (en) * | 2013-02-08 | 2014-08-14 | Richard Bellemare | Methods for metallizing an aluminum paste |
| CN104341803A (en) * | 2014-10-25 | 2015-02-11 | 合肥旭阳铝颜料有限公司 | High-temperature-resistant aluminum pigment and preparation method thereof |
| CN104341801A (en) * | 2014-09-29 | 2015-02-11 | 合肥旭阳铝颜料有限公司 | Fireproof aluminum pigment and preparation method thereof |
-
2017
- 2017-02-14 CN CN201710077395.9A patent/CN106883457A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101089122A (en) * | 2007-06-15 | 2007-12-19 | 杭州海虹精细化工有限公司 | Surface modified aluminium hydroxide fire retardant and its prepn process |
| US20140227827A1 (en) * | 2013-02-08 | 2014-08-14 | Richard Bellemare | Methods for metallizing an aluminum paste |
| CN104341801A (en) * | 2014-09-29 | 2015-02-11 | 合肥旭阳铝颜料有限公司 | Fireproof aluminum pigment and preparation method thereof |
| CN104341803A (en) * | 2014-10-25 | 2015-02-11 | 合肥旭阳铝颜料有限公司 | High-temperature-resistant aluminum pigment and preparation method thereof |
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| 冯亚青 等: "《高等学校教学用书 助剂化学及工艺学》", 30 June 1997 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112480720A (en) * | 2020-11-26 | 2021-03-12 | 上海颜钛实业有限公司 | Preparation method of aluminum paste pigment and product prepared by preparation method |
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