CN110815619A - Method for producing epoxy resin-based composite material by using ultrasonic mixing - Google Patents
Method for producing epoxy resin-based composite material by using ultrasonic mixing Download PDFInfo
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- CN110815619A CN110815619A CN201910954495.4A CN201910954495A CN110815619A CN 110815619 A CN110815619 A CN 110815619A CN 201910954495 A CN201910954495 A CN 201910954495A CN 110815619 A CN110815619 A CN 110815619A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B7/00—Mixing; Kneading
- B29B7/02—Mixing; Kneading non-continuous, with mechanical mixing or kneading devices, i.e. batch type
- B29B7/06—Mixing; Kneading non-continuous, with mechanical mixing or kneading devices, i.e. batch type with movable mixing or kneading devices
- B29B7/08—Mixing; Kneading non-continuous, with mechanical mixing or kneading devices, i.e. batch type with movable mixing or kneading devices shaking, oscillating or vibrating
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B7/00—Mixing; Kneading
- B29B7/30—Mixing; Kneading continuous, with mechanical mixing or kneading devices
- B29B7/34—Mixing; Kneading continuous, with mechanical mixing or kneading devices with movable mixing or kneading devices
- B29B7/36—Mixing; Kneading continuous, with mechanical mixing or kneading devices with movable mixing or kneading devices shaking, oscillating or vibrating
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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
- B29C35/00—Heating, cooling or curing, e.g. crosslinking or vulcanising; Apparatus therefor
- B29C35/02—Heating or curing, e.g. crosslinking or vulcanizing during moulding, e.g. in a mould
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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
- C08K5/16—Nitrogen-containing compounds
- C08K5/17—Amines; Quaternary ammonium compounds
- C08K5/175—Amines; Quaternary ammonium compounds containing COOH-groups; Esters or salts thereof
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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
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/06—Elements
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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
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/14—Glass
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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
- C08L2203/00—Applications
- C08L2203/20—Applications use in electrical or conductive gadgets
- C08L2203/206—Applications use in electrical or conductive gadgets use in coating or encapsulating of electronic parts
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Physics & Mathematics (AREA)
- Oral & Maxillofacial Surgery (AREA)
- Thermal Sciences (AREA)
- Epoxy Resins (AREA)
Abstract
The invention discloses a method for producing an epoxy resin-based composite material by using ultrasonic mixing, which relates to the technical field of epoxy resin-based composite materials and comprises the following steps: (1) preparing a resin component, (2) preparing a curing agent component, (3) preparing a composite material, and (4) curing; according to the invention, on one hand, bubbles generated by stirring can be avoided by utilizing ultrasonic waves, the operation step of removing the bubbles from the material in the existing production process is reduced, the curing effect can be further improved by reducing the bubbles, and the vacuum on the surface of the material formed after curing is avoided; on the other hand can also make the material misce bene, guarantees the mixing uniformity of material when shortening compounding time.
Description
The technical field is as follows:
the invention relates to the technical field of epoxy resin-based composite materials, in particular to a method for producing an epoxy resin-based composite material by using ultrasonic mixing.
Background art:
the composite material is a material with new performance formed by two or more than two materials with different properties through a physical or chemical method on a macroscopic (microscopic) scale. The materials mutually make up for the deficiencies in performance to generate a synergistic effect, so that the comprehensive performance of the composite material is superior to that of the original composition material to meet various different requirements.
The history of composite use dates back to the ancient times. Both rice straw or wheat straw reinforced clay, which has been used from ancient times to date, and reinforced concrete, which has been used for centuries, are compounded from two materials. In the 40's of the 20 th century, glass fiber reinforced plastics (commonly known as glass fiber reinforced plastics) were developed due to the needs of the aviation industry, and the name of composite materials has since emerged. Composite materials are classified into resin-based, metal-based and ceramic-based composite materials according to the difference of matrix materials.
The epoxy resin is used as a composite material resin matrix which is developed earliest and applied most widely, has excellent processability and cohesiveness, and has higher strength and modulus after being cured. However, the epoxy resin is easy to generate bubbles in the mixing and stirring process, and the time for removing the bubbles in vacuum is consumed, so that the viscosity of some systems with quick reaction is increased after degassing, and the operable time is shortened; and physical mechanical stirring is easy to form a streaming dead angle, so that the materials are not uniformly mixed, and the strength of the composite material is not uniform.
The invention content is as follows:
the invention aims to solve the technical problem of providing a method for producing an epoxy resin-based composite material by using ultrasonic mixing, and the epoxy resin-based composite material with high construction efficiency and good use effect is prepared by the cooperation of ultrasonic waves, a resin component and a curing agent component.
The technical problem to be solved by the invention is realized by adopting the following technical scheme:
the method for producing the epoxy resin-based composite material by using ultrasonic mixing comprises the following steps:
(1) preparation of the resin component: uniformly mixing 80-90 parts of bisphenol A epoxy resin and 10-20 parts of reactive diluent by using ultrasonic waves to obtain a resin component;
(2) preparation of the curing agent component: uniformly mixing 55-70 parts of polyether amine and 30-45 parts of alicyclic amine by using ultrasonic waves to obtain a curing agent component;
(3) preparing a composite material: uniformly mixing the resin component and the curing agent component according to the proportion of 100:20-50 by using ultrasonic waves to obtain a mixture, taking 30-45 parts of the mixture, and introducing 50-70 parts of fibers in vacuum;
(4) and (3) a curing process: curing at 40 deg.C for 3-5 hr, and curing at 80 deg.C for 2-4 hr.
The ultrasonic wave is generated by an ultrasonic device with the working frequency of 28kHz or 40kHz and the ultrasonic wave power of 600-1800W.
The fibers are carbon fibers or glass fibers. The use performance of the composite material is improved by introducing carbon fiber or glass fiber, and the use amount of resin is reduced.
The operating conditions of the vacuum introduction are as follows: preheating the resin component to 45 ℃, not preheating the curing agent, preheating the mould to 40 ℃, introducing the fiber in vacuum at 40 ℃, and controlling the vacuum degree to be between-0.05 MPa and-0.1 MPa.
The polyether amine is one or more of D-230, D-400, D-2000 and T-403.
The alicyclic amine is one or more of methyl cyclohexanediamine, cyclohexylamine and m-phenylenediamine.
The polyether amine and the alicyclic amine form a composite amine curing agent, and the composite amine curing agent is used for reducing the curing temperature and shortening the curing time.
The reactive diluent is 1, 4-butanediol diglycidyl ether. 1, 4-butanediol diglycidyl ether is used as a reactive diluent, so that the viscosity of a curing system can be reduced, the fluidity can be increased, and the operability can be improved.
In order to make the reactive diluent have the effect of increasing the fluidity of the resin and improve the impact strength of the resin and make the prepared epoxy resin-based composite material have good impact resistance, the invention tries various substances which are not conventional reactive diluents in the field as the reactive diluent in the test process, and unexpectedly finds that the technical effects of increasing the fluidity of the resin and improving the impact strength of the resin can be simultaneously achieved by using the saturated aqueous solution of hydrolyzed polymaleic anhydride, but the hydrolyzed polymaleic anhydride does not belong to the substances which are known in the field and can be used as the reactive diluent. Therefore, the reactive diluent is a saturated aqueous solution of hydrolyzed polymaleic anhydride.
It is obvious to those skilled in the art that foam is inevitably generated when epoxy resin-based composite materials are formulated or constructed, and the generation of foam seriously affects construction efficiency and causes pinholes to be generated on the surface of the materials formed after curing. To solve this problem, the art generally adopts the way of adding an antifoaming agent. Therefore, the resin component of the invention also comprises 0.5-2 parts of defoaming agent.
The defoaming agent is one or a mixture of more of an organic silicon defoaming agent and a polyether defoaming agent.
In order to obtain better defoaming effect, the invention tries to adopt a plurality of substances which are not the conventional defoaming agents in the field as the defoaming agents in the test process, and judges whether the defoaming agents have defoaming effect or not by combining the defoaming effect. The inventor unexpectedly finds that the N < E- (1-carboxymethyl) -L-lysine can obtain the defoaming effect which is obviously better than that of a silicone defoaming agent or a polyether defoaming agent or a composite defoaming agent formed by mixing the silicone defoaming agent and the polyether defoaming agent when being used as the defoaming agent, whereas N Ε - (1-carboxymethyl) -L-lysine does not belong to the class of silicone defoamers or polyether defoamers, and the application of N Ε - (1-carboxymethyl) -L-lysine as an antifoaming agent is not in the prior art and common knowledge in the field, therefore, the invention realizes the new application of taking N < E- (1-carboxymethyl) -L-lysine as the defoaming agent, and obtains good defoaming effect by matching with ultrasonic waves, thereby avoiding the influence of the existence of foam on the construction efficiency and the curing effect. Thus, the antifoaming agent is N Ε - (1-carboxymethyl) -L-lysine.
The invention has the beneficial effects that: according to the invention, on one hand, bubbles generated by stirring can be avoided by utilizing ultrasonic waves, the operation step of removing the bubbles from the material in the existing production process is reduced, the curing effect can be further improved by reducing the bubbles, and the vacuum on the surface of the material formed after curing is avoided; on the other hand, the materials can be uniformly mixed, so that the mixing time is shortened and the mixing uniformity of the materials is ensured; the epoxy resin-based composite material prepared by the invention can be used as an electronic component packaging material, can be quickly cured at room temperature, can realize firm bonding between parts, and ensures the bonding quality and the bonding durability.
The specific implementation mode is as follows:
in order to make the technical means, the creation characteristics, the achievement purposes and the effects of the invention easy to understand, the invention is further described with the specific embodiments.
The bisphenol A type epoxy resins in the following examples and comparative examples were obtained from bisphenol A type liquid epoxy resin 128 of Wuxi Yehao chemical Co., Ltd, polyetheramine was obtained from polyetheramine D-230 of Shanghai Yi Bio-technology Co., Ltd, carbon fibers were obtained from carbon fiber powder of Xiangsheng carbon fiber technology Co., Ltd, polydimethylsiloxane was obtained from Wantai silicone rubber Co., Ltd, and polyoxypropylene ethylene oxide glyceryl ether was obtained from Wuhan Xinkang Fine chemical Co., Ltd.
Example 1
(1) Preparation of the resin component: uniformly mixing 85g of bisphenol A epoxy resin and 13g of 1, 4-butanediol diglycidyl ether by using ultrasonic waves for 30min to obtain a resin component;
(2) preparation of the curing agent component: uniformly mixing 58g of polyetheramine and 32g of methylcyclohexanediamine by using ultrasonic waves for 30min to obtain a curing agent component;
(3) preparing a composite material: uniformly mixing the resin component and the curing agent component according to the proportion of 100:30 by using ultrasonic waves to obtain a mixture, mixing for 30min, taking 40g of the mixture, and introducing 55g of carbon fibers in vacuum; preheating the resin component to 45 ℃, not preheating the curing agent, preheating the mould to 40 ℃, introducing the fiber in vacuum at 40 ℃, and controlling the vacuum degree to be-0.08 MPa;
(4) and (3) a curing process: curing at 40 deg.C for 4 hr, and curing at 80 deg.C for 3 hr.
Wherein the ultrasonic wave is generated by an ultrasonic device with the working frequency of 40kHz and the ultrasonic power of 1200W.
Comparative example
The vacuum introduction in example 1 was replaced by physical mixing, i.e. step (3) was replaced by "preparation of composite material: the resin component and the curing agent component are uniformly mixed by ultrasonic waves according to the proportion of 100:30 to obtain a mixture, the mixing time is 30min, 40g of the mixture is taken, 55g of carbon fiber is added, and the mixture is mixed by ultrasonic waves for 30min ", and the rest is the same as the example 1.
Example 2
The procedure of example 1 was repeated except that the 1, 4-butanediol diglycidyl ether in example 1 was replaced with a saturated aqueous solution of hydrolyzed polymaleic anhydride (25 ℃ C.), and the mass of the hydrolyzed polymaleic anhydride was the same as that of the 1, 4-butanediol diglycidyl ether.
Example 3
Step (1) in example 1 was replaced with "preparation of resin component: 85g of bisphenol A epoxy resin, 13g of 1, 4-butanediol diglycidyl ether, and 0.5 to 2 parts of a defoaming agent were uniformly mixed by ultrasonic waves for 30 minutes to obtain a resin component, and the defoaming agent was polydimethylsiloxane, and the rest was the same as in example 1.
Example 4
The defoamer of example 3 was replaced with polyoxypropylene ethylene oxide glyceryl ether, and the remainder was the same as in example 3.
Example 5
The antifoam in example 3 was replaced with N Ε - (1-carboxymethyl) -L-lysine, the remainder being as in example 3.
Epoxy resin-based composite materials were prepared using the above examples and comparative examples, respectively.
The defoaming and foam suppressing properties of the resin components prepared in examples 1, 3, 4 and 5 were measured by the following methods: 50mL of the resin component was measured out using a 100mL stoppered cylinder and the cylinder was shaken 10 and 100 times in the vertical direction, left to stand for immediate timing, and the highest graduations V10 and V100 of the foam (V being the sum of the liquid volume and the foam volume) and the times T10 and T100 for complete elimination of the foam were recorded, with the test results shown in Table 1. The smaller the V value is, the better the foam inhibition performance is; the smaller the T value, the better the defoaming property.
The impact resistance of the epoxy resin-based composite materials prepared in example 1, comparative example and example 2 was measured with reference to standard SJ/T11125-1997, and the test results are shown in Table 1.
TABLE 1
| Group of | Izod notched impact Strength | V10 | T10 | V100 | T100 |
| Example 1 | 28.4J/m | 71mL | 63s | mL | 82s |
| Example 2 | 33.5J/m | / | / | / | / |
| Example 3 | / | 56mL | 10s | 58mL | 12s |
| Example 4 | / | 55mL | 8s | 57mL | 9s |
| Example 5 | / | 51mL | 4s | 51mL | 4s |
| Comparative example | 25.9J/m | / | / | / | / |
"/" means not determined.
As can be seen from table 1, in example 2, the technical effect of significantly improving the impact resistance of the composite material can be achieved by using the saturated aqueous solution of hydrolyzed polymaleic anhydride, and the vacuum introduction operation of the fiber can also improve the impact resistance of the composite material; example 5 the technical effect of significantly improving the defoaming and foam suppressing ability of the resin component can be achieved by using N Ε - (1-carboxymethyl) -L-lysine as a defoaming agent, and the defoaming and foam suppressing ability is superior to that of the conventional polydimethylsiloxane and polyoxypropylene ethylene oxide glyceryl ether in the art.
The foregoing shows and describes the general principles and broad features of the present invention and advantages thereof. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (7)
1. The method for producing the epoxy resin-based composite material by using ultrasonic mixing is characterized by comprising the following steps of:
(1) preparation of the resin component: uniformly mixing 80-90 parts of bisphenol A epoxy resin and 10-20 parts of reactive diluent by using ultrasonic waves to obtain a resin component;
(2) preparation of the curing agent component: uniformly mixing 55-70 parts of polyether amine and 30-45 parts of alicyclic amine by using ultrasonic waves to obtain a curing agent component;
(3) preparing a composite material: uniformly mixing the resin component and the curing agent component according to the proportion of 100:20-50 by using ultrasonic waves to obtain a mixture, taking 30-45 parts of the mixture, and introducing 50-70 parts of fibers in vacuum;
(4) and (3) a curing process: curing at 40 deg.C for 3-5 hr, and curing at 80 deg.C for 2-4 hr.
2. The method of claim 1, wherein: the ultrasonic wave is generated by an ultrasonic device with the working frequency of 28kHz or 40kHz and the ultrasonic wave power of 600-1800W.
3. The method of claim 1, wherein: the fibers are carbon fibers or glass fibers.
4. The method of claim 1, wherein: the operating conditions of the vacuum introduction are as follows: preheating the resin component to 45 ℃, not preheating the curing agent, preheating the mould to 40 ℃, introducing the fiber in vacuum at 40 ℃, and controlling the vacuum degree to be between-0.05 MPa and-0.1 MPa.
5. The method of claim 1, wherein: the polyether amine is one or more of D-230, D-400, D-2000 and T-403.
6. The method of claim 1, wherein: the alicyclic amine is one or more of methyl cyclohexanediamine, cyclohexylamine and m-phenylenediamine.
7. The method of claim 1, wherein: the reactive diluent is 1, 4-butanediol diglycidyl ether.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111791416A (en) * | 2020-04-27 | 2020-10-20 | 东莞市维斯德新材料技术有限公司 | Preparation method of carbon fiber composite material |
| CN116178894A (en) * | 2023-02-03 | 2023-05-30 | 安徽恒泰新材料科技股份有限公司 | Epoxy resin composite material and processing device thereof |
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| CN102153833A (en) * | 2010-09-20 | 2011-08-17 | 青岛科技大学 | Carbon fiber (powder)/epoxy resin composite material used for rapid prototyping die |
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2019
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| GB1404575A (en) * | 1971-07-27 | 1975-09-03 | Kodak Ltd | Method of dispersing a pigment in a resin |
| CN101811661A (en) * | 2010-03-11 | 2010-08-25 | 同济大学 | Preparation method of carbon fiber/carbon nano tube/epoxy resin multi-dimensional hybrid composite |
| CN102153833A (en) * | 2010-09-20 | 2011-08-17 | 青岛科技大学 | Carbon fiber (powder)/epoxy resin composite material used for rapid prototyping die |
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