A preparation method and processing equipment for fast curing epoxy resin adhesive

Abstract

The invention relates to the technical field of adhesives, and discloses a preparation method and processing device of a fast-curing epoxy resin adhesive. The invention first uses isobornyl methacrylate, pentaerythritol tetrakis (3-mercaptopropionic acid) ester, triethylamine and chloroform as raw materials to prepare modified pentaerythritol tetrakis (3-mercaptopropionic acid) ester; then mixes a silane coupling agent and an epoxy resin to obtain an epoxy resin modified by a silane coupling agent; then mixes and stirs the epoxy resin modified by a silane coupling agent, N,N-dimethylformamide, modified pentaerythritol tetrakis (3-mercaptopropionic acid) ester, 2-methylimidazole and nano-silicon dioxide to obtain a fast-curing epoxy resin adhesive. Pentaerythritol tetrakis (3-mercaptopropionic acid) ester is modified by isobornyl methacrylate, so that the adhesive has the effect of fast curing; the epoxy resin modified by a silane coupling agent can enhance the viscosity of the adhesive.

Description

Technical Field

[0001] The invention relates to the technical field of adhesives, and in particular to a preparation method and processing equipment for a fast-curing epoxy resin adhesive. Background Art

[0002] Epoxy resin is a commonly used polymer compound. The adhesive made from epoxy resin is known as a universal adhesive. It has good bonding properties, high mechanical properties, chemical corrosion resistance, and is easy to process without causing any pollution to the environment. The adhesive made from epoxy resin has excellent bonding properties with various materials such as metal, glass, ceramics, concrete, and wood.

[0003] However, existing epoxy resin adhesives have certain disadvantages, including brittle cured products, slow curing speed at room temperature and low temperature, etc. The prior art research on epoxy resin adhesives that can be quickly cured at low temperatures is as follows:

[0004] For example, Chinese patent CN105440998B discloses a method for preparing a low-temperature fast-curing epoxy resin adhesive, wherein epoxy resin, silicone resin, modified nitrile rubber, inorganic filler, modified filler, curing agent, etc. are mixed to obtain a low-temperature fast-curing epoxy resin adhesive. Another example is Chinese patent CN103694937B, which discloses an epoxy resin adhesive that can be quickly cured and has good mechanical properties, wherein epoxy resin, organic montmorillonite, curing agent, etc. are mixed to obtain an epoxy resin adhesive that can be quickly cured and has good mechanical properties. However, the epoxy resin adhesives prepared by the above patents all have the disadvantage of weak viscosity, and only by adding montmorillonite, their own mechanical properties are enhanced, making their performance in mechanical aspects such as shear strength and tensile strength not excellent enough. Summary of the invention

[0005] In order to solve the above technical problems, the present invention provides a method for preparing a fast-curing epoxy resin adhesive, comprising the following steps:

[0006] Step 1: mixing isobornyl methacrylate, pentaerythritol tetrakis (3-mercaptopropionic acid) ester, triethylamine and chloroform, stirring, heating and refluxing to obtain a reaction mixture; distilling the reaction mixture under reduced pressure to obtain modified pentaerythritol tetrakis (3-mercaptopropionic acid) ester;

[0007] Step 2: mixing and stirring the silane coupling agent and the epoxy resin to obtain the epoxy resin modified by the silane coupling agent;

[0008] Step 3: Mix and stir the prepared raw materials of silane coupling agent-modified epoxy resin, N,N-dimethylformamide, modified pentaerythritol tetrakis (3-mercaptopropionate), 2-methylimidazole, and nano-silica to obtain a fast-curing epoxy resin adhesive.

[0009] Preferably, in the step 1, the mass ratio of isobornyl methacrylate, pentaerythritol tetrakis(3-mercaptopropionate), triethylamine and chloroform is 50:(11.5-70):(0.5-5):(100-500).

[0010] Preferably, in step 1, the heating reflux temperature is 60-80° C. and the heating reflux time is 20-35 h.

[0011] Preferably, in step 1, the temperature of the vacuum distillation is 50-55° C., and the pressure of the vacuum distillation is -0.06 to -0.08 MPa.

[0012] Preferably, in step 2, the silane coupling agent includes silane coupling agent KH550, and the mass ratio of the silane coupling agent to the epoxy resin is 10-15:100.

[0013] Preferably, in step 2, the mixing and stirring conditions are: temperature of 25-30° C., stirring speed of 300-400 r / min, and stirring time of 60-80 min.

[0014] Preferably, in step three, the mixing mass ratio of epoxy resin modified by silane coupling agent, N,N-dimethylformamide, modified pentaerythritol tetrakis(3-mercaptopropionate), 2-methylimidazole and nano-silicon dioxide is (60-80):10:(10-25):(0.3-1.0):(1-10).

[0015] Preferably, in step three, the mixing and stirring conditions are: temperature of 25-30° C., stirring speed of 300-400 r / min, and stirring time of 15-30 min.

[0016] The present invention also discloses an adhesive processing device, which includes a machine body, a stirring mechanism arranged on the machine body, and a reflux mechanism arranged on the stirring mechanism. The stirring mechanism includes a processing cylinder, a suspension, and a stirring blade. The processing cylinder is fixedly mounted on the machine body, the suspension is rotatably matched in the processing cylinder, and the stirring blade is arranged on the suspension.

[0017] The reflux mechanism comprises a reflux pipe and a fan blade, wherein the reflux pipe is fixedly mounted on the treatment tube, both ends of the reflux pipe are in communication with the treatment tube, the treatment tube is provided with the fan blade, and the fan blade is opposite to a port on one side of the reflux pipe;

[0018] To ensure that when the stirring blades mix and stir the prepared raw materials, the fan blades are driven to rotate at the same time, and at the same time, the suspension drives the stirring blades to swing back and forth.

[0019] Preferably, the stirring mechanism also includes a first driving disk, a first transmission rod, a second driving disk, and a second transmission rod. The first driving disk is rotatably engaged with one side of the suspension, and a plurality of the first transmission rods are rotatably engaged with the first driving disk. The first transmission rods are evenly distributed in a circular shape on the first driving disk. The second driving disk is rotatably engaged with the other side of the suspension, and a plurality of the second transmission rods are rotatably engaged with the second driving disk. The second transmission rods are evenly distributed in a circular shape on the second driving disk. The first driving disk and the second driving disk are located in the same plane.

[0020] Preferably, a rotating ring is arranged between the first transmission rod and the second transmission rod, the first transmission rod is rotatably matched with the rotating ring, the connection between the first transmission rod and the rotating ring is circular and evenly distributed on the rotating ring, the second transmission rod is rotatably matched with the rotating ring, the connection between the second transmission rod and the rotating ring is circular and evenly distributed on the rotating ring, and a plurality of stirring blades are fixedly mounted on the rotating ring, and the stirring blades are circular and evenly distributed on the rotating ring.

[0021] Preferably, a driven gear is rotatably engaged on the other side of the suspension, and the driven gear is dynamically connected to the second driving disk. A fixed gear is rotatably engaged on the other side of the suspension, and the fixed gear is located at a coaxial position at the connection point where the suspension rotatably engages with the processing cylinder, and the fixed gear is meshed with the driven gear. A driving rod is rotatably engaged on the processing cylinder, and the driving rod passes through the wall of the processing cylinder, and the driving rod passes through the wall of the machine body. A power gear is fixedly installed on the driving rod, and the power gear is located in the processing cylinder, and the power gear is meshed with the fixed gear. A stirring motor is fixedly installed in the machine body, and the shaft of the stirring motor is fixedly installed with the driving rod.

[0022] Preferably, a connecting rod is rotatably mounted on the processing cylinder, the connecting rod passes through the wall of the processing cylinder, a first auxiliary gear is fixedly mounted on the connecting rod, the first auxiliary gear is located in the processing cylinder, a second auxiliary gear is fixedly mounted on one side of the suspension, the second auxiliary gear is located at a coaxial position at the connection point where the suspension is rotatably mounted on the processing cylinder, a servo motor is fixedly mounted on the processing cylinder, and the servo motor is fixedly mounted to the connecting rod.

[0023] Preferably, the reflux mechanism also includes a cooling box, a water inlet pipe, and a water outlet pipe. The cooling box is fixedly installed in the machine body, the reflux pipe passes through the wall of the machine body, the reflux pipe passes through the wall of the cooling box, the water inlet pipe is fixedly installed on the top surface of the cooling box, the water inlet pipe is communicated with the cooling box, the water inlet pipe passes through the wall of the machine body, the water outlet pipe is fixedly installed on the side of the cooling box, the water outlet pipe is communicated with the cooling box, and the water outlet pipe passes through the wall of the machine body.

[0024] Preferably, a fixed sleeve is fixedly installed in the processing cylinder, and the fixed sleeve is opposite to one side port of the return pipe. A rotating shaft is rotatably fitted on the fixed sleeve, and a plurality of fan blades are fixedly installed on the rotating shaft. The fan blades are circular and evenly distributed on the rotating shaft. A belt is tensioned between the driving rod and the rotating shaft. A plurality of limit frames are fixedly installed on the processing cylinder, and the belt passes through the limit frames.

[0025] Preferably, a feed pipe is fixedly installed on the upper end of the processing cylinder, and the feed pipe is communicated with the processing cylinder. An electric-controlled valve is fixedly installed on the lower end of the processing cylinder, and the electric-controlled valve is communicated with the processing cylinder. A temperature controller is fixedly installed in the body, a heating plate is fixedly installed on the body, the heating plate is in contact with the bottom end of the processing cylinder, the heating plate is connected to the temperature controller, a temperature meter is fixedly installed on the processing cylinder, and the temperature meter is connected to the temperature controller signal.

[0026] Compared with the prior art, the present invention has the following beneficial effects:

[0027] The raw materials for preparing the epoxy resin adhesive of the present invention include epoxy resin, curing agent, diluent, accelerator and inorganic filler; the epoxy resin is epoxy resin modified by silane coupling agent, modified pentaerythritol tetrakis (3-mercaptopropionic acid) ester is used as curing agent, N, N-dimethylformamide is used as diluent, 2-methylimidazole is used as accelerator, nano silicon dioxide is used as inorganic filler, and the prepared epoxy resin adhesive can be quickly cured;

[0028] Pentaerythritol tetrakis (3-mercaptopropionate) is used as a common adhesive curing agent. With triethylamine as a catalyst and chloroform as a solvent, the thiol group of pentaerythritol tetrakis (3-mercaptopropionate) and the double bond of isobornyl methacrylate undergo Michael addition reaction to obtain an anti-Markovnikov addition product, thereby achieving the modification of pentaerythritol tetrakis (3-mercaptopropionate); on the one hand, the modified pentaerythritol tetrakis (3-mercaptopropionate) extends the molecular chain and increases its molecular weight, thereby enhancing stability; on the other hand, by introducing a non-polar alkyl group, the compatibility of the curing agent with the epoxy resin is improved, which can accelerate the curing speed of the epoxy resin adhesive;

[0029] Epoxy resin modified by silane coupling agent can enhance the adhesion of adhesive; on the one hand, the amino group in the silane coupling agent KH550 molecule can react with the epoxy group of epoxy resin to open the epoxy group; on the other hand, the epoxy resin modified by silane coupling agent can bond with inorganic filler nano-silica to enhance the viscosity of adhesive by forming covalent bonds; in addition, since nano-silica particles have high hardness and heat resistance, they give the adhesive high strength and high temperature aging resistance.

[0030] The adhesive processing equipment of the present invention stirs the prepared raw materials by rotating the stirring blades, and the stirring blades drive the fan blades to rotate, and the fan blades blow into the reflux pipe, so that the volatilized part of the volatile prepared raw materials in the processing tube is blown into the reflux pipe, and is cooled and reliquefied in the reflux pipe and refluxed into the processing tube for reuse. At the same time, the suspension swings back and forth to drive the stirring blades to swing back and forth, so that the stirring blades stir the prepared raw materials more fully, ensuring that the prepared raw materials are fully stirred and avoiding the loss of the prepared raw materials caused by the volatile components in the prepared raw materials and the pollution of the air environment caused by volatilization into the air. BRIEF DESCRIPTION OF THE DRAWINGS

[0031] Figure 1 The present invention is a process flow chart for preparing the fast-curing epoxy resin adhesive;

[0032] Figure 2 It is a line graph of the gelation time of the epoxy resin adhesive prepared in Examples 1-5 of the present invention and Comparative Examples 1-2;

[0033] Figure 3 The figure is a bar graph showing the mechanical properties of the epoxy resin adhesives prepared in Examples 1-5 of the present invention and Comparative Examples 3-4;

[0034] Figure 4 It is a schematic diagram of the internal structure of the processing cylinder of the adhesive processing equipment in the present invention;

[0035] Figure 5 It is a schematic diagram of the structure of the stirring mechanism and the reflux mechanism of the adhesive processing equipment in the present invention;

[0036] Figure 6 for Figure 5 The enlarged structural diagram at A in the middle;

[0037] Figure 7 It is a schematic diagram of the internal structure of the adhesive processing equipment of the present invention;

[0038] Figure 8 It is a schematic diagram of the overall device structure of the adhesive processing equipment in the present invention.

[0039] In the figure: 1. body; 2. stirring mechanism; 21. treatment cylinder; 22. suspension; 23. first drive disk; 24. first transmission rod; 25. second drive disk; 26. second transmission rod; 27. rotating ring; 28. stirring blade; 29. ​​driven gear; 210. fixed gear; 211. driving rod; 212. power gear; 213. stirring motor; 214. connecting rod; 215. first auxiliary gear; 216. second auxiliary gear; 217. servo motor; 3. reflux mechanism; 31. reflux pipe; 32. cooling box; 33. water inlet pipe; 34. water outlet pipe; 35. fixing sleeve; 36. rotating shaft; 37. fan blade; 38. belt; 39. limit frame; 41. feed pipe; 42. electric control valve; 43. temperature controller; 44. heating plate; 45. temperature detector. DETAILED DESCRIPTION

[0040] The technical solutions in the embodiments 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, rather than all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative work are within the scope of protection of the present invention. Example

[0041] A method for preparing a fast-curing epoxy resin adhesive comprises the following steps:

[0042] Step 1, isobornyl methacrylate, pentaerythritol tetrakis (3-mercaptopropionic acid), triethylamine and chloroform are mixed and stirred in a mass ratio of 50:11.5:0.5:100, and heated under reflux at 60° C. for 35 hours to obtain a reaction mixture; the reaction mixture is subjected to reduced pressure distillation at a temperature of 50° C. and a pressure of -0.08 MPa to obtain modified pentaerythritol tetrakis (3-mercaptopropionic acid);

[0043] Step 2: Silane coupling agent KH550 and epoxy resin are mixed and stirred in a mass ratio of 10:100 to obtain epoxy resin modified by silane coupling agent; wherein the mixing and stirring conditions are: temperature of 25° C., stirring speed of 300 r / min, and stirring time of 80 min;

[0044] Step 3: Mix and stir the prepared raw materials of silane coupling agent-modified epoxy resin, N,N-dimethylformamide, modified pentaerythritol tetrakis (3-mercaptopropionic acid) ester, 2-methylimidazole, and nano-silicon dioxide in a mass ratio of 80:10:10:0.3:10 to obtain a fast-curing epoxy resin adhesive:

[0045] The mixing and stirring conditions are as follows: temperature of 25°C, stirring speed of 300 r / min, and stirring time of 30 min. Example

[0046] A method for preparing a fast-curing epoxy resin adhesive comprises the following steps:

[0047] Step 1, isobornyl methacrylate, pentaerythritol tetrakis (3-mercaptopropionic acid), triethylamine and chloroform are mixed and stirred in a mass ratio of 50:25:1.5:200, and heated under reflux at 80° C. for 20 hours to obtain a reaction mixture; the reaction mixture is subjected to reduced pressure distillation at a temperature of 55° C. and a pressure of -0.06 MPa to obtain modified pentaerythritol tetrakis (3-mercaptopropionic acid);

[0048] Step 2: Silane coupling agent KH550 and epoxy resin are mixed and stirred in a mass ratio of 11.4:100 to obtain epoxy resin modified by silane coupling agent; wherein the mixing and stirring conditions are: temperature of 30° C., stirring speed of 400 r / min, and stirring time of 60 min;

[0049] Step 3: Mix and stir the prepared raw materials of silane coupling agent-modified epoxy resin, N,N-dimethylformamide, modified pentaerythritol tetrakis (3-mercaptopropionic acid) ester, 2-methylimidazole, and nano-silicon dioxide in a mass ratio of 76:10:14:0.5:8 to obtain a fast-curing epoxy resin adhesive:

[0050] The mixing and stirring conditions are as follows: temperature of 30°C, stirring speed of 400 r / min, and stirring time of 15 min. Example

[0051] A method for preparing a fast-curing epoxy resin adhesive comprises the following steps:

[0052] Step 1, isobornyl methacrylate, pentaerythritol tetrakis (3-mercaptopropionic acid), triethylamine and chloroform are mixed and stirred in a mass ratio of 50:40:3:300, and heated under reflux at 70° C. for 30 hours to obtain a reaction mixture; the reaction mixture is subjected to reduced pressure distillation at a temperature of 55° C. and a pressure of -0.07 MPa to obtain modified pentaerythritol tetrakis (3-mercaptopropionic acid);

[0053] Step 2: Silane coupling agent KH550 and epoxy resin are mixed and stirred in a mass ratio of 12.8:100 to obtain epoxy resin modified by silane coupling agent; wherein the mixing and stirring conditions are: temperature of 25° C., stirring speed of 350 r / min, and stirring time of 70 min;

[0054] Step 3: Mix and stir the prepared raw materials of silane coupling agent-modified epoxy resin, N,N-dimethylformamide, modified pentaerythritol tetrakis (3-mercaptopropionic acid) ester, 2-methylimidazole, and nano-silicon dioxide in a mass ratio of 72:10:18:0.65:6 to obtain a fast-curing epoxy resin adhesive:

[0055] The mixing and stirring conditions are as follows: temperature of 25°C, stirring speed of 350 r / min, and stirring time of 25 min. Example

[0056] A method for preparing a fast-curing epoxy resin adhesive comprises the following steps:

[0057] Step 1, isobornyl methacrylate, pentaerythritol tetrakis (3-mercaptopropionic acid), triethylamine and chloroform are mixed and stirred in a mass ratio of 50:55:4:400, and heated under reflux at 70° C. for 25 hours to obtain a reaction mixture; the reaction mixture is subjected to reduced pressure distillation at a temperature of 55° C. and a pressure of -0.07 MPa to obtain modified pentaerythritol tetrakis (3-mercaptopropionic acid);

[0058] Step 2: Silane coupling agent KH550 and epoxy resin are mixed and stirred in a mass ratio of 14:100 to obtain epoxy resin modified by silane coupling agent; wherein the mixing and stirring conditions are: temperature of 25° C., stirring speed of 350 r / min, and stirring time of 70 min;

[0059] Step 3: Mix and stir the prepared raw materials of silane coupling agent-modified epoxy resin, N,N-dimethylformamide, modified pentaerythritol tetrakis (3-mercaptopropionic acid) ester, 2-methylimidazole, and nano-silicon dioxide in a mass ratio of 68:10:22:0.8:4 to obtain a fast-curing epoxy resin adhesive:

[0060] The mixing and stirring conditions are as follows: temperature of 25°C, stirring speed of 350 r / min, and stirring time of 25 min. Example

[0061] A method for preparing a fast-curing epoxy resin adhesive comprises the following steps:

[0062] Step 1, isobornyl methacrylate, pentaerythritol tetrakis (3-mercaptopropionic acid), triethylamine and chloroform are mixed and stirred in a mass ratio of 50:70:5:500, and heated under reflux at 70° C. for 25 hours to obtain a reaction mixture; the reaction mixture is subjected to reduced pressure distillation at a temperature of 55° C. and a pressure of -0.07 MPa to obtain modified pentaerythritol tetrakis (3-mercaptopropionic acid);

[0063] Step 2: Silane coupling agent KH550 and epoxy resin are mixed and stirred in a mass ratio of 15:100 to obtain epoxy resin modified by silane coupling agent; wherein the mixing and stirring conditions are: temperature of 25° C., stirring speed of 350 r / min, and stirring time of 70 min;

[0064] Step 3: Mix and stir the prepared raw materials of silane coupling agent-modified epoxy resin, N,N-dimethylformamide, modified pentaerythritol tetrakis (3-mercaptopropionic acid) ester, 2-methylimidazole, and nano-silicon dioxide in a mass ratio of 60:10:25:1:1 to obtain a fast-curing epoxy resin adhesive:

[0065] The mixing and stirring conditions are as follows: temperature of 25°C, stirring speed of 350 r / min, and stirring time of 25 min.

[0066] Comparative Example 1

[0067] A method for preparing an epoxy resin adhesive comprises the following steps:

[0068] Step 1: Silane coupling agent KH550 and epoxy resin are mixed and stirred in a mass ratio of 10:100 to obtain epoxy resin modified by silane coupling agent; wherein the mixing and stirring conditions are: temperature of 25° C., stirring speed of 350 r / min, and stirring time of 70 min;

[0069] Step 2: Mix and stir the epoxy resin modified by the silane coupling agent, N,N-dimethylformamide, pentaerythritol tetrakis (3-mercaptopropionate), 2-methylimidazole, and nano-silicon dioxide in a mass ratio of 80:10:10:0.3:10 to obtain an epoxy resin adhesive:

[0070] The mixing and stirring conditions are as follows: temperature of 25°C, stirring speed of 300 r / min, and stirring time of 30 min.

[0071] Comparative Example 2

[0072] A method for preparing an epoxy resin adhesive comprises the following steps:

[0073] Step 1: Silane coupling agent KH550 and epoxy resin are mixed and stirred in a mass ratio of 10:100 to obtain epoxy resin modified by silane coupling agent; wherein the mixing and stirring conditions are: temperature of 25° C., stirring speed of 350 r / min, and stirring time of 70 min;

[0074] Step 2: Mix and stir the epoxy resin modified by the silane coupling agent, N,N-dimethylformamide, 2-methylimidazole and nano-silicon dioxide in a mass ratio of 80:10:0.3:10 to obtain an epoxy resin adhesive:

[0075] The mixing and stirring conditions are as follows: temperature of 25°C, stirring speed of 300 r / min, and stirring time of 30 min.

[0076] Comparative Example 3

[0077] A method for preparing an epoxy resin adhesive comprises the following steps:

[0078] Step 1, isobornyl methacrylate, pentaerythritol tetrakis (3-mercaptopropionic acid), triethylamine and chloroform are mixed and stirred in a mass ratio of 50:11.5:0.5:100, and heated under reflux at 60° C. for 35 hours to obtain a reaction mixture; the reaction mixture is subjected to reduced pressure distillation at a temperature of 50° C. and a pressure of -0.08 MPa to obtain modified pentaerythritol tetrakis (3-mercaptopropionic acid);

[0079] Step 2: Mix and stir the prepared raw materials epoxy resin, N,N-dimethylformamide, modified pentaerythritol tetrakis (3-mercaptopropionic acid) ester, 2-methylimidazole, and nano-silicon dioxide in a mass ratio of 60:10:25:1:1 to obtain an epoxy resin adhesive:

[0080] The mixing and stirring conditions are as follows: temperature of 25°C, stirring speed of 300 r / min, and stirring time of 30 min.

[0081] Comparative Example 4

[0082] A method for preparing an epoxy resin adhesive comprises the following steps:

[0083] Step 1, isobornyl methacrylate, pentaerythritol tetrakis (3-mercaptopropionic acid), triethylamine and chloroform are mixed and stirred in a mass ratio of 50:11.5:0.5:100, and heated under reflux at 60° C. for 35 hours to obtain a reaction mixture; the reaction mixture is subjected to reduced pressure distillation at a temperature of 50° C. and a pressure of -0.08 MPa to obtain modified pentaerythritol tetrakis (3-mercaptopropionic acid);

[0084] Step 2: Silane coupling agent KH550 and epoxy resin are mixed and stirred in a mass ratio of 10:100 to obtain epoxy resin modified by silane coupling agent; wherein the mixing and stirring conditions are: temperature of 25° C., stirring speed of 300 r / min, and stirring time of 80 min;

[0085] Step 3: Mix and stir the prepared raw materials of silane coupling agent-modified epoxy resin, N,N-dimethylformamide, modified pentaerythritol tetrakis (3-mercaptopropionic acid) ester, and 2-methylimidazole in a mass ratio of 60:10:25:1 to obtain an epoxy resin adhesive:

[0086] The mixing and stirring conditions are as follows: temperature of 25°C, stirring speed of 300 r / min, and stirring time of 30 min.

[0087] In all the above embodiments and comparative examples, isobornyl methacrylate comes from Jinan Pulaihua Chemical Co., Ltd. with the item number 2154; pentaerythritol tetrakis (3-mercaptopropionic acid) ester comes from Shandong Yaotong Co., Ltd. with the item number 2561498; silane coupling agent KH550 comes from Dongguan Kangjin New Materials Technology Co., Ltd. with the item number 550; the epoxy resins are all epoxy resin E-51, which comes from Shandong Haoyao New Materials Co., Ltd. with the item number HY5454; nano-silicon dioxide comes from Jiangsu Tianxing New Materials Co., Ltd., model: TSP-H10, with a particle size of 20 nm.

[0088] The epoxy resin adhesives prepared in Examples 1-5 and Comparative Examples 1-4 were subjected to performance tests:

[0089] (1) Gel time test: Use the BK-1 gel time tester to test the gel time of the adhesive sample at different temperatures. After the equipment temperature rises to the specified temperature, use a syringe to take 0.2mL of the prepared epoxy resin adhesive and drop it on the hot plate. Start stirring after 20 seconds to make the epoxy resin adhesive evenly spread on the hot plate. Make 2-3 turns within 1 second until drawing or clumping occurs. Stop the timing and record the time. The test temperature is 120°C. The test results are shown in Table 1:

[0090] Table 1

[0091] Example 1 Example 2 Example 3 Example 4 Example 5 Comparative Example 1 Comparative Example 2 Gel time (s) 98.2 94.3 90.7 86.5 82.1 105.1 130.1

[0092] As shown in Table 1, the epoxy resin adhesive prepared by the present invention has the characteristics of short gelation time and rapid curing. In Example 5, the modified pentaerythritol tetrakis (3-mercaptopropionate) ester has the highest proportion in the adhesive and the lowest gelation time. However, since the pentaerythritol tetrakis (3-mercaptopropionate) ester was not modified in Comparative Example 1, the compatibility of pentaerythritol tetrakis (3-mercaptopropionate) ester with epoxy resin E-51 was reduced, and the rapid curing effect of the adhesive was reduced; the curing agent pentaerythritol tetrakis (3-mercaptopropionate) ester was not added in Comparative Example 2, so that the adhesive needed a long time to solidify and form a gel.

[0093] (2) The epoxy resin adhesive was cured at 25°C for 30 minutes, and the shear strength of the cured adhesive was tested in accordance with GB7124-86 "Determination of tensile shear strength (metal to metal)";

[0094] (3) Tensile performance test: The tensile performance test was conducted in accordance with GB / T1040.2-2006 "Determination of tensile properties of plastics Part 2: Test conditions for molded and extruded plastics". The tensile speed was 50 mm / min and the curing time of the prepared adhesive was 3 h.

[0095] The test results are shown in Table 2:

[0096] Table 2

[0097] Example 1 Example 2 Example 3 Example 4 Example 5 Comparative Example 3 Comparative Example 4 Shear strength / MPa 35.7 33.5 31..2 29..5 27.7 19.7 23.9 Tensile strength / MPa 79 76 73 70 68 60 62

[0098] As shown in Table 2, the epoxy resin adhesive prepared by the present invention has good shear strength and tensile properties. The epoxy resin selected in Comparative Example 3 is not modified by a silane coupling agent, and its bonding performance decreases, resulting in a decrease in mechanical properties such as shear strength and tensile strength. The epoxy resin modified by a silane coupling agent in Comparative Example 4 does not add nano-silica, and its mechanical properties are poor compared to the epoxy resin adhesive with inorganic fillers added. Example

[0099] This embodiment provides an adhesive processing device that can meet the mixing and stirring treatment of the prepared raw materials in Examples 1-5 and Comparative Examples 1-4 to prepare epoxy resin adhesive.

[0100] like Figure 4 As shown, an adhesive processing device includes a body 1, a stirring mechanism 2 arranged on the body 1, and a reflux mechanism 3 arranged on the stirring mechanism 2. The stirring mechanism 2 includes a processing cylinder 21, a suspension 22, and a stirring blade 28. The processing cylinder 21 is fixedly installed on the body 1, and the suspension 22 is rotatably matched in the processing cylinder 21. The suspension 22 is provided with a stirring blade 28.

[0101] The reflux mechanism 3 includes a reflux pipe 31 and a fan blade 37. The reflux pipe 31 is fixedly mounted on the treatment tube 21. Both ends of the reflux pipe 31 are in communication with the treatment tube 21. The treatment tube 21 is provided with a fan blade 37. The fan blade 37 is opposite to one side port of the reflux pipe 31.

[0102] To ensure that when the stirring blade 28 stirs the prepared raw materials, the fan blade 37 is driven to rotate at the same time, and at the same time, the suspension 22 drives the stirring blade 28 to swing back and forth.

[0103] When using:

[0104] After all the prepared raw materials enter the processing cylinder 21, the stirring blade 28 starts to rotate, and the stirring blade 28 mixes and stirs the prepared raw materials, and the stirring blade 28 drives the fan blade 37 to rotate, and the fan blade 37 blows into the reflux pipe 31, so that the volatilized part of the volatile prepared raw materials in the processing cylinder 21 is blown into the reflux pipe 31, and is cooled and reliquefied in the reflux pipe 31 and refluxed to the processing cylinder 21 for reuse. At the same time, the suspension 22 swings back and forth to drive the stirring blade 28 to swing back and forth, so that the stirring blade 28 mixes and stirs the prepared raw materials more fully, ensuring that the prepared raw materials are fully mixed and stirred, and avoiding the loss of the prepared raw materials caused by the volatile components in the prepared raw materials and the pollution of the air environment caused by volatilization into the air.

[0105] Furthermore, if Figure 4-6 As shown, the stirring mechanism 2 also includes a first driving disk 23, a first transmission rod 24, a second driving disk 25, and a second transmission rod 26. The first driving disk 23 is rotatably engaged on one side of the suspension 22, and a plurality of first transmission rods 24 are rotatably engaged on the first driving disk 23. The first transmission rods 24 are evenly distributed in a circular shape on the first driving disk 23. The second driving disk 25 is rotatably engaged on the other side of the suspension 22, and a plurality of second transmission rods 26 are rotatably engaged on the second driving disk 25. The second transmission rods 26 are evenly distributed in a circular shape on the second driving disk 25. The first driving disk 23 and the second driving disk 25 are located in the same plane.

[0106] Furthermore, the first driving plate 23 is close to one end of the suspension 22 , and the second driving plate 25 is close to the other end of the suspension 22 .

[0107] Furthermore, if Figure 5-6 As shown, a rotating ring 27 is provided between the first transmission rod 24 and the second transmission rod 26, the first transmission rod 24 is rotatably matched with the rotating ring 27, the connection between the first transmission rod 24 and the rotating ring 27 is circular and evenly distributed on the rotating ring 27, the second transmission rod 26 is rotatably matched with the rotating ring 27, the connection between the second transmission rod 26 and the rotating ring 27 is circular and evenly distributed on the rotating ring 27, a plurality of stirring blades 28 are fixedly installed on the rotating ring 27, and the stirring blades 28 are circular and evenly distributed on the rotating ring 27.

[0108] Furthermore, the rotating ring 27 is located on the central vertical plane between the first driving disk 23 and the second driving disk 25, so that after the first transmission rod 24 and the second transmission rod 26 are respectively connected to the rotating ring 27, the first transmission rod 24, the rotating ring 27 and the second transmission rod 26 form a triangular structure, so that the rotating ring 27 forms a fixed position relative to the suspension 22, so that the rotating ring 27 forms a rotating structure of a virtual rotating axis, ensuring that the rotating ring 27 can fully mix and stir the prepared raw materials.

[0109] Among them, the second driving disk 25 drives the second transmission rod 26 to rotate, and cooperates with the first driving disk 23 and the first transmission rod 24 so that the second transmission rod 26 drives the rotating ring 27 to rotate, and the rotating ring 27 drives the stirring blade 28 to rotate, and the stirring blade 28 is used to mix and stir the prepared raw materials.

[0110] Furthermore, if Figure 5 As shown, a driven gear 29 is rotatably engaged on the other side of the suspension 22, and the driven gear 29 is power-connected to the second driving disk 25. A fixed gear 210 is rotatably engaged on the other side of the suspension 22, and the fixed gear 210 is located at a coaxial position at the connection between the suspension 22 and the processing cylinder 21, and the fixed gear 210 is meshed with the driven gear 29. A driving rod 211 is rotatably engaged on the processing cylinder 21, and the driving rod 211 penetrates the wall of the processing cylinder 21, and the driving rod 211 penetrates the wall of the body 1. A power gear 212 is fixedly installed on the driving rod 211, and the power gear 212 is located in the processing cylinder 21, and the power gear 212 is meshed with the fixed gear 210. A stirring motor 213 is fixedly installed in the body 1, and the shaft of the stirring motor 213 is fixedly installed with the driving rod 211.

[0111] Furthermore, the connection between the driving rod 211 and the processing cylinder 21 is sealed.

[0112] Among them, the stirring motor 213 is started, the stirring motor 213 drives the driving rod 211 to rotate, the driving rod 211 drives the power gear 212 to rotate, the power gear 212 drives the fixed gear 210 to rotate, the fixed gear 210 drives the driven gear 29 to rotate, and the driven gear 29 drives the second driving disk 25 to rotate, so that the second driving disk 25 drives the stirring blade 28 to rotate.

[0113] Furthermore, if Figure 5 As shown, a connecting rod 214 is rotatably engaged on the processing cylinder 21, and the connecting rod 214 passes through the wall of the processing cylinder 21. A first auxiliary gear 215 is fixedly installed on the connecting rod 214, and the first auxiliary gear 215 is located in the processing cylinder 21. A second auxiliary gear 216 is fixedly installed on one side of the suspension 22, and the second auxiliary gear 216 is located at a coaxial position at the connection point where the suspension 22 rotatably engages with the processing cylinder 21. A servo motor 217 is fixedly installed on the processing cylinder 21, and the servo motor 217 is fixedly installed with the connecting rod 214.

[0114] Furthermore, the connection between the connecting rod 214 and the processing cylinder 21 is sealed.

[0115] Furthermore, the servo motor 217 performs reciprocating rotation operation.

[0116] Among them, the servo motor 217 is started, the servo motor 217 drives the connecting rod 214 to rotate reciprocatingly, the connecting rod 214 drives the first auxiliary gear 215 to rotate reciprocatingly, the first auxiliary gear 215 drives the second auxiliary gear 216 to rotate reciprocatingly, and the second auxiliary gear 216 drives the suspension 22 to swing back and forth, so that the suspension 22 drives the stirring blade 28 to better perform mixing and stirring processing.

[0117] Furthermore, if Figure 4 , Figure 5 , Figure 7 As shown, the reflux mechanism 3 also includes a cooling box 32, a water inlet pipe 33, and a water outlet pipe 34. The cooling box 32 is fixedly installed in the machine body 1, the reflux pipe 31 passes through the wall of the machine body 1, and the reflux pipe 31 passes through the wall of the cooling box 32. A water inlet pipe 33 is fixedly installed on the top surface of the cooling box 32, the water inlet pipe 33 is communicated with the cooling box 32, and the water inlet pipe 33 passes through the wall of the machine body 1. A water outlet pipe 34 is fixedly installed on the side of the cooling box 32, the water outlet pipe 34 is communicated with the cooling box 32, and the water outlet pipe 34 passes through the wall of the machine body 1.

[0118] The cooling water enters from the water inlet pipe 33 , then enters the cooling box 32 , and then is discharged from the water outlet pipe 34 .

[0119] Furthermore, if Figure 5 , Figure 7 As shown, a fixed sleeve 35 is fixedly installed in the processing cylinder 21, and the fixed sleeve 35 is opposite to one side port of the return pipe 31. A rotating shaft 36 is rotatably fitted on the fixed sleeve 35, and a plurality of fan blades 37 are fixedly installed on the rotating shaft 36. The fan blades 37 are circular and evenly distributed on the rotating shaft 36. A belt 38 is tensioned between the driving rod 211 and the rotating shaft 36. A plurality of limit frames 39 are fixedly installed on the processing cylinder 21, and the belt 38 passes through the limit frames 39.

[0120] Among them, the driving rod 211 drives the belt 38 to rotate, the belt 38 drives the rotating shaft 36 to rotate, and the rotating shaft 36 drives the fan blades 37 to rotate, so that the fan blades 37 blow the volatilized part of the volatile preparation raw materials in the processing cylinder 21 into the return pipe 31, and the cooling water in the cooling box 32 cools and liquefies the volatilized part of the volatile preparation raw materials in the return pipe 31, so that the volatilized part of the volatile preparation raw materials is liquefied and refluxed into the processing cylinder 21.

[0121] Furthermore, if Figure 7-8As shown, a feed pipe 41 is fixedly installed on the upper end of the processing cylinder 21, and the feed pipe 41 is communicated with the processing cylinder 21; an electric control valve 42 is fixedly installed on the lower end of the processing cylinder 21, and the electric control valve 42 is communicated with the processing cylinder 21; a temperature controller 43 is fixedly installed in the body 1; a heating plate 44 is fixedly installed on the body 1, and the heating plate 44 is in contact with the bottom end of the processing cylinder 21, and the heating plate 44 is connected to the temperature controller 43; a temperature detector 45 is fixedly installed on the processing cylinder 21, and the temperature detector 45 is connected to the temperature controller 43 signal.

[0122] Among them, the feed pipe 41 adds the prepared raw materials into the processing cylinder 21, and after a batch of prepared raw materials is processed, the electric control valve 42 is opened to allow the epoxy resin adhesive obtained after processing to flow out from the electric control valve 42, and the temperature sensor 45 monitors the temperature in the processing cylinder 21, and controls the temperature controller 43 in real time, so that the temperature controller 43 controls the heating plate 44 to heat the processing cylinder 21, so as to maintain the temperature in the processing cylinder 21 within the required temperature range.

[0123] Working principle:

[0124] After all the prepared raw materials enter the processing barrel 21, the stirring blade 28 starts to rotate, and the stirring blade 28 mixes and stirs the prepared raw materials, and the stirring blade 28 drives the fan blade 37 to rotate, and the fan blade 37 blows into the reflux pipe 31, so that the volatilized part of the volatile prepared raw materials in the processing barrel 21 is blown into the reflux pipe 31, so that the volatilized part of the volatile prepared raw materials is cooled in the reflux pipe 31 to re-liquefy the volatilized part of the volatile prepared raw materials and return to the processing barrel 21 for reuse. At the same time, the suspension 22 reciprocates to drive the stirring blade 28 to reciprocate, so that the stirring blade 28 mixes and stirs the prepared raw materials more fully;

[0125] The feed pipe 41 adds the prepared raw materials into the processing cylinder 21, and the stirring motor 213 is started. The stirring motor 213 drives the driving rod 211 to rotate, the driving rod 211 drives the power gear 212 to rotate, the power gear 212 drives the fixed gear 210 to rotate, the fixed gear 210 drives the driven gear 29 to rotate, the driven gear 29 drives the second driving disk 25 to rotate, so that the second driving disk 25 drives the stirring blade 28 to rotate, the second driving disk 25 drives the second transmission rod 26 to rotate, and cooperates with the first driving disk 23 and the first transmission rod 24 so that the second transmission rod 26 drives the rotating ring 27 to rotate, the rotating ring 27 drives the stirring blade 28 to rotate, and the stirring blade 28 performs mixing and stirring treatment on the prepared raw materials;

[0126] At the same time, the servo motor 217 is started, the servo motor 217 drives the connecting rod 214 to rotate back and forth, the connecting rod 214 drives the first auxiliary gear 215 to rotate back and forth, the first auxiliary gear 215 drives the second auxiliary gear 216 to rotate back and forth, and the second auxiliary gear 216 drives the suspension 22 to swing back and forth, so that the suspension 22 drives the stirring blade 28 to perform a better mixing and stirring process;

[0127] Furthermore, cooling water enters from the water inlet pipe 33, and then enters the cooling box 32, and then is discharged from the water outlet pipe 34. At the same time, the driving rod 211 drives the belt 38 to rotate, the belt 38 drives the rotating shaft 36 to rotate, and the rotating shaft 36 drives the fan blades 37 to rotate, so that the fan blades 37 blow the volatilized part of the volatile preparation raw material in the processing cylinder 21 into the return pipe 31, and the cooling water in the cooling box 32 cools and liquefies the volatilized part of the volatile preparation raw material in the return pipe 31, so that the volatilized part of the volatile preparation raw material is liquefied and flows back into the processing cylinder 21;

[0128] Then, after a batch of raw materials are mixed and stirred, the electric control valve 42 is opened to allow the epoxy resin adhesive obtained after the mixing and stirring process to flow out from the electric control valve 42, and the temperature sensor 45 monitors the temperature in the processing cylinder 21 and controls the temperature controller 43 in real time, so that the temperature controller 43 controls the heating plate 44 to heat the processing cylinder 21, so as to maintain the temperature in the processing cylinder 21 within the required temperature range.

[0129] Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and variations may be made to the embodiments without departing from the principles and spirit of the present invention, and that the scope of the present invention is defined by the appended claims and their equivalents.

Claims

1. An adhesive processing device, characterized in that: It comprises a machine body, a stirring mechanism arranged on the machine body, and a reflux mechanism arranged on the stirring mechanism; The stirring mechanism comprises a treatment cylinder, a suspension, and a stirring blade. The treatment cylinder is fixedly mounted on the machine body. The suspension is rotatably fitted inside the treatment cylinder, and the stirring blade is arranged on the suspension. The reflux mechanism comprises a reflux pipe and a fan blade, wherein the reflux pipe is fixedly mounted on the treatment tube, both ends of the reflux pipe are in communication with the treatment tube, the treatment tube is provided with the fan blade, and the fan blade is opposite to a port on one side of the reflux pipe; Ensure that when the stirring blade mixes and stirs the prepared raw materials, the fan blade is driven to rotate at the same time, and at the same time, the suspension drives the stirring blade to swing back and forth; The stirring mechanism further includes a first driving disk, a first transmission rod, a second driving disk, and a second transmission rod. The first driving disk is rotatably matched with one side of the suspension, and a plurality of the first transmission rods are rotatably matched with the first driving disk. The first transmission rods are evenly distributed on the first driving disk in a circular shape. The second driving disk is rotatably matched with the other side of the suspension, and a plurality of the second transmission rods are rotatably matched with the second driving disk. The second transmission rods are evenly distributed on the second driving disk in a circular shape. The first driving disk and the second driving disk are located in the same plane. A rotating ring is provided between the first transmission rod and the second transmission rod, the first transmission rods are rotatably matched with the rotating ring, the connection between the first transmission rod and the rotating ring is circular and evenly distributed on the rotating ring, the second transmission rods are rotatably matched with the rotating ring, the connection between the second transmission rod and the rotating ring is circular and evenly distributed on the rotating ring, a plurality of stirring blades are fixedly mounted on the rotating ring, and the stirring blades are circular and evenly distributed on the rotating ring; A driven gear is rotatably matched on the other side of the suspension, and the driven gear is dynamically connected to the second driving disk. A fixed gear is rotatably matched on the other side of the suspension, and the fixed gear is located at a coaxial position where the suspension is rotatably matched on the connection of the treatment cylinder, and the fixed gear is meshed with the driven gear. A driving rod is rotatably matched on the treatment cylinder, and the driving rod passes through the wall of the treatment cylinder, and the driving rod passes through the wall of the machine body. A power gear is fixedly installed on the driving rod, and the power gear is located in the treatment cylinder, and the power gear is meshed with the fixed gear. A stirring motor is fixedly installed in the machine body, and the shaft of the stirring motor is fixedly installed with the driving rod; The treatment cylinder is rotatably equipped with a connecting rod, the connecting rod penetrates the wall of the treatment cylinder, a first auxiliary gear is fixedly installed on the connecting rod, the first auxiliary gear is located in the treatment cylinder, a second auxiliary gear is fixedly installed on one side of the suspension, the second auxiliary gear is located at a coaxial position of the connection part where the suspension is rotatably equipped on the treatment cylinder, a servo motor is fixedly installed on the treatment cylinder, and the servo motor is fixedly installed with the connecting rod; The reflux mechanism further comprises a cooling box, a water inlet pipe and a water outlet pipe. The cooling box is fixedly installed in the machine body, the reflux pipe penetrates the wall of the machine body, the reflux pipe penetrates the wall of the cooling box, the water inlet pipe is fixedly installed on the top of the cooling box, the water inlet pipe is communicated with the cooling box, the water inlet pipe penetrates the wall of the machine body, the water outlet pipe is fixedly installed on the side of the cooling box, the water outlet pipe is communicated with the cooling box, and the water outlet pipe penetrates the wall of the machine body; A fixed sleeve is fixedly installed in the processing cylinder, and the fixed sleeve is opposite to one side port of the return pipe. A rotating shaft is rotatably fitted on the fixed sleeve, and a plurality of fan blades are fixedly installed on the rotating shaft. The fan blades are circular and evenly distributed on the rotating shaft. A belt is tensioned between the driving rod and the rotating shaft. A plurality of limit frames are fixedly installed on the processing cylinder, and the belt passes through the limit frames.

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