CN103805116A - Preparation method of polyborosiloxane modified phenol formaldehyde resin (PF) adhesive with high temperature resistance - Google Patents
Preparation method of polyborosiloxane modified phenol formaldehyde resin (PF) adhesive with high temperature resistance Download PDFInfo
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- CN103805116A CN103805116A CN201210446377.0A CN201210446377A CN103805116A CN 103805116 A CN103805116 A CN 103805116A CN 201210446377 A CN201210446377 A CN 201210446377A CN 103805116 A CN103805116 A CN 103805116A
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Abstract
The invention relates to a preparation method of polyborosiloxane modified phenol formaldehyde resin (PF) adhesive with high temperature resistance, belongs to the technical field of chemistry, and particularly relates to the preparation method of the polyborosiloxane modified phenol formaldehyde resin (PF) adhesive with the high temperature resistance. The invention provides the preparation method of the polyborosiloxane modified phenol formaldehyde resin (PF) adhesive with the high temperature resistance, and the polyborosiloxane modified phenol formaldehyde resin (PF) adhesive is high in yield, and good in product performance. The preparation method of the polyborosiloxane modified phenol formaldehyde resin (PF) adhesive with the high temperature resistance is as follows: a silicone prepolymer is prepared by adding synthesized BSi resin into PF (formaldehyde resin), then heating until the BSi resin is melted, stirring for reaction, dewatering in vacuum, and gradually warming up; when the gelation time is 90s-150s, the reaction is stopped, and the resin is rapidly poured on Teflon cloth to obtain light yellow transparent or translucent resin; nitrile-40 rubber mix and the BSiP resin are respectively dissolved in ethyl acetate, and then proportionally mixed, and a proper amount of a combined filler is added, and ground and dispersed uniformly to obtain the adhesive prepared by the preparation method.
Description
Technical field
the invention belongs to technical field of chemistry, in particular, the present invention relates to the preparation method of polyborosiloxane modified phenolic resins high-temperature resistance adhesive.
Background technology
resol (PF) is artificial synthetic resin the earliest, obtains a wide range of applications in various fields.Along with the needs of development, the modification work of Phenol aldehyde resin is subject to people's attention day by day.Its modification work may be summarized to be two aspects.The one, the toughening modifying of resol, to improve its bonding strength, particularly stripping strength; The 2nd, in resol, introducing hetero-atoms is as Si, B, Al, Ti etc., to improve its temperature tolerance.Roughly have and improve the durothermic method of PF Resin adhesive: (1) adopts phenol, the aldehyde of other structure; (2) adopt organosilane-modified; (3) introduce boron atom modified etc.
Summary of the invention
the present invention is exactly for the problems referred to above, provides a kind of productive rate high, the preparation method of the polyborosiloxane modified phenolic resins high-temperature resistance adhesive of good product performance.
for realizing above-mentioned purpose of the present invention, the present invention adopts following technical scheme, and the preparation method of polyborosiloxane modified phenolic resins high-temperature resistance adhesive of the present invention is.
to the phenol, formaldehyde, the zinc oxide that add calculated amount in four-hole bottle, start stirring, temperature reaction gradually, starts vacuum system and deviates from part water, and residual resin retains wherein for subsequent use.The organosilicon preformed polymer of calculated amount and boric acid are added in there-necked flask, start stirring, progressively heat up, temperature reaction insulation after boric acid all dissolves, dehydration, heats up, vacuum, obtain the BSi resin of water white transparency or White-opalescent, organosilicon preformed polymer is that above-mentioned synthetic BSi resin is added in PF, heats up, to the rear stirring reaction of BSi fusing, vacuum hydro-extraction, progressively heats up.In the time that gel time reaches 90s～150 s, stopped reaction, is poured on resin in teflon cloth fast, obtains faint yellow transparent or semitransparent resin.Butyronitrile-40 rubber unvulcanizate and BSiP resin are dissolved in ethyl acetate respectively, then both are mixed in proportion, and add appropriate combined stuffing, grinding distribution is even, is this work institute preparing adhesive.
beneficial effect of the present invention.
this present invention is short reaction time, and reaction conditions gentleness, has productive rate high, when preparation security good a little, have good promotional value.And it is good that the present invention has bonding strength, the advantage of good heat resistance, these are all that existing resol high-temperature resistance adhesive is incomparable.
Embodiment
the preparation method of polyborosiloxane modified phenolic resins high-temperature resistance adhesive of the present invention is.
to the phenol, formaldehyde, the zinc oxide that add calculated amount in four-hole bottle, start stirring, temperature reaction gradually, starts vacuum system and deviates from part water, and residual resin retains wherein for subsequent use.The organosilicon preformed polymer of calculated amount and boric acid are added in there-necked flask, start stirring, progressively heat up, temperature reaction insulation after boric acid all dissolves, dehydration, heats up, vacuum, obtain the BSi resin of water white transparency or White-opalescent, organosilicon preformed polymer is that above-mentioned synthetic BSi resin is added in PF, heats up, to the rear stirring reaction of BSi fusing, vacuum hydro-extraction, progressively heats up.In the time that gel time reaches 90s～150 s, stopped reaction, is poured on resin in teflon cloth fast, obtains faint yellow transparent or semitransparent resin.Butyronitrile-40 rubber unvulcanizate and BSiP resin are dissolved in ethyl acetate respectively, then both are mixed in proportion, and add appropriate combined stuffing, grinding distribution is even, is this work institute preparing adhesive.
embodiment 1.
to the phenol, formaldehyde, the zinc oxide that add calculated amount in four-hole bottle, start stirring, be warming up to gradually 90 ℃, reaction 3 h, start vacuum system and deviate from part water, and residual resin retains wherein for subsequent use.The organosilicon preformed polymer of calculated amount and boric acid are added in there-necked flask, start stirring, be progressively warming up to 70 ℃, after all dissolving, boric acid is warming up to 233 ℃ of reaction 3h, insulation, dehydration, be warming up to 140 ℃, vacuum reaches 99223 Pa, obtains the BSi resin of water white transparency or White-opalescent, organosilicon preformed polymer is that above-mentioned synthetic BSi resin is added in PF, be warming up to 89 ℃, to the rear stirring reaction 2h of BSi fusing, vacuum hydro-extraction, " C, vacuum tightness reaches 99975 Pa to be progressively warmed up to 120.In the time that gel time reaches 90 s～150 s, stopped reaction, is poured on resin in teflon cloth fast, obtains faint yellow transparent or semitransparent resin.Butyronitrile-40 rubber unvulcanizate and BSiP resin are dissolved in ethyl acetate respectively, then both are mixed in proportion, and add appropriate combined stuffing, grinding distribution is even, is this work institute preparing adhesive.
above content is the further description of the present invention being done in conjunction with concrete preferred implementation; can not assert that specific embodiment of the invention is confined to these explanations; for general technical staff of the technical field of the invention; without departing from the inventive concept of the premise; can also make some simple deduction or replace, all should be considered as belonging to the definite protection domain of claims that the present invention submits to.
Claims (2)
1. the preparation method of polyborosiloxane modified phenolic resins high-temperature resistance adhesive, is characterized in that:
To the phenol, formaldehyde, the zinc oxide that add calculated amount in four-hole bottle, start stirring, temperature reaction gradually, starts vacuum system and deviates from part water, and residual resin retains wherein for subsequent use; The organosilicon preformed polymer of calculated amount and boric acid are added in there-necked flask, start stirring, progressively heat up, temperature reaction insulation after boric acid all dissolves, dehydration, heats up, vacuum, obtain the BSi resin of water white transparency or White-opalescent, organosilicon preformed polymer is that above-mentioned synthetic BSi resin is added in PF, heats up, to the rear stirring reaction of BSi fusing, vacuum hydro-extraction, progressively heats up; In the time that gel time reaches 90s～150 s, stopped reaction, is poured on resin in teflon cloth fast, obtains faint yellow transparent or semitransparent resin; Butyronitrile-40 rubber unvulcanizate and BSiP resin are dissolved in ethyl acetate respectively, then both are mixed in proportion, and add appropriate combined stuffing, grinding distribution is even, is this work institute preparing adhesive.
2. the preparation method of polyborosiloxane modified phenolic resins high-temperature resistance adhesive according to claim 1, it is characterized in that: to the phenol, formaldehyde, the zinc oxide that add calculated amount in four-hole bottle, start stirring, be warming up to gradually 90 ℃, react 3 h, start vacuum system and deviate from part water, residual resin retains wherein for subsequent use; The organosilicon preformed polymer of calculated amount and boric acid are added in there-necked flask, start stirring, be progressively warming up to 70 ℃, after all dissolving, boric acid is warming up to 233 ℃ of reaction 3h, insulation, dehydration, be warming up to 140 ℃, vacuum reaches 99223 Pa, obtains the BSi resin of water white transparency or White-opalescent, organosilicon preformed polymer is that above-mentioned synthetic BSi resin is added in PF, be warming up to 89 ℃, to the rear stirring reaction 2h of BSi fusing, vacuum hydro-extraction, progressively be warmed up to 120 " C, vacuum tightness reaches 99975 Pa; In the time that gel time reaches 90 s～150 s, stopped reaction, is poured on resin in teflon cloth fast, obtains faint yellow transparent or semitransparent resin; Butyronitrile-40 rubber unvulcanizate and BSiP resin are dissolved in ethyl acetate respectively, then both are mixed in proportion, and add appropriate combined stuffing, grinding distribution is even, is this work institute preparing adhesive.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210446377.0A CN103805116A (en) | 2012-11-09 | 2012-11-09 | Preparation method of polyborosiloxane modified phenol formaldehyde resin (PF) adhesive with high temperature resistance |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210446377.0A CN103805116A (en) | 2012-11-09 | 2012-11-09 | Preparation method of polyborosiloxane modified phenol formaldehyde resin (PF) adhesive with high temperature resistance |
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| CN103805116A true CN103805116A (en) | 2014-05-21 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201210446377.0A Pending CN103805116A (en) | 2012-11-09 | 2012-11-09 | Preparation method of polyborosiloxane modified phenol formaldehyde resin (PF) adhesive with high temperature resistance |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115181378A (en) * | 2022-08-03 | 2022-10-14 | 福建冠翔日用塑料制品有限公司 | Waterproof high-temperature-resistant PVC plastic and preparation process thereof |
-
2012
- 2012-11-09 CN CN201210446377.0A patent/CN103805116A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115181378A (en) * | 2022-08-03 | 2022-10-14 | 福建冠翔日用塑料制品有限公司 | Waterproof high-temperature-resistant PVC plastic and preparation process thereof |
| CN115181378B (en) * | 2022-08-03 | 2023-09-08 | 福建冠翔日用塑料制品有限公司 | Waterproof high-temperature-resistant PVC plastic and preparation process thereof |
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Application publication date: 20140521 |