CN111205402A - Wave-transparent unsaturated polyester resin material and preparation method thereof - Google Patents
Wave-transparent unsaturated polyester resin material and preparation method thereof Download PDFInfo
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- CN111205402A CN111205402A CN202010195817.4A CN202010195817A CN111205402A CN 111205402 A CN111205402 A CN 111205402A CN 202010195817 A CN202010195817 A CN 202010195817A CN 111205402 A CN111205402 A CN 111205402A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/01—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to unsaturated polyesters
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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
- C08L51/00—Compositions of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Compositions of derivatives of such polymers
- C08L51/08—Compositions of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Compositions of derivatives of such polymers grafted on to macromolecular compounds obtained otherwise than by reactions only involving unsaturated carbon-to-carbon bonds
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Abstract
The invention discloses a wave-transparent unsaturated polyester resin material and a preparation method thereof, and the wave-transparent unsaturated polyester resin material comprises the following raw materials in parts by weight: 80-120 parts of unsaturated polyester resin, 5-10 parts of epoxy resin, 1-5 parts of styrene, 2-3 parts of surfactant, 0.02-0.1 part of initiator, 0.5-1.5 parts of accelerator and 1-5 parts of curing agent. According to the invention, the unsaturated polyester resin, the epoxy resin, the styrene, the surfactant, the accelerator and the curing agent are pre-prepared and mixed, and the unsaturated polyester resin material with excellent dielectric property is prepared after the polymerization is initiated by the initiator and fully cured.
Description
Technical Field
The invention relates to the technical field of unsaturated polyester resin material synthesis, in particular to a wave-transparent unsaturated polyester resin material and a preparation method thereof.
Background
Compared with an inorganic wave-transparent composite material, the resin-based wave-transparent composite material has a good development prospect and economic benefits. Different structural forms can be designed by utilizing the resin-based wave-transmitting composite material to meet the requirements on the mechanical properties of the material. Meanwhile, the content of each raw material of the composite material can be accurately controlled according to the requirement of wave-transmitting performance, wherein the dielectric performance and other performances of the composite material can be properly designed and adjusted, so that the resin-based composite wave-transmitting material is favored by scientific researchers. At present, resin-based composite wave-transmitting materials are divided into the following categories according to the difference of resin bases:
(1) epoxy resin based wave-transparent composite material
The epoxy resin molecular structure contains epoxy functional groups capable of reacting with various curing agents, so that the epoxy resin molecular structure has good cohesiveness and wear resistance, the process is relatively mature, the wave-transparent composite material prepared by using the epoxy resin molecular structure has low cost, stable size and compact material structure, but the epoxy resin-based wave-transparent composite material has low heat resistance and cannot meet the heat resistance requirement of an aircraft under high Mach number conditions; the impact toughness and the resistance to moist heat are also poor, and the dielectric constant and the dielectric loss value are large.
(2) Cyanate resin-based wave-transparent composite material
The cyanate resin molecules contain two or more cyanate functional groups, cyclization reaction can occur between the cyanate resin molecules at a certain temperature, and finally the cross-linked network macromolecule containing triazine ring is produced. The triazine ring has a highly symmetrical structure, has weak polarizability and does not have dipole moment, so the triazine ring has excellent dielectric properties, namely, the low dielectric constant epsilon is 2.8-3.1F/m, the extremely small dielectric loss (tan delta) is 0.009-0.005, and the glass transition temperature T of the cyanate resingOver 240 ℃. However, the curing process of preparing the wave-transparent composite material by using the cyanate ester resin needs higher curing temperature, but the toughness of the material is greatly reduced by high-temperature curing, the brittleness is higher, and meanwhile, the production cost of the wave-transparent composite material is higher.
(3) Polyimide resin-based wave-transmitting composite material
The polyimide resin is a polymer containing aromatic rings and imide groups on a main chain, has high heat resistance, can resist heat up to 366 ℃, has dielectric property epsilon of 4.1F/m and dielectric loss (tan delta) of 0.008, has good mechanical property, chemical resistance and high dimensional stability, but has curing temperature higher than 300 ℃ when the polyimide resin is used for preparing the wave-transparent composite material, increases the production cost, and has harsh process conditions, thereby bringing certain difficulty to the wide application of the polyimide resin.
(4) Bismaleimide resin-based wave-transmitting composite material
The bismaleimide is one of resin systems derived from polyimide, has good electrical insulation performance, chemical corrosion resistance and high temperature resistance, has the working temperature of 100-250 ℃, and has poor toughness due to the fact that the bismaleimide is used for preparing the wave-transmitting composite material because of the heat resistance of the multifunctional epoxy resin.
(5) Unsaturated resin-based wave-transparent composite material
The unsaturated polyester resin contains a large amount of crosslinked thermosetting plastics in the molecular structure, and the unsaturated bonds are initiated to react by an initiator under proper conditions to generate the crosslinked thermosetting plastics. The wave-transparent composite material prepared by using the unsaturated polyester resin has certain mechanical property and electrical property, but self-polymerization curing is easy to occur in the synthesis process, and the prepared material has the abnormal phenomena of stickiness, generation of a large amount of bubbles and the like, so that the dielectric property and the mechanical property of the wave-transparent composite material are greatly reduced. Meanwhile, the prepared unsaturated polyester resin-based wave-transmitting composite material has poor high-temperature resistance and is easy to ablate.
Based on the fact that the wave-transmitting performance of the existing unsaturated polyester resin material is unstable, and the dielectric property and the mechanical property of the unsaturated polyester resin material are relatively low, the unsaturated polyester resin material with excellent wave-transmitting performance is provided.
Disclosure of Invention
Based on the above problems, the present invention aims to provide a wave-transparent unsaturated polyester resin material and a preparation method thereof, wherein the dielectric constant and the dielectric loss of the unsaturated polyester resin material are effectively reduced, and the dielectric property of the unsaturated polyester resin material is improved.
The wave-transparent unsaturated polyester resin material comprises the following raw materials in parts by weight:
80-120 parts of unsaturated polyester resin, 5-10 parts of epoxy resin, 1-5 parts of styrene, 2-3 parts of surfactant, 0.02-0.1 part of initiator, 0.5-1.5 parts of accelerator and 1-5 parts of curing agent.
Preferably, the solid content of the unsaturated polyester resin is 60-70%, the acid value is 10-30mg KOH/g, the viscosity is 2000-2300mpa.s, and the OH value is 45-55 mgKOH/g.
Preferably, the epoxy value of the epoxy resin is 4.5 to 5.0, and the epoxy value is the amount of epoxy groups contained in 100g of the epoxy resin.
Preferably, the surfactant is one of tween 80, fatty glyceride, span 60 or span 80.
Preferably, the initiator is a solution of methyl ethyl ketone peroxide at a concentration of 5 to 8 wt%.
Preferably, the promoter is cobalt isooctanoate.
Preferably, the curing agent is prepared by mixing dibenzoyl peroxide and benzophenone peroxide according to a molar ratio of 1: 2.
The preparation method of the wave-transparent unsaturated polyester resin material comprises the following steps:
step one, mixing unsaturated polyester resin, epoxy resin and styrene in proportion, and stirring for 10-30min at room temperature to obtain a mixture I;
step two, adding a surfactant and an accelerator into the mixture I according to a proportion, and fully stirring for 10-30min to obtain a mixture II;
step three, adding a curing agent into the mixture II according to a proportion, and fully stirring to obtain a mixture III;
and step four, adding an initiator into the uniformly mixed mixture III, initiating polymerization at the temperature of 0-10 ℃, and placing the polymerized product into a constant temperature and humidity box for heating and curing treatment to obtain the transparent unsaturated polyester resin material.
Preferably, the humidity in the constant temperature and humidity box is 60-70%, and the temperature is 50-70 ℃.
Preferably, the curing time is 1 to 3 hours.
Compared with the prior art, the invention has the following beneficial effects: according to the invention, unsaturated polyester resin, epoxy resin, styrene, a surfactant, an accelerator and a curing agent are pre-prepared and mixed, polymerization reaction is initiated by an initiator and the mixture is fully cured to prepare the unsaturated polyester resin material with excellent dielectric property, and due to the addition of the surfactant and the epoxy resin, the phenomena of stickiness, pinholes, bubbles and the like in the preparation process are avoided, and the prepared material has strong mechanical property due to the initiation polymerization of the styrene.
Detailed Description
The present invention will be further described with reference to the following specific examples.
Example 1
The wave-transparent unsaturated polyester resin material comprises the following raw materials in parts by weight:
100 parts of unsaturated polyester resin, 6 parts of epoxy resin, 4 parts of styrene, 3 parts of surfactant, 0.05 part of initiator, 1.2 parts of cobalt isooctanoate and 3 parts of curing agent. Wherein the solid content of the unsaturated polyester resin is 65 percent, the acid value is 20mg KOH/g, the viscosity is 2000mpa.s, and the OH value is 50 mgKOH/g.
The epoxy value of the epoxy resin is 4.5, and the curing agent is prepared by mixing dibenzoyl peroxide and benzophenone peroxide according to a molar ratio of 1: 2.
The initiator is methyl ethyl ketone peroxide solution with the concentration of 6 wt%.
The preparation method of the wave-transparent unsaturated polyester resin material comprises the following steps:
step one, mixing unsaturated polyester resin, epoxy resin and styrene in proportion, and stirring for 10-30min at room temperature to obtain a mixture I;
step two, adding a surfactant and an accelerator into the mixture I according to a proportion, and fully stirring for 30min to obtain a mixture II;
step three, adding a curing agent into the mixture II according to a proportion, and fully stirring to obtain a mixture III;
and step four, adding an initiator into the uniformly mixed mixture III, initiating polymerization at the temperature of 5 ℃, and placing the polymerized product into a constant temperature and humidity box for heating and curing treatment to obtain the transparent unsaturated polyester resin material, wherein the humidity in the constant temperature and humidity box is 65%, the temperature is 60 ℃, and the curing time is 3 hours.
Example 2
The wave-transparent unsaturated polyester resin material comprises the following raw materials in parts by weight:
80 parts of unsaturated polyester resin, 5 parts of epoxy resin, 1 part of styrene, 2 parts of surfactant, 0.02 part of initiator, 0.5 part of cobalt isooctanoate and 1 part of curing agent. Wherein the solid content of the unsaturated polyester resin is 60 percent, the acid value is 10mg KOH/g, the viscosity is 2300mpa.s, and the OH value is 55 mgKOH/g.
The epoxy value of the epoxy resin is 4.5, and the curing agent is prepared by mixing dibenzoyl peroxide and benzophenone peroxide according to a molar ratio of 1: 2.
The initiator is methyl ethyl ketone peroxide solution with the concentration of 5 wt%.
The preparation method of the wave-transparent unsaturated polyester resin material comprises the following steps:
step one, mixing unsaturated polyester resin, epoxy resin and styrene in proportion, and stirring for 10-30min at room temperature to obtain a mixture I;
step two, adding a surfactant and an accelerator into the mixture I according to a proportion, and fully stirring for 30min to obtain a mixture II;
step three, adding a curing agent into the mixture II according to a proportion, and fully stirring to obtain a mixture III;
and step four, adding an initiator into the uniformly mixed mixture III, initiating polymerization at the temperature of 0 ℃, and placing the polymerized product into a constant temperature and humidity box for heating and curing treatment to obtain the transparent unsaturated polyester resin material, wherein the humidity in the constant temperature and humidity box is 70%, the temperature is 70 ℃, and the curing time is 1 h.
Example 3
The wave-transparent unsaturated polyester resin material comprises the following raw materials in parts by weight:
120 parts of unsaturated polyester resin, 10 parts of epoxy resin, 5 parts of styrene, 2 parts of surfactant, 0.1 part of initiator, 1.5 parts of cobalt isooctanoate and 4 parts of curing agent. Wherein the solid content of the unsaturated polyester resin is 62 percent, the acid value is 25mg KOH/g, the viscosity is 2100mpa.s, and the OH value is 45 mgKOH/g.
The epoxy value of the epoxy resin is 5.0, and the curing agent is prepared by mixing dibenzoyl peroxide and benzophenone peroxide according to a molar ratio of 1: 2.
The initiator is a methyl ethyl ketone peroxide solution with the concentration of 7 wt%.
The preparation method of the wave-transparent unsaturated polyester resin material comprises the following steps:
step one, mixing unsaturated polyester resin, epoxy resin and styrene in proportion, and stirring for 10-30min at room temperature to obtain a mixture I;
step two, adding a surfactant and an accelerator into the mixture I according to a proportion, and fully stirring for 10-30min to obtain a mixture II;
step three, adding a curing agent into the mixture II according to a proportion, and fully stirring to obtain a mixture III;
and step four, adding an initiator into the uniformly mixed mixture III, initiating polymerization at the temperature of 2 ℃, and placing the polymerized product into a constant temperature and humidity box for heating and curing treatment to obtain the transparent unsaturated polyester resin material, wherein the humidity in the constant temperature and humidity box is 62%, the temperature is 55 ℃, and the curing time is 3 hours.
Example 4
The wave-transparent unsaturated polyester resin material comprises the following raw materials in parts by weight:
90 parts of unsaturated polyester resin, 10 parts of epoxy resin, 3 parts of styrene, 3 parts of surfactant, 0.06 part of initiator, 1.2 parts of cobalt isooctanoate and 4 parts of curing agent. Wherein the solid content of the unsaturated polyester resin is 70 percent, the acid value is 15mg KOH/g, the viscosity is 2300mpa.s, and the OH value is 50 mgKOH/g.
The epoxy value of the epoxy resin is 5.0, and the curing agent is prepared by mixing dibenzoyl peroxide and benzophenone peroxide according to a molar ratio of 1: 2.
The initiator is methyl ethyl ketone peroxide solution with the concentration of 5 wt%.
The preparation method of the wave-transparent unsaturated polyester resin material comprises the following steps:
step one, mixing unsaturated polyester resin, epoxy resin and styrene in proportion, and stirring for 10-30min at room temperature to obtain a mixture I;
step two, adding a surfactant and an accelerator into the mixture I according to a proportion, and fully stirring for 20min to obtain a mixture II;
step three, adding a curing agent into the mixture II according to a proportion, and fully stirring to obtain a mixture III;
and step four, adding an initiator into the uniformly mixed mixture III, initiating polymerization at the temperature of 10 ℃, and placing the polymerized product into a constant temperature and humidity box for heating and curing treatment to obtain the transparent unsaturated polyester resin material, wherein the humidity in the constant temperature and humidity box is 65%, the temperature is 65 ℃, and the curing time is 1-3 hours.
Example 5
The wave-transparent unsaturated polyester resin material comprises the following raw materials in parts by weight:
110 parts of unsaturated polyester resin, 10 parts of epoxy resin, 5 parts of styrene, 2 parts of surfactant, 0.05 part of initiator, 1 part of cobalt isooctanoate and 3 parts of curing agent. Wherein the solid content of the unsaturated polyester resin is 70 percent, the acid value is 10mg KOH/g, the viscosity is 2000mpa.s, and the OH value is 45 mgKOH/g.
The epoxy value of the epoxy resin is 5.0, and the curing agent is prepared by mixing dibenzoyl peroxide and benzophenone peroxide according to a molar ratio of 1: 2.
The initiator is methyl ethyl ketone peroxide solution with the concentration of 8 wt%.
The preparation method of the wave-transparent unsaturated polyester resin material comprises the following steps:
step one, mixing unsaturated polyester resin, epoxy resin and styrene in proportion, and stirring for 10-30min at room temperature to obtain a mixture I;
step two, adding a surfactant and an accelerator into the mixture I according to a proportion, and fully stirring for 30min to obtain a mixture II;
step three, adding a curing agent into the mixture II according to a proportion, and fully stirring to obtain a mixture III;
and step four, adding an initiator into the uniformly mixed mixture III, initiating polymerization at the temperature of 5 ℃, and placing the polymerized product into a constant temperature and humidity box for heating and curing treatment to obtain the transparent unsaturated polyester resin material, wherein the humidity in the constant temperature and humidity box is 70%, the temperature is 50 ℃, and the curing time is 3 hours.
The dielectric properties and mechanical properties of the wave-transparent unsaturated polyester resin materials prepared in examples 1 to 5 of the present invention were measured and are shown in Table 1.
TABLE 1
The principles and embodiments of the present invention have been described herein using specific examples, which are provided only to help understand the method and the core concept of the present invention; meanwhile, for a person skilled in the art, according to the idea of the present invention, the specific embodiments and the application range may be changed. In view of the above, the present disclosure should not be construed as limiting the invention.
Claims (10)
1. The wave-transparent unsaturated polyester resin material is characterized by comprising the following raw materials in parts by weight:
80-120 parts of unsaturated polyester resin, 5-10 parts of epoxy resin, 1-5 parts of styrene, 2-3 parts of surfactant, 0.02-0.1 part of initiator, 0.5-1.5 parts of accelerator and 1-5 parts of curing agent.
2. The wave-transparent unsaturated polyester resin material as claimed in claim 1, wherein the unsaturated polyester resin has a solid content of 60-70%, an acid value of 10-30mg KOH/g, a viscosity of 2000-2300mpa.s, and an OH value of 45-55mg KOH/g.
3. The wave-transparent unsaturated polyester resin material according to claim 1, wherein the epoxy value of the epoxy resin is 4.5-5.0.
4. The wave-transparent unsaturated polyester resin material according to claim 1, wherein the surfactant is one of tween 80, fatty acid glyceride, span 60 or span 80.
5. The wave-transparent unsaturated polyester resin material according to claim 1, wherein the initiator is a methyl ethyl ketone peroxide solution having a concentration of 5-8 wt%.
6. The wave-transparent unsaturated polyester resin material according to claim 1, wherein the accelerator is cobalt iso-octoate.
7. The wave-transparent unsaturated polyester resin material according to claim 1, wherein the curing agent is a mixture of dibenzoyl peroxide and benzophenone peroxide in a molar ratio of 1: 2.
8. The method for preparing the wave-transparent unsaturated polyester resin material according to any one of claims 1 to 7, comprising the steps of:
step one, mixing unsaturated polyester resin, epoxy resin and styrene in proportion, and stirring for 10-30min at room temperature to obtain a mixture I;
step two, adding a surfactant and an accelerator into the mixture I according to a proportion, and fully stirring for 10-30min to obtain a mixture II;
step three, adding a curing agent into the mixture II according to a proportion, and fully stirring to obtain a mixture III;
and step four, adding an initiator into the uniformly mixed mixture III, initiating polymerization at the temperature of 0-10 ℃, and placing the polymerized product into a constant temperature and humidity box for heating and curing treatment to obtain the transparent unsaturated polyester resin material.
9. The method for preparing the wave-transparent unsaturated polyester resin material according to claim 8, wherein the humidity in the constant temperature and humidity chamber is 60-70%, and the temperature is 50-70 ℃.
10. The method of claim 8, wherein the curing time is 1-3 hours.
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Cited By (1)
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