CN109735157B - Silicon-nitrogen-phosphorus efficient halogen-free flame retardant for fireproof flame-retardant coating, and preparation method and application thereof - Google Patents
Silicon-nitrogen-phosphorus efficient halogen-free flame retardant for fireproof flame-retardant coating, and preparation method and application thereof Download PDFInfo
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Abstract
The invention relates to a silicon-nitrogen-phosphorus efficient halogen-free flame retardant and a preparation method and application thereof. The invention also discloses a fire retardant for the fire-retardant coating and a preparation method thereof. Epoxy siloxane, triglycidyl isocyanurate and aminoimidazole are added into a reaction vessel and mixed uniformly; and slowly dropwise adding phosphoric acid, heating to 60-70 ℃, and reacting for 3-5 h to obtain the silicon-nitrogen-phosphorus efficient halogen-free flame retardant. And then the self-made flame retardant is applied to the preparation of the fireproof coating. The structure of the high-efficiency flame retardant design molecule integrates an acid source, a carbon source and a gas source, and can promote carbon formation during combustion to form a compact silicon-carbon layer, so that a high polymer material is prevented from generating secondary combustion due to melting and dripping during combustion, and better flame retardant property is provided for the high polymer material; the water resistance and the weather resistance of the coating are not influenced; high flame-retardant efficiency can be formed during combustion, and no halogen is contained, so that the environment is not polluted.
Description
Technical Field
The invention relates to a silicon-nitrogen-phosphorus efficient halogen-free flame retardant for a fireproof flame-retardant coating, and a preparation method and application thereof, and belongs to the technical field of flame retardance of high polymer materials.
Background
The flame retardant is a substance for increasing the flame resistance of a high polymer material and is divided into an additive flame retardant and a reactive flame retardant according to the using method. The additive-type flame retardant mainly comprises a halogen-based flame retardant and a halogen-free flame retardant. In practical application, the halogen flame retardant decomposes to generate hydrogen halide during combustion to eliminate active free radicals generated by the combustion reaction of high polymer materials, has the advantages of high flame retardant efficiency, small using amount, proper price and the like, but has the defects of generating dense smoke, toxic and corrosive gases during combustion, so that the research and development of halogen-free flame retardants, such as phosphorus-series, nitrogen-series, silicon-series and other halogen-free flame retardants are promoted.
Most of the traditional halogen-free flame retardants have the defects of low flame retardant efficiency, large addition amount, low compatibility, degradation of mechanical properties of high polymer materials and the like. At present, the synergistic flame retardance of silicon, nitrogen and phosphorus elements is becoming the development direction of halogen-free flame retardants, such as nitrogen, phosphorus, silicon, phosphorus, nitrogen, silicon, phosphorus and the like, and a large amount of hydrogen chloride gas is inevitably generated in the reaction of silicon source in the preparation process and hydroxyl.
Disclosure of Invention
The purpose of the invention is as follows: the invention aims to solve the technical problem of providing a silicon-nitrogen-phosphorus efficient halogen-free flame retardant. The invention aims to provide a silicon-nitrogen-phosphorus efficient synergistic flame retardant for a water-based fireproof flame-retardant coating, which is prepared from alkoxy silane with an epoxy group, triglycidyl isocyanurate, aminoimidazole and a phosphoric acid oligomer, and has the advantages of high efficiency, no pollution discharge and simple operation. The invention organically combines silicon, nitrogen and phosphorus together, has easily obtained materials, can be applied to the fields of coating, plastics, rubber and the like, and achieves ideal flame retardant effect on the premise of not reducing the performance of high polymer materials and eliminating toxic smoke generated by halogen during combustion.
The invention also aims to solve the technical problem of providing a preparation method and application of the silicon-nitrogen-phosphorus efficient halogen-free flame retardant.
The invention finally aims to solve the technical problem of providing the fireproof flame-retardant coating and the preparation method thereof.
The technical scheme is as follows: in order to solve the technical problems, the invention adopts the technical scheme that: the silicon-nitrogen-phosphorus efficient halogen-free flame retardant is prepared by reacting alkoxy silane with epoxy groups, triglycidyl isocyanurate, aminoimidazole and a compound containing phosphoric acid groups; the mass ratio of the alkoxysilane with an epoxy group, the triglycidyl isocyanurate, the aminoimidazole and the compound containing a phosphoric acid group in the reaction is 1.5-6.2: 0.5-2.5: 0-1.0: 0.1-2.
Wherein the mass ratio of the alkoxy silane with the epoxy group, the triglycidyl isocyanurate, the aminoimidazole and the polyphosphoric acid in the reaction is 3: 2: 0.3: 1.5.
Wherein, the alkoxy silane with epoxy groups is one or more of epoxy siloxane monomer, epoxy siloxane oligomer, epoxy modified silicone resin oligomer, acrylic acid modified epoxy organosilicon and phenolic aldehyde modified epoxy organosilicon.
Wherein the compound containing the phosphoric acid group is one of phosphoric acid, polyphosphoric acid, phosphoric acid monoester or phosphoric acid diester.
Wherein, the epoxy siloxane monomer is KH560 (gamma-glycidoxypropyltrimethoxysilane).
The invention also comprises a preparation method of the silicon-nitrogen-phosphorus efficient halogen-free flame retardant, which comprises the following steps:
adding alkoxy silane with epoxy groups, triglycidyl isocyanurate and aminoimidazole into a reaction vessel, and uniformly stirring and mixing;
and step two, slowly dropwise adding a compound containing phosphoric acid groups, keeping the temperature below 40 ℃, and after dropwise adding, heating to 60-70 ℃ for reaction for 3-5 hours.
The invention also comprises the application of the silicon nitrogen phosphorus high-efficiency halogen-free flame retardant in the preparation of fireproof flame-retardant coating.
The invention also comprises a fireproof flame-retardant coating, which comprises the following raw materials in parts by weight: 35-65 parts of emulsion polymer, 15-65 parts of silicon-nitrogen-phosphorus efficient synergistic flame retardant, 3-8 parts of film-forming assistant, 0.1-0.5 part of wetting agent, 0.1-0.2 part of flatting agent, 0.2-0.5 part of thickening agent, 0.1-0.5 part of defoaming agent, 0.1-0.3 part of bactericide, 0.1-0.5 part of ammonia water and 5-10 parts of deionized water.
The film forming auxiliary agent, the wetting agent, the flatting agent, the defoaming agent, the bactericide and the thickener can comprise any corresponding auxiliary agent types on the market;
preferably, the film-forming aid is alcohol ester-12, the wetting agent is a U3010 aqueous wetting agent, the leveling agent is SN4710, the thickener is U605, the defoamer is 6028, and the bactericide is 6081.
The invention also comprises a preparation method of the fireproof flame-retardant coating, which comprises the following specific steps:
1) adding the emulsion polymer into a container, adding ammonia water and a small amount of water, and uniformly stirring at a low speed of about 100-200 r/min;
2) uniformly mixing the silicon-nitrogen-phosphorus efficient synergistic flame retardant, the film forming aid, the wetting agent, the flatting agent, the defoaming agent, the bactericide and the thickening agent, adding the mixture under stirring at 600-700 r/min, stirring for 15-25 min, filtering and packaging.
Has the advantages that: compared with the prior art, the invention has the following advantages:
1. the preparation of the silicon-nitrogen-phosphorus efficient halogen-free flame retardant adopts alkoxy silane containing epoxy groups, and is different from the traditional method of adopting chlorosilane, no hydrogen chloride gas is generated in the synthesis of the flame retardant, and enterprises realize emission-free production;
2. the high-efficiency halogen-free flame retardant contains three elements of silicon, phosphorus and nitrogen which can play a role in synergistic flame retardance, and can play a good role in synergistic flame retardance; the structure of the high-efficiency flame retardant design molecule integrates an acid source, a carbon source and a gas source, and can promote carbon formation during combustion to form a compact silicon-carbon layer, so that secondary combustion caused by melting and dripping of a high polymer material during combustion is prevented, and better flame retardant performance is provided for the high polymer material; the water resistance and the weather resistance of the coating are not influenced; high flame-retardant efficiency can be formed during combustion, and no halogen is contained, so that the environment is not polluted;
3. according to the invention, epoxy groups on nitrogen elements in the high-efficiency halogen-free flame retardant molecules are hydrolyzed to generate active hydroxyl groups, so that the crosslinking reaction with coating emulsion is facilitated, and the adsorption effect with a substrate is enhanced; the siloxane groups are hydrolyzed to form silicon hydroxyl groups during the molding of the high polymer material, and the silicon hydroxyl groups are condensed to realize self-crosslinking, so that the silicon can promote carbon formation during the combustion to form a compact silicon-carbon layer; the organic silicon and the phosphate ester have good hydrophobic property, the compatibility of the flame retardant and a polymer matrix is enhanced, the migration and precipitation phenomenon of the flame retardant is not easy to generate, and the polymer has lasting flame retardant property.
4. The fireproof coating has the advantages that: the paint prepared by the invention has the advantages of flame retardance, water resistance and moist heat resistance: in the aspect of flame resistance, the flame resistance time index is increased by 5 minutes, so that the time is saved for the escape of personnel on the fire scene; in the aspect of water resistance, the new flame retardant 144h does not peel off, and the traditional flame retardant foams for 72 h; the wet heat resistance is realized, the new flame retardant 144h does not peel off, and the traditional flame retardant foams for 96 h. The coating prepared by the invention has good flame retardance, water resistance and damp-heat resistance.
Detailed Description
The technical solution of the present invention will be described in detail with reference to examples.
In addition, the film-forming assistant is alcohol ester-12 of Islam chemical engineering Co., Ltd, the wetting agent is a U3010 aqueous wetting agent of Minghua of Wuhan sea, the leveling agent is SN4710 of Shanghai deep bamboo chemical engineering Co., Ltd, the thickening agent is U605 of Shanghai deep bamboo chemical engineering Co., Ltd, the defoaming agent is 6028 of Longhai chemical engineering, and the bactericide is Minghua 6081.
Example 1 silicon nitrogen phosphorus high efficiency halogen free flame retardant
Adding KH560, triglycidyl isocyanurate and aminoimidazole into a reaction vessel, and uniformly stirring and mixing;
and step two, slowly dropwise adding the isooctyl phosphate, maintaining the temperature below 40 ℃, and heating to 65 ℃ after dropwise adding to react for 4 hours.
Wherein the mass ratio of KH560, triglycidyl isocyanurate, aminoimidazole and isooctyl phosphate in the reaction is 4.5: 1.5: 0.6: 1.1.
Example 2 silicon nitrogen phosphorus high efficiency halogen free flame retardant
Adding KH560 and triglycidyl isocyanurate into a reaction vessel, and uniformly stirring and mixing;
and step two, slowly dropwise adding the diisocaprylate phosphate, keeping the temperature below 40 ℃, and heating to 70 ℃ after dropwise adding to react for 3.5 hours.
The mass ratio of the KH560 to the triglycidyl isocyanurate to the phosphoric acid diisocaprylate in the reaction is 2.0: 1.5: 0.3.
Example 3 silicon nitrogen phosphorus high efficiency halogen free flame retardant
Step one, adding polyphosphoric acid and isopropanol into a reaction container, and stirring and mixing uniformly;
and step two, slowly dripping a mixture of KH560, aminoimidazole and triglycidyl isocyanurate, maintaining the temperature below 40 ℃, and after dripping, heating to 80 ℃ for reacting for 3 hours.
The mass ratio of KH560, aminoimidazole and triglycidyl isocyanurate, polyphosphoric acid and isopropanol in the reaction is 0.8: 0.3: 2.6: 0.4: 0.5.
Example 4 silicon nitrogen phosphorus high efficiency halogen free flame retardant
Adding phosphoric acid and isopropanol into a reaction vessel, and stirring and mixing uniformly;
and step two, slowly dripping a mixture of KH560 and triglycidyl isocyanurate, maintaining the temperature below 40 ℃, and after dripping is finished, heating to 60 ℃ for reacting for 4.5 hours.
The mass ratio of the KH560 to the triglycidyl isocyanurate to the phosphoric acid to the isopropanol in the reaction is 4.5: 2.6: 0.7: 0.5.
Example 5 fire retardant coating
The preparation of a fireproof flame-retardant coating is as follows:
preparation process of fireproof coating
Step one, adding a commercially available pure acrylic emulsion polymer into a container, adding ammonia water and a small amount of water, and uniformly stirring at a low speed of about 180 r/min;
and step two, uniformly mixing the efficient flame retardant, the film-forming auxiliary agent, the wetting agent, the flatting agent, the thickening agent, the defoaming agent, the bactericide and the thickening agent, adding the mixture while stirring at the speed of 650r/min, stirring for 20min, filtering and packaging.
The fire-retardant coating prepared by the preparation process of the embodiment has reliable storage stability, and can obtain good stability results by testing a thermal storage test at the temperature of 50 ℃. The results of the tests carried out according to GB/T12441-2005 finish type fireproof paint are shown in the following table.
The test results show that the performance index of the developed water-based transparent fireproof coating exceeds the national standard requirement, and the effect of the invention is proved.
Example 6 fire retardant coating a fire retardant coating was prepared according to the following formula:
preparation process of fireproof coating
Step one, adding a dispersing agent into water, and then adding titanium dioxide and feldspar powder to disperse uniformly;
adding the polyurethane modified acrylic emulsion into a container, adding ammonia water and a small amount of water, and uniformly stirring at a low speed of about 150 r/min;
step three, adding the pigment slurry dispersed in the step one into the emulsion in the step two, and stirring uniformly;
and step four, uniformly mixing the efficient flame retardant, the film-forming auxiliary agent, the wetting agent, the flatting agent, the thickening agent, the defoaming agent, the bactericide and the thickening agent, adding the mixture while stirring at the speed of 600r/min, stirring for 15min, filtering and packaging.
The fire-retardant coating prepared by the preparation process of the embodiment has reliable storage stability, and can obtain good stability results by testing a thermal storage test at the temperature of 50 ℃. The results of the tests carried out according to GB/T12441-2005 finish type fireproof paint are shown in the following table.
The test result shows that the performance index of the developed water-based transparent fireproof coating exceeds the national standard requirement.
Example 7
The preparation of a fireproof flame-retardant coating is as follows:
preparation process of fireproof coating
Step one, adding a commercial styrene-acrylic emulsion into a container, adding ammonia water and a small amount of water, and uniformly stirring at a low speed of about 180 r/min;
and step two, uniformly mixing the efficient flame retardant, the film-forming auxiliary agent, the wetting agent, the flatting agent, the thickening agent, the defoaming agent, the bactericide and the thickening agent, adding the mixture while stirring at the speed of 620r/min, stirring for 30min, filtering and packaging.
The fire-retardant coating prepared by the preparation process of the embodiment has reliable storage stability, and can obtain good stability results by testing a thermal storage test at the temperature of 50 ℃. The results of the tests carried out according to GB/T12441-2005 finish type fireproof paint are shown in the following table.
The test results show that the performance index of the developed water-based transparent fireproof coating exceeds the national standard requirement, and the effect of the invention is proved.
Example 8
The preparation of a fireproof flame-retardant coating is as follows:
preparation process of fireproof coating
Adding a commercially available chlorinated rubber emulsion blended acrylic emulsion into a container, adding ammonia water and a small amount of water, and uniformly stirring at a low speed of about 200 r/min;
and step two, uniformly mixing the efficient flame retardant, the film-forming auxiliary agent, the wetting agent, the flatting agent, the thickening agent, the defoaming agent, the bactericide and the thickening agent, adding the mixture while stirring at the speed of 700r/min, stirring for 20min, filtering and packaging.
The fire-retardant coating prepared by the preparation process of the embodiment has reliable storage stability, and can obtain good stability results by testing a thermal storage test at the temperature of 50 ℃. The results of the tests carried out according to GB/T12441-2005 finish type fireproof paint are shown in the following table.
The test results show that the performance index of the developed water-based transparent fireproof coating exceeds the national standard requirement, and the effect of the invention is proved.
Comparative example:
comparative example the aqueous fireproofing coating prepared in example 7 was mixed with a common flame retardant ammonium polyphosphate
From this comparison, it can be seen that the paint prepared by the present invention is superior in flame retardancy, water resistance and wet heat resistance. In the aspect of flame retardance, the flame-resistant time index is increased, so that time can be won for escape of personnel on a fire scene in case of fire; from the viewpoint of water (moisture) resistance, the new flame retardant 144h did not peel off, whereas the conventional flame retardants foamed 72 and 96h, respectively, and lost the protective properties of the coating.
It should be understood that the above examples are only for clearly illustrating the present invention and are not intended to limit the embodiments of the present invention. It will be apparent to those skilled in the art that other variations and modifications may be made in the foregoing disclosure without departing from the spirit or essential characteristics of all embodiments, and that such modifications and variations are within the scope of the invention.
Claims (9)
1. The silicon-nitrogen-phosphorus efficient halogen-free flame retardant is characterized in that the silicon-nitrogen-phosphorus efficient halogen-free flame retardant is prepared by reacting alkoxy silane with an epoxy group, triglycidyl isocyanurate, aminoimidazole and a compound containing a phosphoric acid group; the mass ratio of the alkoxysilane with an epoxy group, the triglycidyl isocyanurate, the aminoimidazole and the compound containing a phosphoric acid group in the reaction is 1.5-6.2: 0.5-2.5: 0-1.0: 0.1-2, wherein the compound containing the phosphoric acid group is phosphoric acid or polyphosphoric acid, and the preparation method of the silicon-nitrogen-phosphorus efficient halogen-free flame retardant comprises the following steps:
adding alkoxy silane with epoxy groups, triglycidyl isocyanurate and aminoimidazole into a reaction vessel, and uniformly stirring and mixing;
and step two, slowly dropwise adding a compound containing phosphoric acid groups, keeping the temperature below 40 ℃, and after dropwise adding, heating to 60-70 ℃ for reaction for 3-5 hours.
2. The silicon nitrogen phosphorus high efficiency halogen-free flame retardant of claim 1, wherein the mass ratio of the alkoxy silane with epoxy group, triglycidyl isocyanurate, aminoimidazole and polyphosphoric acid in the reaction is 3: 2: 0.3: 1.5.
3. the silicon-nitrogen-phosphorus efficient halogen-free flame retardant of claim 1, wherein the alkoxy silane with epoxy groups is one or more of epoxy siloxane monomer, epoxy siloxane oligomer, epoxy modified silicone oligomer, acrylic modified epoxy silicone and phenolic modified epoxy silicone.
4. The efficient silicon nitrogen phosphorus halogen-free flame retardant of claim 3, wherein the epoxysiloxane monomer is KH 560.
5. The preparation method of the silicon-nitrogen-phosphorus efficient halogen-free flame retardant of any one of claims 1 to 4, characterized by comprising the following steps:
adding alkoxy silane with epoxy groups, triglycidyl isocyanurate and aminoimidazole into a reaction vessel, and uniformly stirring and mixing;
and step two, slowly dropwise adding a compound containing phosphoric acid groups, keeping the temperature below 40 ℃, and after dropwise adding, heating to 60-70 ℃ for reaction for 3-5 hours.
6. The use of the silicon-nitrogen-phosphorus high-efficiency halogen-free flame retardant of any one of claims 1 to 4 in the preparation of a fireproof flame-retardant coating.
7. The fireproof flame-retardant coating is characterized by comprising the following raw materials in parts by weight: 35-65 parts of emulsion polymer, 15-65 parts of silicon-nitrogen-phosphorus efficient halogen-free flame retardant according to any one of claims 1-5, 3-8 parts of film forming additive, 0.1-0.5 part of wetting agent, 0.1-0.2 part of flatting agent, 0.2-0.5 part of thickening agent, 0.1-0.5 part of defoaming agent, 0.1-0.3 part of bactericide, 0.1-0.5 part of ammonia water and 5-10 parts of deionized water.
8. The fireproof flame-retardant coating of claim 7, wherein the film-forming aid is alcohol ester-12, the wetting agent is a U3010 aqueous wetting agent, the leveling agent is leveling agent SN4710, the thickener is thickener U605, the defoamer is defoamer 6028, and the bactericide is bactericide 6081.
9. The preparation method of the fireproof flame-retardant coating of claim 7 or 8, which is characterized by comprising the following specific steps:
1) adding the emulsion polymer into a container, adding ammonia water and a small amount of water, and uniformly stirring at a low speed of 100-200 r/min;
2) uniformly mixing the silicon-nitrogen-phosphorus efficient halogen-free flame retardant, the film forming additive, the wetting agent, the leveling agent, the defoaming agent, the bactericide and the thickener according to any one of claims 1 to 4, adding the mixture under stirring at the speed of 600 to 700r/min, stirring for 15 to 25min, filtering and packaging.
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| CN115368570A (en) * | 2022-09-26 | 2022-11-22 | 山东天一化学股份有限公司 | Carbon forming agent of mosaic macromolecular derivative and preparation method thereof |
Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2006107659A1 (en) * | 2005-04-01 | 2006-10-12 | General Electric Company | Resin compositions and methods of use thereof |
| CN101818068A (en) * | 2010-04-26 | 2010-09-01 | 中科院广州化学有限公司 | Phosphoro-silicate hybrid-containing composite fire retardant and preparation method thereof |
| CN102112517B (en) * | 2008-08-01 | 2013-03-27 | 住友电木株式会社 | Resin composition for semiconductor encapsulation and semiconductor device using the same |
| CN103173070A (en) * | 2013-03-13 | 2013-06-26 | 惠州市凯辉化工有限公司 | Water-based flame retardant plastic coating for plastic materials |
| CN103265752A (en) * | 2013-06-04 | 2013-08-28 | 广东聚石化学股份有限公司 | Halogen-free flame retardant thermoplastic polyolefin cable material |
| CN104341595A (en) * | 2014-10-28 | 2015-02-11 | 东华大学 | BAPOPP (2,2-bi[4-(4-aminophenoxy)phenyl]propane) type active halogen-free flame retardant and preparation method thereof |
| CN104341596A (en) * | 2014-10-28 | 2015-02-11 | 东华大学 | DDM (4,4'-diaminodiphenylmethane) type active halogen-free flame retardant and preparation method thereof |
| CN105646581A (en) * | 2016-02-18 | 2016-06-08 | 厦门大学 | Halogen-free and ketone-containing intumescent flame retardant adopting cyanuric acid structure and synthetic method |
| CN107177168A (en) * | 2017-06-29 | 2017-09-19 | 倪群 | A kind of hydridization is grafted anti-oxidant flame retardant epoxy material and preparation method thereof |
| CN107760319A (en) * | 2017-09-15 | 2018-03-06 | 广东聚石化学股份有限公司 | A kind of preparation method of high polymerization degree APP fire retardant |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP5764423B2 (en) * | 2011-08-02 | 2015-08-19 | 日東電工株式会社 | Epoxy resin composition for optical semiconductor device, lead frame for optical semiconductor device or substrate for optical semiconductor device obtained by using the same, and optical semiconductor device |
-
2018
- 2018-12-24 CN CN201811581194.3A patent/CN109735157B/en active Active
Patent Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2006107659A1 (en) * | 2005-04-01 | 2006-10-12 | General Electric Company | Resin compositions and methods of use thereof |
| CN102112517B (en) * | 2008-08-01 | 2013-03-27 | 住友电木株式会社 | Resin composition for semiconductor encapsulation and semiconductor device using the same |
| CN101818068A (en) * | 2010-04-26 | 2010-09-01 | 中科院广州化学有限公司 | Phosphoro-silicate hybrid-containing composite fire retardant and preparation method thereof |
| CN103173070A (en) * | 2013-03-13 | 2013-06-26 | 惠州市凯辉化工有限公司 | Water-based flame retardant plastic coating for plastic materials |
| CN103265752A (en) * | 2013-06-04 | 2013-08-28 | 广东聚石化学股份有限公司 | Halogen-free flame retardant thermoplastic polyolefin cable material |
| CN104341595A (en) * | 2014-10-28 | 2015-02-11 | 东华大学 | BAPOPP (2,2-bi[4-(4-aminophenoxy)phenyl]propane) type active halogen-free flame retardant and preparation method thereof |
| CN104341596A (en) * | 2014-10-28 | 2015-02-11 | 东华大学 | DDM (4,4'-diaminodiphenylmethane) type active halogen-free flame retardant and preparation method thereof |
| CN105646581A (en) * | 2016-02-18 | 2016-06-08 | 厦门大学 | Halogen-free and ketone-containing intumescent flame retardant adopting cyanuric acid structure and synthetic method |
| CN107177168A (en) * | 2017-06-29 | 2017-09-19 | 倪群 | A kind of hydridization is grafted anti-oxidant flame retardant epoxy material and preparation method thereof |
| CN107760319A (en) * | 2017-09-15 | 2018-03-06 | 广东聚石化学股份有限公司 | A kind of preparation method of high polymerization degree APP fire retardant |
Non-Patent Citations (2)
| Title |
|---|
| ＤＯＰＯ－ＰＨＢＡ反应型阻燃剂的合成及其与TGIC复配体系对环氧树脂性能的影响;谭行;《复合材料学报》;20180331;285-294 * |
| Synthesis of an acrylate constructed by phosphaphenanthrene and triazine-trione and its application in intrinsic flame retardant vinyl ester resin;Xiaoxiao Tao，etal;《Polymer Degradation and Stability》;20180628;485-492 * |
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