Flexible epoxy pouring sealant and preparation method thereof

Abstract

The invention provides a flexible epoxy pouring sealant. The flexible epoxy pouring sealant is composed of a component A and a component B in a mass ratio of 1: (0.8-1.2), the component A is prepared from the following raw materials in percentage by mass: 20-40% of epoxy resin; 10-20% of an epoxy diluent; 40-60% of a filler; 0.5 to 1.5 percent of a white carbon black thixotropic agent; 0.5 to 1.5 percent of an anti-aging agent; 0.1-1% of a defoaming agent; 0.1-1% of carbon black; the component B is prepared from the following raw materials in percentage by mass: 10-20% of a polyamide curing agent; 5 to 10% of aminoethyl piperazine; 5-10% of a curing accelerator; 0.5-5% of polyether amine; 5-10% of a modified phenolic aldehyde amine curing agent; 50-70% of a filler; 0.5-3% of a tackifier; 0.1-1% of a defoaming agent; and 0.1-1% of a dispersant. Compared with the prior art, the flexible epoxy pouring sealant provided by the invention adopts specific components with specific contents, realizes relatively good overall interaction, has good flexibility on the basis of meeting basic use performance requirements of the pouring sealant, can be used for relatively well bonding low-surface-energy base materials such as PP (polypropylene) and PTFE (polytetrafluoroethylene), and has the advantages of low surface energy consumption, low cost and the like. The method is suitable for the security camera field.

Description

Technical Field

[0001] The invention relates to the technical field of epoxy potting adhesive, and more specifically to a flexible epoxy potting adhesive and a preparation method thereof. Background Art

[0002] At present, in the field of security cameras, the tail wires at the bottom of the camera housing are mainly fixed by potting glue, which plays the role of structural bonding, waterproofing and airtightness. Since security cameras are mainly used outdoors, there are strict requirements for the aging resistance of the glue. A suitable potting glue needs to have the following properties: high adhesion to metal, plastic and other shell substrates, high hardness, good flexibility, good resistance to high and low temperature impact, excellent water resistance and corrosion resistance, etc. In general, epoxy potting glue is the most suitable.

[0003] However, epoxy adhesives are usually too strong and not tough enough, and are prone to cracking when facing high and low temperature changes. At the same time, with the continuous iteration of customer technology, epoxy adhesives also face the problem of surface adhesion of various difficult-to-bond substrates. At present, it is a major trend in the market for composite materials and polymer plastics to replace traditional metal materials. The camera housing materials used by customers in the field of security cameras have also changed from the original metal aluminum to plastic PC (polycarbonate), and will later change to PP (polypropylene) and even PTFE (polytetrafluoroethylene). As we all know, PTFE is an excellent demolding material, which means that it is difficult to find glue that can bond PTFE. In order to solve this problem of customers, it is necessary to develop epoxy potting glue; but there is currently no epoxy glue on the market that can bond PP and PTFE substrates well. Summary of the invention

[0004] In view of this, the object of the present invention is to provide a flexible epoxy potting adhesive and a preparation method thereof. The flexible epoxy potting adhesive provided by the present invention has good flexibility on the basis of meeting the basic performance requirements of the potting adhesive, and can perform good adhesion to low surface energy substrates such as PP (polypropylene), PTFE (polytetrafluoroethylene), etc., and is suitable for the field of security cameras.

[0005] The present invention provides a flexible epoxy potting adhesive, which is composed of a component A and a component B in a mass ratio of 1: (0.8-1.2);

[0006] The A component is prepared from the following raw materials in percentage by mass:

[0007] Epoxy resin 20~40%;

[0008] Epoxy diluent 10~20%;

[0009] Filler 40~60%;

[0010] White carbon black thixotropic agent 0.5~1.5%;

[0011] Anti-aging agent 0.5~1.5%;

[0012] Defoaming agent 0.1~1%;

[0013] Carbon black 0.1~1%;

[0014] The B component is prepared from the following raw materials in percentage by mass:

[0015] Polyamide curing agent 10~20%;

[0016] Aminoethylpiperazine 5-10%;

[0017] Curing accelerator 5~10%;

[0018] Polyetheramine 0.5~5%;

[0019] Modified phenolic amine curing agent 5~10%;

[0020] Filler 50~70%;

[0021] Thickener 0.5~3%;

[0022] Defoaming agent 0.1~1%;

[0023] Dispersant 0.1~1%.

[0024] Preferably, the epoxy resin is selected from one or more of bisphenol A epoxy resin, bisphenol F epoxy resin, and aliphatic epoxy resin.

[0025] Preferably, the epoxy diluent is selected from one or more of Hubei Green Home LS-622 active diluent, Anhui Xinyuan XY-622 active diluent, Hubei Green Home LS-AGE active diluent, and Anhui Xinyuan XY-748 active diluent.

[0026] Preferably, the filler is selected from aluminum hydroxide and / or calcium carbonate.

[0027] Preferably, the polyetheramine is selected from German BASF EC-130 polyetheramine curing agent and / or American HUNTSMANEDR-148 polyetheramine curing agent.

[0028] The present invention also provides a method for preparing the flexible epoxy potting adhesive described in the above technical solution, comprising the following steps:

[0029] a) mixing epoxy resin, epoxy diluent, filler, white carbon black thixotropic agent, carbon black, anti-aging agent and defoaming agent, and performing a first dispersion treatment to obtain component A;

[0030] The polyamide curing agent, aminoethyl piperazine, curing accelerator, polyether amine, modified phenolic amine curing agent, filler, tackifier, defoamer and dispersant are mixed and subjected to a second dispersion treatment to obtain component B;

[0031] b) Mixing the above component A and component B to obtain a flexible epoxy potting adhesive.

[0032] Preferably, the first dispersing process in step a) is carried out in a double planetary disperser; the temperature of the dispersing process is 20°C to 30°C, the speed is 400rpm to 600rpm, the vacuum degree is -0.08MPa to -0.1MPa, and the time is 2h to 4h;

[0033] Preferably, the second dispersing process in step a) is carried out in a double planetary disperser; the temperature of the dispersing process is 20°C~30°C, the rotation speed is 400rpm~600rpm, the vacuum degree is -0.08MPa~-0.1MPa, and the time is 2h~4h.

[0034] Preferably, the filler, white carbon black thixotropic agent and carbon black in step a) are dried before mixing.

[0035] Preferably, the drying treatment is carried out at a temperature of 90° C. to 110° C. and for a time of 45 h to 50 h.

[0036] The invention provides a flexible epoxy potting adhesive, which consists of an A component and a B component in a mass ratio of 1:(0.8-1.2); the A component is prepared from the following raw materials in mass percentage: 20-40% of epoxy resin; 10-20% of epoxy diluent; 40-60% of filler; 0.5-1.5% of white carbon black thixotropic agent; 0.5-1.5% of anti-aging agent; 0.1-1% of defoaming agent; and 0.1-1% of carbon black; the B component is prepared from the following raw materials in mass percentage: 10-20% of polyamide curing agent; 5-10% of aminoethyl piperazine; 5-10% of curing accelerator; 0.5-5% of polyether amine; 5-10% of modified phenolic amine curing agent; 50-70% of filler; 0.5-3% of tackifier; 0.1-1% of defoaming agent; and 0.1-1% of dispersant. Compared with the prior art, the flexible epoxy potting adhesive provided by the present invention adopts specific components with specific contents to achieve better overall interaction. On the basis of meeting the basic performance requirements of the potting adhesive, it has good flexibility and can perform good adhesion to low surface energy substrates such as PP (polypropylene), PTFE (polytetrafluoroethylene), etc., and is suitable for the field of security cameras.

[0037] In addition, the preparation method provided by the present invention has simple process, mild conditions, easy control, low requirements on equipment, and has broad application prospects. DETAILED DESCRIPTION

[0038] The technical solution of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0039] The present invention provides a flexible epoxy potting adhesive, which is composed of a component A and a component B in a mass ratio of 1: (0.8-1.2);

[0040] The A component is prepared from the following raw materials in percentage by mass:

[0041] Epoxy resin 20~40%;

[0042] Epoxy diluent 10~20%;

[0043] Filler 40~60%;

[0044] White carbon black thixotropic agent 0.5~1.5%;

[0045] Anti-aging agent 0.5~1.5%;

[0046] Defoaming agent 0.1~1%;

[0047] Carbon black 0.1~1%;

[0048] The B component is prepared from the following raw materials in percentage by mass:

[0049] Polyamide curing agent 10~20%;

[0050] Aminoethylpiperazine 5-10%;

[0051] Curing accelerator 5~10%;

[0052] Polyetheramine 0.5~5%;

[0053] Modified phenolic amine curing agent 5~10%;

[0054] Filler 50~70%;

[0055] Thickener 0.5~3%;

[0056] Defoaming agent 0.1~1%;

[0057] Dispersant 0.1~1%.

[0058] The present invention provides a flexible epoxy potting adhesive suitable for low surface energy plastic substrates in the field of security cameras and a preparation method thereof, which mainly solves the problem of poor flexibility and brittleness of traditional epoxy potting adhesives, which leads to cracking and poor air tightness after hot and cold shock aging, and solves the problem of no adhesion of traditional epoxy potting adhesives to low surface energy substrates such as PP (polypropylene), PTFE (polytetrafluoroethylene) and the like; through reasonable formula design, the requirements of flexible potting, high adhesion, high aging resistance and adhesion to low surface energy plastic substrates are met at the same time.

[0059] In the present invention, the flexible epoxy potting adhesive is composed of component A and component B in a mass ratio of 1: (0.8-1.2), preferably 1:1.

[0060] In the present invention, the A component is prepared from the following raw materials in percentage by mass:

[0061] Epoxy resin 20~40%;

[0062] Epoxy diluent 10~20%;

[0063] Filler 40~60%;

[0064] White carbon black thixotropic agent 0.5~1.5%;

[0065] Anti-aging agent 0.5~1.5%;

[0066] Defoaming agent 0.1~1%;

[0067] Carbon black 0.1~1%.

[0068] The present invention has no special restrictions on the sources of the epoxy resin, epoxy diluent, filler, white carbon black thixotropic agent, anti-aging agent, defoaming agent, and carbon black, and commercial products well known to those skilled in the art can be used.

[0069] In the present invention, the epoxy resin is preferably selected from one or more of bisphenol A epoxy resin, bisphenol F epoxy resin, and aliphatic epoxy resin, more preferably bisphenol A epoxy resin and aliphatic epoxy resin, or bisphenol F epoxy resin and aliphatic epoxy resin, or bisphenol A epoxy resin.

[0070] In the present invention, the epoxy diluent is preferably selected from one or more of Hubei Green Home LS-622 active diluent, Anhui Xinyuan XY-622 active diluent, Hubei Green Home LS-AGE active diluent, Anhui Xinyuan XY-748 active diluent, more preferably Hubei Green Home LS-622 active diluent, Hubei Green Home LS-AGE active diluent or Anhui Xinyuan XY-622 active diluent.

[0071] In the present invention, the filler is preferably selected from aluminum hydroxide and / or calcium carbonate, more preferably aluminum hydroxide.

[0072] In the present invention, the white carbon black thixotropic agent is preferably CABOT TS720 white carbon black thixotropic agent or Evonik R202 white carbon black thixotropic agent; the anti-aging agent is preferably Taiwan Double Bond TP-10H anti-aging agent or Jiangyin Alte AO-120 anti-aging agent; the defoaming agent is preferably Germany BYK-1790 defoaming agent or Jiangyin Alte ATA-3265 defoaming agent; the carbon black is preferably Hangzhou HZ-6004 carbon black.

[0073] In the present invention, the B component is prepared from the following raw materials in percentage by mass:

[0074] Polyamide curing agent 10~20%;

[0075] Aminoethylpiperazine 5-10%;

[0076] Curing accelerator 5~10%;

[0077] Polyetheramine 0.5~5%;

[0078] Modified phenolic amine curing agent 5~10%;

[0079] Filler 50~70%;

[0080] Thickener 0.5~3%;

[0081] Defoaming agent 0.1~1%;

[0082] Dispersant 0.1~1%.

[0083] The present invention has no particular restrictions on the sources of the polyamide curing agent, aminoethylpiperazine, curing accelerator, polyetheramine, modified phenolic amine curing agent, filler, tackifier, defoamer, and dispersant, and commercially available products known to those skilled in the art may be used.

[0084] In the present invention, the polyamide curing agent is preferably Evonik Ancamide 910 polyamide curing agent, Jiangyin Alte ATA-H270 polyamide curing agent or Shenzhen Jiadida XH-463 polyamide curing agent; the aminoethyl piperazine is preferably Japan TOSOH AEP aminoethyl piperazine or American HUNTSMAN AEP-HP aminoethyl piperazine; the curing accelerator is preferably Jinyu Material HY-12D dodecylphenol and Evonik Ancamine K54 curing accelerator in a mass ratio of 3:1.

[0085] In the present invention, the polyetheramine is preferably selected from German BASF EC-130 polyetheramine curing agent and / or American HUNTSMAN EDR-148 polyetheramine curing agent, more preferably German BASF EC-130 polyetheramine curing agent or American HUNTSMAN EDR-148 polyetheramine curing agent.

[0086] In the present invention, the modified phenolic amine curing agent is preferably Dalian Liansheng LSW-523-1 modified phenolic amine curing agent; the filler is preferably calcium carbonate; the tackifier is preferably German BYK-4510 tackifier or German BYK-4511 tackifier; the defoamer is preferably Jiangyin Alte ATA-3265 defoamer or German BYK-1790 defoamer; the dispersant is preferably Jiangyin Alte ATA-6747 dispersant or German BYK-9076 dispersant.

[0087] At present, traditional epoxy potting glue needs to solve the following two problems: one is how to make epoxy potting glue into a flexible potting product, and the other is how to improve the adhesion of flexible epoxy potting glue to difficult-to-bond substrates such as PP and PTFE. For problem one, the existing technology selects polyamide as a flexible curing agent, but the reaction speed of polyamide is slow and cannot meet the demand for quick fixation of wiring harnesses by potting glue; for problem two, the existing technology can only improve the adhesion of glue to it by surface plasma / flame treatment or primer treatment of the substrate, but the camera is often a special-shaped structure, and the structure is delicate and small, and it is impossible to perform pre-surface treatment. In view of this, the purpose of the present invention is to first prepare an epoxy potting glue with fast curing speed and good flexibility, and secondly, to improve the adhesion to difficult-to-bond substrates such as PP and PTFE without the need for pre-surface treatment.

[0088] The present invention mainly solves the above problems through two approaches: combined screening of epoxy resins and compounding of curing agents. In addition to selecting the conventional combination of bisphenol A+bisphenol F, the epoxy resin also selects aliphatic epoxy resin for toughening and is matched with an epoxy diluent for improving the reaction rate. In the curing agent component, in order to solve the problem of slow curing speed of polyamide, curing accelerators, polyetheramines, aminoethylpiperazine and other curing agent components are selected and compounded, thereby improving the product flexibility and the curing speed. Finally, in order to improve the adhesion to difficult-to-bond substrates such as PTFE, a modified phenolic amine curing agent is additionally added to the curing agent component.

[0089] Compared with the prior art, the present invention solves the problem of epoxy resin brittleness, can still maintain high bonding strength after high and low temperature impact aging, and has a fast curing speed; more importantly, it still has high bonding strength for extremely difficult-to-bond substrates such as PTFE. Experimental results show that the hardness of the glue can reach more than 50 Shore-D after baking at 60°C for 1 hour, the bonding strength for metal AL is greater than 8MPa, and the shear strength can still be maintained at more than 8MPa after 1000 hours of hot and cold shock. For PTFE substrates, the shear strength can reach more than 3.5MPa without any surface treatment and without applying primer.

[0090] The present invention also provides a method for preparing the flexible epoxy potting adhesive described in the above technical solution, comprising the following steps:

[0091] a) mixing epoxy resin, epoxy diluent, filler, white carbon black thixotropic agent, carbon black, anti-aging agent and defoaming agent, and performing a first dispersion treatment to obtain component A;

[0092] The polyamide curing agent, aminoethyl piperazine, curing accelerator, polyether amine, modified phenolic amine curing agent, filler, tackifier, defoamer and dispersant are mixed and subjected to a second dispersion treatment to obtain component B;

[0093] b) Mixing the above component A and component B to obtain a flexible epoxy potting adhesive.

[0094] The present invention firstly mixes epoxy resin, epoxy diluent, filler, white carbon black thixotropic agent, carbon black, anti-aging agent and defoamer, and performs a first dispersion treatment to obtain component A; at the same time, polyamide curing agent, aminoethyl piperazine, curing accelerator, polyether amine, modified phenolic amine curing agent, filler, tackifier, defoamer and dispersant are mixed, and performs a second dispersion treatment to obtain component B;

[0095] In the present invention, the raw materials are the same as those in the above technical solution and will not be described in detail here.

[0096] In the present invention, the first dispersion treatment process is preferably carried out in a double planetary disperser; the temperature of the dispersion treatment is preferably 20°C~30°C, the rotation speed is preferably 400rpm~600rpm, the vacuum degree is preferably -0.08MPa~-0.1MPa, and the time is preferably 2h~4h; the second dispersion treatment process is preferably carried out in a double planetary disperser; the temperature of the dispersion treatment is preferably 20°C~30°C, the rotation speed is preferably 400rpm~600rpm, the vacuum degree is preferably -0.08MPa~-0.1MPa, and the time is preferably 2h~4h.

[0097] In the present invention, the filler, white carbon black thixotropic agent and carbon black are preferably dried before mixing; the drying temperature is preferably 90° C. to 110° C., and the drying time is preferably 45 h to 50 h.

[0098] The preparation method provided by the invention has simple process, mild conditions, easy control, low requirements on equipment, and has broad application prospects.

[0099] The invention provides a flexible epoxy potting adhesive, which consists of an A component and a B component in a mass ratio of 1:(0.8-1.2); the A component is prepared from the following raw materials in mass percentage: 20-40% of epoxy resin; 10-20% of epoxy diluent; 40-60% of filler; 0.5-1.5% of white carbon black thixotropic agent; 0.5-1.5% of anti-aging agent; 0.1-1% of defoaming agent; and 0.1-1% of carbon black; the B component is prepared from the following raw materials in mass percentage: 10-20% of polyamide curing agent; 5-10% of aminoethyl piperazine; 5-10% of curing accelerator; 0.5-5% of polyether amine; 5-10% of modified phenolic amine curing agent; 50-70% of filler; 0.5-3% of tackifier; 0.1-1% of defoaming agent; and 0.1-1% of dispersant. Compared with the prior art, the flexible epoxy potting adhesive provided by the present invention adopts specific components with specific contents to achieve better overall interaction. On the basis of meeting the basic performance requirements of the potting adhesive, it has good flexibility and can perform good adhesion to low surface energy substrates such as PP (polypropylene), PTFE (polytetrafluoroethylene), etc., and is suitable for the field of security cameras.

[0100] In addition, the preparation method provided by the present invention has simple process, mild conditions, easy control, low requirements on equipment, and has broad application prospects.

[0101] In order to further illustrate the present invention, the following examples are provided for detailed description. The raw materials involved in the following examples of the present invention are as follows:

[0102] Epoxy resin: Nan Ya NPEL-128 bisphenol A epoxy resin, Nan Ya NPEL-127E bisphenol A epoxy resin, Nan Ya NPEF-170 bisphenol F epoxy resin, Japan ADEKA EP-4000 aliphatic epoxy resin;

[0103] Epoxy diluent: Hubei Green Home LS-622 active diluent, Anhui Xinyuan XY-622 active diluent, Hubei Green Home LS-AGE active diluent, Anhui Xinyuan XY-748 active diluent;

[0104] Polyamide curing agent: Evonik Ancamide 910 polyamide curing agent, Shenzhen Jiadida XH-463 polyamide curing agent, China, Jiangyin Alte ATA-H270 polyamide curing agent, China;

[0105] Aminoethylpiperazine: Japan TOSOH AEP, USA HUNTSMAN AEP-HP;

[0106] Curing accelerator: Jinyu Materials HY-12D, Evonik Ancamine K54;

[0107] Polyetheramine: German BASF EC-130 polyetheramine curing agent, American HUNTSMAN EDR-148 polyetheramine curing agent;

[0108] Modified phenolic amine curing agent: Dalian Liansheng LSW-523-1 modified amine curing agent from China;

[0109] Filler: China Foshan Jinge DRHY-367 aluminum hydroxide, China Foshan Jinge DRHY-390 aluminum hydroxide, Omya 1-JI calcium carbonate, Omya 2-JI calcium carbonate;

[0110] White carbon black thixotropic agent: CABOT TS720, Evonik R202;

[0111] Tackifier: German BYK BYK-4510, BYK-4511;

[0112] Defoamer: BYK BYK-1790 from Germany, ATA-3265 from Jiangyin, China;

[0113] Dispersant: BYK BYK-9076 from Germany, ATA-6747 from Jiangyin, China;

[0114] Anti-aging agent: Double Bond TP-10H from Taiwan, China, Alte AO-120 from Jiangyin, China;

[0115] Carbon black: Hangzhou HZ-6004.

[0116] Example 1

[0117] Component A: 23 parts by weight of Nan Ya NPEL-128 bisphenol A epoxy resin, 11 parts by weight of Japan ADEKA EP-4000 aliphatic epoxy resin, 13 parts by weight of China Hubei Green Home LS-622 active diluent, 30 parts by weight of Foshan Jinge DRHY-367 aluminum hydroxide, 20 parts by weight of Foshan Jinge DRHY-390 aluminum hydroxide, 1 part by weight of CABOT TS720 white carbon black thixotropic agent, 1 part by weight of Taiwan Double Bond TP-10H anti-aging agent, 0.5 parts by weight of Germany BYK-1790 defoaming agent, and 0.5 parts by weight of Hangzhou HZ-6004 carbon black.

[0118] Component B: 10 parts by weight of Evonik Ancamide 910 polyamide curing agent, 5 parts by weight of Japan TOSOH AEP aminoethyl piperazine, 6 parts by weight of Jinyu Material HY-12D dodecylphenol, 2 parts by weight of Evonik Ancamine K54 curing accelerator, 2 parts by weight of Germany BASF EC-130 polyetheramine curing agent, 8 parts by weight of Dalian Liansheng LSW-523-1 modified phenolic amine curing agent, 65 parts by weight of Omya 2-JI calcium carbonate, 1 part by weight of Germany BYK-4511 viscosity enhancer, 0.5 parts by weight of Germany BYK-1790 defoamer, and 0.5 parts by weight of Germany BYK-9076 dispersant.

[0119] Example 2

[0120] Component A: 23 parts by weight of Nan Ya NPEF-170 bisphenol F epoxy resin, 11 parts by weight of Japan ADEKA EP-4000 aliphatic epoxy resin, 13 parts by weight of LS-AGE active diluent from Hubei Green Home, China, 30 parts by weight of DRHY-367 aluminum hydroxide from Jinge, Foshan, China, 20 parts by weight of DRHY-390 aluminum hydroxide from Jinge, Foshan, China, 1 part by weight of CABOT TS720 white carbon black thixotropic agent, 1 part by weight of Double Bond TP-10H anti-aging agent from Taiwan, China, 0.5 parts by weight of Alte ATA-3265 defoaming agent from Jiangyin, China, and 0.5 parts by weight of Hangzhou HZ-6004 carbon black.

[0121] Component B: 15 parts by weight of Jiangyin Alte ATA-H270 polyamide curing agent, 5 parts by weight of US HUNTSMAN AEP-HP aminoethyl piperazine, 6 parts by weight of Jinyu Material HY-12D dodecylphenol, 2 parts by weight of Evonik Ancamine K54 curing accelerator, 2 parts by weight of US HUNTSMAN EDR-148 polyetheramine curing agent, 8 parts by weight of Dalian Liansheng LSW-523-1 modified phenolic amine curing agent, 60 parts by weight of Omya 1-JI calcium carbonate, 1 part by weight of German BYK-4510 viscosity enhancer, 0.5 parts by weight of Jiangyin Alte ATA-3265 defoamer, and 0.5 parts by weight of Jiangyin Alte ATA-6747 dispersant.

[0122] Example 3

[0123] Component A: 34 parts by weight of Nan Ya NPEL-127E bisphenol A epoxy resin, 13 parts by weight of Anhui Xinyuan XY-622 active diluent, 30 parts by weight of Foshan Jinge DRHY-367 aluminum hydroxide, 20 parts by weight of Foshan Jinge DRHY-390 aluminum hydroxide, 1 part by weight of Evonik R202 white carbon black thixotropic agent, 1 part by weight of Jiangyin Alte AO-120 anti-aging agent, 0.5 part by weight of Jiangyin Alte ATA-3265 defoaming agent, and 0.5 part by weight of Hangzhou HZ-6004 carbon black.

[0124] Component B: 10 parts by weight of Shenzhen Jiadida XH-463 polyamide curing agent, 5 parts by weight of Japan TOSOH AEP aminoethyl piperazine, 6 parts by weight of Jinyu Material HY-12D dodecylphenol, 2 parts by weight of Evonik Ancamine K54 curing accelerator, 2 parts by weight of German BASF EC-130 polyetheramine curing agent, 8 parts by weight of Dalian Liansheng LSW-523-1 modified phenolic amine curing agent, 65 parts by weight of Omya 2-JI calcium carbonate, 1 part by weight of German BYK-4511 viscosity enhancer, 0.5 parts by weight of German BYK-1790 defoamer, and 0.5 parts by weight of German BYK-9076 dispersant.

[0125] Comparative Example 1

[0126] Component A: 23 parts by weight of Nan Ya NPEL-128 bisphenol A epoxy resin, 11 parts by weight of Japan ADEKA EP-4000 aliphatic epoxy resin, 13 parts by weight of China Hubei Green Home LS-622 active diluent, 30 parts by weight of China Foshan Jinge DRHY-367 aluminum hydroxide, 20 parts by weight of China Foshan Jinge DRHY-390 aluminum hydroxide, 1 part by weight of CABOT TS720 white carbon black thixotropic agent, 1 part by weight of Taiwan Double Bond TP-10H anti-aging agent, 0.5 parts by weight of Germany BYK-1790 defoaming agent, and 0.5 parts by weight of Hangzhou HZ-6004 carbon black.

[0127] Component B: 15 parts by weight of Evonik Ancamide 910 polyamide curing agent, 8 parts by weight of Japan TOSOH AEP aminoethyl piperazine, 6 parts by weight of Jinyu Material HY-12D dodecylphenol, 2 parts by weight of Evonik Ancamine K54 curing accelerator, 2 parts by weight of German BASF EC-130 polyetheramine curing agent, 65 parts by weight of Omya 2-JI calcium carbonate, 1 part by weight of German BYK-4511 viscosity enhancer, 0.5 parts by weight of German BYK-1790 defoamer, and 0.5 parts by weight of German BYK-9076 dispersant.

[0128] Comparative Example 2

[0129] Component A: 23 parts by weight of Nan Ya NPEL-128 bisphenol A epoxy resin, 11 parts by weight of Japan ADEKA EP-4000 aliphatic epoxy resin, 13 parts by weight of China Hubei Green Home LS-622 active diluent, 30 parts by weight of China Foshan Jinge DRHY-367 aluminum hydroxide, 20 parts by weight of China Foshan Jinge DRHY-390 aluminum hydroxide, 1 part by weight of CABOT TS720 white carbon black thixotropic agent, 1 part by weight of Taiwan Double Bond TP-10H anti-aging agent, 0.5 parts by weight of Germany BYK-1790 defoaming agent, and 0.5 parts by weight of Hangzhou HZ-6004 carbon black.

[0130] Component B: 15 parts by weight of Evonik Ancamide 910 polyamide curing agent, 6 parts by weight of Jinyu Material HY-12D dodecylphenol, 2 parts by weight of Evonik Ancamine K54 curing accelerator, 2 parts by weight of German BASF EC-130 polyetheramine curing agent, 8 parts by weight of Dalian Liansheng LSW-523-1 modified phenolic amine curing agent, 65 parts by weight of Omya 2-JI calcium carbonate, 1 part by weight of German BYK-4511 viscosity enhancer, 0.5 parts by weight of German BYK-1790 defoamer, and 0.5 parts by weight of German BYK-9076 dispersant.

[0131] The above formula is shown in Table 1 below.

[0132] Table 1

[0133]

[0134] The specific preparation methods of the two-component epoxy potting adhesives provided in the above embodiments and comparative examples are as follows:

[0135] Component A:

[0136] First, the filler, white carbon black thixotropic agent and carbon black are dried and dehydrated in a drying room at 100°C for 48 hours for use;

[0137] Then, epoxy resin, epoxy diluent, pre-dried filler, white carbon black thixotropic agent, carbon black, anti-aging agent and defoaming agent were added into a double planetary disperser, stirred at 500 rpm at room temperature and evacuated to -0.09 MPa for reaction for 3 hours to obtain component A.

[0138] Component B:

[0139] First, dry and dehydrate the filler in a drying room at 100°C for 48 hours and set aside;

[0140] Then, polyamide curing agent, aminoethyl piperazine, curing accelerator, polyether amine, modified phenolic amine curing agent, pre-dried filler, tackifier, defoamer and dispersant were added into a double planetary disperser, stirred at 500 rpm at room temperature and evacuated to -0.09 MPa for reaction for 3 hours to obtain component B.

[0141] Finally, the above-mentioned component A and component B are evenly mixed in a mass ratio of 1:1 to obtain a two-component epoxy potting adhesive.

[0142] The various properties of the two-component epoxy potting adhesive provided in each embodiment and comparative example were tested, and the testing method is as follows:

[0143] Hardness: GB / T 531.1-2008, Standard for the test method of indentation hardness of vulcanized rubber or thermoplastic rubber;

[0144] Shear strength: GB / T 7124-2008, Determination of tensile shear strength of adhesives (rigid material to rigid material);

[0145] Elongation at break: GB / T 528-2009, Determination of tensile stress-strain properties of vulcanized rubber or thermoplastic rubber;

[0146] Thermal shock aging: GB / T 2423.102-2008, Environmental testing for electrical and electronic products Part 2: Test method Test: Temperature (low temperature, high temperature) / low pressure / vibration (sinusoidal) combined.

[0147] The test results are shown in Table 2 below.

[0148] Table 2

[0149]

[0150] The present invention takes Example 1 as the basic formula. In Example 2, the content of the polyamide curing agent is increased to explore the effect of increasing the flexible curing agent on the overall performance of the glue. In Example 3, the content of the aliphatic epoxy resin is reduced to explore the effect of the flexible epoxy resin on the overall performance of the glue. In Comparative Example 1, the modified phenolic amine curing agent is eliminated to explore its effect on the bonding performance of the PTFE substrate. In Comparative Example 2, aminoethyl piperazine is eliminated to explore its effect on promoting the curing speed.

[0151] From the results in Table 2, we can draw the following conclusions:

[0152] The epoxy resin component selects conventional bisphenol A / bisphenol F epoxy combined with flexible aliphatic epoxy resin, and the curing agent component selects flexible polyamide + aminoethyl piperazine + curing accelerator + modified phenolic amine system. The overall formula system formed can simultaneously meet the characteristics of flexibility, high and low temperature impact resistance, high bonding strength, fast curing speed, and good bonding performance to PTFE substrate, and can well cope with the potting of composite materials in the future security camera field.

[0153] The results of Example 2 show that when the content of polyamide in the curing agent component is increased, the flexibility of the glue becomes better and the adhesion to the metal substrate is higher, but the curing speed will be reduced to a certain extent;

[0154] Example 3 shows that when the content of flexible epoxy resin in the epoxy resin component is reduced, the flexibility of the glue will decrease significantly, the adhesion to the metal substrate will also decrease, and the shear strength will decrease significantly after hot and cold shock;

[0155] The results of control 1 show that the modified phenalkamine curing agent plays a vital role for difficult-to-bond substrates such as PTFE;

[0156] The results of control 2 show that aminoethylpiperazine plays a crucial role in improving the curing speed.

[0157] The above description of the disclosed embodiments enables those skilled in the art to implement or use the present invention. Various modifications to these embodiments will be apparent to those skilled in the art, and the general principles defined herein may be implemented in other embodiments without departing from the spirit or scope of the present invention. Therefore, the present invention will not be limited to the embodiments shown herein, but rather to the widest scope consistent with the principles and novel features disclosed herein.

Claims

1. A flexible epoxy potting adhesive, composed of component A and component B in a mass ratio of 1: (0.8-1.2); The A component is prepared from the following raw materials in percentage by mass: Epoxy resin 20~40%; Epoxy diluent 10~20%; Filler 40~60%; White carbon black thixotropic agent 0.5~1.5%; Anti-aging agent 0.5~1.5%; Defoaming agent 0.1~1%; Carbon black 0.1~1%; The B component is prepared from the following raw materials in percentage by mass: Polyamide curing agent 10~20%; Aminoethylpiperazine 5-10%; Curing accelerator 5~10%; Polyetheramine 0.5~5%; Modified phenolic amine curing agent 5~10%; Filler 50~70%; Thickener 0.5~3%; Defoaming agent 0.1~1%; Dispersant 0.1~1%.

2. The flexible epoxy potting adhesive according to claim 1, characterized in that: The epoxy resin is selected from one or more of bisphenol A epoxy resin, bisphenol F epoxy resin and aliphatic epoxy resin.

3. The flexible epoxy potting adhesive according to claim 1, characterized in that: The epoxy diluent is selected from one or more of Hubei Green Home LS-622 active diluent, Anhui Xinyuan XY-622 active diluent, Hubei Green Home LS-AGE active diluent, and Anhui Xinyuan XY-748 active diluent.

4. The flexible epoxy potting adhesive according to claim 1, characterized in that: The filler is selected from aluminum hydroxide and / or calcium carbonate.

5. The flexible epoxy potting adhesive according to claim 1, characterized in that: The polyetheramine is selected from German BASF EC-130 polyetheramine curing agent and / or American HUNTSMAN EDR-148 polyetheramine curing agent.

6. A method for preparing the flexible epoxy potting adhesive according to any one of claims 1 to 5, comprising the following steps: a) mixing epoxy resin, epoxy diluent, filler, white carbon black thixotropic agent, carbon black, anti-aging agent and defoaming agent, and performing a first dispersion treatment to obtain component A; The polyamide curing agent, aminoethyl piperazine, curing accelerator, polyether amine, modified phenolic amine curing agent, filler, tackifier, defoamer and dispersant are mixed and subjected to a second dispersion treatment to obtain component B; b) Mixing the above component A and component B to obtain a flexible epoxy potting adhesive.

7. The preparation method according to claim 6, characterized in that: The first dispersing process in step a) is carried out in a double planetary disperser; the temperature of the dispersing process is 20°C to 30°C, the rotation speed is 400rpm to 600rpm, the vacuum degree is -0.08MPa to -0.1MPa, and the time is 2h to 4h.

8. The preparation method according to claim 6, characterized in that: The second dispersing process in step a) is carried out in a double planetary disperser; the temperature of the dispersing process is 20°C~30°C, the rotation speed is 400rpm~600rpm, the vacuum degree is -0.08MPa~-0.1MPa, and the time is 2h~4h.

9. The preparation method according to claim 6, characterized in that: In step a), the filler, white carbon black thixotropic agent and carbon black are dried before mixing.

10. The preparation method according to claim 9, characterized in that: The temperature of the drying treatment is 90° C. to 110° C., and the time is 45 h to 50 h.

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