CN108485592A - A kind of long-term resistance to 300 DEG C of paper honeycombs core bar adhesive and preparation method thereof - Google Patents
A kind of long-term resistance to 300 DEG C of paper honeycombs core bar adhesive and preparation method thereof Download PDFInfo
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- CN108485592A CN108485592A CN201810245105.1A CN201810245105A CN108485592A CN 108485592 A CN108485592 A CN 108485592A CN 201810245105 A CN201810245105 A CN 201810245105A CN 108485592 A CN108485592 A CN 108485592A
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- core bar
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- paper honeycombs
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Classifications
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J179/00—Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen, with or without oxygen, or carbon only, not provided for in groups C09J161/00 - C09J177/00
- C09J179/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
- C09J179/08—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
- C09J179/085—Unsaturated polyimide precursors
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/08—Macromolecular additives
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
Abstract
A kind of long-term resistance to 300 DEG C of paper honeycombs core bar adhesive and preparation method thereof, it is related to a kind of adhesive and preparation method thereof, the purpose of the present invention is to solve in current existing core colloid system do not have that the resin of high Tg, high thermo-oxidative stability can be met simultaneously, lead to problems such as core bar glue 300 DEG C of Long-Term Properties it is poor in addition failure, it is made by mass fraction of matrix resin, cyanate, plasticized modifier, rubber elastomer toughener, inorganic nano-filler and solvent.Rubber elastomer is blended with inorganic nano material, mixed sheet is obtained, is put into solvent and dissolves, matrix resin and plasticized modifier is added, is uniformly dissolved.It can spend solidification at 300 DEG C, room temperature shear strength 18MPa, 300 DEG C of intensity 12MPa, paper honeycomb node strength 5.8N/cm (or material damage), 300 DEG C of degree × 1000h, room temperature shear strength 11MPa, 300 DEG C of shear strength 8MPa of high temperature.
Description
Technical field
The present invention relates to a kind of long-term resistance to 300 DEG C of paper honeycombs core bar adhesive and preparation method thereof.
Background technology
Honeycomb core composite material is a kind of sandwich material using honeycomb sandwich structure, and this structure has lightweight, than strong
The features such as degree is high, specific stiffness is high, and endurance, anti-shake performance are good, and can effectively absorb a series of biographies such as shock loading
Advantage not available for commons material has wide application in automobile making, shipbuilding, engineering damping and explosion protection etc.
Foreground, especially high-performance paper honeycomb, are the light-weighted important materials of high-end equipment, and favor is received in Aeronautics and Astronautics field, at
Develop one of indispensable material for Aeronautics and Astronautics.
Honeycomb core strip adhesive is one of the important materials of honeycomb manufacture, heat resistance, toughness, mechanical property and technique etc.
Aspect performance is the key that the quality of honeycomb manufacture.With the fast development of China's aerospace cause, to refractory honeycomb
Core material demand is also increasing, further urgent (such as high-speed flight of especially resistance to 300 DEG C or more the honeycomb demands being used for a long time
Refractory honeycomb sandwich in the components such as device, radome fairing).And China is resistant to the bee of 300 DEG C of long-time services not yet at present
Nest product does not manufacture matched resistance to 300 DEG C yet and uses core bar glue for a long time therewith.
This is primarily due to not have that the tree of high Tg, high thermo-oxidative stability can be met simultaneously in existing core colloid system
Fat, cause core bar glue 300 DEG C of Long-Term Properties it is poor in addition failure.
Invention content
The purpose of the present invention is to solve can not meet high Tg, high fever simultaneously in current existing core colloid system
The resin of oxidative stability leads to problems such as core bar glue and devise a kind of length 300 DEG C of Long-Term Properties are poor or even failure
Phase resistance to 300 DEG C of paper honeycombs core bar adhesive and preparation method thereof, the core bar glue can meet resistance to 300 DEG C of paper honeycombs manufacture and
The demands such as long-time service.
A kind of long-term resistance to 300 DEG C of paper honeycombs core bar adhesive of the present invention, by quality by 100 parts matrix resin, 10
~20 parts of cyanates, 15~35 parts of plasticized modifiers, 10~20 parts of rubber elastomer toughener, 5~15 parts of inorganic nano-fillers
It is made with 400~480 parts of solvents.
A kind of long-term resistance to 300 DEG C of paper honeycombs core adhesive preparation method of the present invention, concrete operation step are as follows:
One, 100 parts of matrix resin, 10~20 parts of cyanates, 15~35 parts of plasticized modifiers, 10~20 are weighed by quality
Part rubber elastomer toughener, 5~15 parts of inorganic nano-fillers and 400~480 parts of solvents;
Two, that quality is made by mechanical blending with inorganic nano material in rubber elastomer that step 1 is weighed is uniform
Mixed sheet;
Three, under agitation, the mixed sheet obtained by step 2 is put into the solvent that step 1 is weighed, is waited for
After dissolving completely, matrix resin and plasticized modifier are sequentially added, is uniformly dissolved, long-term resistance to 300 DEG C of paper honeycomb cores are made
Bar adhesive.
The action principle of the present invention:
The present invention uses resin based on the polyimides that alkynyl blocks, and dissolves in N-Methyl pyrrolidone or N, N- diformazans
Yl acetamide.
The beneficial effects of the invention are as follows:The modified material temperature resistant grade of existing core bar glue can not meet long-term resistance to 300
DEG C or more paper honeycomb manufacture and requirement.The present invention uses the aromatic diamines containing azepine ring structure, poly- with aromatic dianhydride
Conjunction forms polyimides, compared to data and it is reported in the literature use modifying agent, such as span, cyanate, polyimides compares,
With higher material modulus and rigidity, and the introducing of benzimidazole structure, it forms another in addition to benzo imide ring
One coplanar club shaped structure, improves glass transition temperature and heat resistance, it is surprising that more than more than Tg values,
Due to the holding of rigid structure, still there is high modulus value, modulus to drop in 0.5 order of magnitude, make it have and be more than
The performance of Tg or more, so as to meet 300 DEG C~400 DEG C requirements used.In addition, avoiding introducing in aromatic diamines soft
Property group, to ensure in each repetitive unit to be all made of rigid straight chain again to imide ring from imide ring to benzimidazole
Structure forms rigid segment.Further improve integrally-built high-temperature heat-resistance performance.In addition, using the two of symmetrical structure
Amine can further promote the structural order of material, obtain more preferably high heat resistance.
Secondly, the present invention selects group containing angle rotatable or steric hindrance, as aromatic dianhydride simultaneously, not
Have using including the rigid coplanar structure such as pyromellitic acid anhydride, on the one hand can improve the flexibility of segment, pass through adjusting
Number of repeat unit controls molecular weight, makes it have certain solvent solubility;On the other hand, having by introducing can be with heterogeneous material
Expect that surface group, such as hydroxyl, carboxyl form C=O, S=O, C-F etc. of chamical binding, increase interfacial adhesion, improves viscous
Junctor system continuous heat resistance energy.Compared in the past use other types of resin, the present invention relates to azacyclo- polyimides energy
It is more than 390 DEG C enough to have Tg, realizes the coordination of flexible splicing and 300 DEG C long-term thermal oxidation stability.
The present invention includes following advantageous effect:
After tested, high temperature resistant paper honeycomb core bar glue obtained by the present invention can spend solidification, room temperature shear strength at 300 DEG C
18MPa, 300 DEG C of intensity 12MPa, paper honeycomb (polyimides) node strength 5.8N/cm (or material damage), 300 DEG C of degree ×
1000h, room temperature shear strength 11MPa, 300 DEG C of shear strength 8MPa of high temperature, the paper honeycomb core bar glue can for a long time make at 300 DEG C
With.
Specific implementation mode
Specific implementation mode one:A kind of long-term resistance to 300 DEG C of paper honeycombs core bar adhesive of present embodiment, feature exist
In it by mass fraction by 100 parts of matrix resin, 10~20 parts of cyanates, 15~35 parts of plasticized modifiers, 10~20 portions of rubbers
Glue elastomer toughener, 5~15 parts of inorganic nano-fillers and 400~480 parts of solvents are made.
Specific implementation mode two:The present embodiment is different from the first embodiment in that:Matrix resin seals for acetenyl
The polyimides at end, chemical equation are as follows:
The n is 5~99;The Ar1For or;
The Ar2For
It is other same as the specific embodiment one.
Specific implementation mode three:The present embodiment is different from the first embodiment in that:The cyanate is by phenolic aldehyde
One or more mixing in type cyanate, bisphenol E-type cyanate and tetramethyl bisphenol-f type cyanate are mixed by any ratio.
It is other same as the specific embodiment one.
Specific implementation mode four:The present embodiment is different from the first embodiment in that:The rubber elastomer is by ring
One or more mixtures that oxygroup nitrile rubber closes in solid nbr carboxyl terminal are mixed by any ratio.Other and specific reality
It is identical to apply mode one.
Specific implementation mode five:The present embodiment is different from the first embodiment in that:The inorganic nano-filler by
Aerosil, asbestos powder one or two kinds of mixtures be mixed by any ratio.It is other same as the specific embodiment one.
Specific implementation mode six:The present embodiment is different from the first embodiment in that:The solvent is N- methyl pyrroles
One or both of pyrrolidone and DMAC N,N' dimethyl acetamide are mixed by any ratio.It is other with one phase of specific implementation mode
Together.
Specific implementation mode seven:The present embodiment is different from the first embodiment in that:It is by mass fraction by 100 parts
Matrix resin, 10~15 parts of cyanates, 10~15 parts of rubber elastomer toughener, 5~10 parts of inorganic nano-fillers and 420~
480 parts of solvents are made.It is other same as the specific embodiment one.
Specific implementation mode eight:A kind of preparation method of high temperature resistant paper honeycomb core bar adhesive of present embodiment, specifically
Operating procedure is as follows:
One, 100 parts of matrix resin, 10~20 parts of cyanates, 10~20 parts of rubber elastomers is weighed by mass fraction to increase
Tough dose, 5~15 parts of inorganic nano-fillers and 400~480 parts of solvents;
Two, that quality is made by mechanical blending with inorganic nano material in rubber elastomer that step 1 is weighed is uniform
Mixed sheet;
Three, under agitation, the mixed sheet obtained by step 2 is put into the solvent that step 1 is weighed, is waited for
After dissolving completely, matrix resin and plasticized modifier are sequentially added, is uniformly dissolved, long-term resistance to 300 DEG C of paper honeycomb cores are made
Bar adhesive.
Specific implementation mode nine:Present embodiment is unlike specific implementation mode eight:100 parts are weighed by mass fraction
Matrix resin, 10~15 parts of cyanates, 10~15 parts of rubber elastomer toughener, 5~10 parts of inorganic nano-fillers and 420~
480 parts of solvents.It is other identical as specific implementation mode eight.
Specific implementation mode ten:Present embodiment is unlike specific implementation mode eight:Matrix resin seals for acetenyl
The polyimides at end, chemical equation are as follows:
The n is 5~99;The Ar1For or;
The Ar2For
It is other identical as specific implementation mode eight.
Specific implementation mode 11:Present embodiment is unlike specific implementation mode eight:The cyanate is by phenol
One or more mixing in aldehyde type cyanate, bisphenol E-type cyanate and tetramethyl bisphenol-f type cyanate are mixed by any ratio.
It is other identical as specific implementation mode eight.
Specific implementation mode 12:Present embodiment is unlike specific implementation mode eight:The rubber elastomer by
One or more mixtures that epoxy group nitrile rubber closes in solid nbr carboxyl terminal are mixed by any ratio.It is other with it is specific
Embodiment eight is identical.
Specific implementation mode 13:Present embodiment is unlike specific implementation mode eight:The inorganic nano-filler
It is mixed by any ratio by one or two kinds of mixtures of aerosil, asbestos powder.It is other identical as specific implementation mode eight.
Specific implementation mode 14:Present embodiment is unlike specific implementation mode eight:The solvent is N- methyl
One or both of pyrrolidones and DMAC N,N' dimethyl acetamide are mixed by any ratio.It is other with eight phase of specific implementation mode
Together.
The content of present invention is not limited only to the content of the respective embodiments described above, the group of one of them or several specific implementation modes
Contract sample can also realize the purpose of invention.
Beneficial effects of the present invention are verified using following instance:
Embodiment one:
A kind of high temperature resistant paper honeycomb core adhesive preparation method described in the present embodiment, concrete operation step are as follows:
One, by mass fraction weigh 100 parts matrix resin, 15 parts of cyanates, 15 parts of rubber elastomer toughener, 10 parts
Inorganic nano-filler and 460 parts of solvents;
Two, that quality is made by mechanical blending with inorganic nano material in rubber elastomer that step 1 is weighed is uniform
Mixed sheet;
Three, under agitation, the mixed sheet obtained by step 2 is put into the solvent that step 1 is weighed, is waited for
After dissolving completely, matrix resin and cyanate ester resin are sequentially added, is uniformly dissolved, a kind of high temperature resistant paper honeycomb core bar glue is made
Stick.
The polyimides structure that matrix resin described in the present embodiment is blocked by the acetenyl described in specific embodiment
At;Cyanate is made of Novolac Cyanate Eater Resin and double E type cyanates, the ratio of Novolac Cyanate Eater Resin and double E type cyanates
It is 9:1;Rubber elastomer is that epoxy group nitrile rubber is formed with solid nbr carboxyl terminal, epoxy group nitrile rubber and solid
The ratio of nbr carboxyl terminal is 6:4;Inorganic filler is that aerosil and asbestos powder form, aerosil and stone
Continuous powder ratio is 2:1;Solvent is N-Methyl pyrrolidone.
The present embodiment high temperature resistant paper honeycomb core bar adhesive is tested:
Test method:GB/T 7144-2008 adhesive tensile shear strengths test methods (rigid material-rigid material);
GJB444-1988 adhesive drawing by high temperature method for testing shear strength (metal-metal);GJB130.3-86 is glued aluminium honeycomb core
Child node strength test method.
The high temperature resistant paper honeycomb core bar glue developed can spend solidification at 300 DEG C, and room temperature shear strength 18MPa, 300 DEG C by force
12MPa, paper honeycomb (polyimides) node strength 5.8N/cm (or material damage), 300 DEG C of degree × 1000h are spent, room temperature shearing is strong
11MPa, 300 DEG C of shear strength 8MPa of high temperature are spent, which can be used for a long time at 300 DEG C.
Embodiment two:
A kind of high temperature resistant paper honeycomb core adhesive preparation method described in the present embodiment, concrete operation step are as follows:
Step as in the first embodiment, matrix resin be Degussa P84, other same embodiments one.
Node colloidality obtained by the present embodiment can be:Its room temperature shear strength 17MPa, 300 DEG C of intensity 9MPa, paper honeycomb
(polyimides) node strength 5.0N/cm, 300 DEG C of degree × 1000h, room temperature shear strength 5MPa, 300 DEG C of shear strengths of high temperature
2MPa。
Claims (10)
1. a kind of long-term resistance to 300 DEG C of paper honeycombs core bar adhesive, it is characterised in that it presses mass fraction by 100 parts of main body tree
Fat, 10~20 parts of cyanates, 15~35 parts of plasticized modifiers, 10~20 parts of rubber elastomer toughener, 5~15 parts of inorganic nanos
Filler and 400~480 parts of solvents are made.
2. a kind of long-term resistance to 300 DEG C of paper honeycombs core bar adhesive according to claim 1, it is characterised in that matrix resin
For the polyimides of acetenyl sealing end, chemical equation is as follows:
The n is 5~99;The Ar1For or;
The Ar2For
3. a kind of long-term resistance to 300 DEG C of paper honeycombs core bar adhesive according to claim 1, it is characterised in that the cyanogen
Acid esters is by one or more mixing in Novolac Cyanate Eater Resin, bisphenol E-type cyanate and tetramethyl bisphenol-f type cyanate by arbitrary
Than mixing.
4. a kind of long-term resistance to 300 DEG C of paper honeycombs core bar adhesive according to claim 1, it is characterised in that the rubber
Elastomer closes one or more mixtures in solid nbr carboxyl terminal by epoxy group nitrile rubber and is mixed by any ratio.
5. a kind of long-term resistance to 300 DEG C of paper honeycombs core bar adhesive according to claim 1, it is characterised in that described inorganic
Nano filling is mixed by any ratio by one or two kinds of mixtures of aerosil, asbestos powder.
6. a kind of long-term resistance to 300 DEG C of paper honeycombs core bar adhesive according to claim 1, it is characterised in that the solvent
For being mixed by any ratio for one or both of N-Methyl pyrrolidone and DMAC N,N' dimethyl acetamide.
7. a kind of long-term resistance to 300 DEG C of paper honeycombs core bar adhesive according to claim 1, it is characterised in that it presses quality
Number is by 100 parts of matrix resin, 10~15 parts of cyanates, 10~15 parts of rubber elastomer toughener, 5~10 parts of inorganic nanos
Filler and 420~480 parts of solvents are made.
8. a kind of preparation method of long-term resistance to 300 DEG C of paper honeycombs core bar adhesive, it is characterised in that concrete operation step is as follows:
One, by mass fraction weigh 100 parts matrix resin, 10~20 parts of cyanates, 10~20 parts of rubber elastomer toughener,
5~15 parts of inorganic nano-fillers and 400~480 parts of solvents;
Two, the uniform mixing of quality is made by mechanical blending with inorganic nano material in the rubber elastomer that step 1 is weighed
Film;
Three, under agitation, the mixed sheet obtained by step 2 is put into the solvent that step 1 is weighed, it is to be dissolved
After completely, matrix resin and plasticized modifier are sequentially added, is uniformly dissolved, long-term resistance to 300 DEG C of paper honeycombs core bar glue is made
Stick.
9. a kind of preparation method of long-term resistance to 300 DEG C of paper honeycombs core bar adhesive according to claim 8, feature exist
In the matrix resin, 10~15 parts of cyanates, 10~15 parts of rubber elastomer toughener, 5~10 that weigh 100 parts by mass fraction
Part inorganic nano-filler and 420~480 parts of solvents.
10. a kind of long-term resistance to 300 DEG C of paper honeycombs preparation method of core bar adhesive according to claim 8, feature
It is that matrix resin is the polyimides of acetenyl sealing end, chemical equation is as follows:
The n is 5~99;The Ar1For or;
The Ar2For
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CN111574953A (en) * | 2020-04-30 | 2020-08-25 | 航天材料及工艺研究所 | High-temperature-resistant honeycomb core strip glue, and preparation method and application thereof |
CN111634078A (en) * | 2020-04-30 | 2020-09-08 | 航天材料及工艺研究所 | Ultra-light high-temperature-resistant honeycomb core material and preparation method thereof |
CN112029473A (en) * | 2020-07-23 | 2020-12-04 | 航天材料及工艺研究所 | High-temperature-resistant thin-wall glass cloth honeycomb core strip glue and preparation method and application thereof |
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CN112029473A (en) * | 2020-07-23 | 2020-12-04 | 航天材料及工艺研究所 | High-temperature-resistant thin-wall glass cloth honeycomb core strip glue and preparation method and application thereof |
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