CN109483782A - Rubbery state resin cast preparation - Google Patents
Rubbery state resin cast preparation Download PDFInfo
- Publication number
- CN109483782A CN109483782A CN201811471034.3A CN201811471034A CN109483782A CN 109483782 A CN109483782 A CN 109483782A CN 201811471034 A CN201811471034 A CN 201811471034A CN 109483782 A CN109483782 A CN 109483782A
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- CN
- China
- Prior art keywords
- resin
- mold
- rubbery state
- temperature
- autoclave
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- 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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Classifications
-
- 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
- B29C39/02—Shaping by casting, i.e. introducing the moulding material into a mould or between confining surfaces without significant moulding pressure; Apparatus therefor for making articles of definite length, i.e. discrete articles
-
- 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
-
- 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
Abstract
The present invention relates to a kind of rubbery state resin cast preparations, belong to the field of production of high molecular material.Bubble is excluded using autoclave high-temperature pressurizing deaeration technology.Specific method is implemented to include mold preparation, resin cast, resin pretreatment, the preparation of autoclave tooling, resin solidification and demoulding.The invention of this method is mainly at a temperature of 45 DEG C, viscosity >=100Pa.s resin system, and the casting resin of preparation is smooth, bubble-free, provides more reliable data, more can really reflect the performance of resin.It solves the sordid problem of rubbery state resin system casting matrix bottom removal of bubbles, has broken the undesirable situation of rubbery state casting resin production effect, this method is equally applicable to middle low viscosity resin system.
Description
Technical field
The present invention relates to the field of production of high molecular material, are a kind of rubbery state casting resin preparation in detail
Method.
Background technique
It is well known that as polymer matrix composites are in the neck such as automobile, ship, rail traffic, new energy, Aeronautics and Astronautics
Domain application deepens continuously, and reisn base material is also continued to develop to high-performance, multi-functional special material direction.Traditional tree
Aliphatic radical body has been unable to meet performance requirement, therefore the introducing of modified component is essential, and the introducing of modified component also can not just be kept away
Exempt from that resin viscosity is caused significantly to increase.At room temperature, the viscosity of Special Resin material is the tens of conventional resins viscosity of material
Times even hundreds of times, normally referred to as rubbery state resin.
The Mechanics Performance Testing of casting resin is the main characterization approach of resin material performance, the performance energy of resin material
No true reflection depends on casting resin exemplar quality.Therefore, the production of casting resin is in resin matrix research and development
One important link.
The difficult point of casting resin production be how de-bubbled, it is traditional and when making rubbery state casting resin
Vacuum defoamation method and evacuation and centrifugal degassing method are not applicable.Vacuum defoamation method easily causes rubbery state resin matrix component split-phase, centrifugation
Then deaeration amount is few and because shearing force increases resin temperature for deaeration, influences resin property.
Summary of the invention
For overcome the deficiencies in the prior art, the present invention provides a kind of rubbery state resin cast preparation, gets rid of pumping
Vacuum causes the conventional method of subnormal ambient bubble removing, and using high temperature and pressure (positive pressure) environment inside autoclave, setting is suitable
Curing process curve, a kind of casting preparation that can really reflect rubbery state resin property is provided.
The technical solution adopted by the present invention to solve the technical problems is: a kind of rubbery state resin cast preparation,
It is characterized by comprising following step:
A. mold prepares:
1) all contact surfaces of die bottom plate and metal die frame and resin are coated release agent by coating release agent.
2) then metal die frame is placed on air guide cloth and goes forward side by side by the laying air guide cloth on smooth, smooth die bottom plate
Row is fixed.
3) ready whole set of die is put into baking oven and is preheated.
B. resin cast:
Rubbery state resin is put into the mold being preheated.
C. resin pre-processes:
The mold that will be filled with rubbery state resin is put into 50 DEG C -140 DEG C of baking oven, is filled up completely rubbery state resin in a mold
And guarantee that resin surface is smooth.
D. autoclave tooling prepares:
Leveling tool mold is placed in autoclave body, and then casting resin mold members are placed in tooling.
E. resin solidification:
Curing process parameter is set on autoclave control panel according to curing process curve, after technological parameter is provided with, is opened
Beginning curing schedule.
F. it demoulds:
The high viscosity resins casting matrix plate being cured is removed from the molds.
The rubbery state resin material is viscosity >=100Pa.s resin system at a temperature of 45 DEG C, and resin system is
One of epoxy resin, phenolic resin, bismaleimide resin, cyanate ester resin, benzoxazine resin etc. are a variety of.
In rubbery state resin cast preparation of the present invention, including mold preparation, resin cast, resin are located in advance
Reason, the preparation of autoclave tooling, resin solidification and demoulding step: the curing process curve are as follows:
1. according to the heating rate β of 0.5 DEG C/min-3 DEG C/min1It is warming up to 60 DEG C -140 DEG C of T1It pressurizes when temperature, pressurization is big
The range of small P is 0.1MPa-9MPa；
2. as the T for being warming up to 70 DEG C -140 DEG C2Pressure release, blowdown step times N >=1 in solidification process are carried out when temperature；
3. the repressurization P MPa after constant temperature 5-90min, and continue constant temperature 5-90min；
4. with the heating rate β of 0.5 DEG C/min-5 DEG C/min size2It is warming up to the T of 80 DEG C of -220 DEG C of ranges3Solidification temperature is laggard
Row solidification 60min-500min.With β2Heating rate heated up and in the cured period, with the pressure of 0.1MPa-9MPa size
Power P pressurizes；
5. according to the rate of temperature fall β of 0.5 DEG C/min-2.5 DEG C/min3Cooling, when being down to autoclave temperature≤60 DEG C, is let out
Pressure.
The invention has the advantages that simple process, de-aeration and solidification process are continuously finished in same equipment, automatically
Change degree is high, and operating method is simple, and the resin cast weight of production is high, lot stability is good, it is possible to provide more reliable number
According to the performance of more true reflection resin.
Detailed description of the invention
Present invention will be further explained below with reference to the attached drawings and examples.
Fig. 1 is curing process curve graph of the invention.
Specific embodiment
Embodiment 1:
One, mold prepares:
1) die bottom plate and metal die frame and all contact surfaces of resin are coated release agent by coating release agent.
2) then metal die frame is placed on air guide cloth and goes forward side by side by the laying air guide cloth on smooth, smooth die bottom plate
Row mold is fixed
3) ready whole set of die is put into 60 DEG C of baking ovens, preheats 15min.
Two, resin cast:
Rubbery state resin is put into the mold being preheated.
Three, resin pre-processes:
The mold that will be filled with rubbery state resin is put into 40min in the baking oven that temperature is 100 DEG C, and resin is filled up completely in a mold simultaneously
And guarantee that resin surface is smooth.
Four, autoclave tooling prepares:
Leveling tool mold is placed in autoclave body, and then casting resin mold members are placed in tooling.
Five, resin solidification:
According to curing process curve, curing process parameter, curing process are set on autoclave control panel are as follows:
Pressurization when being a. warming up to 80 DEG C according to 0.5 DEG C/min heating rate, pressurization size are 0.5 MPa；
B. when being warming up to 85 DEG C of progress pressure releases；
C.85 repressurization after DEG C constant temperature 20min, pressure size 0.5MPa, then 85 DEG C of continuation constant temperature 5min；
D. 170 DEG C are warming up to from 85 DEG C with the heating of 1 DEG C/min heating rate, pressure size 0.5MPa；
E.170 DEG C constant temperature 180min, pressure size 0.5MPa；
F. room temperature is cooled to from 170 DEG C with 2 DEG C/min heating rate, solidification process terminates.When temperature is down to 50 DEG C, pressure release.
Six, it demoulds:
The high viscosity resins casting matrix plate being cured is removed from the molds.
Embodiment 2:
One, mold prepares:
1) die bottom plate and metal die frame and all contact surfaces of resin are coated release agent by coating release agent.
2) then metal die frame is placed on air guide cloth and goes forward side by side by the laying air guide cloth on smooth, smooth die bottom plate
Row mold is fixed
3) ready whole set of die is put into 60 DEG C of baking ovens, preheats 15min.
Two, resin cast:
Rubbery state resin is put into the mold being preheated.
Three, resin pre-processes:
The mold that will be filled with rubbery state resin is put into 40min in the baking oven that temperature is 100 DEG C, and resin is filled up completely in a mold simultaneously
And guarantee that resin surface is smooth.
Four, autoclave tooling prepares:
Leveling tool mold is placed in autoclave body, and then casting resin mold members are placed in tooling.
Five, resin solidification:
According to curing process curve, curing process parameter, curing process are set on autoclave control panel are as follows:
Pressurization when being a. warming up to 80 DEG C according to 1 DEG C/min heating rate, pressurization size are 0.5 MPa；
B. when being warming up to 85 DEG C of progress pressure releases；
C.85 it pressurizes after DEG C constant temperature 10min, pressure size 0.5MPa, then 85 DEG C of continuation constant temperature 15min, pressure release again；
D. 170 DEG C are warming up to from 85 DEG C with the heating of 1 DEG C/min heating rate, the pressurization when temperature rises to 120 DEG C, pressure size is
0.5MPa；
E.170 DEG C constant temperature 180min, pressure size 0.5MPa；
F. room temperature is cooled to from 170 DEG C with 2 DEG C/min heating rate, solidification process terminates.When temperature is down to 50 DEG C, pressure release.
Six, it demoulds:
The high viscosity resins casting matrix plate being cured is removed from the molds.
Embodiment 3:
One, mold prepares:
1) die bottom plate and metal die frame and all contact surfaces of resin are coated release agent by coating release agent.
2) then metal die frame is placed on air guide cloth and goes forward side by side by the laying air guide cloth on smooth, smooth die bottom plate
Row mold is fixed
3) ready whole set of die is put into 60 DEG C of baking ovens, preheats 15min.
Two, resin cast:
Rubbery state resin is put into the mold being preheated.
Three, resin pre-processes:
The mold that will be filled with rubbery state resin is put into 40min in the baking oven that temperature is 100 DEG C, and resin is filled up completely in a mold simultaneously
And guarantee that resin surface is smooth.
Four, autoclave tooling prepares:
Leveling tool mold is placed in autoclave body, and then casting resin mold members are placed in tooling.
Five, resin solidification:
According to curing process curve, curing process parameter, curing process are set on autoclave control panel are as follows:
Pressurization when being a. warming up to 80 DEG C according to 1 DEG C/min heating rate, pressurization size are 0.7 MPa；
B. when being warming up to 85 DEG C of progress pressure releases；
C.85 repressurization after DEG C constant temperature 20min, pressure size 0.7MPa, then 85 DEG C of continuation constant temperature 10min, let out again
Pressure；
D. 170 DEG C are warming up to from 85 DEG C with the heating of 0.5 DEG C/min heating rate, the pressurization when temperature is warming up to 95 DEG C, pressure is big
Small is 0.7MPa；
E.170 DEG C constant temperature 200min, pressure size 0.7MPa；
F. room temperature is cooled to from 170 DEG C with 2 DEG C/min heating rate, solidification process terminates.When temperature is down to 50 DEG C, pressure release.
Six, it demoulds:
The high viscosity resins casting matrix plate being cured is removed from the molds.
Embodiment 4:
One, mold prepares:
1) die bottom plate and metal die frame and all contact surfaces of resin are coated release agent by coating release agent.
2) then metal die frame is placed on air guide cloth and goes forward side by side by the laying air guide cloth on smooth, smooth die bottom plate
Row mold is fixed
3) ready whole set of die is put into 60 DEG C of baking ovens, preheats 15min.
Two, resin cast:
Rubbery state resin is put into the mold being preheated.
Three, resin pre-processes:
The mold that will be filled with rubbery state resin is put into 40min in the baking oven that temperature is 100 DEG C, and resin is filled up completely in a mold simultaneously
And guarantee that resin surface is smooth.
Four, autoclave tooling prepares:
Leveling tool mold is placed in autoclave body, and then casting resin mold members are placed in tooling.
Five, resin solidification:
According to curing process curve, curing process parameter, curing process are set on autoclave control panel are as follows:
Pressurization when being a. warming up to 80 DEG C according to 1 DEG C/min heating rate, pressurization size are 0.7 MPa；
B. when being warming up to 90 DEG C of progress pressure releases；
C.90 repressurization after DEG C constant temperature 30min, pressure size 0.7MPa, then 90 DEG C of continuation constant temperature 10min, let out again
Pressure；
D. 170 DEG C are warming up to from 90 DEG C with the heating of 0.5 DEG C/min heating rate, the pressurization when temperature is warming up to 95 DEG C, pressure is big
Small is 0.7MPa；
E.170 DEG C constant temperature 200min, pressure size 0.7MPa；
F. room temperature is cooled to from 170 DEG C with 2 DEG C/min heating rate, solidification process terminates.When temperature is down to 50 DEG C, pressure release.
Six, it demoulds:
The high viscosity resins casting matrix plate being cured is removed from the molds.
Mainly for the resin system of viscosity >=100Pa.s (45 DEG C of@), the casting resin of preparation is flat for the invention of this method
Whole, bubble-free provides more reliable data, more can really reflect the performance of resin.Solves rubbery state resinite
It is the sordid problem of casting matrix bottom removal of bubbles, has broken the undesirable situation of rubbery state casting resin production effect,
This method is equally applicable to middle low viscosity resin system.
Claims (2)
1. a kind of rubbery state resin cast preparation, which is characterized in that including following consecutive steps:
Mold prepares:
All contact surfaces of die bottom plate and metal die frame and resin are coated into release agent；
Then metal die frame is placed on air guide cloth and carries out mold by the laying air guide cloth on smooth, smooth die bottom plate
It is fixed；
Mold preheating；
Resin cast:
Rubbery state resin is put into the mold being preheated；
Resin pretreatment:
The mold that will be filled with rubbery state resin is put into 50 DEG C -140 DEG C of baking oven, is filled up completely resin in a mold and is protected
It is smooth to demonstrate,prove rubbery state resin surface；
Autoclave tooling prepares:
Leveling tool mold is placed in autoclave body, and then casting matrix mold members are placed in tooling；
Resin solidification:
According to curing process curve, curing process parameter, the pressure process of curing process curve are set on autoclave control panel
Discontinuously, there is blowdown step, blowdown step times N >=1 in solidification process is specifically provided that
According to the heating rate β of 0.5 DEG C/min-3 DEG C/min1It is warming up to 60 DEG C -140 DEG C of T1It pressurizes when temperature, pressurize size P
Range be 0.1MPa-9MPa；
As the T for being warming up to 70 DEG C -140 DEG C2Pressure release, blowdown step number >=1 in solidification process are carried out when temperature；
In T2Repressurization P MPa after constant temperature 5-90min at DEG C, and continue constant temperature 5-90min；
With the heating rate β of 0.5 DEG C/min-5 DEG C/min size2It is warming up to the T of 80 DEG C of -220 DEG C of ranges3It is carried out after solidification temperature
Solidify 60min-500min, with β2Heating rate heated up and in the cured period, with the pressure of 0.1MPa-9MPa size
P pressurizes；
According to the rate of temperature fall β of 0.5 DEG C/min-2.5 DEG C/min3Cooling carries out pressure release when autoclave temperature≤60 DEG C；
Demoulding:
The high viscosity resins casting matrix plate being cured is removed from the molds.
2. rubbery state resin cast preparation according to claim 1, it is characterised in that the rubbery state resinous wood
Material is viscosity >=100Pa.s resin system at a temperature of 45 DEG C, and resin system is epoxy resin, phenolic resin, span tree
One of rouge, cyanate ester resin, benzoxazine resin etc. are a variety of.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811471034.3A CN109483782A (en) | 2018-12-04 | 2018-12-04 | Rubbery state resin cast preparation |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811471034.3A CN109483782A (en) | 2018-12-04 | 2018-12-04 | Rubbery state resin cast preparation |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109483782A true CN109483782A (en) | 2019-03-19 |
Family
ID=65699223
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811471034.3A Pending CN109483782A (en) | 2018-12-04 | 2018-12-04 | Rubbery state resin cast preparation |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2002018120A2 (en) * | 2000-09-01 | 2002-03-07 | Honeywell International Inc. | Rapid densification of porous bodies (preforms) with high viscosity resins or pitches using a resin transfer molding process |
| CN102042443A (en) * | 2010-12-20 | 2011-05-04 | 辽宁康泰塑胶科技有限公司 | Thermoplastic micro foaming injection pipe fitting and preparation method thereof |
| CN103958150A (en) * | 2012-11-09 | 2014-07-30 | 夏普株式会社 | Molding manufacturing equipment and molding manufacturing method |
| CN107984662A (en) * | 2017-12-14 | 2018-05-04 | 威海光威复合材料股份有限公司 | High viscosity formulated resin casting preparation |
| CN108407336A (en) * | 2018-02-24 | 2018-08-17 | 航天特种材料及工艺技术研究所 | A kind of stereo fabric enhancing phenolic resin composite and preparation method |
-
2018
- 2018-12-04 CN CN201811471034.3A patent/CN109483782A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2002018120A2 (en) * | 2000-09-01 | 2002-03-07 | Honeywell International Inc. | Rapid densification of porous bodies (preforms) with high viscosity resins or pitches using a resin transfer molding process |
| CN102042443A (en) * | 2010-12-20 | 2011-05-04 | 辽宁康泰塑胶科技有限公司 | Thermoplastic micro foaming injection pipe fitting and preparation method thereof |
| CN103958150A (en) * | 2012-11-09 | 2014-07-30 | 夏普株式会社 | Molding manufacturing equipment and molding manufacturing method |
| CN107984662A (en) * | 2017-12-14 | 2018-05-04 | 威海光威复合材料股份有限公司 | High viscosity formulated resin casting preparation |
| CN108407336A (en) * | 2018-02-24 | 2018-08-17 | 航天特种材料及工艺技术研究所 | A kind of stereo fabric enhancing phenolic resin composite and preparation method |
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Application publication date: 20190319 |