CN102604430B - Aluminic ester modified antimony trioxide and preparation method thereof - Google Patents
Aluminic ester modified antimony trioxide and preparation method thereof Download PDFInfo
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- CN102604430B CN102604430B CN201210013803.1A CN201210013803A CN102604430B CN 102604430 B CN102604430 B CN 102604430B CN 201210013803 A CN201210013803 A CN 201210013803A CN 102604430 B CN102604430 B CN 102604430B
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- antimony trioxide
- coupling agent
- antimonous oxide
- modification
- aluminic
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Abstract
The invention discloses an aluminic ester modified antimony trioxide, which takes antimony trioxide and an aluminic ester coupling agent as raw materials. The preparation method comprises the following steps that: antimony trioxide with a particle size of 1 to 5 mum is flatly paved at a thickness of 1 to 20 mm, and is pre-treated for 1 to 5 minutes in a microwave field with a microwave intensity of 5 to 50kW per square meter; and the pre-treated 100 parts of antimony trioxide and 0.5 to 3 parts of aluminic ester coupling agent are mixed, are modified for 10 to 30 minutes at a temperature of 110 to 130 DEG C and a stirring speed of 800 to 1500 r/min, and are cooled to obtain the aluminic ester modified antimony trioxide with a contact angle of greater than 140 degrees. The modified antimony trioxide is used for plastic flame retardant modification, the tensile strength and the breaking elongation are 10% higher than those of the unmodified antimony trioxide, and the vertical flammability level achieves the highest level. Since the cheap aluminic ester coupling agent and a dry modification method are used, the cost is low, the safety is good, and the pollution is free.
Description
Technical field
The present invention relates to a kind of fire retarding synergist and preparation method thereof, particularly Aluminate modification antimonous oxide and preparation method thereof.
Background technology
Antimonous oxide is applied in flame-retardant polymer mainly as fire retarding synergist, it is the fire retarding synergist of halogen flame excellence, although itself there is no flame retardant properties, at superpolymer, (do not comprise the superpolymer that self contains halogen, as clorafin, polyvinyl chloride etc.) in singly add antimonous oxide flame retardant properties without obvious change, but with the composite use of other fire retardants, can play and help flame retardant effect, especially with the composite use of bromide fire retardant, can make the flame retardant properties of brominated flame-retardant (as decabromodiphenyl oxide) improve more than 30%.Therefore, antimonous oxide is widely used aspect fire-retardant at general-purpose plastics, engineering plastics, thermoplastic elastomer, epoxy resin, unsaturated polyester and textiles etc. as fire retarding synergist.
Antimonous oxide powder surface is wetting ability, if directly mix fabricated product in high molecule plastic, thereby because dispersion effect is bad, cause the mechanical property of goods to decline, flame retardant effect does not reach requirement yet, can not embody the specific function of antimonous oxide powder material.For improving antimonous oxide and organic macromolecule consistency and dispersiveness, must carry out antimonous oxide powder surface organically-modifiedly, powder surface characteristic is changed, meet the application requiring of various performances.At present, the method for organic modification of surface of antimonous oxide is wet method, for the modification coupling agent of surface modification, has silane, titanic acid ester etc.As < < fire retardant material and technology > > (the 5th phase 7-10 page in 1996) have delivered the surface modification technology research of retardant synergist ANTIMONY TRIOXIDE SB 203 99.8 PCT, in xylene solvent, use respectively by silane, titanic acid ester and stearic acid modified dose and carry out Sb
2o
3wet-process modified, use titanic acid ester and organosilane-modified effect all better; < < additives for plastics > > (the 5th phase 46-48 page in 2008) has reported coupling agent surface modification Sb
2o
3research, in solvent normal heptane, 1% titanate coupling agent and Sb
2o
3at 60 ℃ wet-process modified 30 minutes, then drying and obtaining contact angle was the modified product of 142 °.Although large through wet-process modified antimonous oxide contact angle, its properties-correcting agent is expensive, and uses a large amount of organic solvents in modifying process, and environment is caused to potential threat, promotes the use of thereby affected it.
Summary of the invention
The object of the invention is, antimonous oxide fire retarding synergist that a kind of fire-retardant synergistic is effective, production cost is low and preparation method thereof is provided, particularly adopt aluminate coupling agent surface modification antimonous oxide and preparation method thereof.
Antimonous oxide fire retarding synergist of the present invention is that to take antimonous oxide and aluminate coupling agent be raw material, and aluminate coupling agent directly mixes with antimonous oxide particle, and concrete technology is as follows:
(1) pre-treatment of antimonous oxide: the antimonous oxide that is 1～5 μ m by particle diameter is paved, thickness is 1～20mm, at microwave intensity, is 5～50kW/m
2microwave field in radiation 1～5 minute;
(2) dry method modification: 100 parts of antimonous oxides and 0.5～3 part of aluminate coupling agent that pre-treatment is good mix, in temperature, be that 110～130 ℃, stirring velocity are 800～1500 revs/min of lower modifications 10～30 minutes, coolingly obtain the Aluminate modification antimonous oxide that contact angle is greater than 140 °.
The aluminate coupling agent that antimonous oxide fire retarding synergist of the present invention adopts, its general molecular formula is: (C
3h
7o)
xal (OCOR
1)
m(OCOR
2)
n(OAB)
y, x+m+n=3 wherein, y=0～2; R is long-chain hydrocarbon, and carbon atom number is generally between 14～22; A, B are hydrocarbon short chain, and carbon atom number is between 6～8.
Modification antimonous oxide fire retarding synergist of the present invention is for plastic flame modification, and its tensile strength and elongation at break are all high more than 10% than the antimonous oxide that there is no modification, and it is highest that vertical combustion grade reaches.
The modification antimonous oxide fire retarding synergist that the present invention prepares, is used aluminate coupling agent lower by 40～70% than silane and titanate coupling agent price.
The modification antimonous oxide fire retarding synergist that the present invention prepares, adopt dry method modification, without solvent, although adopted Microwave Pretreatment, because the Microwave Pretreatment time is short, and energy preheating material, compare with the wet method of a large amount of organic solvents of use, not only cost is low, and security is good, pollution-free.
Embodiment
Embodiment 1
The antimonous oxide that is 2 μ m by particle diameter is paved, and thickness is 5mm, at microwave intensity, is 25kW/m
2microwave field in radiation 3 minutes; Then good 100 parts of antimonous oxides and the 1.5 parts of aluminate coupling agents of pre-treatment being mixed, is that 120 ℃, stirring velocity are 1100 revs/min of lower modifications 20 minutes in temperature, coolingly obtains the Aluminate modification antimonous oxide that contact angle is greater than 142 °.
Embodiment 2
The antimonous oxide that is 3 μ m by particle diameter is paved, and thickness is 10mm, at microwave intensity, is 35kW/m
2microwave field in radiation 3 minutes; Then good 100 parts of antimonous oxides and the 2.5 parts of aluminate coupling agents of pre-treatment being mixed, is that 130 ℃, stirring velocity are 1300 revs/min of lower modifications 25 minutes in temperature, coolingly obtains the Aluminate modification antimonous oxide that contact angle is greater than 144 °.
Claims (1)
1. a preparation method for aluminate coupling agent modification antimonous oxide, is characterized in that the modification of antimonous oxide be take aluminate coupling agent as raw material, and aluminate coupling agent directly mixes with antimonous oxide particle, and specific implementation Step By Condition is as follows:
(1) pre-treatment of antimonous oxide: the antimonous oxide that is 1～5 μ m by particle diameter is paved, thickness is 1～20mm, at microwave intensity, is 5～50kW/m
2microwave field in radiation 1～5 minute;
(2) dry method modification: 100 parts of antimonous oxides and 0.5～3 part of aluminate coupling agent that pre-treatment is good mix, in temperature, be that 110～130 ℃, stirring velocity are 800～1500 revs/min of lower modifications 10～30 minutes, the cooling Aluminate modification antimonous oxide that obtains.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201210013803.1A CN102604430B (en) | 2012-01-17 | 2012-01-17 | Aluminic ester modified antimony trioxide and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210013803.1A CN102604430B (en) | 2012-01-17 | 2012-01-17 | Aluminic ester modified antimony trioxide and preparation method thereof |
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| Publication Number | Publication Date |
|---|---|
| CN102604430A CN102604430A (en) | 2012-07-25 |
| CN102604430B true CN102604430B (en) | 2014-04-02 |
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Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103224716B (en) * | 2013-05-09 | 2015-06-10 | 芜湖华烨新材料有限公司 | Titanate modified antimony trioxide and preparation method thereof |
| CN106810721A (en) * | 2016-12-20 | 2017-06-09 | 广西华锑科技有限公司 | A kind of surface modifying method of the special antimony oxide of nylon plastic(s) |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102015913A (en) * | 2008-04-25 | 2011-04-13 | 3M创新有限公司 | Process for the surface modification of particles |
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| WO2008068154A2 (en) * | 2006-12-06 | 2008-06-12 | Ciba Holding Inc. | Changing surface properties by functionalized nanoparticles |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102015913A (en) * | 2008-04-25 | 2011-04-13 | 3M创新有限公司 | Process for the surface modification of particles |
Non-Patent Citations (1)
| Title |
|---|
| 王泽霖.玻璃钢原材料及选用.《玻璃钢原材料及选用》.化学工业出版社,2009,第343页. * |
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