CN102153729B - Semi-enclosed organic amine curing agent and application thereof to anti-corrosive coating - Google Patents
Semi-enclosed organic amine curing agent and application thereof to anti-corrosive coating Download PDFInfo
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- CN102153729B CN102153729B CN 201110052512 CN201110052512A CN102153729B CN 102153729 B CN102153729 B CN 102153729B CN 201110052512 CN201110052512 CN 201110052512 CN 201110052512 A CN201110052512 A CN 201110052512A CN 102153729 B CN102153729 B CN 102153729B
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Abstract
The invention discloses a semi-enclosed organic amine curing agent, which is characterized by being obtained by mixing and reacting the following substances in percentage by weight: 15-40 percent of epoxy resin, 5-12 percent of amine, 15-35 percent of ketone and 20-35 percent of solvent, wherein the epoxy resin is bisphenol A epoxy resin or bisphenol F epoxy resin; the amine is diethylenetriamine or triethylene tetramine; the ketone is methyl isobutyl ketone or ethyl methyl ketone; and the solvent is toluene or xylene or a mixture of toluene and xylene in any ratio or normal butanol or isobutyl alcohol or a mixture of normal butanol and isobutyl alcohol in any ratio. Semi-enclosed organic amine obtained by multi-step synthesis is cross-linked with epoxy resin and naturally dried into a film, the cross-linked product is de-capsulated into primary amine for further curing with moisture in the air or moisture on the surface of a substrate, and the curing agent is partially enclosed, so that the service life of reactive double-component paint can be greatly prolonged after mixing; and epoxy resin is introduced into the curing agent to form a multi-aromatic ring anti-corrosive prepolymer, so that the corrosion resistance of a final film forming substance is further enhanced.
Description
Technical field
The present invention relates to protective system film forming matter preparation and coating preparation technical field, be specifically related to key ingredient, composition semiclosed-type organic amine curing agent, preparation method and the application in protective system thereof of the low protective system of surface treatment.
Background technology
Protective system is that the departments such as modern industry, traffic, the energy, oceanographic engineering use a kind of coating very widely, account for 30% anti-corrosive paint of epoxy resin and be cured as the overwhelming majority with epoxy group(ing) and amine, wherein solidifying agent works to the application property of anti-corrosive paint of epoxy resin, antiseptic property etc. the very important effect of doing.
In prior art, at first require before corrosion protective coating technology strictly to process being coated matrix surface; When selecting corrosion-resistant epoxy paint, the overwhelming majority is that epoxy resin and organic amine film-forming are that base-material and rust-stabilising pigment, filler and auxiliary agent etc. consist of corrosion protection coating.Wanting the preservative effect concrete grammar that anticorrosive coating with less expensive reaches high requirement has following several:
1, in anticorrosive coating, thereby suitably reduce pre-treatment requirement reduction expense, see the preservative effect that can reach good.
2, extend the usage period of many component epoxies protective system, reduce the waste of protective system in the construction use.
3, improve the antiseptic property of film-forming resin in protective system, reach the preservative effect of long period, thus obtain in the reduction of long-term anticorrosion cost.
Owing to requiring seasoning anticorrosive coating technique more in the anticorrosive coating design, anti-corrosive paint of epoxy resin has again outstanding Anticorrosive Character, bisphenol A type epoxy resin can anti-higher corrosion temperature (100 ~ 120 ℃), also has certain acid resistance, alkali resistance performance etc. and is used widely.But the corrosion-resistant temperature of the epoxy resin of prior art is still lower, can not satisfy the needs of higher corrosion-resistant temperature (160 ℃ of left and right), anti-strong acid, highly basic; And require higher to the pre-treatment that is coated matrix surface in the corrosion-resistant epoxy paint coating decoration.Therefore, need to the key ingredient solidifying agent of corrosion-resistant epoxy paint be further processed, could adapt to the anticorrosion needs of low-treated surface steel.
Summary of the invention
The corrosion-resistant temperature that the present invention is directed to epoxy curing agent of the prior art is lower, can not satisfy the needs of higher corrosion-resistant temperature, anti-strong acid, highly basic, in coating decoration, the pre-treatment that is coated matrix surface is had relatively high expectations, increased the deficiencies such as construction cost, provide a kind of key ingredient as protective system, semiclosed-type organic amine curing agent and the application in protective system thereof.
The object of the present invention is achieved like this: semiclosed-type organic amine curing agent, it is characterized in that being obtained by the material hybrid reaction of following weight percent,
| Epoxy resin | 15~40% |
| Amine | 5~12% |
| Ketone | 15~35% |
| Solvent | 20~35% |
Described epoxy resin can be selected bisphenol A epoxide resin, or bisphenol F epoxy resin, or other suitable epoxy resin;
Described amine can be selected diethylenetriamine, triethylene tetramine, or other suitable amine;
Described ketone can be selected hexone, methylethylketone, or other suitable ketone;
Described solvent can be selected toluene or dimethylbenzene, or toluene and dimethylbenzene is with the mixture of arbitrary proportion, or propyl carbinol or isopropylcarbinol, or propyl carbinol and isopropylcarbinol are with the mixture of arbitrary proportion.
The synthetic process of semiclosed-type organic amine curing agent of the present invention is characterized in that comprising the steps:
Step 1: the amine that will proportionally take and ketone drop in reactor, stir, and are warmed up to 110 ~ 180 ℃, react 4 ~ 10 hours, discharge water from water trap at set intervals; React complete after, be cooled to below 50 ℃ filter, discharging, obtain a kind of sealing primary amine, keep the semiclosed-type organic amine curing agent of secondary amine, this organic amine curing agent is the ketoimine lower-molecular substance;
Step 2: the used for epoxy resin dissolution with solvents that will proportionally take, be warming up to 85 ~ 100 ℃, moisture is in addition removed in backflow, be cooled to again the semiclosed-type organic amine curing agent that adds step 1 to obtain below 80 ℃, keep reaction for some time at 50 ~ 100 ℃, as 40 ~ 100 minutes, maintenance refluxed to remove moisture, was cooled to below 40 ℃ to pack.
The present invention contains the rust proof paint of semiclosed-type organic amine curing agent, it is characterized in that being comprised of the first component and the component B that include semiclosed-type organic amine curing agent:
The moiety of first component and weight percent are:
| Solvent | 35~45% |
| Semiclosed-type organic amine curing agent | 55~65% |
| Low-temperature curing promotor | 2~6% |
Wherein solvent is propyl carbinol, isopropylcarbinol, and methyl iso-butyl ketone (MIBK), a kind of in dimethylbenzene, or wherein two or three mix with arbitrary proportion;
Low-temperature curing promotor is: tertiary amine or phenolic hydroxyl group trimethylamine are as MDP-30[2,4,6-three (N, N-dimethyl) methylamino phenol], K-54; And enjoy this graceful product: Accelerator 960-1 (standard tertiary amine), Accelerator 2950 (patent protection product).
The moiety of component B and weight percent are:
| Epoxy resin | 25~45% |
| Red iron oxide | 8~15% |
| Aluminium triphosphate | 8~~15% |
| Talcum powder | 5~25% |
| Wetting dispersing auxiliary | 0.1~0.5% |
| Functional resin | 3~8% |
| Anti-precipitation auxiliary agent | 0.5~1.5% |
| The froth breaking auxiliary agent | 0.1~0.2% |
| Leveling auxiliary agent | 0.1~0.5% |
| Solvent | 8~25% |
Wherein functional resin is: any in terpolycyantoamino-formaldehyde resin, xylene formaldehyde resin, aldehyde ketone resin; Or wherein two or three mix with arbitrary proportion;
Wherein dispersing auxiliary is: any in anti-coacervation polyether polyols with reduced unsaturation dispersion agent, unsaturated polyester acid amides and acid esters salt wetting dispersing agent or wherein two kinds mix with arbitrary proportion;
Wherein anti-precipitation auxiliary agent is: any in aerosil, acid amides modified waxes liquid, hydrogenated castor oil; Or wherein two or three mix with arbitrary proportion;
Froth breaking auxiliary agent wherein: be any in silicone antifoam agent, antifoaming agent of non-silicone; Or wherein two kinds mix with arbitrary proportion;
Wherein leveling auxiliary agent is: any in modified organic silicon flow agent, fluorine-carbon macromolecule compound flow agent or wherein two kinds mix with arbitrary proportion;
Solvent is dimethylbenzene, propyl carbinol, and methyl iso-butyl ketone (MIBK), isopropylcarbinol, a kind of in aromatic solvent S-100A, or wherein two or three mix with arbitrary proportion;
First, component B mixing quality ratio is: first
:Second=1
: (3 ~ 9)
With respect to prior art, the present invention has following features:
1, by synthetic homemade type semienclosed organic amine of several steps and cross linking of epoxy resin seasoning film forming.
2, be that primary amine further solidifies by moisture in air or substrate surface moisture deblocking, and due to the curing agent part sealing, after the two component paints of response type mix, the serviceable time extend greatly.
3, this two component epoxies antifouling paste is applicable to the low-treated surface base material, and some substrate surface or construction environment humidity that can't reach the high request pre-treatment are also being reached good effect more than 80%.
4, adopt introducing epoxy resin formation multi-aromatic ring protection against corrosion prepolymer in solidifying agent, make the antiseptic property of final film forming matter further improve.
Embodiment
Semiclosed-type organic amine curing agent of the present invention is characterized in that being obtained by the material hybrid reaction of following weight percent,
| Epoxy resin | 15~40% |
| Amine | 5~12% |
| Ketone | 15~35% |
| Solvent | 20~35% |
Described epoxy resin is bisphenol A epoxide resin, or bisphenol F epoxy resin, or other suitable epoxy resin;
Described amine is diethylenetriamine, triethylene tetramine, or other suitable amine;
Described ketone is hexone, methylethylketone, or other suitable ketone;
Described solvent is toluene or dimethylbenzene, or toluene and dimethylbenzene is with the mixture of arbitrary proportion, or propyl carbinol or isopropylcarbinol, or propyl carbinol and isopropylcarbinol are with the mixture of arbitrary proportion.
The synthetic method of semiclosed-type organic amine curing agent of the present invention, it comprises the steps:
Step 1: the amine that will proportionally take and ketone drop in reactor, stir, and are warmed up to 110 ~ 180 ℃, react 4 ~ 10 hours, discharge water from water trap at set intervals; React complete after, be cooled to below 50 ℃ filter, discharging, obtain a kind of semiclosed-type organic amine curing agent that seals primary amine, keeps secondary amine, this organic amine curing agent is the ketoimine lower-molecular substance;
Step 2: the used for epoxy resin dissolution with solvents that will proportionally take, be warming up to 85 ~ 100 ℃, moisture is in addition removed in backflow, be cooled to again the semiclosed-type organic amine curing agent that adds step 1 to obtain below 80 ℃, keep reaction for some time at 50 ~ 100 ℃, maintenance refluxes to remove moisture, is cooled to below 40 ℃ to pack.
The protective system that contains semiclosed-type organic amine curing agent of the present invention is comprised of first, second two components:
Wherein the composition of first component and weight percent are:
| Solvent | 25~35% |
| Semiclosed-type organic amine curing agent | 65~75% |
| Low-temperature curing promotor | 0~3% |
Wherein solvent is propyl carbinol, isopropylcarbinol, and methyl iso-butyl ketone (MIBK), a kind of in dimethylbenzene, or wherein two or three mix with arbitrary proportion;
Wherein low-temperature curing promotor is: tertiary amine or phenolic hydroxyl group trimethylamine, as: MDP-30[2,4,6-three (N, N-dimethyl) methylamino phenol], K-54; And enjoy this graceful product: Accelerator 960-1 (standard tertiary amine), Accelerator 2950 (patent protection product).
The composition of component B and weight percent are:
| Epoxy resin | 25~45% |
| Titanium dioxide | 0~~15% |
| Furnace treated black | 0~2.0% |
| Red iron oxide | 0~15% |
| Aluminium triphosphate | 8~~15% |
| Talcum powder | 5~25% |
| Wetting dispersing auxiliary | 0.1~0.5% |
| Functional resin | 3~8% |
| Anti-precipitation auxiliary agent | 0.2~1.5% |
| The froth breaking auxiliary agent | 0.1~0.2% |
| Leveling auxiliary agent | 0.1~0.5% |
| Solvent | 8~25% |
Wherein functional resin is: any in terpolycyantoamino-formaldehyde resin, xylene formaldehyde resin, aldehyde ketone resin; Or wherein two or three mix with arbitrary proportion;
Wherein dispersing auxiliary is: any in a new generation anti-coacervation polyether polyols with reduced unsaturation dispersion agent, unsaturated polyester acid amides and acid esters salt wetting dispersing agent or wherein two kinds mix with arbitrary proportion;
Anti-precipitation auxiliary agent wherein: be any in aerosil, acid amides modified waxes liquid, hydrogenated castor oil; Or wherein two or three mix with arbitrary proportion;
Froth breaking auxiliary agent wherein: be any in silicone antifoam agent, antifoaming agent of non-silicone; Or wherein two kinds mix with arbitrary proportion;
Wherein leveling auxiliary agent is: any in modified organic silicon flow agent, fluorine-carbon macromolecule compound flow agent or wherein two kinds mix with arbitrary proportion;
Solvent is dimethylbenzene, propyl carbinol, and methyl iso-butyl ketone (MIBK), isopropylcarbinol, a kind of in the S-100A solvent, or wherein two or three mix with arbitrary proportion;
First, component B mixing quality ratio is: first
:Second=1
: (3 ~ 9)
Embodiment 1:
1, the preparation of type semienclosed special organic amine curing agent
(1) take triethylene tetramine 200Kg, hexone 800Kg, drop in stainless steel cauldron, pad hexone in water trap, start and stir, be warming up to backflow, and keep refluxing, (adjusting this interval time according to temperature and water outlet situation) discharged water from water trap once every 30 minutes, along with reaction is carried out, temperature in the kettle rises gradually, when reaching 140 ℃, temperature begins timing, reacted about 6 hours, the accumulative total aquifer yield reaches can lowering the temperature more than 10.5% of always feeding intake, filter below temperature to 40 ℃, discharging, with packaging spare after air in the nitrogen replacement pail pack.
(2) take E-20 epoxy resin 400Kg, toluene 250Kg, in stainless steel cauldron, pad toluene in water trap, beginning crawl when being warming up to 85 ℃ stirs, if without extremely formal startup stirring, keep refluxing and dewatered 1 hour, the product 280Kg that adds preparation in (1) when being cooled to 60 ℃, slowly heating, stopped heating when temperature rises to 60 ℃, and emptying jacket steam, allow intensification naturally in still, if can suitably heat when the temperature rising is slow, keep reaction for some time, as kept refluxing 1 hour, use in case of necessity dimethylbenzene, butanols, one or more arbitrary proportion mixtures 100Kg in hexone dilutes, pack, obtain the special organic amine curing agent of a kind of type semienclosed type (epoxy ketoimine prepolymer).
2, the preparation of first component
Take the special organic amine curing agent 700Kg of type semienclosed type, solvent 290Kg in the stainless steel still of the use nitrogen purge of low-temperature curing promotor 10Kg input cleaning, drying, stirs, filter after the assay was approved, with packing after air in the nitrogen replacement pail pack.
3, the preparation of component B
taking red iron oxide 155Kg is tinting pigment, epoxy resin 250Kg as anticorrosion base-material, hydrogenated castor oil 3Kg as anti-precipitation effect, talcum powder 220Kg as stopping composition, as rust-stabilising pigment aluminium triphosphate 150kg, polycarboxylate sky happy-70 as wetting dispersing auxiliary is 3Kg, non-organic silicon ketone EFKA-2020 as the froth breaking auxiliary agent is 0.5Kg, methyl isobutyl ketone solvent 218.5Kg (gross weight 1000Kg) as solvent mixes and stirs, change in paint mixing cylinder below being dispersed to fineness 50 μ m with sand mill, add merit performance resin xylene formaldehyde resin 30Kg, add totally 0.5 Kg as the fluorocarbon polymer EFKA-3600 of leveling auxiliary agent, isopropylcarbinol 10Kg (gross weight 1000Kg) as solvent.
3, above-mentioned first, component B is mixed in proportion, get first component 1Kg in reality and mix with component B 5Kg, the first component
:Second=1
:5, adjust working viscosity 17 ~ 30S (determining according to working-yard temperature) and filter laggard line space gas spraying application.
Proportioning of the present invention, the first component
:The concrete numerical value that second can be selected is, 1
:3,1
:3.2,1
:3.5,1
:3.8,1
:4,1
:4.2,1
:4.5,1
:4.8,1
:5,1
:5.2,1
:5.5,1
:5.8,1
:6,1
:6.5,1
:6.8,1
:7,1
:7.5,1
:8 etc., can satisfy actual needs, realize the object of the invention.
Embodiment 2:
1, the preparation of type semienclosed special organic amine curing agent
(1) take diethylenetriamine 350Kg, hexone 650Kg, drop in stainless steel cauldron, pad hexone in water trap, start and stir, be warming up to backflow, and keep refluxing, (adjusting this interval time according to temperature and water outlet situation) discharged water from water trap once every 30 minutes, along with reaction is carried out, temperature in the kettle rises gradually, when reaching 140 ℃, temperature begins timing, 6 the reaction hour more than, the accumulative total aquifer yield reaches can lowering the temperature more than 10.5% of always feeding intake, filter below temperature to 40 ℃, discharging, with packaging spare after air in the nitrogen replacement pail pack.
(2) take E-20 epoxy resin 350Kg, dimethylbenzene 250Kg, in stainless steel cauldron, pad dimethylbenzene in water trap, beginning crawl when being warming up to 85 ℃ stirs, if without extremely formal startup stirring, keep refluxing and dewatered 1 hour, the product 300Kg that adds preparation in (1) when being cooled to 60 ℃, slowly heating, stopped heating immediately when temperature rises to 60 ℃, and emptying jacket steam, allow intensification naturally in still, if can suitably heat when the temperature rising is slow, reaction for some time, as kept refluxing 1 hour, use in case of necessity dimethylbenzene, butanols, one or more arbitrary proportion mixtures 100Kg in hexone dilutes, pack, obtain a kind of type semienclosed special organic amine curing agent (epoxy ketoimine prepolymer).
2, the preparation of first component
Take type semienclosed special organic amine curing agent 800Kg, solvent 190Kg in the stainless steel still of the use nitrogen purge of low-temperature curing promotor 10Kg input cleaning, drying, stirs, and filters after the assay was approved, with packing after air in the nitrogen replacement pail pack.
3, the preparation of component B
take titanium dioxide 150Kg and furnace treated black 5Kg as tinting pigment, take anticorrosion base-material epoxy resin 250Kg, hydrogenated castor oil 3Kg as anti-precipitation effect, talcum powder 220Kg as stopping composition, as rust-stabilising pigment aluminium triphosphate 150kg, sky happy-70 as wetting dispersing auxiliary is total to 3Kg, EFKA-2020 as the froth breaking auxiliary agent is total to 0.5Kg, methyl isobutyl ketone solvent 218.5Kg (gross weight 1000Kg) as solvent mixes and stirs, change in paint mixing cylinder below being dispersed to fineness 50 μ m with sand mill, add merit performance resin xylene formaldehyde resin 30Kg, add totally 0.5 Kg as the EFKA-3600 of leveling auxiliary agent, isopropylcarbinol 10Kg (gross weight 1000Kg) as solvent.
3, above-mentioned first, component B is mixed in proportion, get first component 1Kg in reality and mix with component B 5Kg, the first component
:Second=1
:5, adjust working viscosity 17 ~ 30S (determining according to working-yard temperature) and filter laggard line space gas spraying application.
Proportioning of the present invention, the first component
:The concrete numerical value that second can be selected is, 1
:3,1
:3.2,1
:3.5,1
:3.8,1
:4,1
:4.2,1
:4.5,1
:4.8,1
:5,1
:5.2,1
:5.5,1
:5.8,1
:6,1
:6.5,1
:6.8,1
:7,1
:7.5,1
:8 etc., can satisfy actual needs, realize the object of the invention.
Two component epoxide resin protective systems of the present invention are quoted GB/T 1724-1979, GB/T 1725-2007, GB/T 1771-2007 detects paint vehicle, and its fineness is 50 μ m, and non-volatile part is 70%, meets Q/CYQ 286-2009 standard; Quote GB/T 1728-1979, GB/T 1731-1993, GB/T 1732-1993, GB/T1730-2007, GB/T1720-1996, GB/T1733-1993, GB/T1763-1996, GB/T 1771-2007 detect paint film, its surface drying time is 60min., do solid work and be 24h., snappiness is 1mm, shock-resistance is 50cm, hardness is 0.5, sticking power is 1 grade, water-fast 720h. is non-foaming, wrinkle resistant, non-corrosive, salt water resistance 720h. is qualified, qualified Q/CYQ 286-2009 standard-requireds that meet of salt spray resistance 500h..
Claims (1)
1. protective system that contains semiclosed-type organic amine curing agent is characterized in that:
A, formed by first, second two components:
Wherein the composition of first component and weight percent are:
Wherein solvent is propyl carbinol, isopropylcarbinol, and methyl iso-butyl ketone (MIBK), a kind of in dimethylbenzene, or wherein two or three mix with arbitrary proportion;
Wherein low-temperature curing promotor is: tertiary amine;
The composition of component B and weight percent are:
Wherein functional resin is: any in terpolycyantoamino-formaldehyde resin, xylene formaldehyde resin, aldehyde ketone resin; Or wherein two or three mix with arbitrary proportion;
Wherein dispersing auxiliary is: any in anti-coacervation polyether polyols with reduced unsaturation dispersion agent, unsaturated polyester acid amides and acid esters salt wetting dispersing agent or wherein two kinds mix with arbitrary proportion;
Anti-precipitation auxiliary agent wherein: be any in aerosil, acid amides modified waxes liquid, hydrogenated castor oil; Or wherein two or three mix with arbitrary proportion;
Froth breaking auxiliary agent wherein: be any in silicone antifoam agent, antifoaming agent of non-silicone; Or wherein two kinds mix with arbitrary proportion;
Wherein leveling auxiliary agent is: any in modified organic silicon flow agent, fluorine-carbon macromolecule compound flow agent or wherein two kinds mix with arbitrary proportion;
Solvent is dimethylbenzene, propyl carbinol, and methyl iso-butyl ketone (MIBK), isopropylcarbinol, a kind of in aromatic solvent S-100A, or wherein two or three mix with arbitrary proportion;
B, the semiclosed-type organic amine curing agent in the first component are wherein obtained by the material hybrid reaction of following weight percent, and each component concentration sum is 100%;
Described epoxy resin is bisphenol A epoxide resin, or bisphenol F epoxy resin;
Described amine is diethylenetriamine, or triethylene tetramine;
Described ketone is hexone, or methylethylketone;
Described solvent is toluene or dimethylbenzene, or toluene and dimethylbenzene is with the mixture of arbitrary proportion, or propyl carbinol or isopropylcarbinol, or propyl carbinol and isopropylcarbinol are with the mixture of arbitrary proportion;
C, first, component B mixing quality ratio are: first
:Second=1
: (3 ~ 9).
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| CN109153038A (en) | 2015-12-31 | 2019-01-04 | 汉高股份有限及两合公司 | Low-temperature bake autodeposition coatings |
| CN105505200A (en) * | 2016-01-09 | 2016-04-20 | 安徽万诚达新型材料有限公司 | Epoxy seal paint and preparation method thereof |
| CN107523187B (en) * | 2017-09-08 | 2020-05-26 | 重庆三峡油漆股份有限公司 | Enhanced thermal insulation reflective coating |
| CN108948950A (en) * | 2018-06-08 | 2018-12-07 | 徐潇潇 | A kind of formula based on improvement coating tolerance |
| CN109134829B (en) * | 2018-08-17 | 2021-05-11 | 重庆南方漆业有限公司 | Anti-tack epoxy curing agent and preparation method and application thereof |
| CN110724433B (en) * | 2019-10-15 | 2021-10-01 | 江苏大亚新型包装材料有限公司 | Antifouling weather-resistant protective coating for reaction kettle equipment and preparation method thereof |
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| CN101781508B (en) * | 2010-01-18 | 2012-03-28 | 中国海洋石油总公司 | Epoxy protective coating system for high-power nuclear power station |
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| CN101054487A (en) * | 2007-04-30 | 2007-10-17 | 袁兴 | Method of preparing low temperature solidifying environment protection type cathode electrophoresis coating |
| CN101274998A (en) * | 2008-03-21 | 2008-10-01 | 中国科学院广州化学研究所 | Heat-resistant flame-proof phosphorus- and silicon-containing hybrid curing agent for epoxy type electronic polymer material and preparation thereof |
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