CN107722551B - A kind of toughening type pentaerythrite acrolein resin and preparation method thereof - Google Patents
A kind of toughening type pentaerythrite acrolein resin and preparation method thereof Download PDFInfo
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- CN107722551B CN107722551B CN201711044571.5A CN201711044571A CN107722551B CN 107722551 B CN107722551 B CN 107722551B CN 201711044571 A CN201711044571 A CN 201711044571A CN 107722551 B CN107722551 B CN 107722551B
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- 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
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/05—Alcohols; Metal alcoholates
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Abstract
The invention discloses a kind of toughening type pentaerythrite acrolein resins, are prepared by following components according to parts by weight: pentaerythrite acrolein resin: 75~95 parts, toughener: 5~25 parts, catalytic curing agent: 3~5 parts.The present invention also provides the preparation methods of toughening type pentaerythrite acrolein resin.Compared with prior art, the present invention carries out resin modified and the specific preparation process of selection by the way that low-molecular material benzyl alcohol is added, the mechanical property of pentaerythrite acrolein resin can be significantly improved, the toughness of especially resin increases substantially, so that pentaerythrite acrolein resin can adapt to more violent high and low temperature environment impact.
Description
Technical field
The present invention relates to polymeric material fields, and in particular to a kind of toughening type pentaerythrite acrolein resin and its preparation
Method.
Background technique
Pentaerythrite acrolein resin is the multiple groups part pre-polymer mixture being polymerized by pentaerythrite and methacrylaldehyde, season
Combination can generate different products to penta tetrol in different proportions from methacrylaldehyde, such as a methacrylaldehyde pentaerythrite, two methacrylaldehyde seasons
Penta tetrol etc..In pentaerythrite acrolein resin system contain polyhydroxy and alkenyl, can heat in presence of an acid catalyst or with it is more
Hydroxy compounds reaction is cured as a kind of highly transparent and has good mechanical property, heat resistance, chemical proof and electricity
The rigid plastics of performance.The solidified resin is widely used as surface coating, adhesive, electrical device pouring sealant and moulding article etc..
However, the reaction that intersects of inner part subchain forms three-dimensional network to pentaerythrite acrolein resin in the curing process
Structure, so that it has the characteristics that intensity is high, physical and chemical performance is stable, but the problem of exist simultaneously poor toughness, to limit
The application range of the resin.Therefore the toughness for improving pentaerythrite acrolein resin also becomes colleague both at home and abroad and closes for a long time
The hot spot of the heart.It is less for the research report in terms of pentaerythrite acrolein resin toughening at present.
Summary of the invention
For the toughness for improving pentaerythrite acrolein resin, expand its application range, the present invention provides a kind of effective toughening
The method of pentaerythrite acrolein resin.Had using pentaerythrite acrolein resin material prepared by method of the invention higher
Toughness, in the curing process and solidification laggard trip temperature mutation impact is not in crackle.
To achieve the above object, The technical solution adopted by the invention is as follows:
A kind of toughening type pentaerythrite acrolein resin, is prepared by following components according to parts by weight:
Pentaerythrite acrolein resin: 75~95 parts, toughener: 5~25 parts, catalytic curing agent: 3~5 parts.
Further technical solution is:
The pentaerythrite acrolein resin polymerize the pre- of generation with methacrylaldehyde for pentaerythrite under acid catalysis
Aggressiveness, molecular weight are 300~500；
The toughener is benzyl alcohol；
The catalytic curing agent is dithyl sulfate.
The present invention also provides the preparation methods of toughening type pentaerythrite acrolein resin, mainly comprise the steps that
(1) pretreatment of pentaerythrite acrolein resin: resin is placed in 40 DEG C~50 DEG C baking ovens preheats first, later
200 mesh screens are crossed to remove bulky grain aggregation, resin is then handled into 30min or more under vacuum conditions, vacuum degree≤-
0.090MPa, temperature is 50 DEG C~60 DEG C, so that wherein small molecule component is removed, it is spare；
(2) catalytic curing agent removes water process: catalytic curing agent is handled 30min or more, vacuum degree under vacuum conditions
≤ -0.090Mpa, temperature are 50 DEG C~60 DEG C, spare to remove wherein hydrone.
(3) ingredient: the pretreated resin is weighed in proportion, water removal treated catalytic curing agent and toughening
Agent is poured into mold after mixing evenly；
(4) it is vacuum-treated: the mold equipped with resin system is placed in processing 30min or more, vacuum degree under vacuum condition
≤ -0.090Mpa, temperature is 40 DEG C~60 DEG C, to remove air and low-molecular material therein；
(5) it is heating and curing: the sample after vacuum processing being put into 70 ± 2 DEG C of insulating box, heat 5h~8h, resin is handed over
Join curing molding.
The present invention prepares the pentaerythrite third modified based on addition low-molecular material by selecting benzyl alcohol as toughener
Olefine aldehydr resin, the mechanical property that can be effectively improved pentaerythrite acrolein resin improve its toughness；
Resin and catalytic curing agent are pre-processed using vacuum condition, low-molecular material therein is removed, original can be improved
The effective component of material；
Mixed resin system is handled using vacuum condition, it can be ensured that cured product processability is good, populated, no gas
In addition the density of cured product can be improved in hole.
Compared with prior art, the present invention carries out resin modified and the specific system of selection by the way that low-molecular material benzyl alcohol is added
Standby technique, the toughness that can significantly improve the mechanical property of pentaerythrite acrolein resin, especially resin increase substantially, thus
So that pentaerythrite acrolein resin can adapt to more violent high and low temperature environment impact.
Detailed description of the invention
Fig. 1 is pentaerythrite acrolein resin cured product figure.
Fig. 2 is different formulations component material viscosity change curve.
Specific embodiment
In order to be more clear the objectives, technical solutions, and advantages of the present invention, the present invention is done in detail below with reference to embodiment
Thin description.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not intended to limit the present invention.
Embodiment 1
A kind of toughening type pentaerythrite acrolein resin, formula composition are as follows: pentaerythrite acrolein resin: 91 parts, benzene
Methanol: 9 parts, dithyl sulfate: 4.5 parts.
The toughening type pentaerythrite acrolein resin preparation mainly comprises the steps that
(1) resin: being placed in 50 DEG C of baking ovens preheat first by the pretreatment of pentaerythrite acrolein resin, crosses 200 later
Then resin is handled 30min or more to remove bulky grain aggregation by mesh screen under vacuum conditions, and vacuum degree≤-
0.090Mpa, temperature is 50 DEG C, so that wherein small molecule component is removed, it is spare；
(2) catalytic curing agent removes water process: catalytic curing agent is handled 30min or more, vacuum degree under vacuum conditions
≤ -0.090Mpa, temperature are 50 DEG C, spare to remove wherein hydrone.
(3) ingredient: the pretreated resin is weighed in proportion, water removal treated catalytic curing agent and toughening
Agent is poured into mold after mixing evenly；
(4) it is vacuum-treated: the mold equipped with resin system is placed in processing 30min or more, vacuum degree under vacuum condition
≤ -0.090Mpa, temperature is 55 DEG C, to remove air and low-molecular material therein；
(5) it is heating and curing: the sample after vacuum processing being put into 70 DEG C of insulating box, heat 6h, resin crosslinking curing
Molding, such as Fig. 1.
The indices of gained toughening type pentaerythrite acrolein resin are as follows:
(1) material viscosity variation such as Fig. 2, initial viscosity are 106 centipoises, and viscosity is respectively after solidification 0.5h, 1.5h, 1.8h
110 centipoises, 1364 centipoises, 13382 centipoises；
(2) mechanical property: tensile strength 56.50MPa, fracture elongation 5.12%；
(3) -40~70 DEG C of film process of temperature jump impact, appearance flawless, chip off-falling.
Embodiment 2
A kind of toughening type pentaerythrite acrolein resin, formula composition are as follows: pentaerythrite acrolein resin: 87 parts, benzene
Methanol: 13 parts, dithyl sulfate: 4.4 parts.
The preparation method is the same as that of Example 1.
Gained cured product indices are as follows:
(1) material viscosity variation such as Fig. 2, initial viscosity are 74 centipoises, are sticked after solidification 0.5h, 1h, 1.5h, 1.8h, 1.9h
Degree is respectively 96 centipoises, 162 centipoises, 1002 centipoises, 8964 centipoises, 31325 centipoises；
(2) mechanical property: tensile strength 14.82MPa, fracture elongation 32.51%；
(3) -40~70 DEG C of film process of temperature jump impact, appearance flawless, chip off-falling.
Embodiment 3
A kind of toughening type pentaerythrite acrolein resin, formula composition are as follows: pentaerythrite acrolein resin: 83 parts, benzene
Methanol: 17 parts, dithyl sulfate: 4.2 parts.
The preparation method is the same as that of Example 1.
Gained cured product indices are as follows:
(1) material viscosity variation such as Fig. 2, initial viscosity are 70 centipoises, viscosity after solidification 0.5h, 1h, 1.5h, 2h, 2.3h
Respectively 88 centipoises, 106 centipoises, 376 centipoises, 3131 centipoises, 31500 centipoises；
(2) mechanical property: tensile strength 4.11MPa, fracture elongation 63.17%；
(3) -40~70 DEG C of film process of temperature jump impact, appearance flawless, chip off-falling.
Embodiment 4
A kind of toughening type pentaerythrite acrolein resin, formula composition are as follows: pentaerythrite acrolein resin: 80 parts, benzene
Methanol: 20 parts, dithyl sulfate: 4 parts.
The preparation method is the same as that of Example 1.
Gained cured product indices are as follows:
(1) material viscosity variation such as Fig. 2, initial viscosity is 38 centipoises, after solidifying 0.5h, 1h, 1.5h, 2h, 2.3h, 2.5h
Viscosity is respectively 40 centipoises, 56 centipoises, 156 centipoises, 836 centipoises, 4167 centipoises, 16600 centipoises；
(2) mechanical property: tensile strength 1.86MPa, fracture elongation 84.65%；
(3) -40~70 DEG C of film process of temperature jump impact, appearance flawless, chip off-falling.
Although reference be made herein to invention has been described for explanatory embodiment of the invention, and above-described embodiment is only this hair
Bright preferable embodiment, embodiment of the present invention are not limited by the above embodiments, it should be appreciated that those skilled in the art
Member can be designed that a lot of other modification and implementations, these modifications and implementations will fall in principle disclosed in the present application
Within scope and spirit.
Claims (2)
1. a kind of toughening type pentaerythrite acrolein resin, it is characterised in that: by following components preparation according to parts by weight
At:
Pentaerythrite acrolein resin: 75~95 parts, toughener: 5~25 parts, catalytic curing agent: 3~5 parts；
The pentaerythrite acrolein resin is the performed polymer that pentaerythrite polymerize generation with methacrylaldehyde under acid catalysis,
Molecular weight is 300~500, and the toughener is benzyl alcohol, and the catalytic curing agent is dithyl sulfate.
2. the preparation method of toughening type pentaerythrite acrolein resin described in claim 1, it is characterised in that the following steps are included:
(1) pretreatment of pentaerythrite acrolein resin: resin is placed in 40 DEG C~50 DEG C baking ovens preheats first, later mistake
Then resin is handled 30min or more to remove bulky grain aggregation by 200 mesh screens under vacuum conditions, and vacuum degree≤-
0.090MPa, temperature is 50 DEG C~60 DEG C, so that wherein small molecule component is removed, it is spare；
(2) catalytic curing agent removes water process: catalytic curing agent is handled into 30min or more under vacuum conditions, vacuum degree≤-
0.090MP a, temperature are 50 DEG C~60 DEG C, spare to remove wherein hydrone；
(3) ingredient: weighing the pretreated resin, water removal treated catalytic curing agent and toughener in proportion,
It pours into mold after mixing evenly；
(4) it is vacuum-treated: the mold equipped with resin system being placed under vacuum condition and handles 30min or more, vacuum degree≤-
0.090MP a, temperature is 40 DEG C~60 DEG C, to remove air and low-molecular material therein；
(5) it is heating and curing: the sample after vacuum processing being put into 70 ± 2 DEG C of insulating box, heat 5h~8h, resin crosslinking is solid
Chemical conversion type.
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| CN108976472A (en) * | 2018-06-07 | 2018-12-11 | 中国工程物理研究院化工材料研究所 | The curing method of plasticizer and pentaerythrite acrolein resin |
| CN109485809A (en) * | 2018-11-14 | 2019-03-19 | 中国工程物理研究院化工材料研究所 | Ionic liquid-catalyzed solidification pentaerythrite acrolein resin of one kind and preparation method thereof |
| CN110698797B (en) * | 2019-10-30 | 2022-05-03 | 中国工程物理研究院化工材料研究所 | Preparation method of carboxylated carbon nanotube modified pentaerythritol acrolein resin |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105001591A (en) * | 2015-08-03 | 2015-10-28 | 中国工程物理研究院化工材料研究所 | Ionic liquid toughening type pentaerythritol acrolein resin and curing method thereof |
| CN106977875A (en) * | 2017-04-13 | 2017-07-25 | 中国工程物理研究院化工材料研究所 | A kind of low-temperature catalyzed solidification aldol resin system and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105001591A (en) * | 2015-08-03 | 2015-10-28 | 中国工程物理研究院化工材料研究所 | Ionic liquid toughening type pentaerythritol acrolein resin and curing method thereof |
| CN106977875A (en) * | 2017-04-13 | 2017-07-25 | 中国工程物理研究院化工材料研究所 | A kind of low-temperature catalyzed solidification aldol resin system and preparation method thereof |
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