CN109722209A - A kind of YASI organic imides silica gel and preparation method thereof - Google Patents
A kind of YASI organic imides silica gel and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to a kind of YASI organic imides silica gel and preparation method thereof, by 1,3- bis- (2,4- diamino phenoxy) benzene 13BDAPB, both-end aminopropyl polydimethylsiloxone YASI, maleic anhydride, aromatic diamine, aromatic dicarboxylic acid anhydride and 3- aminopropyltrialkoxysilane reaction product and organic solvent composition.Raw material sources of the invention are convenient, and simple process is easy to operate, and product comprehensive performance is good, can be applied to the bonding of glass, ceramics, composite material, extraordinary polarity weaving prepreg and its composite material base, have good market application prospect.
Description
Technical field
The invention belongs to adhesive area, in particular to a kind of YASI organic imides silica gel and preparation method thereof.
Background technique
Adhesive system is widely used in the every field of national economy: either high-technology field or general
Its trace can be seen in technical field, either defence and military or civilian industry or even daily life.
Related adhesive system or containing silicone resin system have had many research reports, also there is many patents of invention:
Chinese invention patent CN102786902A discloses a kind of organosilicon Organic fluoride epoxy adhesive and preparation method thereof.
Yan Rui, Yu Xinhai et al. [preparation of novel epoxy adhesive and performance study, insulating materials, 2012,45 (2):
12-14,18] a kind of neo-epoxy resin adhesive and preparation method thereof is disclosed, and systematic research has been carried out to its performance.
Chinese invention patent CN106220851A discloses a kind of siliceous epoxy acid imide matrix resin of YASI type and its system
Preparation Method is characterized mainly in that:
(1) by bis- (3- amino-4-hydroxylphenyl) hexafluoropropane of 2,2-, o-cresol, bis- [4- (the 3,4- dicarboxyl benzene of 2,2-
Oxygroup) phenyl] propane dianhydride and maleic anhydride be put into reaction kettle, be passed through nitrogen, stir, be heated to 80 DEG C, be added dropwise different
Quinoline is heated to 100 DEG C -110 DEG C, after being stirred to react 5-12 hours, is cooled to 60 DEG C, reactant is poured into and fills precipitating agent
In precipitating kettle, solids is precipitated in stirring, is filtered, and vacuum drying obtains imide oligomer object；
(2) will be bis- (γ-aminopropyl) polydimethylsiloxone YASI, epoxy resin be put into reaction kettle, in 80 DEG C-
After 100 DEG C are stirred reaction 0.5-1 hours, imide oligomer object is added and continues to be stirred to react 1-2 hours, 3- ammonia is then added
Propyl trialkoxy silane is stirred to react 5-15 minutes, is cooled to room temperature, is added curing agent, is uniformly mixed.
Yu Xinhai et al. [preparation of organosilicon epoxy system adhesive and performance study, insulating materials, 2012,45 (2):
1-3,11] a kind of adhesive composition of organic siliconresin modified epoxy is disclosed, and its performance is studied, simultaneously
The superior adhesive of comprehensive performance is obtained.
Xu Meifang et al. [the cure kinetics research of polyimide-epoxy resin adhesive, chemistry and bonding, 2011,33
(2): 17-20 a kind of polyimide-epoxy resin adhesive] is disclosed, and cure kinetics research has been carried out to it.
Chinese invention patent CN104844801A discloses a kind of Silicone Containing Polyimides copper coated foil plate, it is characterised in that: by
Copper foil, alkali-free glass cloth and Silicone Containing Polyimides resin composition；Wherein, it is 1:1-5 that Silicone Containing Polyimides resin, which is by mass ratio,
A, B component polymerization reaction and obtain；And component A is reacted with aromatic dianhydride by the organosilicon diamines that molar ratio is 1:2 and is obtained；B
Component is by molar ratio are as follows: the aromatic diamine of 2:1.8-1.9:0.1-0.3 is reacted with aromatic dianhydride, maleic anhydride and obtained.
Chinese invention patent CN101397486A discloses a kind of preparation side of bi-component solvent-free epoxy resin adhesive
Method is primarily characterized in that: it includes component A and B component, and wherein component A contains novolac epoxy resin, alicyclic type epoxy resin
And nbr carboxyl terminal；B component is 4,4 '-bis- (2,4- diamino phenoxy) diphenyl ether aromatic polyvalent amine hardeners.Rouge
The additive amount of ring-like epoxy resin and nbr carboxyl terminal is respectively the 20-35% and 12% (quality hundred of novolac epoxy resin
Score).The additive amount of 4,4 '-bis- (2,4- diamino phenoxy) diphenyl ether aromatic polyvalent amine hardeners is epoxy novolac
Chinese patent CN101397486A discloses a kind of preparation method of bi-component solvent-free epoxy resin adhesive,
Be characterized mainly in that: it includes component A and B component, and wherein component A contains novolac epoxy resin, alicyclic type epoxy resin and end
Carboxy nitrile rubber；B component is bis- (2,4- diamino phenoxy) the benzene aromatic polyvalent amine hardeners of 1,4-.Alicyclic ring type asphalt mixtures modified by epoxy resin
The additive amount of rouge and nbr carboxyl terminal is respectively the 20-35% and 12% (mass percent) of novolac epoxy resin.1,4-
The additive amount of bis- (2,4- diamino phenoxy) benzene aromatic polyvalent amine hardeners is the 15-20% (quality of novolac epoxy resin
Percentage), gained adhesive system good manufacturability.But its heat resistance is ideal not enough.
Yu Xinhai et al. [development [J] of high-temperature resistant single-component epoxy adhesive is bonded, 2008,29 (12): 16-19] is public
The preparation method for having opened a kind of high-temperature resistant single-component epoxy adhesive, is primarily characterized in that: being sealing end with maleic anhydride (MA)
Agent, with bis- [4- (4- amino-benzene oxygen) phenyl] third of bis- (3- amino-4-hydroxylphenyl) hexafluoropropane (BAHPFP) of 2,2-, 2,2-
Bis- [4- (3,4- di carboxyl phenyloxy) phenyl] propane dianhydrides (BPADA) of alkane (BAPOPP), 2,2- are that main Material synthesis obtains
Phenolic hydroxy group polyetherimide resin (HPEI)；With synthesized obtained HPEI for resistant, toughened dose, with N, N, N', N'- tetra-
Glycidyl -4,4'- diaminodiphenylmethane (TGDDM), hydrogenated bisphenol A epoxy resin (HBPAE), latent curing agent
Deng, preparation obtained the high-temperature resistant single-component epoxy adhesive of excellent combination property.
This method, although containing the polyetherimide resin of active reactive group (hydroxyl, unsaturated double-bond) by synthesis
(HPEI), toughening modifying has been carried out to epoxy resin, and has achieved preferable technical effect.But there is also some disadvantages:
(1) reactable group is limited, and the content of especially unsaturated double-bond is relatively low.Because maleic anhydride is as sealing end
Agent come using, the dosage of maleic anhydride is seldom.
The monomers such as bis- (3- amino-4-hydroxylphenyl) hexafluoropropane (BAHPFP) of (2) 2,2- are expensive, lead to polyethers acyl
The cost of imide resin (HPEI) and adhesive is very high, is unfavorable for large-scale promotion application, can only be confined to certain special dimensions.
Chinese invention patent CN106220047A discloses a kind of YASI type granolith plate and preparation method thereof, main
It is characterized in that:
(1) epoxy resin and bis- (γ-aminopropyl) polydimethylsiloxone YASI are put into reaction kettle, stirring is mixed
It closes, in 115 DEG C after -125 DEG C of reactions 0.5-1 hours, is cooled to 60 DEG C hereinafter, addition latent curing agent LRC30 and liquid acid
Acid anhydride is uniformly mixed, and obtains YASI type resin；
(2) after mixing by YASI type resin and granite powder, it being put into stainless steel flat plate frame, pressing is preforming,
Heat-pressure curing molding；Wherein, the temperature range of heating is room temperature to 180 DEG C；The pressure limit of pressurization be 0.5MPa extremely
5MPa；Curing time is 2-5 hours.
Summary of the invention
Technical problem to be solved by the invention is to provide a kind of YASI organic imides silica gel and preparation method thereof, this has
Machine silica gel comprehensive performance is good, can be applied to glass, ceramics, composite material, extraordinary polarity weaving prepreg and its composite material
The bonding of substrate has good market application prospect.
The present invention provides a kind of YASI organic imides silica gel, the organic silica gel is 1:0.1-0.5:2 by molar ratio:
5-10:6.5-12:1-2 bis- (2,4- diamino phenoxy) the benzene 13BDAPB of 1,3-, both-end aminopropyl polydimethylsiloxone
The reaction product of YASI, maleic anhydride, aromatic diamine, aromatic dicarboxylic acid anhydride and 3- aminopropyltrialkoxysilane, and
Organic solvent composition.
The aromatic diamine is selected from m-phenylene diamine (MPD), p-phenylenediamine, 2- methylresorcinol diamines, 2,4,6- trimethyl isophthalic
Diamines, 3,4 '-diaminodiphenyl ethers, 4,4 '-diaminodiphenyl ethers, 3,3 '-diaminodiphenyl ethers, 4,4 '-benzidines, 3,
3 '-dimethyl -4,4 '-benzidine, 4,4 '-diaminodiphenylmethane, 4,4 '-diamino -4 "-hydroxyl triphenylmenthane, 4,
It is 4 '-diaminodiphenylsulfones, 3,3 '-diaminodiphenylsulfones, 3,3 '-dimethyl -4,4 '-diaminodiphenylmethane, 3,3 '-two chloro-
4,4 '-diaminodiphenylmethane, 3,3 ', 5,5 '-tetramethyls -4,4 '-diaminodiphenylmethane, 2,6- bis- (4- amino-benzene oxygens)
Bis- (3- amino-benzene oxygen) benzonitriles of benzonitrile, 2,6-, 2- (4- aminophenyl) -5- aminobenzimidazole, 3,3 '-diamino -
Bis- (3- amino-4-hydroxylphenyl) propane of 4,4 '-dihydroxybiphenyls, 2,2-, bis- (3- amino-4-hydroxylphenyl) hexafluoros third of 2,2-
Bis- (3- amino-benzene oxygen) benzene of alkane, 1,3-, bis- (4- amino-benzene oxygen) benzene of 1,3-, 1,4- bis- (4- amino-benzene oxygen) benzene, 1,3-
Bis- (2- trifluoromethyl-4-aminophenoxyl) benzene of bis- (2- trifluoromethyl-4-aminophenoxyl) benzene, 1,4-, bis- (the 4- amino of 2,6-
Phenoxy group) toluene, bis- (4- amino-benzene oxygen) toluene of 2,5-, 3,5- bis- (2- trifluoromethyl-4-aminophenoxyl) benzoic acid, 2,
Bis- (2- trifluoromethyl-4-aminophenoxyl) toluene of 6-, bis- (2- trifluoromethyl-4-aminophenoxyl) toluene of 2,5-, 2,2- are bis-
Bis- [4- (2- trifluoromethyl-4-aminophenoxyl) phenyl] propane of [4- (4- amino-benzene oxygen) phenyl] propane, 2,2-, 2,2- are bis-
[4- (3- amino-benzene oxygen) phenyl] propane, 4,4 '-bis- (4- amino-benzene oxygen) diphenyl-methanes, 4,4 '-bis- (3- aminobenzene oxygen
Base) diphenyl-methane, 4,4 '-bis- (2- trifluoromethyl-4-aminophenoxyl) diphenyl-methanes, the bis- [4- (4- amino-benzene oxygen) of 2,2-
Phenyl] hexafluoropropane, bis- [4- (2- trifluoromethyl-4-aminophenoxyl) phenyl] hexafluoropropane of 2,2-, bis- [4- (the 3- ammonia of 2,2-
Phenoxyl) phenyl] hexafluoropropane, 4,4 '-bis- (4- amino-benzene oxygen) diphenyl sulphone (DPS)s, 4,4 '-bis- (3- amino-benzene oxygen) hexichol
Sulfone, 4,4 '-bis- (2- trifluoromethyl-4-aminophenoxyl) diphenyl sulphone (DPS)s, 4,4 '-bis- (4- amino-benzene oxygen) diphenyl sulfides, 4,4 '-
Bis- (3- amino-benzene oxygen) diphenyl sulfides, 4,4 '-bis- (2- trifluoromethyl-4-aminophenoxyl) diphenyl sulfides, 4,4 '-bis- (4-
Amino-benzene oxygen) diphenyl ether, 4,4 '-bis- (3- amino-benzene oxygen) diphenyl ether, 4,4 '-bis- (2- trifluoromethyl -4- aminobenzene oxygen
Base) it is diphenyl ether, 4,4 '-bis- (4- amino-benzene oxygen) benzophenone, 4,4 '-bis- (3- amino-benzene oxygen) benzophenone, 4,4 '-bis-
(2- trifluoromethyl-4-aminophenoxyl) benzophenone, 4,4 '-bis- (4- amino-benzene oxygen) biphenyl, 4,4 '-bis- (3- aminobenzenes
Oxygroup) biphenyl, one or more of 4,4 '-bis- (2- trifluoromethyl-4-aminophenoxyl) biphenyl.
The aromatic dicarboxylic acid anhydride be selected from pyromellitic acid anhydride, 3,3 ', 4,4 '-tetracarboxylic diphenyl ether dianhydrides, 3,3 ', 4,
Bis- (3,4- dicarboxyphenyi) hexafluoros third of 4 '-tetracarboxylic diphenyl sulfone dianhydrides, 3,3 ', 4,4 '-tetracarboxylic benzophenone dianhydrides, 2,2-
Bis- [4- (3,4- di carboxyl phenyloxy) phenyl] hexafluoropropane dianhydrides of alkane dianhydride, 3,3 ', 4,4 '-tetracarboxylic biphenyl dianhydrides, 2,2-,
Bis- [4- (3,4- di carboxyl phenyloxy) phenyl] propane dianhydrides of 2,2-, 1,4- bis- (3,4- di carboxyl phenyloxy) benzene dianhydrides, 1,3-
Double-(3,4- di carboxyl phenyloxy) benzene dianhydride, 4,4 '-bis- (3,4- di carboxyl phenyloxy) biphenyl dianhydrides, 4,4 '-bis- (3,4- bis-
Carboxyphenoxy) diphenyl sulfone dianhydride, 4,4 '-bis- (3,4- di carboxyl phenyloxy) diphenyl ether dianhydrides, 4,4 '-bis- (3,4- dicarboxyls
Phenoxy group) diphenyl ether dianhydride, one or more of 4,4 '-bis- (3,4- di carboxyl phenyloxy) benzophenone dianhydrides.
The 3- aminopropyltrialkoxysilane is selected from 3- aminopropyl trimethoxysilane, 3- aminopropyl triethoxysilane
One or both of.
The organic solvent is selected from N, N-dimethylformamide, N, N dimethyl acetamide, tetrahydrofuran, methyl tetrahydro furan
It mutters, one or more of n-methyl-2-pyrrolidone, N- ethyl-2-pyrrolidone, dimethyl sulfoxide.
The mass ratio of the organic solvent and reactant is 2.5-9.5:1；Wherein, reactant refers to 1,3- bis- (2,4- bis-
Amino-benzene oxygen) benzene 13BDAPB, both-end aminopropyl polydimethylsiloxone YASI, maleic anhydride, aromatic diamine, virtue
Fragrant race's dibasic anhydride and 3- aminopropyltrialkoxysilane.
The molecular structural formula of the both-end aminopropyl polydimethylsiloxone YASI are as follows:
Wherein, m is and the natural number less than 15 greater than 1.
The present invention also provides a kind of preparation methods of YASI organic imides silica gel, include the following steps:
According to the ratio, bis- (2,4- diamino phenoxy) the benzene 13BDAPB of 1,3- and organic solvent are put into reaction kettle, room temperature
After lower stirring and dissolving, maleic anhydride is added, reacts 15min-30min after stirring and dissolving at room temperature, both-end aminopropyl is then added
Polydimethylsiloxone YASI, aromatic diamine after stirring and dissolving, are added aromatic dicarboxylic acid anhydride, are stirred to react at room temperature
After -4.0 hours 1.0 hours, be added 3- aminopropyltrialkoxysilane, be stirred to react at room temperature -2 hours 0.5 hour to get
YASI organic imides silica gel.
Beneficial effect
(1) present invention has a good hot mechanical performance, and excellent combination property, can be applied to glass, ceramics, compound
The bonding of material, extraordinary polarity weaving prepreg and its composite material base, has good market application prospect；
(2) preparation process of the invention is simple, at low cost, easy to operate, reaction raw materials convenient sources, can set general
Standby middle completion preparation process, is advantageously implemented industrialized production；
(3) 3- aminopropyltrialkoxysilane, both-end aminopropyl poly two are introduced in adhesive molecular structure of the invention
Methylsiloxane YASI provides not only the cured crosslinking reactivity group of adhesive system or silicon oxygen silicon base group is made to enter high score
Sub- skeleton structure, and good anchor cooperation use or affinity interaction can be generated with substrate, to improve the interface performance of bonding plane with
Adhesive strength is of great benefit to.
Specific embodiment
Present invention will be further explained below with reference to specific examples.It should be understood that these embodiments are merely to illustrate the present invention
Rather than it limits the scope of the invention.In addition, it should also be understood that, after reading the content taught by the present invention, those skilled in the art
Member can make various changes or modifications the present invention, and such equivalent forms equally fall within the application the appended claims and limited
Range.
Embodiment 1
By bis- (2,4- diamino phenoxy) benzene (13BDAPB) of the 1,3- of 32.2 grams (0.1 moles), 420 grams of methyl tetrahydros
Furans and 900 grams of n,N dimethylformamide are put into reaction kettle, and at room temperature after stirring and dissolving, 19.6 grams of (0.2 mole) horses are added
Carry out acid anhydrides, react 15min after stirring and dissolving at room temperature, 11.3 grams of (0.01 mole) both-end aminopropyl poly dimethyl are then added
Siloxanes (YASI, m average value be 13), after stirring and dissolving is complete, be added 40.0 grams of (0.2 mole) 3,4 '-diaminodiphenyl ethers,
Bis- (4- amino-benzene oxygen) benzonitriles of 31.7 grams of (0.1 mole) 2,6-, 36.6 grams of bis- (3- amino-4-hydroxies of (0.1 mole) 2,2-
Phenyl) hexafluoropropane and 40.0 grams of (0.1 moles) 4,4 '-bis- (4- amino-benzene oxygen) diphenyl sulfides after stirring and dissolving, are added
209.3 grams (0.65 mole) 3,3 ', 4,4 '-tetracarboxylic benzophenone dianhydrides, stirring and dissolving, is stirred to react 1.0 hours at room temperature
Afterwards, 22.1 grams of (0.1 mole) 3- aminopropyl triethoxysilanes are added, are stirred to react 2 hours at room temperature to get viscous to 1763 grams
Thick YASI organic imides silica gel, is denoted as SA-1.
Embodiment 2
By bis- (2,4- diamino phenoxy) benzene (13BDAPB) of the 1,3- of 32.2 grams (0.1 moles), 1000 grams of tetrahydro furans
It mutters, 1000 grams of N, N dimethyl acetamide and 1000 grams of N- ethyl-2-pyrrolidones are put into reaction kettle, at room temperature stirring and dissolving
Afterwards, 19.6 grams of (0.2 mole) maleic anhydrides are added, react 30min after stirring and dissolving at room temperature, are then added 20.8 gram (0.03
Mole) (YASI, m average value are 7), after stirring and dissolving is complete, to be added 58.0 grams to both-end aminopropyl polydimethylsiloxone
(0.2 mole) 4,4 '-diamino -4 "-hydroxyl triphenylmenthane, 100.0 grams of (0.5 mole) 3,4 '-diaminodiphenyl ethers and 120.0
After stirring and dissolving, 186.0 grams of (0.6 moles) 3,3 ' are added in gram (0.3 mole) 4,4 '-bis- (4- amino-benzene oxygen) diphenyl sulfides,
4,4 '-tetracarboxylic diphenyl ether dianhydrides and 193.2 grams (0.6 mole) 3,3 ', 4,4 '-tetracarboxylic benzophenone dianhydrides, are stirred at room temperature
Dissolution is mixed, after being stirred to react 4.0 hours, 44.2 grams of (0.2 mole) 3- aminopropyl triethoxysilanes are added, stirring is anti-at room temperature
0.5 hour is answered to get to 3774 grams of sticky YASI organic imides silica gel, is denoted as SA-2.
Embodiment 3
By bis- (2,4- diamino phenoxy) benzene (13BDAPB) of the 1,3- of 32.2 grams (0.1 moles), 1600 grams of tetrahydro furans
It mutters, the organic solvent of 2000 grams of n,N dimethylformamide and 2000 grams of N- ethyl-2-pyrrolidones is put into reaction kettle, room temperature
After lower stirring and dissolving, 19.6 grams of (0.2 mole) maleic anhydrides are added, react 20min after stirring and dissolving at room temperature, is then added
(YASI, m average value are 4), after stirring and dissolving is complete, to add to 23.5 grams of (0.05 mole) both-end aminopropyl polydimethylsiloxones
Enter bis- (4- amino-benzene oxygen) hexichol of 40.0 grams of (0.2 mole) 3,4 '-diaminodiphenyl ethers, 120.0 grams of (0.3 moles) 4,4 '-
Thioether and 43.2 grams of (0.2 mole) 3,3 '-diamino -4,4 '-dihydroxybiphenyls, after stirring and dissolving, being added 225.4 grams, (0.7 rubs
You) 3,3 ', 4,4 '-tetracarboxylic benzophenone dianhydrides, bis- [4- (3,4- di carboxyl phenyloxy) benzene of 78.0 grams of (0.15 mole) 2,2-
Base] propane dianhydride, stirring and dissolving, after being stirred to react 2.0 hours, is added 22.1 grams of three second of (0.1 mole) 3- aminopropyl at room temperature
Oxysilane and 17.9 grams of (0.1 mole) 3- aminopropyl trimethoxysilanes, are stirred to react 1.5 hours at room temperature to get arriving
6222 grams of sticky YASI organic imides silica gel, are denoted as SA-3.
Embodiment 4
The YASI organic imides silica gel of suitable 1~embodiment of embodiment 3, i.e. SA-1~SA-3, and difference are taken respectively
It is uniformly applied in standard stainless steel test piece, overlaps, clamp, be put into convection oven and solidified: being started to warm up from room temperature
To 80 DEG C, after being kept for 1 hour, 150 DEG C are continuously heating to, after being kept for 2 hours, is continuously heating to 200 DEG C, after being kept for 0.5 hour,
260 DEG C are continuously heating to, after being kept for 0.5 hour, cooled to room temperature.Using electronic tensile machine, room temperature is carried out to it respectively
Tensile shear strength test under the conditions of (25 DEG C) and high temperature (250 DEG C), the results are shown in Table 1.
The YASI organic imides silica gel of suitable 1~embodiment of embodiment 3, i.e. SA-1~SA-3, and difference are taken respectively
It is equably impregnated on glass cloth, is overlapped and clamped with standard stainless steel test piece, be put into convection oven and solidified: being opened from room temperature
Beginning is warming up to 80 DEG C, after being kept for 1 hour, is continuously heating to 150 DEG C, after being kept for 2 hours, is continuously heating to 200 DEG C, keeps 0.5
After hour, 260 DEG C are continuously heating to, after being kept for 0.5 hour, cooled to room temperature.Using electronic tensile machine, respectively to its into
Tensile shear strength test under the conditions of row room temperature (25 DEG C) and high temperature (250 DEG C), the results are shown in Table 1.
Using Guilin Electro Scientific research institute produce megger test its solidfied material volume resistivity ρ v (1MHz, 25
DEG C), the results are shown in Table 1.
The dielectric loss (D) of its solidfied material is tested using the TH2828S tester of Changzhou Tong Hui Electron equipment Co., Ltd
(1MHz, 25 DEG C), the results are shown in Table 1.
Deionized water (25 DEG C) are soaked in after the square coupons weighing (W1) of above-mentioned drying using precision electronic balance
In, it after 72 hours, takes out, dries surface with filter paper, weigh (W2), water absorption rate is calculatedData it is as shown in table 1.
Climatic chamber (85 is placed in after the square coupons weighing (G1) of above-mentioned drying using precision electronic balance
DEG C, RH85%) in, it after 72 hours, takes out, dries surface with filter paper, weigh (G2), the data of hydroscopicity (ψ) are calculated such as
Shown in table 1.
The performance data of table 1YASI organic imides silica gel
Claims (8)
1. a kind of YASI organic imides silica gel, it is characterised in that: the organic silica gel is 1:0.1-0.5:2:5- by molar ratio
Bis- (2,4- diamino phenoxy) the benzene 13BDAPB of the 1,3- of 10:6.5-12:1-2, both-end aminopropyl polydimethylsiloxone
The reaction product of YASI, maleic anhydride, aromatic diamine, aromatic dicarboxylic acid anhydride and 3- aminopropyltrialkoxysilane, and
Organic solvent composition.
2. a kind of YASI organic imides silica gel according to claim 1, it is characterised in that: the aromatic diamine choosing
From m-phenylene diamine (MPD), p-phenylenediamine, 2- methylresorcinol diamines, 2,4,6- trimethyl m-phenylene diamine (MPD), 3,4 '-diaminodiphenyl ethers, 4,
4 '-diaminodiphenyl ethers, 3,3 '-diaminodiphenyl ethers, 4,4 '-benzidines, 3,3 '-dimethyl -4,4 '-diamino connection
Benzene, 4,4 '-diaminodiphenylmethane, 4,4 '-diamino -4 "-hydroxyl triphenylmenthane, 4,4 '-diaminodiphenylsulfones, 3,3 '-two
Aminodiphenyl sulfone, 3,3 '-dimethyl -4,4 '-diaminodiphenylmethane, 3,3 '-two chloro- 4,4 '-diaminodiphenylmethane, 3,
Bis- (4- amino-benzene oxygen) benzonitriles of 3 ', 5,5 '-tetramethyls -4,4 '-diaminodiphenylmethane, 2,6-, bis- (the 3- aminobenzenes of 2,6-
Oxygroup) benzonitrile, 2- (4- aminophenyl) -5- aminobenzimidazole, 3,3 '-diamino -4,4 '-dihydroxybiphenyl, 2,2- be bis-
Bis- (3- amino-4-hydroxylphenyl) hexafluoropropane of (3- amino-4-hydroxylphenyl) propane, 2,2-, bis- (the 3- aminobenzene oxygen of 1,3-
Base) benzene, bis- (4- amino-benzene oxygen) benzene of 1,3-, bis- (4- amino-benzene oxygen) benzene of 1,4-, the bis- (2- trifluoromethyl -4- amino of 1,3-
Phenoxy group) benzene, bis- (2- trifluoromethyl-4-aminophenoxyl) benzene of 1,4-, bis- (4- amino-benzene oxygen) toluene of 2,6-, 2,5- be bis-
Bis- (2- trifluoromethyl-4-aminophenoxyl) benzoic acid of (4- amino-benzene oxygen) toluene, 3,5-, the bis- (2- trifluoromethyl -4- of 2,6-
Amino-benzene oxygen) toluene, bis- (2- trifluoromethyl-4-aminophenoxyl) toluene of 2,5-, bis- [4- (4- amino-benzene oxygen) benzene of 2,2-
Base] propane, bis- [4- (2- trifluoromethyl-4-aminophenoxyl) phenyl] propane of 2,2-, bis- [4- (3- amino-benzene oxygen) benzene of 2,2-
Base] it is propane, 4,4 '-bis- (4- amino-benzene oxygen) diphenyl-methanes, 4,4 '-bis- (3- amino-benzene oxygen) diphenyl-methanes, 4,4 '-bis-
Bis- [4- (4- amino-benzene oxygen) phenyl] hexafluoropropane of (2- trifluoromethyl-4-aminophenoxyl) diphenyl-methane, 2,2-, 2,2- are bis-
Bis- [4- (3- amino-benzene oxygen) phenyl] hexafluoros third of [4- (2- trifluoromethyl-4-aminophenoxyl) phenyl] hexafluoropropane, 2,2-
Alkane, 4,4 '-bis- (4- amino-benzene oxygen) diphenyl sulphone (DPS)s, 4,4 '-bis- (3- amino-benzene oxygen) diphenyl sulphone (DPS)s, 4,4 '-bis- (2- fluoroforms
Base -4- amino-benzene oxygen) diphenyl sulphone (DPS), 4,4 '-bis- (4- amino-benzene oxygen) diphenyl sulfides, 4,4 '-bis- (3- amino-benzene oxygens) two
Diphenyl sulfide, 4,4 '-bis- (2- trifluoromethyl-4-aminophenoxyl) diphenyl sulfides, 4,4 '-bis- (4- amino-benzene oxygen) diphenyl ether,
4,4 '-bis- (3- amino-benzene oxygen) diphenyl ether, 4,4 '-bis- (2- trifluoromethyl-4-aminophenoxyl) diphenyl ether, 4,4 '-bis- (4-
Amino-benzene oxygen) benzophenone, 4,4 '-bis- (3- amino-benzene oxygen) benzophenone, 4,4 '-bis- (2- trifluoromethyl -4- aminobenzenes
Oxygroup) benzophenone, 4,4 '-bis- (4- amino-benzene oxygen) biphenyl, 4,4 '-bis- (3- amino-benzene oxygen) biphenyl, 4,4 '-bis- (2-
One or more of trifluoromethyl-4-aminophenoxyl) biphenyl.
3. a kind of YASI organic imides silica gel according to claim 1, it is characterised in that: the aromatic dicarboxylic acid anhydride choosing
From pyromellitic acid anhydride, 3,3 ', 4,4 '-tetracarboxylic diphenyl ether dianhydrides, 3,3 ', 4,4 '-tetracarboxylic diphenyl sulfone dianhydrides, 3,3 ',
4,4 '-tetracarboxylic benzophenone dianhydrides, 2,2- bis- (3,4- dicarboxyphenyi) hexafluoropropane dianhydrides, 3,3 ', 4,4 '-tetracarboxylics connection
Bis- [4- (3,4- di carboxyl phenyloxy) phenyl] hexafluoropropane dianhydrides of benzene dianhydride, 2,2-, bis- [4- (the 3,4- dicarboxyl benzene oxygen of 2,2-
Base) phenyl] propane dianhydride, bis- (3,4- di carboxyl phenyloxy) benzene dianhydrides of 1,4-, 1,3- be bis--(3,4- di carboxyl phenyloxy) benzene two
Acid anhydride, 4,4 '-bis- (3,4- di carboxyl phenyloxy) biphenyl dianhydrides, 4,4 '-bis- (3,4- di carboxyl phenyloxy) diphenyl sulfone dianhydrides, 4,
4 '-bis- (3,4- di carboxyl phenyloxy) diphenyl ether dianhydrides, 4,4 '-bis- (3,4- di carboxyl phenyloxy) diphenyl ether dianhydrides, 4,4 '-
One or more of bis- (3,4- di carboxyl phenyloxy) benzophenone dianhydrides.
4. a kind of YASI organic imides silica gel according to claim 1, it is characterised in that: three alcoxyl of 3- aminopropyl
Base silane is selected from one or both of 3- aminopropyl trimethoxysilane, 3- aminopropyl triethoxysilane.
5. a kind of YASI organic imides silica gel according to claim 1, it is characterised in that: the organic solvent is selected from N,
N-dimethylformamide, N, N dimethyl acetamide, tetrahydrofuran, methyltetrahydrofuran, n-methyl-2-pyrrolidone, N- ethyl-
One or more of 2-Pyrrolidone, dimethyl sulfoxide.
6. a kind of YASI organic imides silica gel according to claim 1, it is characterised in that: the organic solvent with react
The mass ratio of object is 2.5-9.5:1；Wherein, reactant refers to bis- (2,4- diamino phenoxy) the benzene 13BDAPB of 1,3-, both-end ammonia
Propyl polydimethylsiloxone YASI, maleic anhydride, aromatic diamine, aromatic dicarboxylic acid anhydride and 3- aminopropyl tri-alkoxy
Silane.
7. a kind of acid imide organic silica gel according to claim 1, it is characterised in that: the both-end aminopropyl poly diformazan
The molecular structural formula of radical siloxane YASI are as follows:
Wherein, m is and the natural number less than 15 greater than 1.
8. a kind of preparation method of YASI organic imides silica gel as described in claim 1, includes the following steps:
According to the ratio, bis- (2,4- diamino phenoxy) the benzene 13BDAPB of 1,3- and organic solvent are put into reaction kettle, are stirred at room temperature
After mixing dissolution, maleic anhydride is added, reacts 15min-30min after stirring and dissolving at room temperature, both-end aminopropyl poly is then added
Dimethyl siloxane YASI, aromatic diamine after stirring and dissolving, are added aromatic dicarboxylic acid anhydride, it is small to be stirred to react 1.0 at room temperature
When -4.0 hours after, be added 3- aminopropyltrialkoxysilane, being stirred to react at room temperature -2 hours 0.5 hour has to get YASI
Machine acid imide silica gel.
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