Room temperature curing two-component epoxy potting adhesive based on modified dimer acid epoxy and application thereof

Abstract

The application provides a room temperature curing two-component epoxy pouring sealant based on modified dimer acid epoxy and application thereof, which comprises components A and B; the raw materials for preparing the component A comprise 23-27% of a compound with the structure of formula I, 23-27% of glycidyl ether, 47.5-48.3% of hollow glass microbeads, 0.08-0.12% of a rheological additive and 1.8-2.3% of a flame retardant; the raw materials for preparing the component B comprise 33-37% of epoxy soybean oil modified dimer acid, 42-48% of dimer acid modified polyamide and 18-23% of a toughening agent. The pouring sealant has excellent open time, high board-core glass strength, flat tensile strength, flat compression strength, good sound insulation performance, excellent point load and static load experiment performance and high board-core shear force by using the compound with the structure of formula I, the epoxy soybean oil modified dimer acid with the structure of formula II and the dimer acid modified polyamide with the structure of formula III.

Description

Technical Field

[0001] This invention belongs to the field of potting compound technology, and particularly relates to a room temperature curing two-component epoxy potting compound based on modified dimer acid epoxy and its application. Background Technology

[0002] Traditional rail transit systems use a honeycomb aluminum panel + epoxy potting compound solution. Because the honeycomb aluminum panel provides good support, the traditional epoxy potting compound only needs to achieve the bonding function and does not require additional compressive or tensile strength.

[0003] However, in order to reduce weight, the supporting honeycomb aluminum panel has been replaced with a perforated PP panel, which needs to be filled with glue to bond to the substrate. At the same time, the glue needs to have sufficient tensile strength, compressive strength and toughness to meet the actual application scenarios. Summary of the Invention

[0004] In view of this, the purpose of the present invention is to provide a room temperature curing two-component epoxy potting compound of dimer acid epoxy and its application. The potting compound has excellent open time, high plate-core glass strength, tensile strength and compressive strength, good sound insulation performance, excellent performance in point load and static load tests, and also has high plate-core shear force.

[0005] This invention provides a room temperature curing two-component epoxy potting compound based on modified dimer acid epoxy, comprising component A and component B;

[0006] By mass fraction, the raw materials for preparing component A include 23-27% of a compound having the structure of formula I, 23-27% of glycidyl ether, 47.5-48.3% of hollow glass microspheres, 0.08-0.12% of rheology modifier, and 1.8-2.3% of flame retardant;

[0007] Formula I;

[0008] The raw materials for component B include 33-37% epoxidized soybean oil-modified dimer acid, 42-48% dimer acid-modified polyamide, and 18-23% toughening agent.

[0009] Preferably, the epoxidized soybean oil modified dimer acid has the structure of Formula II:

[0010] Formula II;

[0011] In Formula II, R is the remaining group of the dimer acid after removing the two carboxyl groups;

[0012] It is a partial group of epoxidized soybean oil.

[0013] Preferably, the dimer acid-modified polyamide has the structure of Formula III:

[0014] Formula III;

[0015] In Formula III, R represents the remaining group of the dimer acid after removing the two carboxyl groups.

[0016] Preferably, the rheology modifier is selected from BYK rheology modifiers, and more preferably from RHEOBYK-R 605 or 607;

[0017] The flame retardant is selected from Sanko Japan, brand name HCA, and its component is DOPO;

[0018] The toughening agent is selected from core-shell structured rubber, specifically from the Japanese brand Kanekachi MX153.

[0019] Preferably, the compound having the structure of Formula I is prepared by the following method:

[0020] Under choline catalysis, dimer glycol and epichlorohydrin react to obtain chlorohydrin ether, and then add NaOH aqueous solution to obtain epoxy-terminated dimer glycol modified epoxy. After vacuum distillation, washing with water, separation, and drying, a compound with the structure of formula I is obtained.

[0021] Preferably, the epoxidized soybean oil-modified dimer acid having the structure of Formula II is prepared by the following method:

[0022] Epoxidized soybean oil and dimer acid were mixed and heated to a viscosity of 4300-4800 cps. The mixture was then cooled and capped with 2,3-dimethylcyclohexylamine to obtain epoxidized soybean oil modified dimer acid with the structure of formula II.

[0023] Preferably, the heating reaction temperature is 105~115℃ and the time is 28~33min.

[0024] Preferably, the dimer acid-modified polyamide having the structure of Formula III is prepared by the following method:

[0025] Dimer acid and hexamethylenediamine are mixed and reacted under vacuum. The viscosity of the system is above 6000 cps. The system is then capped with 2,3-dimethylcyclohexylamine. The reaction is stopped when the viscosity no longer increases, yielding a dimer acid-modified polyamide with the structure of formula III.

[0026] Preferably, the reaction temperature under vacuum is 65~75℃ and the reaction time is 110~130min.

[0027] This invention provides an application of the room temperature curing two-component epoxy potting compound described above in the potting of rail transit flooring.

[0028] This invention provides a room-temperature curing two-component epoxy potting compound based on modified dimer acid epoxy, comprising component A and component B. By mass fraction, component A comprises 23-27% of a compound having the structure of formula I, 23-27% glycidyl ether, 47.5-48.3% hollow glass microspheres, 0.08-0.12% rheology modifier, and 1.8-2.3% flame retardant. Component B comprises 33-37% epoxidized soybean oil-modified dimer acid, 42-48% dimer acid-modified polyamide, and 18-23% toughening agent. By employing a compound having the structure of formula I, epoxidized soybean oil-modified dimer acid having the structure of formula II, and dimer acid-modified polyamide having the structure of formula III, this invention enables the potting compound to exhibit excellent open time, high sheet-to-core glass strength, high tensile strength, and high compressive strength, good sound insulation performance, excellent performance in point load and static load tests, and high sheet-to-core shear force. Attached Figure Description

[0029] Figure 1 This is a schematic diagram of the structure of the rail transit floor provided by the present invention. Detailed Implementation

[0030] This invention provides a room temperature curing two-component epoxy potting compound based on modified dimer acid epoxy, comprising component A and component B;

[0031] By mass fraction, the raw materials for preparing component A include 23-27% of a compound having the structure of formula I, 23-27% of glycidyl ether, 47.5-48.3% of hollow glass microspheres, 0.08-0.12% of rheology modifier, and 1.8-2.3% of flame retardant;

[0032] Formula I;

[0033] The raw materials for component B include 33-37% of a three-dimensional curing agent (epoxidized soybean oil modified dimer acid), 42-48% of a linear curing agent (dimer acid modified polyamide), and 18-23% of a toughening agent.

[0034] This invention provides a room temperature curing two-component epoxy potting compound based on modified dimer acid epoxy, comprising component A.

[0035] The raw material for preparing component A in this invention comprises 23-27% of a compound having the structure of Formula I, specifically at a content of 23%, 24%, 25%, 26%, or 27%. This compound can increase the toughness of the potting compound and improve its impact resistance. The compound having the structure of Formula I has the following structure:

[0036] Formula I.

[0037] The compound having the structure of Formula I described in this invention is prepared by the following method:

[0038] Under choline catalysis, dimer glycol and epichlorohydrin react to obtain chlorohydrin ether, and then add NaOH aqueous solution to obtain epoxy-terminated dimer glycol modified epoxy. After vacuum distillation, washing with water, separation, and drying, a compound with the structure of formula I is obtained.

[0039] The dimer glycol used in this invention is selected from the brand Radianol 1990, CAS number 147853-32-5, with a molecular weight of approximately 550. The reaction temperature of the dimer glycol and epichlorohydrin in this invention is 30-40°C, and the reaction time is 4-6 hours. The vacuum distillation temperature in this invention is 40-60°C; this invention removes the solvent and residual epichlorohydrin through vacuum distillation.

[0040] The raw material for preparing component A in this invention includes 23-27% glycidyl ether, specifically 23%, 24%, 25%, 26%, or 27%; it can reduce viscosity and improve processing performance. The glycidyl ether used in this invention is HUNTSMAN glycidyl ether.

[0041] The raw materials for preparing component A in this invention include 47.5% to 48.3% hollow glass microspheres, specifically 47.5%, 47.6%, 47.8%, 47.9%, 48.0%, 48.1%, 48.2%, or 48.3%. The hollow glass microspheres, as fillers, enable the potting compound to be lighter.

[0042] The raw materials for preparing component A in this invention include 0.08-0.12% rheology modifier, specifically 0.08%, 0.09%, 0.10%, 0.11%, or 0.12%; it can improve thixotropic properties. The rheology modifier in this invention is selected from BYK rheology modifiers; preferably RHEOBYK-R 605 or 607 rheology modifiers, which can balance the stress generated during curing and sizing.

[0043] The raw materials for preparing component A in this invention include 1.8-2.3% flame retardant; the specific content can be 1.8%, 1.9%, 2.0%, 2.1%, 2.2%, or 2.3%; the flame retardant is an environmentally friendly flame retardant, giving the potting compound flame-retardant function. The flame retardant used in this invention is selected from the phosphorus-based flame retardant Japanese Sanko brand HCA, and its component is DOPO.

[0044] The room temperature curing two-component epoxy potting compound provided by the present invention includes component B; the raw materials for preparing component B include 33-37% epoxidized soybean oil modified dimer acid, 42-48% dimer acid modified polyamide and 18-23% toughening agent.

[0045] The raw materials for preparing component B in this invention include 33-37% epoxidized soybean oil-modified dimer acid, specifically 33%, 34%, 35%, 36%, or 37%. The epoxidized soybean oil-modified dimer acid is a curing agent. The epoxidized soybean oil-modified dimer acid has a structure of formula II:

[0046] Formula II;

[0047] In Formula II, R is the remaining group of the dimer acid after removing the two carboxyl groups; the number of carbons in the dimer acid is preferably 36;

[0048] It is a partial group of epoxidized soybean oil.

[0049] The epoxidized soybean oil-modified dimer acid with Formula II structure described in this invention is prepared by the following method:

[0050] Epoxidized soybean oil and dimer acid were mixed and heated to a viscosity of 4300-4800 cps. The mixture was then cooled and capped with 2,3-dimethylcyclohexylamine to obtain epoxidized soybean oil modified dimer acid with the structure of formula II.

[0051] The preferred reaction route for epoxidized soybean oil and dimer acid used in this invention is as follows:

[0052] .

[0053] In this invention, the molar ratio of the curing agent epoxidized soybean oil to dimer acid is 1:1.6; the equivalent amount of 2,3-dimethylcyclohexylamine added is 0.1. In this invention, the heating reaction temperature is 105~115℃, specifically 105℃, 110℃, or 115℃; the time is 28~33min, specifically 28min, 29min, 30min, 31min, 32min, or 33min. In this invention, the system viscosity is preferably 4300~4800 cps (at 40℃), specifically 4300 cps, 4350 cps, 4400 cps, 4450 cps, 4600 cps, 4650 cps, 4700 cps, 4750 cps, or 4800 cps; end-capping is performed after cooling to 70℃.

[0054] The raw materials for preparing component B in this invention include 42-48% of a curing agent, dimer acid-modified polyamide, specifically 42%, 43%, 44%, 45%, 46%, 47%, or 48%; it is a high-performance curing agent with strong toughening and impact resistance. The dimer acid-modified polyamide described in this invention has the structure of formula III:

[0055] Formula III;

[0056] In Formula III, R is the remaining group of the dimer acid after removing the two carboxyl groups; the number of carbons in the dimer acid is preferably 36.

[0057] The dimer acid-modified polyamide having the structure of Formula III described in this invention is prepared by the following method:

[0058] Dimer acid and hexamethylenediamine are mixed and reacted under vacuum. The viscosity of the system is above 6000 cps. The system is then capped with 2,3-dimethylcyclohexylamine. The reaction is stopped when the viscosity no longer increases, yielding a dimer acid-modified polyamide with the structure of formula III.

[0059] In this invention, the molar ratio of dimeric acid to hexamethylenediamine is 1.1:1; the equivalent amount of 2,3-dimethylcyclohexylamine added is 0.1. In this invention, the reaction temperature under vacuum is 65~75℃, specifically 65℃, 70℃, or 75℃; the reaction time is 110~130 min, specifically 110 min, 115 min, 120 min, 125 min, or 130 min.

[0060] The reaction route of the dimer acid-modified polyamide having the structure of Formula III described in this invention is as follows:

[0061] .

[0062] In this invention, the raw materials for preparing component B include 18-23% toughening agent, specifically 18%, 19%, 20%, 21%, 22%, or 23%. The toughening agent is selected from core-shell structured rubber, which can improve the impact strength of the potting compound at low temperatures; in a specific embodiment, the toughening agent is Kanekachi MX153 from Japan.

[0063] The room-temperature curing two-component epoxy potting compound based on modified dimer acid epoxy described in this invention is preferably prepared according to the following method:

[0064] Component A is obtained by uniformly mixing 23-27% of a compound having the structure of Formula I, 23-27% of glycidyl ether, 47.5-48.3% of hollow glass microspheres, 0.08-0.12% of rheology modifier and 1.8-2.3% of flame retardant;

[0065] Component B is obtained by uniformly mixing 33-37% of epoxidized soybean oil modified dimer acid, 42-48% of dimer acid modified polyamide, and 18-23% of toughening agent.

[0066] Component A and component B are mixed to obtain a room-temperature curing two-component epoxy potting compound based on modified dimer acid epoxy.

[0067] In this invention, the mass ratio of component A to component B is 3:1.

[0068] The room-temperature curing two-component potting compound provided by this invention comprises epoxy-terminated raw materials including compounds with the structure of Formula I; the curing agents include epoxidized soybean oil-modified dimer acid and epoxidized soybean oil-modified dimeramide. This enables the two curing agents to achieve the potting effect. This invention regulates the reaction activity and controls the curing rate by adjusting the reaction steric hindrance and the secondary amine generated in the reaction.

[0069] This invention provides an application of the room temperature curing two-component epoxy potting compound described above in the potting of rail transit flooring.

[0070] Specifically, the rail transit floor of the present invention includes a first fireproof board, a first adhesive board, a polypropylene board, a second adhesive board, and a second fireproof board arranged in sequence.

[0071] A two-component epoxy potting compound is used to pot the first adhesive plate, the polypropylene plate, and the second adhesive plate.

[0072] See Figure 1 , Figure 1 This is a schematic diagram of the structure of the rail transit floor provided in this invention.

[0073] In this invention, the two-component epoxy potting compound plays a supporting role in the floor, strengthens the compression modulus of the foam board, and has a certain compression deformation, which meets the requirements of vehicle aging.

[0074] To further illustrate the present invention, the following detailed description, in conjunction with embodiments, of a room-temperature curing two-component epoxy potting compound based on modified dimer acid epoxy and its applications, is provided by the present invention, but should not be construed as limiting the scope of protection of the present invention.

[0075] Preliminary example

[0076] Dimeric acid glycol (Oleon's brand RADIANO L 1990, CAS number: 147853-32-5, molecular weight approximately 550) was mixed with epichlorohydrin, and choline was added as a catalyst. After the formation of chlorohydrin ether, NaOH aqueous solution was added and stirred to generate epoxy-terminated dimer acid glycol modified epoxy. Then, the solvent and residual epichlorohydrin were removed by liquid-liquid vacuum distillation. After washing with water, the mixture was separated and dried in a vacuum oven to obtain a compound with the structure of formula I.

[0077] Epoxidized soybean oil and dimer acid were added to the system in a molar ratio of 1:1.6. The system was heated under vacuum at 110°C for 30 minutes. When the viscosity of the system reached 4500 cps (at 40°C), the temperature was lowered to 70°C and 0.1 equivalent of 2,3-dimethylcyclohexylamine was added for end-capping. The reaction was stopped when the viscosity of the system stopped increasing, resulting in epoxidized soybean oil modified dimer acid with the structure of formula II.

[0078] Dimeric acid and hexamethylenediamine were added to the system at a molar ratio of 1.1:1. The reaction was initiated at 70°C under vacuum and carried out for 2 hours. When the viscosity of the system reached above 6000 cps (at 40°C), 0.1 equivalents of 2,3-dimethylcyclohexylamine were added for end-capping. The reaction was stopped once the viscosity no longer increased, yielding a dimer acid-modified polyamide with the structure of formula III.

[0079] Example 1

[0080] Component A was obtained by mixing 25% of the compound with the structure of Formula I prepared in the preparatory example, 25% of HUNTSMAN glycidyl ether, 47.9% of HX-60M hollow glass microspheres (purchased from Hebei Haoxing), 0.1% of BYK rheology modifier (RHEOBYK-R 605), and 2% of reactive phosphorus flame retardant (Japan Sanko HCA).

[0081] Component B is obtained by mixing 35% of epoxidized soybean oil modified dimer acid with Formula II structure, 45% of dimer acid modified polyamide with Formula III structure, and 20% of core-shell structure rubber (Kanebuchi MX153, Japan).

[0082] Mix component A and component B at a mass ratio of 3:1 to obtain a room temperature curing two-component epoxy potting compound.

[0083] The properties of the potting compound prepared in Example 1 were tested, and the results are shown in Table 1:

[0084] Table 1

[0085]

[0086] Comparative Example 1

[0087] Compared with Example 1, the difference is that the compound with the structure of Formula I in the raw materials for preparing component A is replaced with dimer acid modified epoxy resin (Loho EDP-171).

[0088] The potting compound prepared in Comparative Example 1 was subjected to performance testing, and the results are shown in Table 2:

[0089] Table 2

[0090]

[0091] Comparative Example 2

[0092] Compared to Example 1, the difference lies in that the epoxidized soybean oil-modified dimer acid with the Formula II structure in the raw materials for component B is replaced with a flexible modifier (Hycar). ® 1300x3).

[0093] The potting compound prepared in Comparative Example 2 was subjected to performance testing, and the results are shown in Table 3:

[0094] Table 3

[0095]

[0096] Comparative Example 3

[0097] Compared with Example 1, the difference is that the dimer acid modified polyamide with the formula III structure in the raw materials for preparing component B is replaced with a polyamide curing agent (Jegao J-1158).

[0098] The potting compound prepared in Comparative Example 3 was subjected to performance testing in this invention, and the results are shown in Table 4:

[0099] Table 4

[0100]

[0101] Comparative Example 4

[0102] Compared with Example 1, the difference is that the dimer acid modified polyamide with the structure of Formula III in the raw materials for preparing component B is replaced with a modified polyamide curing agent (Hensamine-5115B).

[0103] The potting compound prepared in Comparative Example 4 was subjected to performance testing in this invention, and the results are shown in Table 5:

[0104] Table 5

[0105]

[0106] As can be seen from the above embodiments, the present invention provides a room-temperature curing two-component epoxy potting compound based on modified dimer acid epoxy, comprising component A and component B. By mass fraction, component A comprises 23-27% of a compound having the structure of formula I, 23-27% glycidyl ether, 47.5-48.3% hollow glass microspheres, 0.08-0.12% rheology modifier, and 1.8-2.3% flame retardant. Component B comprises 33-37% epoxidized soybean oil-modified dimer acid, 42-48% dimer acid-modified polyamide, and 18-23% toughening agent. By employing a compound having the structure of formula I, epoxidized soybean oil-modified dimer acid having the structure of formula II, and dimer acid-modified polyamide having the structure of formula III, the potting compound exhibits excellent open time, high sheet-to-core glass strength, high tensile strength, and high compressive strength, good sound insulation performance, excellent performance in point load and static load tests, and high sheet-to-core shear force.

[0107] The above description is only a preferred embodiment of the present invention. It should be noted that for those skilled in the art, several improvements and modifications can be made without departing from the principle of the present invention, and these improvements and modifications should also be considered within the scope of protection of the present invention.

Claims

1. A room-temperature curing two-component epoxy potting compound based on modified dimer acid epoxy, comprising component A and component B; By mass fraction, the raw materials for preparing component A include 23-27% of a compound having the structure of formula I, 23-27% of glycidyl ether, 47.5-48.3% of hollow glass microspheres, 0.08-0.12% of rheology modifier, and 1.8-2.3% of flame retardant; Formula I; The raw materials for component B include 33-37% epoxidized soybean oil-modified dimer acid, 42-48% dimer acid-modified polyamide, and 18-23% toughening agent.

2. The room temperature curing two-component epoxy potting compound according to claim 1, characterized in that, The epoxidized soybean oil modified dimer acid has a structure of formula II: Formula II; In Formula II, R is the remaining group of the dimer acid after removing the two carboxyl groups; It is a partial group of epoxidized soybean oil.

3. The room temperature curing two-component epoxy potting compound according to claim 1, characterized in that, The dimer acid-modified polyamide has the structure of formula III: Formula III; In Formula III, R is the remaining group of the dimer acid after removing the two carboxyl groups.

4. The room temperature curing two-component epoxy potting compound according to claim 1, characterized in that, The rheology modifier is selected from BYK rheology modifiers; The flame retardant is selected from Sanko Japan, brand name HCA, and its component is DOPO; The toughening agent is selected from core-shell structured rubber, specifically the Japanese brand Kanekachi MX153.

5. The room-temperature curing two-component epoxy potting compound according to claim 1, characterized in that, Compounds having the structure of Formula I are prepared by the following method: Under choline catalysis, dimer glycol and epichlorohydrin react to obtain chlorohydrin ether, and then add NaOH aqueous solution to obtain epoxy-terminated dimer glycol modified epoxy. After vacuum distillation, washing with water, separation, and drying, a compound with the structure of formula I is obtained.

6. The room temperature curing two-component epoxy potting compound according to claim 2, characterized in that, Epoxidized soybean oil-modified dimer acid with the structure of Formula II was prepared by the following method: Epoxidized soybean oil and dimer acid were mixed and heated to a viscosity of 4300-4800 cps. The mixture was then cooled and capped with 2,3-dimethylcyclohexylamine to obtain epoxidized soybean oil modified dimer acid with the structure of formula II.

7. The room temperature curing two-component epoxy potting compound according to claim 6, characterized in that, The heating reaction temperature is 105~115℃, and the time is 28~33min.

8. The room temperature curing two-component epoxy potting compound according to claim 3, characterized in that, Dimeric acid-modified polyamides having the structure of Formula III are prepared by the following method: Dimer acid and hexamethylenediamine are mixed and reacted under vacuum. The viscosity of the system is above 6000 cps. The system is then capped with 2,3-dimethylcyclohexylamine. The reaction is stopped when the viscosity no longer increases, yielding a dimer acid-modified polyamide with the structure of formula III.

9. The room temperature curing two-component epoxy potting compound according to claim 8, characterized in that, The reaction temperature under vacuum is 65~75℃, and the reaction time is 110~130min.

10. The application of the room temperature curing two-component epoxy potting compound according to any one of claims 1 to 9 in the potting of rail transit floor.

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