CN111825954A - Normal-temperature curing resin system for copying antenna reflecting surface and preparation method thereof - Google Patents

Normal-temperature curing resin system for copying antenna reflecting surface and preparation method thereof Download PDF

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Publication number
CN111825954A
CN111825954A CN202010617159.3A CN202010617159A CN111825954A CN 111825954 A CN111825954 A CN 111825954A CN 202010617159 A CN202010617159 A CN 202010617159A CN 111825954 A CN111825954 A CN 111825954A
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China
Prior art keywords
parts
resin system
epoxy resin
antenna
reflecting surface
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Pending
Application number
CN202010617159.3A
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Chinese (zh)
Inventor
徐宏涛
郝旭峰
鞠博文
张尉博
王晓蕾
戴晶滨
李钱福
吴泽州
梁燕民
田杰
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Shanghai Prospective Innovation Research Institute Co ltd
Shanghai Composite Material Science and Technology Co Ltd
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Shanghai Prospective Innovation Research Institute Co ltd
Shanghai Composite Material Science and Technology Co Ltd
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Priority to CN202010617159.3A priority Critical patent/CN111825954A/en
Publication of CN111825954A publication Critical patent/CN111825954A/en
Pending legal-status Critical Current

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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
    • C08L63/00—Compositions of epoxy resins; Compositions of derivatives of epoxy resins
    • C08L63/04—Epoxynovolacs
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
    • C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
    • C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
    • C08G59/50—Amines
    • C08G59/5006—Amines aliphatic
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
    • C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
    • C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
    • C08G59/50—Amines
    • C08G59/5026—Amines cycloaliphatic
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
    • C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
    • C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
    • C08G59/50—Amines
    • C08G59/5046—Amines heterocyclic
    • C08G59/5053—Amines heterocyclic containing only nitrogen as a heteroatom
    • C08G59/5073—Amines heterocyclic containing only nitrogen as a heteroatom having two nitrogen atoms in the ring
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01Q—ANTENNAS, i.e. RADIO AERIALS
    • H01Q15/00—Devices for reflection, refraction, diffraction or polarisation of waves radiated from an antenna, e.g. quasi-optical devices
    • H01Q15/14—Reflecting surfaces; Equivalent structures
    • 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
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00—Polymer mixtures characterised by other features
    • C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group

Abstract

The invention discloses a normal-temperature curing resin system for copying an antenna reflecting surface and a preparation method thereof, wherein the normal-temperature curing resin system comprises the following components in parts by weight: a: 90-110 parts of phenolic epoxy resin and 30-40 parts of alicyclic epoxy resin; b: 4-6 parts of triethylene tetramine and 30-40 parts of alicyclic amine curing agent. The epoxy resin system obtained by the invention can be used for a normal-temperature replication molding process of the antenna reflecting surface to obtain the high-precision antenna reflecting panel.

Description

Normal-temperature curing resin system for copying antenna reflecting surface and preparation method thereof
Technical Field
The invention belongs to the technical field of high polymer materials, particularly relates to a normal-temperature curing resin system, and particularly relates to a normal-temperature curing resin system for copying an antenna reflecting surface and a preparation method thereof.
Background
The resin-based composite material has the characteristics of small density, large specific stiffness, high specific strength, small thermal expansion coefficient (approaching zero through design) and the like, and becomes the most ideal material for preparing the antenna reflecting surface with high precision and high stability. The antenna reflecting surface replication process is mainly characterized in that a thin medium layer is injected between a warped antenna reflecting surface and a mold to replicate the precision of the mold, and finally, a high-precision antenna reflecting surface which is basically consistent with the precision of the mold is obtained.
Epoxy resin is the most ideal dielectric material for the antenna reflecting surface replication process due to good adhesion, heat resistance, chemical resistance and mechanical properties, but the existing normal-temperature cured epoxy resin system has short operation time, and the high-temperature cured epoxy resin system cannot be cured at normal temperature, so that a resin system which can be cured at normal temperature and has long operation time is urgently needed.
In the existing normal temperature curing epoxy resin system, for example, patent document CN107556954A discloses an epoxy structural adhesive for aramid fiber honeycomb composite material, which comprises the following components: the mass ratio is 1: 1.5-3: 2-5 of matrix epoxy resin, heat-resistant epoxy resin and rubber toughening agent. The epoxy structural adhesive prepared by the method has high bonding strength and high temperature resistance after being cured at normal temperature, and the preparation method is simple to operate, so that the bonding material can be cured at normal temperature and used at high temperature, and the peel strength of the bonding material is enhanced. However, the digital normal-temperature use time is short, about 30min, and the normal-temperature copying requirement of the antenna reflecting surface cannot be met (5 h for vacuum defoaming, 1h for operation, and 6h for supply and demand).
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a normal-temperature curing resin system for copying an antenna reflecting surface and a preparation method thereof.
The purpose of the invention is realized by the following technical scheme:
the invention provides a normal-temperature curing resin system for copying an antenna reflecting surface, which comprises the following components in parts by weight:
90-110 parts of phenolic epoxy resin;
30-40 parts of alicyclic epoxy resin;
34-46 parts of a curing agent.
Preferably, the normal temperature curing resin system for antenna reflecting surface replication comprises the following components in parts by weight:
100 parts of phenolic epoxy resin;
35 parts of alicyclic epoxy resin;
40 parts of curing agent.
Preferably, the novolac type epoxy resin is F-44 or F-51 epoxy resin.
Preferably, the viscosity of the alicyclic epoxy resin at 25 ℃ is less than or equal to 400 mPa.s; the alicyclic epoxy resin is 3, 4-epoxy cyclohexyl formic acid-3 ', 4' -epoxy cyclohexyl methyl ester, vinyl cyclohexene diepoxide and bis (2, 3-epoxy cyclopentyl) ether.
Preferably, the curing agent comprises the following components in a weight ratio of 4-6: 30-40 parts of triethylene tetramine and alicyclic amine curing agent.
Preferably, in the curing agent, the weight ratio of triethylene tetramine to alicyclic amine curing agent is 5: 35.
preferably, the viscosity of the alicyclic amine curing agent at 25 ℃ is less than or equal to 100 mPa.s; the alicyclic amine curing agent is menthane diamine, isophorone diamine and N-aminoethyl piperazine.
The invention also provides a preparation method of the normal-temperature curing resin system for copying the antenna reflecting surface, which comprises the following steps:
s1, weighing the raw materials according to the weight parts of the components in the claim 1;
s2, mixing the novolac epoxy resin and the alicyclic epoxy resin, and stirring to obtain a component A;
s3, adding triethylene tetramine into the alicyclic amine curing agent, and stirring until the mixture is uniformly mixed to form a component B;
and S4, mixing the component A and the component B to form the normal temperature curing resin system for copying the antenna reflecting surface.
Preferably, in step S2, the heating temperature is 40 ℃ to 50 ℃; the stirring speed is 2000-4000 revolutions per minute, and the stirring time is 10-20 min;
in step S3, the stirring speed is 2000-4000 rpm, and the stirring time is 10-15 min.
The invention also provides application of the normal-temperature curing resin system in antenna reflecting surface replication.
Compared with the prior art, the invention has the following beneficial effects:
(1) according to the invention, through compounding of the phenolic epoxy resin and the alicyclic epoxy resin, the viscosity of the resin system at normal temperature can be reduced, so that normal-temperature operation is achieved, and the normal-temperature service time of the resin system is prolonged; and by adding two specific curing agents, the resin system can be cured at normal temperature for a long time, and the requirements of a normal-temperature replication process are met.
(2) The epoxy resin system obtained by the invention can be used for more than 12 hours at normal temperature;
(3) the resin system prepared by the invention can reach the use temperature of more than 120 ℃ after certain post-curing treatment.
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that variations and modifications can be made by persons skilled in the art without departing from the spirit of the invention. All falling within the scope of the present invention.
Example 1
This example provides an ambient temperature curing resin system, the components and parts by weight of which are shown in Table 1. The preparation method comprises the following steps:
1) mixing phenolic epoxy resin F-44100 parts and 3, 4-epoxy cyclohexyl formic acid-3 ', 4' -epoxy cyclohexyl methyl ester (viscosity at 25 ℃ is 400mPa.s)35 parts, and mechanically stirring (rotating speed of 2000 r/min) for 15min for later use;
2) mixing 4 parts of triethylene tetramine and 35 parts of menthane diamine (MDA, viscosity of 19mPa.s at 25 ℃) curing agent, mechanically stirring (rotating speed 4000 r/min) for 10min, and standing for 24 h;
3) the two mixed liquids are put into a refrigerator for storage and standby, and can be used for the high-precision replication process of the antenna reflecting surface subsequently.
Example 2
This example provides a normal temperature curing medium-high temperature epoxy resin system, the components and parts by weight of which are shown in table 1. The preparation method comprises the following steps:
1) mixing phenolic epoxy resin F-51100 parts and 3, 4-epoxy cyclohexyl formic acid-3 ', 4' -epoxy cyclohexyl methyl ester (viscosity at 25 ℃ is 400mPa.s)35 parts, and mechanically stirring (rotating speed of 2000 r/min) for 15min for later use;
2) mixing 5 parts of triethylene tetramine and 40 parts of menthane diamine (MDA, viscosity of 19mPa.s at 25 ℃) curing agent, mechanically stirring (rotating speed 4000 r/min) for 10min, and standing for 24 h;
3) the two mixed liquids are put into a refrigerator for storage and standby, and can be subsequently used for a high-precision reflecting surface high-copy ratio process.
Example 3
This example provides an ambient temperature curing resin system, the components and parts by weight of which are shown in Table 1. The preparation method comprises the following steps:
1) mixing phenolic epoxy resin F-44110 parts and 3, 4-epoxy cyclohexyl formic acid-3 ', 4' -epoxy cyclohexyl methyl ester (viscosity at 25 ℃ is 400mPa.s)30 parts, and mechanically stirring (rotating speed of 3000 r/min) for 20min for later use;
2) mixing 4 parts of triethylene tetramine and 32 parts of menthane diamine (MDA, viscosity of 19mPa.s at 25 ℃) curing agent, mechanically stirring (rotating speed of 2000 r/min) for 15min, and standing for 24 h;
3) the two mixed liquids are put into a refrigerator for storage and standby, and can be used for the high-precision replication process of the antenna reflecting surface subsequently.
Example 4
This example provides an ambient temperature curing resin system, the components and parts by weight of which are shown in Table 1. The preparation method comprises the following steps:
1) mixing phenolic epoxy resin F-4490 parts and 40 parts of 3, 4-epoxy cyclohexyl formic acid-3 ', 4' -epoxy cyclohexyl methyl ester (the viscosity at 25 ℃ is 400mPa.s), and mechanically stirring (the rotation speed is 4000 r/min) for 10min for later use;
2) mixing 6 parts of triethylene tetramine and 30 parts of menthane diamine (MDA, viscosity of 19mPa.s at 25 ℃) curing agent, mechanically stirring (rotating speed of 2000 r/min) for 15min, and standing for 24 hours;
3) the two mixed liquids are put into a refrigerator for storage and standby, and can be used for the high-precision replication process of the antenna reflecting surface subsequently.
Example 5
This example is prepared substantially identically to example 1, except that: in step 2) of this example vinylcyclohexene diepoxide was used in place of 3,4 epoxycyclohexylcarboxylic acid-3 ', 4' -epoxycyclohexylmethyl ester.
Example 6
This example is prepared substantially identically to example 1, except that: in step 2) of this example bis (2, 3-epoxycyclopentyl) ether was used in place of 3,4 epoxycyclohexylcarboxylic acid-3 ', 4' -epoxycyclohexylmethyl ester.
Example 7
This example is prepared substantially identically to example 1, except that: isofluorylketodiamine was used in place of menthanediamine in step 2) of this example.
Example 8
This example is prepared substantially identically to example 1, except that: in step 2) of this example, N-aminoethylpiperazine was used instead of menthanediamine.
Comparative example 1
The components and parts by weight of the comparative example are shown in table 1, and the preparation method is basically the same as that of example 4 except that: the content of 3, 4-epoxycyclohexylmethyl 3 ', 4' -epoxycyclohexylcarboxylate used in this comparative example was 45 parts.
Comparative example 2
The components and parts by weight of this comparative example are shown in table 1, and the preparation method is substantially the same as that of example 3 except that: the content of 3, 4-epoxycyclohexylmethyl 3 ', 4' -epoxycyclohexylcarboxylate used in this comparative example was 25 parts.
Comparative example 3
The components, the parts by weight and the preparation method of the comparative example are basically the same as those of the example 2, and the difference is only that: 8 parts of triethylene tetramine are used in this comparative example.
Comparative example 4
The components, the parts by weight and the preparation method of the comparative example are basically the same as those of the example 2, and the difference is only that: e-51 used in this comparative example was substituted for the novolac type epoxy resin F-51.
Comparative example 5
The components and parts by weight of the comparative example are shown in table 1, and the preparation method is basically the same as that of example 2 except that: the comparative example contained only menthane diamine.
Comparative example 6
The components and the parts by weight of the comparative example are the same as the preparation method of the example 2, and the difference is only that: in this comparative example, diethylenetriamine was used instead of triethylenetetramine.
TABLE 1
Figure BDA0002564172660000061
And (3) effect comparison:
the properties of the epoxy resin system prepared in example 1 were comparable to conventional epoxy resin systems (AG-80/DDS/BF)3MEA) were compared, the specific test method was: separately, cast bodies were prepared and the tensile strength and tensile modulus were measured. The results are shown in Table 2.
TABLE 2
Figure BDA0002564172660000062
Figure BDA0002564172660000071
The invention has many applications, and the above description is only a preferred embodiment of the invention. It should be noted that the above examples are only for illustrating the present invention, and are not intended to limit the scope of the present invention. It will be apparent to those skilled in the art that various modifications can be made without departing from the principles of the invention and these modifications are to be considered within the scope of the invention.

Claims (10)

1. A normal temperature curing resin system for copying an antenna reflecting surface is characterized by comprising the following components in parts by weight:
90-110 parts of phenolic epoxy resin;
30-40 parts of alicyclic epoxy resin;
34-46 parts of a curing agent.
2. The normal temperature curing resin system for antenna reflecting surface replication of claim 1, characterized by comprising the following components in parts by weight:
100 parts of phenolic epoxy resin;
35 parts of alicyclic epoxy resin;
40 parts of curing agent.
3. A room temperature curing resin system for antenna reflector replication as claimed in claim 1 or 2, wherein the novolac type epoxy resin is F-44 or F-51 epoxy resin.
4. The ambient-temperature-curable resin system for antenna reflector replication according to claim 1 or 2, wherein the viscosity of the alicyclic epoxy resin at 25 ℃ is not more than 400 mpa.s; the alicyclic epoxy resin is 3,4 epoxy group cyclohexyl formic acid-3’，4’Epoxycyclohexylmethyl ester, vinylcyclohexene diepoxide, bis (2, 3-epoxycyclopentyl) ether.
5. The normal-temperature curing resin system for antenna reflecting surface replication as claimed in claim 1, wherein the curing agent comprises the following components in a weight ratio of 4-6: 30-40 parts of triethylene tetramine and alicyclic amine curing agent.
6. The normal temperature curing resin system for antenna reflection surface replication of claim 5, wherein the curing agent comprises triethylene tetramine and alicyclic amine in a weight ratio of 5: 35.
7. the ambient curing resin system for antenna reflection surface replication according to claim 5 or 6, wherein the viscosity of the alicyclic amine curing agent at 25 ℃ is 100mpa.s or less; the alicyclic amine curing agent is menthane diamine, isophorone diamine and N-aminoethyl piperazine.
8. A method for preparing a room temperature curing resin system for antenna reflection surface replication according to claim 1, comprising the steps of:
s1, weighing the raw materials according to the weight parts of the components in the claim 1;
s2, mixing the novolac epoxy resin and the alicyclic epoxy resin, and stirring to obtain a component A;
s3, adding triethylene tetramine into the alicyclic amine curing agent, and stirring until the mixture is uniformly mixed to form a component B;
and S4, mixing the component A and the component B to form the normal temperature curing resin system for copying the antenna reflecting surface.
9. The method for preparing a normal temperature curing resin system for antenna reflection surface replication according to claim 8, wherein in step S2, the heating temperature is 40 ℃ to 50 ℃; the stirring speed is 2000-4000 revolutions per minute, and the stirring time is 10-20 min;
in step S3, the stirring speed is 2000-4000 rpm, and the stirring time is 10-15 min.
10. Use of an ambient curing resin system according to claim 1 for replication of a reflecting surface of an antenna.
CN202010617159.3A 2020-06-30 2020-06-30 Normal-temperature curing resin system for copying antenna reflecting surface and preparation method thereof Pending CN111825954A (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105440584A (en) * 2015-12-10 2016-03-30 上海复合材料科技有限公司 Low-shrinkage epoxy resin system and preparation method thereof
CN107629412A (en) * 2017-09-29 2018-01-26 安徽众博新材料有限公司 A kind of high-strength epoxy isolator material and preparation method thereof
CN107936479A (en) * 2017-12-06 2018-04-20 上海复合材料科技有限公司 A kind of low shrinkage epoxy resin and preparation method thereof
CN108794983A (en) * 2018-05-30 2018-11-13 广东博汇新材料科技股份有限公司 Quick-setting composition epoxy resin and preparation method thereof
CN110474169A (en) * 2019-07-09 2019-11-19 上海复合材料科技有限公司 A kind of high-precision composite material antenna reflective face forming method

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105440584A (en) * 2015-12-10 2016-03-30 上海复合材料科技有限公司 Low-shrinkage epoxy resin system and preparation method thereof
CN107629412A (en) * 2017-09-29 2018-01-26 安徽众博新材料有限公司 A kind of high-strength epoxy isolator material and preparation method thereof
CN107936479A (en) * 2017-12-06 2018-04-20 上海复合材料科技有限公司 A kind of low shrinkage epoxy resin and preparation method thereof
CN108794983A (en) * 2018-05-30 2018-11-13 广东博汇新材料科技股份有限公司 Quick-setting composition epoxy resin and preparation method thereof
CN110474169A (en) * 2019-07-09 2019-11-19 上海复合材料科技有限公司 A kind of high-precision composite material antenna reflective face forming method

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Application publication date: 20201027