CN107722551A - 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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- CN107722551A CN107722551A CN201711044571.5A CN201711044571A CN107722551A CN 107722551 A CN107722551 A CN 107722551A CN 201711044571 A CN201711044571 A CN 201711044571A CN 107722551 A CN107722551 A CN 107722551A
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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 resin, it is prepared by the following components counted in parts by weight：Pentaerythrite acrolein resin：75~95 parts, toughener：5~25 parts, catalytic curing agent：3~5 parts.Present invention also offers the preparation method of toughening type pentaerythrite acrolein resin.Compared with prior art, the present invention carries out resin modified and the specific preparation technology of selection by adding low-molecular material phenmethylol, 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 field, and in particular to a kind of toughening type pentaerythrite acrolein resin and its preparation
Method.
Background technology
Pentaerythrite acrolein resin is the more component pre-polymer mixtures 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..Contain polyhydroxy and alkenyl in pentaerythrite acrolein resin system, can heat in presence of an acid catalyst or with it is more
Hydroxy compounds reacts, and 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 inside points subchain forms three-dimensional network to pentaerythrite acrolein resin in the curing process
Structure so that it has the characteristics of intensity is high, physical and chemical performance is stable, but the problem of poor toughness simultaneously be present, so as to limit
The application of the resin.Therefore the toughness for improving pentaerythrite acrolein resin is also closed for a long time as colleague both at home and abroad
The focus of the heart.It is less for the research report in terms of pentaerythrite acrolein resin toughness reinforcing at present.
The content of the invention
To improve the toughness of pentaerythrite acrolein resin, expand its application, the present invention provides a kind of effective toughness reinforcing
The method of pentaerythrite acrolein resin.The pentaerythrite acrolein resin material prepared using the method for the present invention has 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 present invention is as follows：
A kind of toughening type pentaerythrite acrolein resin, is prepared by the following components counted in parts by weight：
Pentaerythrite acrolein resin：75~95 parts, toughener：5~25 parts, catalytic curing agent：3~5 parts.
Further technical scheme is：
Described pentaerythrite acrolein resin is that pentaerythrite polymerize the pre- of generation with methacrylaldehyde under acid catalysis
Aggressiveness, molecular weight are 300~500；
Described toughener is phenmethylol；
Described catalytic curing agent is dithyl sulfate.
Present invention also offers the preparation method of toughening type pentaerythrite acrolein resin, mainly include the following steps that：
(1) pretreatment of pentaerythrite acrolein resin：Resin is placed in 40 DEG C~50 DEG C baking ovens first and preheated, afterwards
200 eye mesh screens are crossed to remove bulky grain aggregation, resin is then handled into more than 30min under vacuum, vacuum≤-
0.090MPa, temperature is 50 DEG C~60 DEG C, standby so as to remove wherein small molecule component；
(2) catalytic curing agent removes water process：Catalytic curing agent is handled into more than 30min, vacuum under vacuum
≤ -0.090Mpa, temperature are 50 DEG C~60 DEG C, standby to remove wherein hydrone.
(3) dispensing：Described pretreated resin is weighed in proportion, except the catalytic curing agent and toughness reinforcing after water process
Agent, poured into after stirring in mould；
(4) application of vacuum：Mould equipped with resin system is positioned over processing more than 30min, vacuum 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：Sample after application of vacuum is put into 70 ± 2 DEG C of insulating box, heats 5h~8h, resin is handed over
Join curing molding.
The present invention prepares the pentaerythrite third being modified based on addition low-molecular material by selecting phenmethylol to be used 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, remove low-molecular material therein, original can be improved
The active ingredient of material；
Mixed resin system is handled using vacuum condition, it can be ensured that cured product processability is good, populated, no gas
Hole, the density of solidified after-product can be improved in addition.
Compared with prior art, the present invention carries out resin modified and the specific system of selection by adding low-molecular material phenmethylol
Standby technique, the mechanical property of pentaerythrite acrolein resin can be significantly improved, the toughness of especially resin increases substantially, so as to
So that pentaerythrite acrolein resin can adapt to more violent high and low temperature environment impact.
Brief description of the drawings
Fig. 1 is pentaerythrite acrolein resin solidified after-product figure.
Fig. 2 is different formulations component material viscosity change curve.
Embodiment
In order that the objects, technical solutions and advantages of the present invention become apparent from, the present invention is done in detail 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, its formula composition are：Pentaerythrite acrolein resin：91 parts, benzene
Methanol：9 parts, dithyl sulfate：4.5 part.
Described toughening type pentaerythrite acrolein resin is prepared and mainly included the following steps that：
(1) pretreatment of pentaerythrite acrolein resin：Resin is placed in 50 DEG C of baking ovens first and preheated, crosses 200 afterwards
Then resin is handled more than 30min by eye mesh screen under vacuum to remove bulky grain aggregation, and vacuum≤-
0.090Mpa, temperature is 50 DEG C, standby so as to remove wherein small molecule component；
(2) catalytic curing agent removes water process：Catalytic curing agent is handled into more than 30min, vacuum under vacuum
≤ -0.090Mpa, temperature are 50 DEG C, standby to remove wherein hydrone.
(3) dispensing：Described pretreated resin is weighed in proportion, except the catalytic curing agent and toughness reinforcing after water process
Agent, poured into after stirring in mould；
(4) application of vacuum：Mould equipped with resin system is positioned over processing more than 30min, vacuum under vacuum condition
≤ -0.090Mpa, temperature is 55 DEG C, to remove air and low-molecular material therein；
(5) it is heating and curing：Sample after application of vacuum is put into 70 DEG C of insulating box, heats 6h, resin crosslinks solidification
Shaping, such as Fig. 1.
The indices of gained toughening type pentaerythrite acrolein resin are as follows：
(1) material viscosity change such as Fig. 2, initial viscosity is 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) the temperature jump impact of -40~70 DEG C of film process, outward appearance flawless, chip off-falling.
Embodiment 2
A kind of toughening type pentaerythrite acrolein resin, its formula composition are：Pentaerythrite acrolein resin：87 parts, benzene
Methanol：13 parts, dithyl sulfate：4.4 part.
Preparation method is the same as embodiment 1.
Gained cured product indices are as follows：
(1) material viscosity change such as Fig. 2, initial viscosity is 74 centipoises, is 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) the temperature jump impact of -40~70 DEG C of film process, outward appearance flawless, chip off-falling.
Embodiment 3
A kind of toughening type pentaerythrite acrolein resin, its formula composition are：Pentaerythrite acrolein resin：83 parts, benzene
Methanol：17 parts, dithyl sulfate：4.2 part.
Preparation method is the same as embodiment 1.
Gained cured product indices are as follows：
(1) material viscosity change such as Fig. 2, initial viscosity is 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) the temperature jump impact of -40~70 DEG C of film process, outward appearance flawless, chip off-falling.
Embodiment 4
A kind of toughening type pentaerythrite acrolein resin, its formula composition are：Pentaerythrite acrolein resin：80 parts, benzene
Methanol：20 parts, dithyl sulfate：4 parts.
Preparation method is the same as embodiment 1.
Gained cured product indices are as follows：
(1) material viscosity change such as Fig. 2, initial viscosity is 38 centipoises, after solidification 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) the temperature jump impact of -40~70 DEG C of film process, outward 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, embodiments of the present invention are simultaneously not restricted to the described embodiments, it should be appreciated that people in the art
Member can be designed that a lot of other modifications and embodiment, and these modifications and embodiment will fall in principle disclosed in the present application
Within scope and spirit.
Claims (5)
- A kind of 1. toughening type pentaerythrite acrolein resin, it is characterised in that：Prepared by the following components counted in parts by weight and Into：Pentaerythrite acrolein resin：75~95 parts, toughener：5~25 parts, catalytic curing agent：3~5 parts.
- 2. toughening type pentaerythrite acrolein resin according to claim 1, it is characterised in that：Described pentaerythrite acrolein resin is the performed polymer that pentaerythrite polymerize generation with methacrylaldehyde under acid catalysis, Molecular weight is 300~500.
- 3. toughening type pentaerythrite acrolein resin according to claim 1, it is characterised in that：Described toughener is phenmethylol.
- 4. toughening type pentaerythrite acrolein resin according to claim 1, it is characterised in that：Described catalytic curing agent is dithyl sulfate.
- 5. the preparation method of toughening type pentaerythrite acrolein resin, its feature exist described in Claims 1-4 any claim In comprising the following steps：(1) pretreatment of pentaerythrite acrolein resin：Resin is placed in 40 DEG C~50 DEG C baking ovens first and preheated, afterwards mistake Then resin is handled more than 30min by 200 eye mesh screens under vacuum to remove bulky grain aggregation, and vacuum≤- 0.090MPa, temperature is 50 DEG C~60 DEG C, standby so as to remove wherein small molecule component；(2) catalytic curing agent removes water process：Catalytic curing agent is handled into more than 30min under vacuum, vacuum≤- 0.090Mpa, temperature are 50 DEG C~60 DEG C, standby to remove wherein hydrone.(3) dispensing：Described pretreated resin is weighed in proportion, except the catalytic curing agent and toughener after water process, Poured into after stirring in mould；(4) application of vacuum：Mould equipped with resin system is positioned under vacuum condition and handles more than 30min, vacuum≤- 0.090Mpa, temperature is 40 DEG C~60 DEG C, to remove air and low-molecular material therein；(5) it is heating and curing：Sample after application of vacuum is put into 70 ± 2 DEG C of insulating box, heats 5h~8h, resin crosslinks are solid Chemical conversion type.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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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 |
| CN110698797A (en) * | 2019-10-30 | 2020-01-17 | 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 |
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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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| 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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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN110698797A (en) * | 2019-10-30 | 2020-01-17 | 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 |
| 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 |
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