Curable slurry of epoxy resin-polyvinyl butyral composite material and preparation method thereof
By using a small molecule amine-based curing agent in epoxy resin to dissolve polyvinyl butyral, the curable slurry preparation of epoxy resin-polyvinyl butyral composite without solvent is achieved, the problem of solvent use in the prior art is solved, and the material performance and construction convenience are improved.
Patent Information
- Application Number
- CN202510095112.8
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-01-21
- Publication Date
- 2025-04-11
- Estimated Expiration
- 2045-01-21
AI Technical Summary
In the prior art, the method of adding polyvinyl butyral to epoxy resin requires the use of a large amount of organic solvents, resulting in environmental pollution and degradation of material properties, and is not suitable for room temperature curing and open construction.
By preparing a curable slurry of epoxy resin-polyvinyl butyral composite material, a small molecule amine-based curing agent is used as a solvent for polyvinyl butyral, and it is introduced into the epoxy resin to achieve room temperature curing without solvent.
This method avoids solvent residue problems, improves the mechanical properties and durability of epoxy resin, is suitable for room temperature curing and open construction, and is safe and environmentally friendly.
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Figure BDA0005252629920000091
Abstract
Description
Technical Field
[0001] The present application belongs to the field of epoxy resins, and specifically relates to a curable slurry of an epoxy resin-polyvinyl butyral composite material and a preparation method thereof. Background Art
[0002] Epoxy resin has excellent mechanical properties such as compression, tension, and bonding, as well as durability properties such as corrosion resistance, hydrolysis resistance, and heat resistance, and is widely used in the fields of construction, chemical industry, and shipbuilding. However, epoxy resin has a high glass transition temperature, is brittle in low-temperature environments, and is prone to cracking, which limits its application in low-temperature environments; in addition, room-temperature curing epoxy resins, which are commonly used for repair, reinforcement, bonding, and corrosion protection in construction projects, have strong sag properties before they are fully cured, making it difficult to construct on the facade, and easily causing defects such as thin top and thick bottom or unevenness.
[0003] Polyvinyl butyral has a low glass transition temperature, good flexibility, tensile strength, bonding strength and impact strength, and has good light resistance, water resistance, heat resistance, cold resistance and film-forming properties. The molecular chain of polyvinyl butyral contains a large number of polar groups such as acetal, hydroxyl, ester, etc., and has good compatibility with epoxy resin. It is suitable for improving the problems of epoxy resin such as large brittleness and easy cracking. Polyvinyl butyral can also thicken and improve rheological properties when added to room temperature curing epoxy resin, making the epoxy resin slurry thixotropic, not easy to sag, and easier for facade construction. In addition, polyvinyl butyral is colorless and transparent and does not affect the appearance of epoxy resin.
[0004] However, the existing method of adding polyvinyl butyral to epoxy resin mainly adopts the solvent method, that is, polyvinyl butyral is dissolved in a solvent to form a solution and then added to the epoxy resin, or polyvinyl butyral and epoxy resin are dissolved in a solvent to form a solution, and then the solvent is removed while heating and curing. This method requires the use of a large amount of organic solvents, which not only requires high-temperature removal of the solvent, but also requires additional processes to recover or harmlessly discharge the solvent, and there is a problem of solvent residue, which is easy to cause environmental pollution, and the solvent residue is also unfavorable to the mechanical properties and durability of the epoxy resin material. In addition, the solvent method is not suitable for application scenarios such as room temperature curing and open construction.
[0005] Therefore, there is an urgent need to provide a technology that can add polyvinyl butyral to epoxy resin without a solvent and can be cured at room temperature to form a curable slurry of epoxy resin-polyvinyl butyral composite material that has performance that meets application requirements and is safe and environmentally friendly. Summary of the invention
[0006] In view of the above-mentioned shortcomings or deficiencies of the prior art, the technical problem to be solved by the present application is to provide a curable slurry of an epoxy resin-polyvinyl butyral composite material and a preparation method thereof.
[0007] To solve the above technical problems, this application is implemented through the following technical solutions:
[0008] The present application proposes a curable slurry of an epoxy resin-polyvinyl butyral composite material, comprising: a component A and a component B; the component A comprises raw materials in the following mass proportions: an epoxy resin: 100; an epoxy-based reactive diluent: 0-30; the component B comprises raw materials in the following mass proportions: a small molecule amine curing agent: 10-50; a polymer amine curing agent: 0-40; polyvinyl butyral: 1-10; and an amino silane coupling agent: 0-10.
[0009] Specifically, in the above-mentioned curable slurry, the epoxy resin is a solvent-free epoxy resin with a functionality of not less than 2.
[0010] Specifically, the curable slurry, wherein the epoxy resin comprises one or more combinations of the following substances: bisphenol A glycidyl ether, hydrogenated or halogenated or hydrocarbon-substituted bisphenol A glycidyl ether, bisphenol F glycidyl ether, hydrogenated or halogenated or hydrocarbon-substituted bisphenol F glycidyl ether, bisphenol S glycidyl ether, hydrogenated or halogenated or hydrocarbon-substituted bisphenol S glycidyl ether, hydrogenated or halogenated or hydrocarbon-substituted hydrocarbyl diglycidyl ether, polyphenol glycidyl ether, Glycidyl ether of water, glycidyl ether of linear phenolic resin, glycidyl ether of aliphatic polyol, glycidyl ester of aliphatic polyacid, glycidyl amine type epoxy resin with a functionality of not less than 2, alicyclic epoxy resin with a functionality of not less than 2, epoxidized olefin with a functionality of not less than 2, triglycidyl isocyanurate, hydantoin epoxy resin with a functionality of not less than 2, terminal epoxy polyether or polyester with a functionality of not less than 2, epoxy polysiloxane with a functionality of not less than 2.
[0011] Specifically, the above-mentioned curable slurry, wherein the epoxy-based reactive diluent includes one or more combinations of the following substances: glycidyl ether of a polyol having a carbon number not greater than 10 and a functionality not less than 2, polyethylene glycol having a viscosity not greater than 300 mPa·s at 25°C, polypropylene glycol diglycidyl ether having a viscosity not greater than 300 mPa·s at 25°C, silicone glycidyl ether having a viscosity not greater than 300 mPa·s at 25°C and a functionality not less than 2, and di(2-epoxypropyl) ether.
[0012] Specifically, the above-mentioned curable slurry, wherein the small molecule amine curing agent includes one or more combinations of the following substances: a monoamine with a carbon number of 2 to 18 and containing one primary amine group, and a polyamine with a carbon number of 2 to 18 and containing no less than 2 tertiary or lower amine groups.
[0013] Specifically, in the above-mentioned curable slurry, the polymer amine curing agent includes one or more combinations of the following substances: amino silicone oil, solvent-free polyethyleneimine, solvent-free amino silane coupling agent condensation product, and polyamide with a freezing point not greater than 40°C.
[0014] Specifically, in the above-mentioned curable slurry, the polyvinyl butyral comprises one or more combinations of the following substances: polyvinyl butyral with a molecular weight of 5000 to 250000; the polyvinyl butyral is in powder form, fine granules or flakes.
[0015] Specifically, the curable slurry, wherein the amino-silane coupling agent comprises: 1 R 2 x Si(OR 3 ) 3-x Silane coupling agent; wherein R 1 is a hydrocarbon group having 2 to 12 carbon atoms and containing one primary amino group, or R 1 is a hydrocarbon group having 2 to 12 carbon atoms and containing at least 2 tertiary or lower amine groups; R 2 and R 3 Each of them is a hydrocarbon group having 1 to 4 carbon atoms; the range of x is 0≤x≤2.
[0016] The present application also proposes a method for preparing a curable slurry of an epoxy resin-polyvinyl butyral composite material, comprising the following steps:
[0017] Weigh component A and component B respectively; wherein component A comprises the following raw materials in the following mass ratios: epoxy resin 100; epoxy-based reactive diluent 0-30; component B comprises the following raw materials in the following mass ratios: small molecule amine curing agent 10-50; polymer amine curing agent 0-40; polyvinyl butyral 1-10; amino silane coupling agent 0-10;
[0018] Prepare the A component; when the A component has more than one raw material, mix all the raw materials of the A component and stir them thoroughly to obtain the A component;
[0019] Prepare the B component; mix the small molecule amine curing agent and the polyvinyl butyral and stir them thoroughly until the polyvinyl butyral is fully dissolved to form a first transparent solution; when the amount of the amino silane coupling agent is not 0, mix the amino silane coupling agent with the small molecule amine curing agent and the polyvinyl butyral and stir them thoroughly until the polyvinyl butyral is fully dissolved to form a second transparent solution; when the amount of the polymer amine curing agent is not 0, mix the polymer amine curing agent with the first transparent solution or the second transparent solution and stir them thoroughly to obtain the B component;
[0020] The component A and the component B are mixed and stirred thoroughly to obtain a curing slurry of the epoxy resin-polyvinyl butyral composite material.
[0021] Optionally, in the above-mentioned preparation method, the preparation process of component A is assisted by heating before mixing with component B, and the heating temperature is not higher than the deterioration temperature of the raw materials used; and / or the polyvinyl butyral is ground and crushed before mixing; and / or the polyvinyl butyral is assisted by heating during the mixing process, and the heating temperature is not higher than the deterioration temperature of the raw materials used; and / or the polyvinyl butyral is assisted by ultrasound during the mixing process.
[0022] Optionally, in the above-mentioned preparation method, when the viscosity of the epoxy resin or polymer amine curing agent is too high, it is solid at room temperature or dissolves slowly, making it difficult to stir evenly in the mixing step, heating is added during mixing, and the heating temperature is not higher than the deterioration temperature of the raw materials used.
[0023] Optionally, in the above-mentioned preparation method, when component A has a high viscosity or solidifies at room temperature and is difficult to mix evenly with component B, the temperature during mixing is adjusted to ensure that component A is easy to mix evenly with component B and the curing time of the obtained curable slurry is shortened without affecting operability.
[0024] Compared with the prior art, this application has the following technical effects:
[0025] (1) In the curable slurry of the epoxy resin-polyvinyl butyral composite material of the present application, polyvinyl butyral is introduced into the epoxy resin, and the good flexibility, tensile strength, bonding strength and impact strength of polyvinyl butyral, as well as the characteristics of being rich in polar groups, having good compatibility with epoxy resin, and increasing the thixotropy of epoxy resin, are utilized to improve the shortcomings of epoxy resin such as greater brittleness under low temperature environment, easy cracking, and strong sag in facade construction, thereby meeting the needs of low-temperature application and facade construction of epoxy resin materials, improving the mechanical properties and durability of epoxy resin without affecting the appearance of epoxy resin, and expanding its application range.
[0026] (2) In the curable slurry of the epoxy resin-polyvinyl butyral composite material of the present application, an epoxy resin cured with an amine curing agent is selected, and the epoxy resin-amine alternating polymerization is carried out based on the addition reaction of the epoxy group-primary amine group / secondary amine group. The reaction can proceed spontaneously at room temperature. There is an induction period with slow viscosity growth at the beginning of the reaction, and then the reaction is rapid and uniform to achieve a high conversion rate. It can be cured at room temperature or by heating, and has a wide range of applications. The reaction can spontaneously achieve a high conversion rate. By adjusting the ratio of the epoxy group-primary amine group / secondary amine group, it is basically possible to achieve no organic amine residue, thereby avoiding the slow release of toxic and volatile organic amines into the environment after the epoxy resin is cured, which is safe and environmentally friendly.
[0027] (3) In the curable slurry of the epoxy resin-polyvinyl butyral composite material of the present application, an epoxy resin cured with an amine curing agent is selected, and the property of polyvinyl alcohol being soluble in small molecule organic amines is utilized, and the small molecule amine curing agent is used as a solvent for polyvinyl butyral to introduce it into the epoxy resin. Unlike the currently commonly used method of dissolving polyvinyl butyral with the help of an additional solvent and adding it to the epoxy resin, the present application does not require the addition of any additional solvent, and therefore does not require high-temperature solvent removal, does not require additional processes for solvent recovery or harmless solvent discharge, and does not have a solvent residue problem. It is safe, energy-saving, and environmentally friendly, and can also avoid the adverse effects of solvent residue on the mechanical properties and durability of the epoxy resin material, and is particularly suitable for application scenarios such as room temperature curing and open construction.
[0028] (4) The curable slurry of the epoxy resin-polyvinyl butyral composite material of the present application is modified based on the existing epoxy resin and has wide applicability to various existing epoxy resins and amine curing agents. DETAILED DESCRIPTION
[0029] The technical solutions in the embodiments of the present application are described clearly and completely below. Obviously, the described embodiments are only part of the embodiments of the present application, not all of the embodiments. Based on the embodiments in the present application, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present application.
[0030] Unless otherwise specified, the raw materials used in the following examples and comparative examples are all commercially available industrial-grade chemical raw materials.
[0031] Example 1
[0032] The following raw materials were weighed respectively: 100 g of epoxy resin 6002; 50 g of small molecule amine curing agent 593; and 10 g of polyvinyl butyral TB-14.
[0033] Epoxy resin 6002 is component A.
[0034] Mix curing agent 593 and TB-14 and stir thoroughly until TB-14 is fully dissolved to form a transparent solution to obtain component B.
[0035] The A component and the B component are mixed and stirred thoroughly to obtain a curable slurry of the epoxy resin-polyvinyl butyral composite material.
[0036] Example 2
[0037] The following raw materials were weighed separately: 90g epoxy resin E-51; 10g triglycidyl isocyanurate; 15g small molecule amine curing agent diethylenetriamine; 5g polymer amine curing agent polyamide 651; 5g polymer amine curing agent polyethyleneimine (600 molecular weight); 1g polyvinyl butyral TB-14.
[0038] E51 and triglycidyl isocyanurate were mixed and stirred thoroughly to obtain component A. During the mixing process, the mixture was heated to 70±10°C and the obtained component A was maintained at 50±5°C.
[0039] Diethylenetriamine and TB-14 were mixed and stirred thoroughly until TB-14 was fully dissolved to form a transparent solution; then they were mixed with polyamide 651 and polyethyleneimine (600 molecular weight) and stirred thoroughly to obtain component B, and heated to 55±5°C during the mixing process.
[0040] The A component and the B component are mixed and stirred thoroughly to obtain a curable slurry of the epoxy resin-polyvinyl butyral composite material.
[0041] Example 3
[0042] The following raw materials were weighed separately: 100g epoxy resin E51; 30g epoxy reactive diluent 669 (ethylene glycol diglycidyl ether); 10g small molecule amine curing agent T-31; 40g polymer amine curing agent polyamide 650; 1g polyvinyl butyral TB-17; 10g amino silane coupling agent KH-550 [γ-aminopropyltriethoxysilane].
[0043] Mix E51 and diluent 669 and stir thoroughly to obtain component A.
[0044] Mix T-31, TB-17 and KH-550 and stir thoroughly until TB-17 is fully dissolved to form a transparent solution, then mix it with polyamide 650 and stir thoroughly to obtain component B.
[0045] The A component and the B component are mixed and stirred thoroughly to obtain a curable slurry of the epoxy resin-polyvinyl butyral composite material.
[0046] Example 4
[0047] The following raw materials were weighed separately: 50g epoxy resin E-51, 50g epoxy resin E-12; 30g epoxy reactive diluent 750 (butylene glycol diglycidyl ether); 20g small molecule amine curing agent 593; 20g polymer amine curing agent polyamide 651; 4g polyvinyl butyral TB-14; 10g amino silane coupling agent KH-792 [N-β-(aminoethyl)-γ-aminopropyltrimethoxysilane].
[0048] Mix E51, E-12 and diluent 750 and stir thoroughly to obtain component A. Heat to 70±10℃ during mixing.
[0049] The curing agent 593, TB-14 and KH-792 were mixed and stirred thoroughly until TB-17 was fully dissolved to form a transparent solution, and then mixed with polyamide 651 and stirred thoroughly to obtain component B.
[0050] The A component and the B component are mixed and stirred thoroughly to obtain a curable slurry of the epoxy resin-polyvinyl butyral composite material.
[0051] Example 5
[0052] The following raw materials were weighed separately: 100g epoxy resin E51; 30g epoxy reactive diluent 749 (neopentyl glycol diglycidyl ether); 30g small molecule amine curing agent T-31; 8g polyvinyl butyral TB-12; 10g amino silane coupling agent KH-792 {N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane}.
[0053] Mix E51 and diluent 749 and stir thoroughly to obtain component A.
[0054] Mix T-31, TB-12 and KH-792 and stir thoroughly until TB-12 is fully dissolved to form a transparent solution to obtain component B.
[0055] The A component and the B component are mixed and stirred thoroughly to obtain a curable slurry of the epoxy resin-polyvinyl butyral composite material.
[0056] Example 6
[0057] The following raw materials were weighed separately: 100g epoxy resin 6002; 20g epoxy reactive diluent 503 (1,6-hexanediol diglycidyl ether), 10g epoxy reactive diluent epoxy double head [1,3-bis(3-glycidyloxypropyl)tetramethyldisiloxane]; 35g small molecule amine curing agent T-31; 2g polyvinyl butyral TB-17; 3g amino silane coupling agent KH-792 [N-β-(aminoethyl)-γ-aminopropyltrimethoxysilane], 7g amino silane coupling agent KH-550 [γ-aminopropyltriethoxysilane].
[0058] Mix epoxy resin 6002, diluent 503 and epoxy double seal and stir well to obtain component A.
[0059] Mix T-31, TB-17, KH-792, KH-550 and stir thoroughly until TB-17 is fully dissolved to form a transparent solution to obtain component B.
[0060] The A component and the B component are mixed and stirred thoroughly to obtain a curable slurry of the epoxy resin-polyvinyl butyral composite material.
[0061] Comparative Example 1
[0062] Weigh the following raw materials respectively: 100g epoxy resin 6002; 50g small molecule amine curing agent 593.
[0063] The two are mixed and stirred thoroughly to obtain epoxy resin curable slurry.
[0064] Comparative Example 2
[0065] The following raw materials were weighed separately: 100g epoxy resin E51; 10g small molecule amine curing agent T-31; 40g polymer amine curing agent polyamide 650; 30g epoxy reactive diluent 669 (ethylene glycol diglycidyl ether); 10g amino silane coupling agent KH-550 [γ-aminopropyltriethoxysilane].
[0066] The above raw materials are mixed and stirred thoroughly to obtain epoxy resin curable slurry.
[0067] Comparative Example 3
[0068] The following raw materials were weighed separately: 100 g epoxy resin E51; 30 g small molecule amine curing agent T-31; 30 g epoxy reactive diluent 749 (neopentyl glycol diglycidyl ether); 10 g amino silane coupling agent KH-792 {N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane}.
[0069] The above raw materials are mixed and stirred thoroughly to obtain epoxy resin curable slurry.
[0070] The curing conditions and some mechanical properties after curing of the curable slurries described in Examples 1 to 6 and Comparative Examples 1 to 3 are shown in Table 1.
[0071] Table 1 Curing conditions of curable slurries of Examples 1 to 6 and Comparative Examples 1 to 3 and some mechanical properties after curing
[0072]
[0073] The curable slurry of the epoxy resin-polyvinyl butyral composite material proposed in the present application introduces polyvinyl butyral into the epoxy resin, and utilizes the good flexibility, tensile strength and other mechanical properties of polyvinyl butyral and its good compatibility with epoxy resin and increased thixotropy of epoxy resin to improve the shortcomings of epoxy resin such as high brittleness and easy cracking in low-temperature environments. Compared with the epoxy resin of the same proportion without polyvinyl butyral, whether it is directly cured by pure slurry, or cured after adding fillers or made into fiberglass, it has higher mechanical properties such as low-temperature compressive strength and flexural strength, meets the application requirements of epoxy resin materials in low-temperature environments, improves the mechanical properties and durability of epoxy resin without affecting the appearance of epoxy resin, and expands its application range.
[0074] In the curable slurry of the epoxy resin-polyvinyl butyral composite material of the present application, the small molecule amine curing agent and the amino silane coupling agent are good solvents for polyvinyl butyral and can form a homogeneous and transparent solution, while the epoxy resin, the polymer amine curing agent and the epoxy-based reactive diluent cannot directly dissolve the polyvinyl butyral, and are only used to dilute the above solution and disperse the polyvinyl butyral therein, and precipitate a small part of the polyvinyl butyral to form a thixotropic gel, so that the curable slurry of the epoxy resin-polyvinyl butyral composite material has thixotropic properties when it is not cured. Denaturation, and as the small molecule amine curing agent as the solvent of polyvinyl butyral is continuously consumed by the polymerization reaction of epoxy resin, polyvinyl butyral is continuously precipitated in situ, and the thickening performance is gradually enhanced. When the slurry is thickly applied on the facade, it can effectively counteract the viscosity decrease caused by the exothermic temperature rise of the reaction, so that the slurry always remains non-sagging during the curing process, solving the problem of strong sag in the facade construction of ordinary epoxy resin, meeting the application needs of epoxy resin materials in facade construction, improving its appearance properties such as flatness and uniformity after curing, and expanding the application range of epoxy resin materials.
[0075] In the preparation method of the curable slurry of the epoxy resin-polyvinyl butyral composite material of the present application, the small molecule amine curing agent of the epoxy resin is also used as the solvent of the polyvinyl butyral to introduce it into the epoxy resin, thereby avoiding the additional addition of solvent, and there is no need for high-temperature solvent removal and additional process recovery or harmless discharge of solvent. There is no problem of solvent residue, which is safe, energy-saving and environmentally friendly. It can also avoid the adverse effects of solvent residue on the mechanical properties and durability of the epoxy resin material. The organic amine itself participates in the reaction as an epoxy resin curing agent and can achieve a high conversion rate. Under the appropriate ratio, it can basically achieve no organic amine residue, which is also safe and environmentally friendly. Therefore, it is particularly suitable for application scenarios such as room temperature curing and open construction.
[0076] The curable slurry of the epoxy resin-polyvinyl butyral composite material of the present application is modified based on the existing epoxy resin, and has wide universality for various existing epoxy resins and amine curing agents.
[0077] The curable slurry of the epoxy resin-polyvinyl butyral composite material of the present application can be used alone as an adhesive or a resin casting, or can be combined with fillers or fiber-reinforced materials to produce coatings, polymer mortars, and fiberglass as materials. It is widely used in the fields of repair, reinforcement, corrosion protection, and appearance beautification of construction, water transportation, roads and bridges, and other projects, and has broad application prospects.
[0078] The above embodiments are only used to illustrate the technical solution of the present application but not to limit it. The present application is described in detail with reference to the preferred embodiments. It should be understood by those skilled in the art that the technical solution of the present application can be modified or replaced by equivalents without departing from the spirit and scope of the technical solution of the present application, and should be included in the scope of the claims of the present application.
Claims
1. A curable slurry of epoxy resin-polyvinyl butyral composite material, characterized in that: include: A component and B component; The A component includes the following raw materials in the following mass ratios: Epoxy resin: 100; Epoxy reactive diluent: 0-30; The B component includes the following raw materials in the following mass ratios: Small molecule amine curing agent: 10-50; Polymer amine curing agent: 0~40; Polyvinyl butyral: 1-10; Amine silane coupling agent: 0~10.
2. The curable slurry of epoxy resin-polyvinyl butyral composite material according to claim 1, characterized in that: The epoxy resin is a solvent-free epoxy resin with a functionality of not less than 2.
3. The curable slurry of epoxy resin-polyvinyl butyral composite material according to claim 1 or 2, characterized in that: The epoxy resin comprises one or more combinations of the following substances: bisphenol A glycidyl ether, hydrogenated or halogenated or hydrocarbon-substituted bisphenol A glycidyl ether, bisphenol F glycidyl ether, hydrogenated or halogenated or hydrocarbon-substituted bisphenol F glycidyl ether, bisphenol S glycidyl ether, hydrogenated or halogenated or hydrocarbon-substituted bisphenol S glycidyl ether, hydrogenated or halogenated or hydrocarbon-substituted hydroquinone diglycidyl ether, polyphenol glycidyl ether, linear phenol resin glycidyl ether, aliphatic polyol glycidyl ether, aliphatic polyacid glycidyl ester, glycidylamine type epoxy resin with a functionality of not less than 2, alicyclic epoxy resin with a functionality of not less than 2, epoxidized olefin with a functionality of not less than 2, triglycidyl isocyanurate, hydantoin epoxy resin with a functionality of not less than 2, terminal epoxy polyether or polyester with a functionality of not less than 2, and epoxy polysiloxane with a functionality of not less than 2.
4. The curable slurry of epoxy resin-polyvinyl butyral composite material according to claim 1, characterized in that: The epoxy-based reactive diluent includes one or more combinations of the following substances: glycidyl ether of a polyol having a carbon number not greater than 10 and a functionality not less than 2, polyethylene glycol having a viscosity not greater than 300 mPa·s, polypropylene glycol diglycidyl ether having a viscosity not greater than 300 mPa·s, silicone glycidyl ether having a viscosity not greater than 300 mPa·s and a functionality not less than 2, and di(2-epoxypropyl) ether.
5. The curable slurry of epoxy resin-polyvinyl butyral composite material according to claim 1, characterized in that: The small molecule amine curing agent includes one or more combinations of the following substances: a monoamine having 2 to 18 carbon atoms and containing one primary amine group, and a polyamine having 2 to 18 carbon atoms and containing no less than 2 tertiary or lower amine groups.
6. The curable slurry of epoxy resin-polyvinyl butyral composite material according to claim 1, characterized in that: The polymer amine curing agent includes one or more combinations of the following substances: amino silicone oil, solvent-free polyethyleneimine, solvent-free amino silane coupling agent condensation product, and polyamide with a solidification point not greater than 40°C.
7. The curable slurry of epoxy resin-polyvinyl butyral composite material according to claim 1, characterized in that: The polyvinyl butyral comprises one or more combinations of the following substances: polyvinyl butyral with a molecular weight of 5000 to 250000; the polyvinyl butyral is in powder form, fine granule form or flake form.
8. The curable slurry of epoxy resin-polyvinyl butyral composite material according to claim 1, characterized in that: The amino silane coupling agent comprises: a structural formula of R 1 R 2 x Si(OR 3 ) 3-x Silane coupling agent; wherein R 1 is a hydrocarbon group having 2 to 12 carbon atoms and containing one primary amino group, or R 1 A hydrocarbon group having 2 to 12 carbon atoms and containing at least 2 tertiary or lower amine groups; R 2 and R 3 All are hydrocarbon groups with 1 to 4 carbon atoms; The range of x is 0≤x≤2.
9. A method for preparing a curable slurry of epoxy resin-polyvinyl butyral composite material, characterized in that: The steps include: Weigh component A and component B respectively; wherein component A comprises the following raw materials in the following mass ratios: epoxy resin 100; epoxy reactive diluent 0-30; component B comprises the following raw materials in the following mass ratios: small molecule amine curing agent 10-50; polymer amine curing agent 0-40; polyvinyl butyral 1-10; Amine silane coupling agent 0~10; Prepare the A component; when the A component has more than one raw material, mix all the raw materials of the A component and stir them thoroughly to obtain the A component; Prepare the B component; mix the small molecule amine curing agent and the polyvinyl butyral and stir them thoroughly until the polyvinyl butyral is fully dissolved to form a first transparent solution; when the amount of the amino silane coupling agent is not 0, mix the amino silane coupling agent with the small molecule amine curing agent and the polyvinyl butyral and stir them thoroughly until the polyvinyl butyral is fully dissolved to form a second transparent solution; when the amount of the polymer amine curing agent is not 0, mix the polymer amine curing agent with the first transparent solution or the second transparent solution and stir them thoroughly to obtain the B component; The component A and the component B are mixed and stirred thoroughly to obtain a curing slurry of the epoxy resin-polyvinyl butyral composite material.
10. The preparation method according to claim 9, characterized in that: The preparation process of component A is supplemented by heating and then mixing with component B; And / or, the polyvinyl butyral is ground or pulverized before mixing; And / or, the polyvinyl butyral is assisted by heating during the mixing process; And / or, the polyvinyl butyral is assisted by ultrasound during the mixing process.
Citation Information
Patent Citations
Liquid epoxy resin composition and electronic component using the same
JP2012172054A
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