CN107201019A - A kind of preparation method of oligomer flame-retardant polycarbonate material - Google Patents
A kind of preparation method of oligomer flame-retardant polycarbonate material Download PDFInfo
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- CN107201019A CN107201019A CN201710609122.4A CN201710609122A CN107201019A CN 107201019 A CN107201019 A CN 107201019A CN 201710609122 A CN201710609122 A CN 201710609122A CN 107201019 A CN107201019 A CN 107201019A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L69/00—Compositions of polycarbonates; Compositions of derivatives of polycarbonates
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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
- C08K3/32—Phosphorus-containing compounds
- C08K2003/321—Phosphates
- C08K2003/322—Ammonium phosphate
- C08K2003/323—Ammonium polyphosphate
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
Abstract
The invention discloses a kind of preparation method of oligomer flame-retardant polycarbonate material, APP, antimony oxide are mixed and are distributed in oligomer by the present invention, effectively raise dispersiveness of the inorganic fire-retarded auxiliary agent between polymer, the stability_intensity of finished product is improved, the fire retardant performance of finished product is improved.
Description
Technical field
The invention belongs to Material Field, and in particular to a kind of preparation method of oligomer flame-retardant polycarbonate material.
Background technology
Makrolon is the high molecular polymer containing carbonate group in strand, can be divided into fat according to the structure of ester group
The polytypes such as race, aromatic series, aliphatic-aromatic.Wherein due to aliphatic and the machinery of aliphatic-aromatic makrolon
Performance is relatively low, so as to limit its application in terms of engineering plastics.Only aromatic copolycarbonate is industrialized at present
Production.Due to the particularity on polycarbonate structure, as the most fast general engineering of growth rate in five large-engineering plastics
Plastics；
Its current growth momentum is very swift and violent, just promptly extends and is dissolved into Technological Problems In Computer Manufacturing, Aero-Space, blue light etc.
In terms of industrial industrialization, it is related to many high-technology fields, additionally since the particularity of its performance, in the common of other resins
Under effect, to carrying out the mode with blending, copolymer or alloy type product are formed, makes its performance more perfect, the product of gained
Performance is very excellent, and the environment of a variety of specific application areas can be adapted to completely, simultaneously for manufacturing cost, properties will
Ask is also to comply fully with standard.Contain phenyl ring on configuration aspects, the main chain of makrolon, in its combustion reaction, can carry out
Be condensed into aroma type charcoal material, it is higher with respect to charring rate, and can self-extinguishment, the standard that its flame retardant rating can reach, relatively
In common thermoplastic polymers, although its anti-flammability relative ideal under contrast, it is still in flammable category, and poly- carbon
Acid esters material in combustion, can be melted and hot melt outflow of dripping, it is more likely that cause the material combustion on periphery, neighbouring material
After material is ignited, cause the generation of fire, for this point, at present in above-mentioned application field, still it is difficult to reach ideal
Fire-retardant fireproof standard；
Therefore apply central in production and to the true extension of material, it is necessary to combustion phenomena and property for material
Matter, flame retardant treatment is carried out to it.But the poor compatibility of traditional inorganic combustion inhibitor and polyester matrix, it is easily reduced the stabilization of finished product
Property.
The content of the invention
In view of the defects and deficiencies of the prior art, the present invention intends to provide a kind of oligomer fire-retardant polycarbonate material
The preparation method of material.
To achieve the above object, the present invention uses following technical scheme：
A kind of preparation method of oligomer flame-retardant polycarbonate material, comprises the following steps：
(1) polyoxyethylene sorbitan monoleate of 1-2 parts by weight is taken, in the deionized water for being added to 16-20 times of its weight, is stirred；
(2) methyl benzoic acid, the antimony oxide mixing of 1-2 parts by weight of 6-8 parts by weight are taken, is incubated at 50-60 DEG C
Stirring 10-20 minutes, adds the perfluoroalkyl ethyl alcohol of 4-6 parts by weight, and rise temperature is 80-90 DEG C, 30-40 points of insulated and stirred
Clock, is added in the aqueous solution of polyoxyethylene sorbitan monoleate, ultrasonic 1-2 minutes, obtains esterification dispersion liquid；
(3) APP of 1-3 parts by weight is taken, in the deionized water for being added to 17-20 times of its weight, is stirred, with
Temperature is raised after above-mentioned esterification dispersion liquid mixing, formalin that 10-17 parts by weight are added dropwise, that concentration is 10-13%, completion of dropping
Spend for 60-70 DEG C, insulated and stirred 30-40 minutes obtains flame-retardant modified esterification dispersion liquid；
(4) above-mentioned flame-retardant modified esterification dispersion liquid is added in reactor, mixed with the Methyl stannum mercaptide of 0.8-1 parts by weight
Close, in the tetrahydrofuran for being added to compound weight 60-70%, regulation temperature of reaction kettle is 80-85 DEG C, and insulated and stirred 1-2 is small
When, discharging is distilled off drying 30-40 minutes at tetrahydrofuran, 90-100 DEG C of vacuum, obtains fire-retardant oligomer；
(5) above-mentioned fire-retardant oligomer, the makrolon of 100-110 parts by weight, the silane coupler of 2-3 parts by weight are taken
Kh570 is mixed, and in the absolute ethyl alcohol for being added to 1.7-2 times of compound weight, insulated and stirred 20-30 minutes at 60-70 DEG C, is gone out
Precipitation is washed in material, filtering, and air drying obtains oligomer flame-retardant polycarbonate material.
Advantages of the present invention：
The present invention using methyl benzoic acid, perfluoroalkyl ethyl alcohol as raw material, obtain esterification dispersion liquid, then by formaldehyde at
Reason, using Methyl stannum mercaptide as condensing agent, mixes with APP, flame-retardant modified esterification dispersion liquid is obtained, then with makrolon
Mixing, obtains composite；
APP, antimony oxide are mixed and are distributed in oligomer by the present invention, effectively raise inorganic fire-retarded help
Dispersiveness of the agent between polymer, improves the stability_intensity of finished product, improves the fire retardant performance of finished product.
Embodiment
Embodiment 1
A kind of preparation method of oligomer flame-retardant polycarbonate material, comprises the following steps：
(1) polyoxyethylene sorbitan monoleate of 1 parts by weight is taken, in the deionized water for being added to 20 times of its weight, is stirred；
(2) methyl benzoic acid, the antimony oxide mixing of 2 parts by weight, 20 points of insulated and stirred at 60 DEG C of 6 parts by weight are taken
Clock, adds the perfluoroalkyl ethyl alcohol of 6 parts by weight, rise temperature is 90 DEG C, and insulated and stirred 40 minutes is added to polyoxyethylene sorbitan monoleate
The aqueous solution in, ultrasound 2 minutes, obtain esterification dispersion liquid；
(3) APP of 1-3 parts by weight is taken, in the deionized water for being added to 20 times of its weight, is stirred, it is and above-mentioned
It is 70 DEG C to be esterified rise temperature after dispersion liquid mixing, 17 parts by weight of dropwise addition, the formalin that concentration is 13%, completion of dropping,
Insulated and stirred 40 minutes, obtains flame-retardant modified esterification dispersion liquid；
(4) above-mentioned flame-retardant modified esterification dispersion liquid is added in reactor, mixed with the Methyl stannum mercaptide of 0.8 parts by weight
Close, in the tetrahydrofuran for being added to compound weight 70%, regulation temperature of reaction kettle is 85 DEG C, insulated and stirred 2 hours, discharging,
It is distilled off drying 30 minutes at tetrahydrofuran, 90 DEG C of vacuum, obtains fire-retardant oligomer；
(5) above-mentioned fire-retardant oligomer, the makrolon of 100 parts by weight, the silane coupler Kh570 mixing of 2 parts by weight are taken,
In the absolute ethyl alcohol for being added to 1.7 times of compound weight, insulated and stirred 30 minutes at 70 DEG C discharge, and filtering will precipitate water
Wash, air drying, obtain oligomer flame-retardant polycarbonate material.
Embodiment 2
A kind of preparation method of oligomer flame-retardant polycarbonate material, comprises the following steps：
(1) polyoxyethylene sorbitan monoleate of 1 parts by weight is taken, in the deionized water for being added to 16 times of its weight, is stirred；
(2) methyl benzoic acid, the antimony oxide mixing of 1 parts by weight, 10 points of insulated and stirred at 50 DEG C of 6 parts by weight are taken
Clock, adds the perfluoroalkyl ethyl alcohol of 4 parts by weight, rise temperature is 80 DEG C, and insulated and stirred 30 minutes is added to polyoxyethylene sorbitan monoleate
The aqueous solution in, ultrasound 1 minute, obtain esterification dispersion liquid；
(3) APP of 1-3 parts by weight is taken, in the deionized water for being added to 17 times of its weight, is stirred, it is and above-mentioned
It is 60 DEG C to be esterified rise temperature after dispersion liquid mixing, 10 parts by weight of dropwise addition, the formalin that concentration is 10%, completion of dropping,
Insulated and stirred 30 minutes, obtains flame-retardant modified esterification dispersion liquid；
(4) above-mentioned flame-retardant modified esterification dispersion liquid is added in reactor, mixed with the Methyl stannum mercaptide of 0.8 parts by weight
Close, in the tetrahydrofuran for being added to compound weight 60%, regulation temperature of reaction kettle is 80 DEG C, insulated and stirred 1 hour, discharging,
It is distilled off drying 30 minutes at tetrahydrofuran, 90 DEG C of vacuum, obtains fire-retardant oligomer；
(5) above-mentioned fire-retardant oligomer, the makrolon of 100 parts by weight, the silane coupler Kh570 mixing of 2 parts by weight are taken,
In the absolute ethyl alcohol for being added to 2 times of compound weight, insulated and stirred 20 minutes at 60 DEG C are discharged, and precipitation is washed in filtering,
Air drying, obtains oligomer flame-retardant polycarbonate material.
Performance test：
The performance test knot for the oligomer flame-retardant polycarbonate material that the 1-2 methods according to embodiments of the present invention of table 1 are prepared
Really
Claims (1)
1. a kind of preparation method of oligomer flame-retardant polycarbonate material, it is characterised in that comprise the following steps：
(1) polyoxyethylene sorbitan monoleate of 1-2 parts by weight is taken, in the deionized water for being added to 16-20 times of its weight, is stirred；
(2) methyl benzoic acid, the antimony oxide mixing of 1-2 parts by weight, the insulated and stirred at 50-60 DEG C of 6-8 parts by weight are taken
10-20 minutes, the perfluoroalkyl ethyl alcohol of 4-6 parts by weight is added, rise temperature is 80-90 DEG C, insulated and stirred 30-40 minutes,
It is added in the aqueous solution of polyoxyethylene sorbitan monoleate, it is ultrasonic 1-2 minutes, obtain esterification dispersion liquid；
(3) APP of 1-3 parts by weight is taken, in the deionized water for being added to 17-20 times of its weight, is stirred, it is and above-mentioned
Being esterified rise temperature after dispersion liquid mixing, dropwise addition 10-17 parts by weight, the formalin that concentration is 10-13%, completion of dropping is
60-70 DEG C, insulated and stirred 30-40 minutes obtains flame-retardant modified esterification dispersion liquid；
(4) above-mentioned flame-retardant modified esterification dispersion liquid is added in reactor, mixed with the Methyl stannum mercaptide of 0.8-1 parts by weight,
In the tetrahydrofuran for being added to compound weight 60-70%, regulation temperature of reaction kettle is 80-85 DEG C, insulated and stirred 1-2 hours,
Discharging, is distilled off drying 30-40 minutes at tetrahydrofuran, 90-100 DEG C of vacuum, obtains fire-retardant oligomer；
(5) the silane coupler Kh570 of above-mentioned fire-retardant oligomer, the makrolon of 100-110 parts by weight, 2-3 parts by weight is taken to mix
Close, in the absolute ethyl alcohol for being added to 1.7-2 times of compound weight, insulated and stirred 20-30 minutes at 60-70 DEG C, discharging, mistake
Filter, precipitation is washed, and air drying obtains oligomer flame-retardant polycarbonate material.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710609122.4A CN107201019A (en) | 2017-07-24 | 2017-07-24 | A kind of preparation method of oligomer flame-retardant polycarbonate material |
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| CN201710609122.4A CN107201019A (en) | 2017-07-24 | 2017-07-24 | A kind of preparation method of oligomer flame-retardant polycarbonate material |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108659345A (en) * | 2018-06-05 | 2018-10-16 | 安徽艾伊德动力科技有限公司 | A kind of pdu harness fireproof material and preparation method thereof |
| CN109777069A (en) * | 2018-12-28 | 2019-05-21 | 方万漂 | A kind of flame-retardant polycarbonate material and preparation method thereof |
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| CN104479323A (en) * | 2014-12-08 | 2015-04-01 | 苏州新区佳合塑胶有限公司 | Flame-retardant plastic for electronic product casing |
| CN105086806A (en) * | 2015-08-10 | 2015-11-25 | 安徽锦洋氟化学有限公司 | Organic fluorine modified polyurethane stain and water resisting coating |
| CN106633753A (en) * | 2016-09-29 | 2017-05-10 | 青岛海之源智能技术有限公司 | Flame-retarding polycarbonate plastics and preparation method thereof |
| CN106867221A (en) * | 2017-01-20 | 2017-06-20 | 广东优科艾迪高分子材料有限公司 | A kind of flame retardant type polycarbonate compositions |
| CN106947164A (en) * | 2017-05-12 | 2017-07-14 | 安徽机电职业技术学院 | A kind of preparation method of organic phosphatization flame retardant automotive anti-friction material |
-
2017
- 2017-07-24 CN CN201710609122.4A patent/CN107201019A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104479323A (en) * | 2014-12-08 | 2015-04-01 | 苏州新区佳合塑胶有限公司 | Flame-retardant plastic for electronic product casing |
| CN105086806A (en) * | 2015-08-10 | 2015-11-25 | 安徽锦洋氟化学有限公司 | Organic fluorine modified polyurethane stain and water resisting coating |
| CN106633753A (en) * | 2016-09-29 | 2017-05-10 | 青岛海之源智能技术有限公司 | Flame-retarding polycarbonate plastics and preparation method thereof |
| CN106867221A (en) * | 2017-01-20 | 2017-06-20 | 广东优科艾迪高分子材料有限公司 | A kind of flame retardant type polycarbonate compositions |
| CN106947164A (en) * | 2017-05-12 | 2017-07-14 | 安徽机电职业技术学院 | A kind of preparation method of organic phosphatization flame retardant automotive anti-friction material |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108659345A (en) * | 2018-06-05 | 2018-10-16 | 安徽艾伊德动力科技有限公司 | A kind of pdu harness fireproof material and preparation method thereof |
| CN109777069A (en) * | 2018-12-28 | 2019-05-21 | 方万漂 | A kind of flame-retardant polycarbonate material and preparation method thereof |
| CN109777069B (en) * | 2018-12-28 | 2021-04-20 | 方万漂 | Flame-retardant polycarbonate material and preparation method thereof |
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Application publication date: 20170926 |
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