CN107603539A - A kind of thermostable phenolic resin adhesive and preparation method thereof - Google Patents
A kind of thermostable phenolic resin adhesive and preparation method thereof Download PDFInfo
- Publication number
- CN107603539A CN107603539A CN201710730818.2A CN201710730818A CN107603539A CN 107603539 A CN107603539 A CN 107603539A CN 201710730818 A CN201710730818 A CN 201710730818A CN 107603539 A CN107603539 A CN 107603539A
- Authority
- CN
- China
- Prior art keywords
- phenolic resin
- resin adhesive
- parts
- thermostable
- thermostable phenolic
- 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.)
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- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 title claims abstract description 35
- 239000005011 phenolic resin Substances 0.000 title claims abstract description 33
- 229920001568 phenolic resin Polymers 0.000 title claims abstract description 33
- 239000000853 adhesive Substances 0.000 title claims abstract description 23
- 230000001070 adhesive effect Effects 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims description 13
- 239000000463 material Substances 0.000 claims abstract description 14
- 239000002994 raw material Substances 0.000 claims abstract description 9
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910000077 silane Inorganic materials 0.000 claims abstract description 8
- 229920006324 polyoxymethylene Polymers 0.000 claims abstract description 5
- 239000002253 acid Substances 0.000 claims description 12
- 229920001187 thermosetting polymer Polymers 0.000 claims description 7
- 238000002454 metastable transfer emission spectrometry Methods 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- CPUDPFPXCZDNGI-UHFFFAOYSA-N triethoxy(methyl)silane Chemical compound CCO[Si](C)(OCC)OCC CPUDPFPXCZDNGI-UHFFFAOYSA-N 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 3
- 230000004044 response Effects 0.000 claims description 2
- ZXPDYFSTVHQQOI-UHFFFAOYSA-N diethoxysilane Chemical compound CCO[SiH2]OCC ZXPDYFSTVHQQOI-UHFFFAOYSA-N 0.000 claims 2
- 239000004836 Glue Stick Substances 0.000 claims 1
- 230000004580 weight loss Effects 0.000 abstract description 12
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 abstract description 4
- 229910010271 silicon carbide Inorganic materials 0.000 abstract description 4
- 238000002679 ablation Methods 0.000 abstract description 3
- 239000000919 ceramic Substances 0.000 abstract description 2
- 229910052761 rare earth metal Inorganic materials 0.000 abstract description 2
- 150000002910 rare earth metals Chemical class 0.000 abstract description 2
- YYLGKUPAFFKGRQ-UHFFFAOYSA-N dimethyldiethoxysilane Chemical group CCO[Si](C)(C)OCC YYLGKUPAFFKGRQ-UHFFFAOYSA-N 0.000 description 4
- 239000000499 gel Substances 0.000 description 4
- 150000007513 acids Chemical class 0.000 description 3
- 238000007711 solidification Methods 0.000 description 3
- 230000008023 solidification Effects 0.000 description 3
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 238000004026 adhesive bonding Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- -1 phenolic aldehyde Chemical class 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
Landscapes
- Phenolic Resins Or Amino Resins (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention discloses a kind of thermostable phenolic resin adhesive, the adhesive is made by the raw material including following parts by weight：100 parts of phenolic resin；200 300 parts of yittrium oxide collosol and gel；13 18 parts of silane coupler；10 15 parts of polyformaldehyde.The present invention introduces high heat-resisting auxiliary material rare earth material yittrium oxide and organosilicon structures in phenolic resin structure, resistance to elevated temperatures is further lifted, 800 DEG C of thermal weight loss≤12%, 1000 DEG C of thermal weight loss≤20%, yittrium oxide and silicon carbide ceramics structural material are resolved into more than 1200 DEG C, ablation resistance is increased substantially very much, suitable for the bonding between multiple material.
Description
Technical field
The invention belongs to adhesive area, and in particular to a kind of thermostable phenolic resin adhesive and preparation method thereof.
Background technology
A kind of thermosetting phenolic resin oxygen-containing polymers high as Residual carbon are often used as using under extreme condition resistance to
The heat-insulated high polymer material of ablation, it is bonded, has many advantages, such as available for multiple material, can be with high temperature resistant, gluing relay is big, can be real
Existing high temperature rapid link, suitable for military industry fields such as Aero-Space.
The content of the invention
It is an object of the invention to provide more excellent synvaren of a kind of resistance to elevated temperatures and preparation method thereof.
In order to solve the above-mentioned technical problem, the invention provides following technical scheme：
A kind of thermostable phenolic resin adhesive, is made by the raw material including following parts by weight：
Preferably, the phenolic resin is wolframic acid modified thermosetting phenolic resin.
Preferably, the silane coupler is dimethyldiethoxysilane and/or MTES.
Preferably, the silane coupler is by dimethyldiethoxysilane 8-10 parts by weight and MTES
5-8 parts by weight form.
The preparation method of above-mentioned thermostable phenolic resin adhesive, comprises the following steps：
(1) yittrium oxide collosol and gel is mixed with silane coupler, heating response under acid condition；
(2) material that step (1) obtains is mixed with phenolic resin and polyformaldehyde, that is, obtains described high temperature resistance phenolic aldehyde tree
Fat adhesive.
Preferably, the reaction temperature of step (1) is 60-80 DEG C, and reaction in about 4 hours is complete.
The wolframic acid modified thermosetting phenolic resin can by phenol, formaldehyde, wolframic acid by 10: 10: 1 weight ratio in catalyst
The lower reaction of effect obtains.
The present invention introduces high heat-resisting auxiliary material rare earth material yittrium oxide and organosilicon structures in phenolic resin structure, resistance to
High-temperature behavior is further lifted, and 800 DEG C of thermal weight loss≤12%, 1000 DEG C thermal weight loss≤20%, oxidation is resolved into more than 1200 DEG C
Yttrium and silicon carbide ceramics structural material, ablation resistance are increased substantially very much, suitable for the bonding between multiple material.
Embodiment
The preferred embodiments of the present invention are illustrated below, it will be appreciated that preferred embodiment described herein is only used
In the description and interpretation present invention, it is not intended to limit the present invention.
Wolframic acid modified thermosetting phenolic resin used in the present invention can obtain by the following method：
100 grams of phenol, 100 grams of formaldehyde, 2 grams of zinc oxide (as catalyst), 10 grams of wolframic acids are mixed, react 8 at 100 DEG C
After hour, it is evaporated under reduced pressure to 104 DEG C, you can.
Yittrium oxide collosol and gel used is purchased from this promise New Chemical Material science and technology Co., Ltd of Dalian, and valid density is
20wt%.Other raw materials are ordinary commercial products.
Embodiment 1
A kind of thermostable phenolic resin adhesive, raw material proportioning are as follows：
Preparation process：250g yittrium oxide collosol and gels are dipped in 10g dimethyldiethoxysilanes and 6g methyl triethoxies
Silane mixture liquid, stirs, and at acid 60 DEG C of (pH3-3.5) condition, reacts 4h；By obtained material and 100g wolframic acids
Uniformly mixing obtains thermostable phenolic resin adhesive for modified thermosetting phenolic resin and 15g polyformaldehyde powder.
Performance indications (in air ambient)：
After 180 DEG C solidify 2 hours,
800 DEG C of thermal weight losses 9.2%,
1000 DEG C of thermal weight losses 15.1%,
1200 DEG C of heating generation Y2O3And SiC.
Embodiment 2
A kind of thermostable phenolic resin adhesive, raw material proportioning are as follows：
Preparation process is as follows：
300g yittrium oxide collosol and gels are dipped in 9g dimethyldiethoxysilanes and 8g MTESs mix
Liquid, stir, at acid 80 DEG C of (pH3-3.5) condition, react 4h；
Obtained material is uniformly mixed with 100g wolframic acids modified thermosetting phenolic resin and 10g polyformaldehyde powder and obtained
Thermostable phenolic resin adhesive.
Performance indications (air ambient)：
After 180 DEG C of solidification 2h,
800 DEG C of thermal weight losses 9.05%,
1000 DEG C of thermal weight losses 14.2%,
1200 DEG C of heating changes are into Y2O3And SiC.
Embodiment 3
A kind of thermostable phenolic resin adhesive, raw material proportioning are as follows：
Preparation process is same as Example 2.
Performance indications (air ambient)：
After 180 DEG C of solidification 2h,
800 DEG C of thermal weight losses 11.54%,
1000 DEG C of thermal weight losses 17.12%.
Embodiment 4
A kind of thermostable phenolic resin adhesive, raw material proportioning are as follows：
Preparation process is same as Example 2.
Performance indications (air ambient)：
After 180 DEG C of solidification 2h,
800 DEG C of thermal weight losses 11.94%,
1000 DEG C of thermal weight losses 19.13%.
Embodiment 5
A kind of thermostable phenolic resin adhesive, raw material proportioning are as follows：
Preparation process is same as Example 2.
Finally it should be noted that：The preferred embodiments of the present invention are the foregoing is only, are not intended to limit the invention,
Although the present invention is described in detail with reference to the foregoing embodiments, for those skilled in the art, it still may be used
To be modified to the technical scheme described in foregoing embodiments, or equivalent substitution is carried out to which part technical characteristic.
Within the spirit and principles of the invention, any modification, equivalent substitution and improvements made etc., it should be included in the present invention's
Within protection domain.
Claims (7)
1. a kind of thermostable phenolic resin adhesive, is made by the raw material including following parts by weight：
2. thermostable phenolic resin adhesive according to claim 1, it is characterised in that：The phenolic resin changes for wolframic acid
Property thermosetting phenolic resin.
3. thermostable phenolic resin adhesive according to claim 1, it is characterised in that：The silane coupler is diformazan
Base diethoxy silane and/or MTES.
4. thermostable phenolic resin adhesive according to claim 3, it is characterised in that：The silane coupler is by diformazan
Base diethoxy silane 8-10 parts by weight and MTES 5-8 parts by weight composition.
5. the preparation method of thermostable phenolic resin adhesive, comprises the following steps described in claim 1-4：
(1) yittrium oxide collosol and gel is mixed with silane coupler, heating response under acid condition；
(2) material that step (1) obtains is mixed with phenolic resin and polyformaldehyde, that is, obtains described thermostable phenolic resin glue
Stick.
6. the preparation method of thermostable phenolic resin adhesive according to claim 5, it is characterised in that：Step (1) it is anti-
It is 60-80 DEG C to answer temperature.
7. the preparation method of thermostable phenolic resin adhesive according to claim 5, it is characterised in that：Step (1) is in pH
Under=3~3.5, reaction.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710730818.2A CN107603539A (en) | 2017-08-23 | 2017-08-23 | A kind of thermostable phenolic resin adhesive and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710730818.2A CN107603539A (en) | 2017-08-23 | 2017-08-23 | A kind of thermostable phenolic resin adhesive and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107603539A true CN107603539A (en) | 2018-01-19 |
Family
ID=61065822
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710730818.2A Pending CN107603539A (en) | 2017-08-23 | 2017-08-23 | A kind of thermostable phenolic resin adhesive and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107603539A (en) |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4307206A (en) * | 1979-07-10 | 1981-12-22 | Oshika Shinko Co., Ltd. | Urea-formaldehyde resin adhesive |
| CN101792647A (en) * | 2010-03-30 | 2010-08-04 | 黑龙江省科学院石油化学研究院 | Aluminic acid and methyl silicone resin binary modification phenol formaldehyde adhesive and preparation method thereof |
| CN104016676A (en) * | 2013-03-01 | 2014-09-03 | 鹤山市龙腾科技有限公司 | Ultrahigh-temperature far-infrared catalytic radiation ring |
| CN104387074A (en) * | 2011-04-21 | 2015-03-04 | 株式会社普利司通 | Ceramic sintered body and method of manufacturing ceramic sintered body |
| CN104419365A (en) * | 2013-09-04 | 2015-03-18 | 黑龙江工程学院 | Inorganic-organic hybrid high-temperature resistant adhesive for SiC splicing and application method thereof |
| CN104877583A (en) * | 2015-06-16 | 2015-09-02 | 黑龙江省科学院石油化学研究院 | High-temperature-resistant phenolic unsupported structural adhesive film and preparation method thereof |
-
2017
- 2017-08-23 CN CN201710730818.2A patent/CN107603539A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4307206A (en) * | 1979-07-10 | 1981-12-22 | Oshika Shinko Co., Ltd. | Urea-formaldehyde resin adhesive |
| CN101792647A (en) * | 2010-03-30 | 2010-08-04 | 黑龙江省科学院石油化学研究院 | Aluminic acid and methyl silicone resin binary modification phenol formaldehyde adhesive and preparation method thereof |
| CN104387074A (en) * | 2011-04-21 | 2015-03-04 | 株式会社普利司通 | Ceramic sintered body and method of manufacturing ceramic sintered body |
| CN104016676A (en) * | 2013-03-01 | 2014-09-03 | 鹤山市龙腾科技有限公司 | Ultrahigh-temperature far-infrared catalytic radiation ring |
| CN104419365A (en) * | 2013-09-04 | 2015-03-18 | 黑龙江工程学院 | Inorganic-organic hybrid high-temperature resistant adhesive for SiC splicing and application method thereof |
| CN104877583A (en) * | 2015-06-16 | 2015-09-02 | 黑龙江省科学院石油化学研究院 | High-temperature-resistant phenolic unsupported structural adhesive film and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 唐磊 等: "《耐高温隔热材料技术》", 31 July 2013, 国防工业出版社 * |
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| AD01 | Patent right deemed abandoned |
Effective date of abandoning: 20211001 |
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