CN110183619A - A kind of fire-retardant epoxy resin solidfied material and its preparation method and application of phosphorus nitrogen one - Google Patents
A kind of fire-retardant epoxy resin solidfied material and its preparation method and application of phosphorus nitrogen one Download PDFInfo
- Publication number
- CN110183619A CN110183619A CN201910363350.7A CN201910363350A CN110183619A CN 110183619 A CN110183619 A CN 110183619A CN 201910363350 A CN201910363350 A CN 201910363350A CN 110183619 A CN110183619 A CN 110183619A
- Authority
- CN
- China
- Prior art keywords
- curing agent
- phosphorus nitrogen
- epoxy resin
- mass parts
- solidfied material
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- 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
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
- C08G59/50—Amines
- C08G59/5026—Amines cycloaliphatic
-
- 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
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
- C08G59/50—Amines
- C08G59/5033—Amines aromatic
-
- 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
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
- C08G59/50—Amines
- C08G59/504—Amines containing an atom other than nitrogen belonging to the amine group, carbon and hydrogen
-
- 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
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
- C08G59/50—Amines
- C08G59/5046—Amines heterocyclic
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Epoxy Resins (AREA)
Abstract
The invention belongs to technical field of polymer materials, disclose a kind of fire-retardant epoxy resin solidfied material and its preparation method and application of phosphorus nitrogen one, the antiflaming epoxy resin curing agent includes 60~80 mass parts of epoxy resin, 15~25 mass parts of curing agent, 0.01~15 mass parts of phosphorus nitrogen one curing agent；Wherein, shown in the molecular structure such as formula (1) of the phosphorus nitrogen one curing agent:
Description
Technical field
The invention belongs to technical field of polymer materials, more particularly, to a kind of flame retardant type asphalt mixtures modified by epoxy resin of phosphorus nitrogen one
Rouge solidfied material and its preparation method and application.
Background technique
Epoxy resin, which refers to, contains two or more epoxy groups in chemical structure, and can be under certain condition
It reacts to obtain the compound of three-dimensional crosslinked network solidfied material with epoxy curing agent, is in polymer matrix composite using most
One of extensive resin, has high bond strength, good electrical insulation capability, excellent physical mechanical property, and price is low
It is honest and clean, easy to process, shrinking percentage is low, the coefficient of expansion is small, resistant to chemical etching, the advantages that possessing outstanding chemistry and dimensional stability,
It is therefore widely used in the neck such as electronic apparatus material, coating, adhesive, the basis material of composite material and civil material
Domain.
But epoxy resin is mainly made of three kinds of carbon, hydrogen, oxygen elements, belongs to combustible material, limit oxygen index only has
19.5, epoxy resin discharges a large amount of combustion heat after being ignited, and flame is spread rapidly, causes a large amount of molten drop, dense smoke and
Noxious material seriously threatens human life's property safety, damages surrounding ecological environment, significantly limits answering for epoxy resin
With.Therefore, it is necessary to carry out flame retardant treatment to epoxy resin.Early stage people introduce halogen-containing fire retardant in epoxy resin to improve
The flame retardant property of epoxy resin, but since halogen-containing fire retardant toxicity is big, seriously polluted, gradually by institute containing phosphorus type flame retardant
Instead of.Containing the efficient flame-retarding agent that phosphorus type flame retardant is environment friendly and pollution-free as new generation of green, it has been widely studied and applied.
And be generally all lacking compared with facile hydrolysis and oxidation, water resistance and compatibility performance containing phosphorus type flame retardant, directly add
Its physical mechanical property, chemical property etc. can be damaged by entering to epoxy resin.Therefore, nontoxic fire-retardant of exploitation New-type halide-free
Epoxy resin is of great significance.
Summary of the invention
In order to solve above-mentioned the shortcomings of the prior art and disadvantage, primary and foremost purpose of the present invention is to provide a kind of phosphorus nitrogen one
The fire retarding epoxide resin solidfied material of body.
Another object of the present invention is to provide a kind of preparation sides of the fire retarding epoxide resin solidfied material of above-mentioned phosphorus nitrogen one
Method.
A further object of the present invention is to provide a kind of applications of the fire retarding epoxide resin solidfied material of above-mentioned phosphorus nitrogen one.
The purpose of the present invention is realized by following technical proposals:
A kind of fire retarding epoxide resin solidfied material of phosphorus nitrogen one, the antiflaming epoxy resin curing agent includes epoxy resin 60
~80 mass parts, 15~25 mass parts of curing agent, 0.01~15 mass parts of phosphorus nitrogen one curing agent；Wherein, the phosphorus nitrogen one
Shown in the molecular structure of body curing agent such as formula (1):
Preferably, the antiflaming epoxy resin curing agent includes 63~75 mass parts of epoxy resin, 18~23 matter of curing agent
Measure part, 0.05~12 mass parts of phosphorus nitrogen one curing agent.
It is further preferable that the antiflaming epoxy resin curing agent includes 65~70 mass parts of epoxy resin, curing agent 20~
22 mass parts, 0.1~10 mass parts of phosphorus nitrogen one curing agent.
Preferably, the epoxy resin is one or more of E44, E51, CYD127, CYD128, E20 or E12.
Preferably, the curing agent is in diaminodiphenylmethane, 4,4- diaminobenzene sulfone or diaminomethyl thiacyclohexane
More than one.
The preparation method of the fire retarding epoxide resin solidfied material of the phosphorus nitrogen one, comprises the following specific steps that:
S1. it by the phosphorus nitrogen one curing agent of epoxy resin sum, is packed into thermometer, blender, three mouthfuls of heating device
In flask, 120~160 DEG C are warming up to, and open vacuum pump, are stirred at vacuum degree < -0.08MPa, until bubble-free generates；
S2. temperature is reduced again to 80~100 DEG C, is added with stirring curing agent, until curing agent is completely dissolved, 120~
Solidify at 150 DEG C to get the fire retarding epoxide resin solidfied material of phosphorus nitrogen one.
Preferably, the time of stirring described in step S1 is 0.5~1h.
Preferably, the cured time described in step S2 is 2~6h.
The fire retarding epoxide resin solidfied material of the phosphorus nitrogen one is in electronic apparatus material, coating, adhesive, composite material
Basis material or civil material field in application.
Compared with prior art, the invention has the following advantages:
1. fire retarding epoxide resin solidfied material of the invention is halogen-free, the harmful substances such as antimony oxide, environmentally protective, resistance
Combustion performance can reach UL94V-0 grade, P content only 1% when limit oxygen index LOI can reach 35.9%, with excellent anti-flammability
Energy.
2. the present invention uses curing agent (diaminodiphenylmethane, 4,4- diaminobenzene sulfone, diaminomethyl thiacyclohexane) and phosphorus
Nitrogen one curing agent co-curing epoxy resin, flame-retardant composition concentrate on curative systems, just have under lower phosphorus content excellent
Flame retardant property, the basic performance of epoxy resin will not be damaged.
3. fire retarding epoxide resin curing process of the invention is simple, production is stablized, and without volatilizable ingredient, can be widely applied to
The fields such as electronic apparatus material, coating, adhesive, the basis material of composite material and civil material.
Specific embodiment
The contents of the present invention are further illustrated combined with specific embodiments below, but should not be construed as limiting the invention.
Unless otherwise specified, the conventional means that technological means used in embodiment is well known to those skilled in the art.Except non-specifically
Illustrate, reagent that the present invention uses, method and apparatus is the art conventional reagents, method and apparatus.
Embodiment 1
1. weigh 0.8g (0.02mol) formaldehyde to be dissolved in 20ml ethyl alcohol, be poured into equipped with reflux condensing tube, thermometer and
In the 100ml three-necked flask of magneton.3.13g (0.02mol) 4- amino -2,2,6,6- tetramethyl piperidine is weighed again is dissolved in 10ml second
It in alcohol, is added drop-wise in three-necked flask with syringe at room temperature, after 0.5h is added dropwise, is warming up to 50 DEG C of reaction 2h, generation contains
Nitrogen intermediate；
2. 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide is added in the resulting nitrogenous intermediate of step S1
(DOPO) 4.32g (0.02mol) is added after 20ml ethyl alcohol is completely dissolved and is heated to 80 DEG C of reaction 8h, is cooled to room after completion of the reaction
Temperature.It is rotated at 50 DEG C, then puts it into 45 DEG C of vacuum ovens for 24 hours, obtain crocus solid, it is integrally solid that phosphorus nitrogen is made
Agent.
Embodiment 2
By the miscellaneous -10- phospha of 9, the 10- dihydro-9-oxy of the CYD127 epoxy resin of 75.44 mass parts and 7.14 mass parts
Phenanthrene -10- oxide is fitted into the three-necked flask for having thermometer, blender, heating device, is warming up to 130 DEG C, and is opened true
Sky pump stirs 0.5h in vacuum degree < -0.08MPa, until bubble-free generates.Temperature is reduced to 90 DEG C, is added with stirring
The diaminodiphenylmethane of 17.42 mass parts is finally poured into until diaminodiphenylmethane is completely dissolved and is pre-heated to 100 DEG C
Mold in, solidify 2h at 130 DEG C to get the fire retarding epoxide resin solidfied material of phosphorus nitrogen one.
Embodiment 3
By the phosphorus nitrogen one curing agent of the E44 epoxy resin of 77.98 mass fractions and 3.13 mass parts, it is packed into and has temperature
Meter, blender, heating device three-necked flask in, be warming up to 130 DEG C, and open vacuum pump, in vacuum degree < -0.08MPa, stir
0.5h is mixed, until bubble-free generates.Temperature is reduced to 90 DEG C, is added with stirring the diaminodiphenylmethane of 18.89 mass fractions,
Until diaminodiphenylmethane is completely dissolved, finally pour into the mold for being pre-heated to 100 DEG C, solidify at 130 DEG C 2h to get
The fire retarding epoxide resin solidfied material of phosphorus nitrogen one.
Embodiment 4
By the phosphorus nitrogen one curing agent of the E51 epoxy resin of 76.13 mass parts and 6.25 mass parts, it is packed into and has temperature
Meter, blender, heating device three-necked flask in, be warming up to 130 DEG C, and open vacuum pump, in vacuum degree < -0.08MPa, stir
0.5h is mixed, until bubble-free generates.Temperature is reduced to 90 DEG C, is added with stirring the diaminodiphenylmethane of 17.62 mass fractions,
Until diaminodiphenylmethane is completely dissolved, finally pour into the mold for being pre-heated to 100 DEG C, solidify at 130 DEG C 2h to get
The fire retarding epoxide resin solidfied material of phosphorus nitrogen one.
Embodiment 5
The phosphorus nitrogen one curing agent of the CYD127 epoxy resin of 74.28 mass parts and 9.38 mass parts is packed into temperature
It spends in the three-necked flask of meter, blender, heating device, is warming up to 130 DEG C, and open vacuum pump, in vacuum degree < -0.08MPa,
0.5h is stirred, until bubble-free generates.Temperature is reduced to 90 DEG C, is added with stirring the diamino hexichol first of 16.34 mass fractions
Alkane finally pours into the mold for being pre-heated to 100 DEG C until diaminodiphenylmethane is completely dissolved, solidifies 2h at 130 DEG C,
Up to the fire retarding epoxide resin solidfied material of phosphorus nitrogen one.
Embodiment 6
The phosphorus nitrogen one curing agent of the CYD128 epoxy resin of 72.43 mass parts and 12.50 mass parts is packed into temperature
It spends in the three-necked flask of meter, blender, heating device, is warming up to 130 DEG C, and open vacuum pump, in vacuum degree < -0.08MPa,
0.5h is stirred, until bubble-free generates.Temperature is reduced to 90 DEG C, is added with stirring the diamino hexichol first of 15.07 mass fractions
Alkane finally pours into the mold for being pre-heated to 100 DEG C until diaminodiphenylmethane is completely dissolved, solidifies 2h at 130 DEG C,
Up to the fire retarding epoxide resin solidfied material of phosphorus nitrogen one.
Embodiment 7
The phosphorus nitrogen one curing agent of the E12 epoxy resin of 80 mass parts and 15 mass parts is packed into thermometer, stirring
Device, heating device three-necked flask in, be warming up to 150 DEG C, and open vacuum pump, in vacuum degree < -0.08MPa, stir 1h, directly
It is generated to bubble-free.Temperature is reduced to 100 DEG C, is added with stirring 4, the 4- diaminobenzene sulfone of 20 mass fractions, until 4,4- bis-
Aminobenzene sulfone is completely dissolved, and is finally poured into the mold for being pre-heated to 100 DEG C, solidifies 1h at 150 DEG C to get phosphorus nitrogen one
Fire retarding epoxide resin solidfied material.
Embodiment 8
The phosphorus nitrogen one curing agent of the E51 epoxy resin of 60 mass parts and 15 mass parts is packed into thermometer, stirring
Device, heating device three-necked flask in, be warming up to 150 DEG C, and open vacuum pump, in vacuum degree < -0.08MPa, stir 1h, directly
It is generated to bubble-free.Temperature is reduced to 100 DEG C, is added with stirring the diaminomethyl thiacyclohexane of 15 mass fractions, until diamino first
Basic ring hexane is completely dissolved, and is finally poured into the mold for being pre-heated to 100 DEG C, solidifies 3h at 120 DEG C to get phosphorus nitrogen one
Fire retarding epoxide resin solidfied material.
Embodiment 9
The phosphorus nitrogen one curing agent of the E12 epoxy resin of 70 mass parts and 10 mass parts is packed into thermometer, stirring
Device, heating device three-necked flask in, be warming up to 150 DEG C, and open vacuum pump, in vacuum degree < -0.08MPa, stir 1h, directly
It is generated to bubble-free.Temperature is reduced to 100 DEG C, is added with stirring the diaminomethyl thiacyclohexane of 15 mass fractions, until diamino first
Basic ring hexane is completely dissolved, and is finally poured into the mold for being pre-heated to 100 DEG C, solidifies 3h at 120 DEG C to get phosphorus nitrogen one
Fire retarding epoxide resin solidfied material.
Embodiment 10
The phosphorus nitrogen one curing agent of the E20 epoxy resin of 75 mass parts and 12 mass parts is packed into thermometer, stirring
Device, heating device three-necked flask in, be warming up to 150 DEG C, and open vacuum pump, in vacuum degree < -0.08MPa, stir 1h, directly
It is generated to bubble-free.Temperature is reduced to 100 DEG C, is added with stirring the diaminomethyl thiacyclohexane of 25 mass fractions, until diamino first
Basic ring hexane is completely dissolved, and is finally poured into the mold for being pre-heated to 100 DEG C, solidifies 3h at 120 DEG C to get phosphorus nitrogen one
Fire retarding epoxide resin solidfied material.
Embodiment 11
By the phosphorus nitrogen one curing agent of the E44 epoxy resin of 77.98 mass fractions and 1 mass parts, be packed into thermometer,
Blender, heating device three-necked flask in, be warming up to 130 DEG C, and open vacuum pump, in vacuum degree < -0.08MPa, stirring
0.5h, until bubble-free generates.Temperature is reduced to 90 DEG C, is added with stirring the diaminodiphenylmethane of 18.89 mass fractions, directly
It is completely dissolved, is finally poured into the mold for being pre-heated to 100 DEG C to diaminodiphenylmethane, solidify 2h at 130 DEG C to get phosphorus
The fire retarding epoxide resin solidfied material of nitrogen one.
Embodiment 12
By the phosphorus nitrogen one curing agent of the E44 epoxy resin of 60 mass fractions and 0.01 mass parts, be packed into thermometer,
Blender, heating device three-necked flask in, be warming up to 130 DEG C, and open vacuum pump, in vacuum degree < -0.08MPa, stirring
0.5h, until bubble-free generates.Temperature is reduced to 90 DEG C, is added with stirring the diaminodiphenylmethane of 18.89 mass fractions, directly
It is completely dissolved, is finally poured into the mold for being pre-heated to 100 DEG C to diaminodiphenylmethane, solidify 2h at 130 DEG C to get phosphorus
The fire retarding epoxide resin solidfied material of nitrogen one.
Embodiment 13
By the phosphorus nitrogen one curing agent of the E44 epoxy resin of 63 mass fractions and 0.05 mass parts, be packed into thermometer,
Blender, heating device three-necked flask in, be warming up to 130 DEG C, and open vacuum pump, in vacuum degree < -0.08MPa, stirring
0.5h, until bubble-free generates.Temperature is reduced to 90 DEG C, is added with stirring the diaminodiphenylmethane of 18 mass fractions, until
Diaminodiphenylmethane is completely dissolved, and is finally poured into the mold for being pre-heated to 100 DEG C, solidifies 2h at 130 DEG C to get phosphorus nitrogen
The fire retarding epoxide resin solidfied material of one.
Embodiment 14
By the phosphorus nitrogen one curing agent of the E44 epoxy resin of 65 mass fractions and 0.1 mass parts, be packed into thermometer,
Blender, heating device three-necked flask in, be warming up to 130 DEG C, and open vacuum pump, in vacuum degree < -0.08MPa, stirring
0.5h, until bubble-free generates.Temperature is reduced to 90 DEG C, is added with stirring the diaminodiphenylmethane of 20 mass fractions, until
Diaminodiphenylmethane is completely dissolved, and is finally poured into the mold for being pre-heated to 100 DEG C, solidifies 2h at 130 DEG C to get phosphorus nitrogen
The fire retarding epoxide resin solidfied material of one.
Embodiment 15
By the phosphorus nitrogen one curing agent of the E44 epoxy resin of 70 mass fractions and 10 mass parts, it is packed into thermometer, stirs
In the three-necked flask for mixing device, heating device, 130 DEG C are warming up to, and open vacuum pump, in vacuum degree < -0.08MPa, stirring
0.5h, until bubble-free generates.Temperature is reduced to 90 DEG C, is added with stirring the diaminodiphenylmethane of 22 mass fractions, until
Diaminodiphenylmethane is completely dissolved, and is finally poured into the mold for being pre-heated to 100 DEG C, solidifies 2h at 130 DEG C to get phosphorus nitrogen
The fire retarding epoxide resin solidfied material of one.
Embodiment 16
By the phosphorus nitrogen one curing agent of the E44 epoxy resin of 75 mass fractions and 12 mass parts, it is packed into thermometer, stirs
In the three-necked flask for mixing device, heating device, 130 DEG C are warming up to, and open vacuum pump, in vacuum degree < -0.08MPa, stirring
0.5h, until bubble-free generates.Temperature is reduced to 90 DEG C, is added with stirring the diaminodiphenylmethane of 23 mass fractions, until
Diaminodiphenylmethane is completely dissolved, and is finally poured into the mold for being pre-heated to 100 DEG C, solidifies 2h at 130 DEG C to get phosphorus nitrogen
The fire retarding epoxide resin solidfied material of one.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, it is other it is any without departing from the spirit and principles of the present invention made by change, modification, substitution, combination and simplify,
It should be equivalent substitute mode, be included within the scope of the present invention.
Claims (9)
1. a kind of fire retarding epoxide resin solidfied material of phosphorus nitrogen one, which is characterized in that the antiflaming epoxy resin curing agent includes
60~80 mass parts of epoxy resin, 15~25 mass parts of curing agent, 0.01~15 mass parts of phosphorus nitrogen one curing agent；Wherein, institute
Shown in the molecular structure such as formula (1) for the phosphorus nitrogen one curing agent stated:
2. the fire retarding epoxide resin solidfied material of phosphorus nitrogen one according to claim 1, which is characterized in that the flame retardant epoxy
Resin curing agent includes 63~75 mass parts of epoxy resin, 18~23 mass parts of curing agent, phosphorus nitrogen one curing agent 0.05~12
Mass parts.
3. the fire retarding epoxide resin solidfied material of phosphorus nitrogen one according to claim 2, which is characterized in that the flame retardant epoxy
Resin curing agent includes 65~70 mass parts of epoxy resin, 20~22 mass parts of curing agent, 0.1~10 matter of phosphorus nitrogen one curing agent
Measure part.
4. the fire retarding epoxide resin solidfied material of phosphorus nitrogen one according to claim 1, which is characterized in that the asphalt mixtures modified by epoxy resin
Rouge is one or more of E44, E51, CYD127, CYD128, E20 or E12.
5. the fire retarding epoxide resin solidfied material of phosphorus nitrogen one according to claim 1, which is characterized in that the curing agent
For one or more of diaminodiphenylmethane, 4,4- diaminobenzene sulfone or diaminomethyl thiacyclohexane.
6. the preparation method of the fire retarding epoxide resin solidfied material of phosphorus nitrogen one according to claim 1-5, special
Sign is, comprises the following specific steps that:
S1. by the phosphorus nitrogen one curing agent of epoxy resin sum, it is packed into the three-necked flask for having thermometer, blender, heating device
In, 120~160 DEG C are warming up to, and open vacuum pump, are stirred at vacuum degree < -0.08MPa, until bubble-free generates；
S2. temperature is reduced again to 80~100 DEG C, is added with stirring curing agent, until curing agent is completely dissolved, at 120~150 DEG C
It is lower to solidify to get the fire retarding epoxide resin solidfied material of phosphorus nitrogen one.
7. the preparation method of the fire retarding epoxide resin solidfied material of phosphorus nitrogen one according to claim 6, which is characterized in that step
The time of stirring described in rapid S1 is 0.5~1h.
8. the preparation method of the fire retarding epoxide resin solidfied material of phosphorus nitrogen one according to claim 6, which is characterized in that step
The cured time described in rapid S2 is 2~6h.
9. the fire retarding epoxide resin solidfied material of the described in any item phosphorus nitrogen one of claim 1-5 electronic apparatus material, coating,
Application in adhesive, the basis material of composite material or civil material field.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910363350.7A CN110183619A (en) | 2019-04-30 | 2019-04-30 | A kind of fire-retardant epoxy resin solidfied material and its preparation method and application of phosphorus nitrogen one |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910363350.7A CN110183619A (en) | 2019-04-30 | 2019-04-30 | A kind of fire-retardant epoxy resin solidfied material and its preparation method and application of phosphorus nitrogen one |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN110183619A true CN110183619A (en) | 2019-08-30 |
Family
ID=67715453
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910363350.7A Pending CN110183619A (en) | 2019-04-30 | 2019-04-30 | A kind of fire-retardant epoxy resin solidfied material and its preparation method and application of phosphorus nitrogen one |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110183619A (en) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20030120021A1 (en) * | 2001-09-20 | 2003-06-26 | Chun-Shan Wang | Phosphorus-containing flame-retardant hardeners, epoxy resins, advanced epoxy resins and cured epoxy resins |
| CN102702678A (en) * | 2012-05-25 | 2012-10-03 | 厦门大学 | Halogen-free flame retardant toughened epoxy resin based composite material and preparation method thereof |
| CN103333461A (en) * | 2013-06-20 | 2013-10-02 | 天津市凯华绝缘材料有限公司 | Epoxy resin composition with high flame-retardant property and preparation method thereof |
| CN105017723A (en) * | 2015-06-26 | 2015-11-04 | 四川东材科技集团股份有限公司 | Insulation stressed member used for extra-high voltage direct current power transmission and transformation, and preparation method thereof |
| CN109021287A (en) * | 2018-06-08 | 2018-12-18 | 福建师范大学 | A kind of phosphorus nitrogen sulfur type fire retardant and its application in the epoxy |
-
2019
- 2019-04-30 CN CN201910363350.7A patent/CN110183619A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20030120021A1 (en) * | 2001-09-20 | 2003-06-26 | Chun-Shan Wang | Phosphorus-containing flame-retardant hardeners, epoxy resins, advanced epoxy resins and cured epoxy resins |
| CN102702678A (en) * | 2012-05-25 | 2012-10-03 | 厦门大学 | Halogen-free flame retardant toughened epoxy resin based composite material and preparation method thereof |
| CN103333461A (en) * | 2013-06-20 | 2013-10-02 | 天津市凯华绝缘材料有限公司 | Epoxy resin composition with high flame-retardant property and preparation method thereof |
| CN105017723A (en) * | 2015-06-26 | 2015-11-04 | 四川东材科技集团股份有限公司 | Insulation stressed member used for extra-high voltage direct current power transmission and transformation, and preparation method thereof |
| CN109021287A (en) * | 2018-06-08 | 2018-12-18 | 福建师范大学 | A kind of phosphorus nitrogen sulfur type fire retardant and its application in the epoxy |
Non-Patent Citations (2)
| Title |
|---|
| HUO, SIQI ET AL.: ""Synthesis of a novel reactive flame retardant containing phosphaphenanthrene and piperidine groups and its application in epoxy resin"", 《POLYMER DEGRADATION AND STABILITY》 * |
| 霍思奇: ""DOPO基本征型阻燃环氧树脂体系的设计制备及其性能研究"", 《中国博士学位论文全文数据库 工程科技I辑》 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Liu et al. | Preparation, thermal properties, and flame retardance of epoxy–silica hybrid resins | |
| KR101915920B1 (en) | CERAMICIZED SILICON RESIN COMPOSITION AND PREPREG AND LAMINATE USING THE SAME | |
| CN102863906B (en) | Low-cost environment-friendly water glass wood adhesive and preparation method thereof | |
| CN103467926B (en) | A kind of Phosphor-nitrogen halogen-free flame-retardant epoxy resin | |
| CN108795134A (en) | A kind of solvent-free fireproof coating | |
| CN108504257A (en) | A kind of fire resistant coating and preparation method thereof | |
| CN106633673B (en) | A kind of epoxy resin and preparation method thereof based on phospha phenanthrene derivative and inorganic fire retardants compositional flame-retardant | |
| CN110256814A (en) | A kind of preparation method of the derivative modified fire retarding epoxide resin of DOPO containing piperazine structure | |
| CN109467574A (en) | It is a kind of novel based on vanillic aldehyde reactive flame retardant and its preparation, application | |
| CN102181128A (en) | Epoxy resin premix and preparation technology of the epoxy resin premix | |
| Liu et al. | Phosphorus‐containing polyaryloxydiphenylsilanes with high flame retardance arising from a phosphorus–silicon synergistic effect | |
| CN103525298B (en) | Thermostable anticorrosive coating and preparation method | |
| CN110183619A (en) | A kind of fire-retardant epoxy resin solidfied material and its preparation method and application of phosphorus nitrogen one | |
| Chiang et al. | Flame retardance and thermal degradation of new epoxy containing silicon and phosphorous hybrid ceramers prepared by the sol-gel method | |
| CN103059790A (en) | Heat-resistant, flame resistant and anti-brittle fracture modified epoxy resin adhesive and preparation method thereof | |
| EP3049256A1 (en) | A self-healing epoxy resin composition | |
| CN107400194A (en) | New-type halide-free reaction-type flame-retarding curing agent and preparation method thereof | |
| WO2023083325A1 (en) | Flame retardant and use thereof, and fire-resistant epoxy resin | |
| CN115160543A (en) | Preparation method and application of environment-friendly flame-retardant amine curing agent | |
| CN107501526A (en) | A kind of new DOPO types epoxy curing agent and preparation method thereof | |
| CN100506914C (en) | Smoke-inhibition type halogen-free flame-proof polycarbonate | |
| CN106833466A (en) | A kind of high-ductility fire retarding epoxide resin adhesive | |
| WO2017101742A1 (en) | Quick-drying-type anti-corrosion paint and preparation method therefor | |
| CN112430381A (en) | Preparation method of intrinsic organic-inorganic smoke-suppression flame-retardant epoxy resin composite material | |
| CN114685937A (en) | Flame-retardant epoxy resin composite material and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20190830 |
|
| RJ01 | Rejection of invention patent application after publication |