CN107118507A - Nanometer toughening type pentaerythrite acrolein resin and preparation method thereof - Google Patents
Nanometer toughening type pentaerythrite acrolein resin and preparation method thereof Download PDFInfo
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- CN107118507A CN107118507A CN201710461546.0A CN201710461546A CN107118507A CN 107118507 A CN107118507 A CN 107118507A CN 201710461546 A CN201710461546 A CN 201710461546A CN 107118507 A CN107118507 A CN 107118507A
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- acrolein resin
- pentaerythrite acrolein
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L61/00—Compositions of condensation polymers of aldehydes or ketones; Compositions of derivatives of such polymers
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C39/00—Shaping by casting, i.e. introducing the moulding material into a mould or between confining surfaces without significant moulding pressure; Apparatus therefor
- B29C39/22—Component parts, details or accessories; Auxiliary operations
- B29C39/38—Heating or cooling
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C39/00—Shaping by casting, i.e. introducing the moulding material into a mould or between confining surfaces without significant moulding pressure; Apparatus therefor
- B29C39/22—Component parts, details or accessories; Auxiliary operations
- B29C39/42—Casting under special conditions, e.g. vacuum
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- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Casting Or Compression Moulding Of Plastics Or The Like (AREA)
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Abstract
The invention discloses the preparation method of a kind of nanometer of toughening type pentaerythrite acrolein resin, comprise the following steps：Dispensing；Surfactant it is scattered；Nano-rubber particle it is scattered；The immersion fluid and pentaerythrite acrolein resin of nano-rubber and surfactant are heated to 45~50 DEG C, then both are well mixed, catalyst is subsequently added into and is well mixed, and constant temperature obtains mixed material to 45~50 DEG C；Moulding by casting is carried out to mixed material using vacuum casting device, it is 48~50 DEG C to control mixed material temperature, and vacuum≤- 0.092MPa, the mould needed for shaping is preheated to 43~48 DEG C；It is heating and curing and has obtained described nanometer toughening type pentaerythrite acrolein resin.The present invention is significantly improved by using the toughness of pentaerythrite acrolein resin obtained by the toughness reinforcing pentaerythrite acrolein resin of nanometer fluororubber 23 14, and the higher intensity of holding pentaerythrite acrolein resin while toughness is improved.
Description
Technical field
The invention belongs to polymeric material field, and in particular to a kind of nanometer toughening type pentaerythrite acrolein resin and its
Preparation method.
Background technology
Pentaerythrite acrolein resin is a kind of common thermosetting resin, and it has big intensity height, density, physics and change
Learn the good advantage of stability.Current pentaerythrite acrolein resin is widely used in the army and the people's production every field, and it can make
For surface corrosion-resistant erosion resisting coating, insulating materials, high-strength die etc., also can as solid rocket propellant and composite explosives bonding
Agent.The interior molecules chain of pentaerythrite acrolein resin imparts its intensity height, physical chemistry in network structure, the structure is intersected
The characteristics of performance is stable, but there is rigidity and cross the problem of high tenacity is not enough in the structure, because toughness deficiency limits Ji Wusi
Application of the alcohol acrolein resin in wide range of areas.Therefore the toughness for improving pentaerythrite acrolein resin for a long time is domestic
The focus that outer colleague is concerned about.
In recent years, the report using nano-rubber particulate reinforcement macromolecule resin is more and more, is matched from matrix resin
Preferable nano-rubber particulate reinforcement macromolecule resin can not reduced while resin toughness is significantly improved its viscosity so as to
Its processing characteristics is not influenceed.There is not been reported for the current method using nanometer toughening technology modification pentaerythrite acrolein resin.
The invention provides a kind of nanometer toughening type pentaerythrite acrolein resin and preparation method thereof, this method can significantly improve season
The toughness of penta tetrol acrolein resin.
The content of the invention
It is an object of the invention to provide a kind of preferable pentaerythrite acrolein resin of toughness, national defence and civil area are met
Requirement to its performance.
It is yet another object of the invention to provide a kind of preparation method of the preferable pentaerythrite acrolein resin of toughness.
In order to reach above-mentioned technique effect, the present invention takes following technical scheme：
The preparation method of a kind of nanometer of toughening type pentaerythrite acrolein resin, comprises the following steps：
Step A：Dispensing：Raw material is weighed according to following mass fractions：Pentaerythrite acrolein resin：85~88 parts, nanometer
Rubber grain：11~14 parts, catalyst：1.7~2.2 parts, 0.015 part of surfactant；
Step B：Surfactant it is scattered：Surfactant is dissolved in diethyl phthalate at room temperature and stirred
Mix uniform, obtain surfactant solution；
Step C：Nano-rubber particle it is scattered：Nano-rubber particle surfactant solution is infiltrated and stirred
It is even, obtain the immersion fluid of nano-rubber and surfactant；
Step D：The immersion fluid and pentaerythrite acrolein resin of nano-rubber and surfactant are heated to 45~50
DEG C, then both are well mixed, catalyst is subsequently added into and is well mixed, and constant temperature obtains mixed material to 45~50 DEG C；
Step E：Moulding by casting is carried out to mixed material using vacuum casting device, it is 48~50 to control mixed material temperature
DEG C, vacuum≤- 0.092MPa, the mould needed for shaping is preheated to 43~48 DEG C；
Step F：It is heating and curing：Mould after moulding by casting is placed in 5~8h of heating at 50~55 DEG C of temperature, then slowly
Room temperature is cooled to, it is to have obtained described nanometer toughening type pentaerythrite acrolein resin then to mold, clear up.
Further technical scheme is that described pentaerythrite acrolein resin have passed through following processing：By Ji Wusi
Alcohol acrolein resin is preheated to 48~53 DEG C, then crosses 80 mesh sieves；Then the stir process 1h under vacuum≤- 0.090MPa.
Further technical scheme is that described nano particle is fluororubber 23 14, and its average grain diameter is 60~80nm.
Further technical scheme is that described surfactant is soybean lecithin.
Further technical scheme is that described catalyst is dithyl sulfate.
Present invention also offers the nanometer that the preparation method of described nanometer toughening type pentaerythrite acrolein resin is obtained
Toughening type pentaerythrite acrolein resin.
The present invention will be further explained below.
By to pentaerythrite acrolein resin preheat sieving and degassing process can effectively remove the degree of cross linking therein compared with
High particle and bubble therein, improves the quality of molding part.
The present invention is by selecting nanometer fluororubber 23 14 as the toughening material of pentaerythrite acrolein resin, one side fluorine
Rubber grain can form ideal interface with pentaerythrite acrolein resin, can form larger interface therebetween and make
Firmly so that the addition of fluorubber particle does not influence the tensile strength of resin.On the other hand, fluorubber particle has suitable viscous
Elasticity, it can produce stress concentration effect in pentaerythrite acrolein resin, trigger particle surrounding resin matrix yielding, from
And substantial amounts of deformation energy is absorbed, the toughness of material is significantly increased.Simultaneous selection particle diameter is 60~80nm fluorubber particle, and it has
There is suitable specific surface area, particle of particle diameter, which is added, in this will not cause the viscosity of pentaerythrite acrolein resin performed polymer to increase,
So as to not interfere with the machine-shaping property of resin.
Surfactant is dissolved in diethyl phthalate, then infiltrates decentralized processing, Neng Gouti with nano-rubber particle
High nano-rubber particle and mixing uniformity of the surfactant in resin.
Moulding by casting is carried out to mixed material using vacuum casting device, can avoid producing bubble in forming process, carry
High Forming Quality.
Curing molding is carried out at 50~55 DEG C of temperature using constant temperature, can prevent nano-rubber particle from producing sedimentation, together
Crosslink density after Shi Tigao shapings.
Surfactant is not that can only select soybean lecithin, but relative other surfaces activating agent, the table of soybean lecithin
Active function best its in face can effectively prevent the reunion in resin of nano particle, make scattered more uniform.
Catalyst is not that can only select dithyl sulfate in the present invention, dithyl sulfate have relatively low catalytic temperature and
Higher catalytic efficiency, selection dithyl sulfate can make resin system that there is the longer technique laundering period to advantageously ensure that cast
The quality of molding process.
The present invention compared with prior art, with following beneficial effect：
The present invention is by using pentaerythrite methacrylaldehyde obtained by the toughness reinforcing pentaerythrite acrolein resin of nanometer fluororubber 23 14
The toughness of resin is significantly improved, and is maintained to while toughness is improved higher strong of pentaerythrite acrolein resin
Degree.
Embodiment
With reference to embodiments of the invention, the invention will be further elaborated.
Embodiment 1：
Dispensing：Raw material is weighed according to following mass fractions：Pentaerythrite acrolein resin：86 parts, nanometer fluororubber 23 14：
12 parts, dithyl sulfate：2 parts, soybean lecithin：0.015 part.Pentaerythrite acrolein resin have passed through following processing：In advance
Then heat cross 80 mesh sieves to 50 DEG C, then the stir process 1h in the case where vacuum is -0.092Mpa.
Surfactant it is scattered：Soybean lecithin is dissolved at room temperature in diethyl phthalate and stirred
It is even, obtain soybean lecithin solution；
Nano-rubber particle it is scattered：By fluororubber 23 14 is with soybean lecithin solution impregnation and stirs, fluorine is obtained
The immersion fluid of rubber and soybean lecithin；
The immersion fluid and pentaerythrite acrolein resin of fluorubber and soybean lecithin are heated to 48 DEG C, then incite somebody to action both
It is well mixed, it is subsequently added into catalyst and is well mixed, and constant temperature obtains mixed material to 45 DEG C；
Moulding by casting is carried out to mixed material using vacuum casting device, it is 48~50 DEG C to control mixed material temperature, very
Reciprocal of duty cycle≤- 0.092MPa, the mould needed for shaping is preheated to 45 DEG C；
It is heating and curing：Mould after moulding by casting is placed at 53 DEG C of temperature and heats 8h, is then slowly cooled to room temperature, so
Molding, clearing up afterwards is to have obtained described nanometer toughening type pentaerythrite acrolein resin.
Every quality index of the nanometer toughening type pentaerythrite acrolein resin of gained is as follows：
(1) material initial viscosity ηα=150 centipoises (25 DEG C)；
(2) actual density ρ=1.321g/cm of 65mm × 15mm × 5mm films3；
(3) mechanical property：Tensile breakage intensity 63.54MPa, compression strength 87.56MPa, fracture elongation 8.8%, glass
75 DEG C of glass temperature；Storage modulus 2686MPa (25 DEG C).
Embodiment 2：
Dispensing：Raw material is weighed according to following mass fractions：Pentaerythrite acrolein resin：87 parts, nanometer fluororubber 23 14：
11.2 parts, dithyl sulfate：1.8 parts, soybean lecithin：0.015 part.Pentaerythrite acrolein resin have passed through following places
Reason：48 DEG C are preheated to, 80 mesh sieves are then crossed, then the stir process 1h in the case where vacuum is -0.092Mpa.
Surfactant it is scattered：Soybean lecithin is dissolved at room temperature in diethyl phthalate and stirred
It is even, obtain soybean lecithin solution；
Nano-rubber particle it is scattered：By fluororubber 23 14 is with soybean lecithin solution impregnation and stirs, fluorine is obtained
The immersion fluid of rubber and soybean lecithin；
The immersion fluid and pentaerythrite acrolein resin of fluorubber and soybean lecithin are heated to 46 DEG C, then incite somebody to action both
It is well mixed, it is subsequently added into catalyst and is well mixed, and constant temperature obtains mixed material to 46 DEG C；
Moulding by casting is carried out to mixed material using vacuum casting device, it is 48~50 DEG C to control mixed material temperature, very
Reciprocal of duty cycle≤- 0.092MPa, the mould needed for shaping is preheated to 46 DEG C；
It is heating and curing：Mould after moulding by casting is placed at 55 DEG C of temperature and heats 7h, is then slowly cooled to room temperature, so
Molding, clearing up afterwards is to have obtained described nanometer toughening type pentaerythrite acrolein resin.
Every quality index of the nanometer toughening type pentaerythrite acrolein resin of gained is as follows：
(1) material initial viscosity ηα=138 centipoises (25 DEG C)；
(2) actual density ρ=1.325g/cm of 65mm × 15mm × 5mm films3；
(3) mechanical property：Tensile breakage intensity 60.86MPa, compression strength 86.54MPa, fracture elongation 9.2%, glass
73 DEG C of glass temperature；Storage modulus 2532MPa (25 DEG C).
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 preferably 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 modification and embodiment, and these modifications and embodiment will fall in principle disclosed in the present application
Within scope and spirit.
Claims (6)
1. the preparation method of a kind of nanometer of toughening type pentaerythrite acrolein resin, it is characterised in that comprise the following steps：
Step A：Dispensing：Raw material is weighed according to following mass fractions：Pentaerythrite acrolein resin：85~88 parts, nano-rubber
Particle：11~14 parts, catalyst：1.7~2.2 parts, 0.015 part of surfactant；
Step B：Surfactant it is scattered：Surfactant is dissolved at room temperature in diethyl phthalate and stirred
It is even, obtain surfactant solution；
Step C：Nano-rubber particle it is scattered：Nano-rubber particle surfactant solution is infiltrated and stirred, is obtained
To the immersion fluid of nano-rubber and surfactant；
Step D：The immersion fluid and pentaerythrite acrolein resin of nano-rubber and surfactant are heated to 45~50 DEG C, so
Both are well mixed afterwards, catalyst is subsequently added into and is well mixed, and constant temperature obtains mixed material to 45~50 DEG C；
Step E：Moulding by casting is carried out to mixed material using vacuum casting device, it is 48~50 DEG C to control mixed material temperature,
Vacuum≤- 0.092MPa, the mould needed for shaping is preheated to 43~48 DEG C；
Step F：It is heating and curing：Mould after moulding by casting is placed in 5~8h of heating at 50~55 DEG C of temperature, then Slow cooling
To room temperature, it is to have obtained described nanometer toughening type pentaerythrite acrolein resin then to mold, clear up.
2. the preparation method of according to claim 1 nanometer of toughening type pentaerythrite acrolein resin, it is characterised in that institute
The pentaerythrite acrolein resin stated have passed through following processing：Pentaerythrite acrolein resin is preheated to 48~53 DEG C, so
80 mesh sieves are crossed afterwards；Then the stir process 1h under vacuum≤- 0.090MPa.
3. the preparation method of according to claim 1 nanometer of toughening type pentaerythrite acrolein resin, it is characterised in that institute
The nano particle stated is fluororubber 23 14, and its average grain diameter is 60~80nm.
4. the preparation method of according to claim 1 nanometer of toughening type pentaerythrite acrolein resin, it is characterised in that institute
The surfactant stated is soybean lecithin.
5. the preparation method of according to claim 1 nanometer of toughening type pentaerythrite acrolein resin, it is characterised in that institute
The catalyst stated is dithyl sulfate.
6. a kind of preparation method of nanometer toughening type pentaerythrite acrolein resin according to any one of Claims 1 to 5
The nanometer toughening type pentaerythrite acrolein resin of acquisition.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710461546.0A CN107118507B (en) | 2017-06-16 | 2017-06-16 | Nanometer toughening type pentaerythrite acrolein resin and preparation method thereof |
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| CN201710461546.0A CN107118507B (en) | 2017-06-16 | 2017-06-16 | Nanometer toughening type pentaerythrite acrolein resin and preparation method thereof |
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| CN107118507B CN107118507B (en) | 2018-12-25 |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1221451A1 (en) * | 2001-01-09 | 2002-07-10 | Mitsui Chemicals, Inc. | Novolak Aralkyl resin, preparation process thereof, and composition containing said resin |
| 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 |
| CN105038656A (en) * | 2015-09-22 | 2015-11-11 | 中国工程物理研究院化工材料研究所 | Room temperature curing bonding system for PBX and preparing method of room temperature curing bonding system |
-
2017
- 2017-06-16 CN CN201710461546.0A patent/CN107118507B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1221451A1 (en) * | 2001-01-09 | 2002-07-10 | Mitsui Chemicals, Inc. | Novolak Aralkyl resin, preparation process thereof, and composition containing said resin |
| CN1252110C (en) * | 2001-01-09 | 2006-04-19 | 三井化学株式会社 | Novolac aralkyl resin, its preparing method and composition containing said resin |
| 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 |
| CN105038656A (en) * | 2015-09-22 | 2015-11-11 | 中国工程物理研究院化工材料研究所 | Room temperature curing bonding system for PBX and preparing method of room temperature curing bonding system |
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| CN107118507B (en) | 2018-12-25 |
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