CN113913141A - Preparation process of epoxy resin pouring sealant - Google Patents

Preparation process of epoxy resin pouring sealant Download PDF

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Publication number
CN113913141A
CN113913141A CN202111407526.8A CN202111407526A CN113913141A CN 113913141 A CN113913141 A CN 113913141A CN 202111407526 A CN202111407526 A CN 202111407526A CN 113913141 A CN113913141 A CN 113913141A
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China
Prior art keywords
component
dispersion
epoxy resin
dispersing
main body
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CN202111407526.8A
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Chinese (zh)
Inventor
葛凡
邬国明
杨李懿
马苗
顾鸣杰
徐伟
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Zhejiang Rongtai Technical Industry Co ltd
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Zhejiang Rongtai Technical Industry Co ltd
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Priority to CN202111407526.8A priority Critical patent/CN113913141A/en
Publication of CN113913141A publication Critical patent/CN113913141A/en
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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J163/00—Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D19/00—Degasification of liquids
    • B01D19/0042—Degasification of liquids modifying the liquid flow
    • B01D19/0052—Degasification of liquids modifying the liquid flow in rotating vessels, vessels containing movable parts or in which centrifugal movement is caused
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D19/00—Degasification of liquids
    • B01D19/02—Foam dispersion or prevention
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02—Non-macromolecular additives
    • C09J11/04—Non-macromolecular additives inorganic
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/08—Macromolecular additives
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C08K2003/2227—Oxides; Hydroxides of metals of aluminium
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/28—Nitrogen-containing compounds
    • C08K2003/282—Binary compounds of nitrogen with aluminium
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/38—Boron-containing compounds
    • C08K2003/382—Boron-containing compounds and nitrogen
    • C08K2003/385—Binary compounds of nitrogen with boron
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00—Specific properties of additives
    • C08K2201/002—Physical properties
    • C08K2201/005—Additives being defined by their particle size in general

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Dispersion Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Mixers Of The Rotary Stirring Type (AREA)

Abstract

The application relates to the technical field of epoxy resin pouring sealant production, in particular to a preparation process of epoxy resin pouring sealant. A preparation process of epoxy resin pouring sealant comprises the following steps of preparing a component A and a component B; step two, adding the component B into a high-speed dispersing device to perform high-speed dispersion and deaeration with the component A, controlling the rotating speed at 350-480rpm, controlling the absolute vacuum degree at 50-200mbar and the deaeration time at 15-100min to obtain a finished product; the high-speed dispersing device used in the preparation process comprises a dispersing kettle main body, a driving motor and a combined dispersing assembly, wherein the driving motor is fixedly connected with the combined dispersing assembly through a coupler; the combined dispersing component is positioned inside the dispersing kettle main body. This application adopts the high-speed dispersion devices of independently researching and developing to carry out high-efficient dispersion deaeration to the material, guarantees the accurate nature and the product quality of batching, can promote the efficiency of dispersion deaeration simultaneously.

Description

Preparation process of epoxy resin pouring sealant
Technical Field
The application relates to the technical field of epoxy resin pouring sealant production, in particular to a preparation process of epoxy resin pouring sealant.
Background
The epoxy pouring sealant is an epoxy resin liquid packaging or potting material which is prepared by taking epoxy resin as a main component and adding various functional auxiliaries and a proper curing agent. The related technology discloses a high-toughness, impact-resistant and high-flexibility epoxy pouring sealant, which comprises a component A and a component B, wherein the mass ratio of the component A to the component B is (10:1) - (20:1), and the component A comprises the following raw materials: 0-130 parts of toughened epoxy resin, 5-20 parts of bisphenol A type epoxy resin, 1-18 parts of reactive diluent, 1-10 parts of thixotropic agent and 320 parts of alumina; the component B comprises the following raw materials: 20-50 parts of flexible curing agent, 25-50 parts of hyperbranched curing agent and 1-5 parts of accelerator.
Aiming at the epoxy resin pouring sealant in the related technology, the applicant finds that the related technical scheme has the following defects: in the actual production process, the amount of the filler alumina is found to be large, and when the conventional dispersion plate (refer to fig. 1) is adopted for dispersion, part of the filler is found to be deposited at the center of the lower circle of the dispersible tablet, so that the materials cannot be uniformly dispersed and defoamed, and the ingredient efficiency and the quality of the final product are influenced.
Disclosure of Invention
In order to solve the problems that materials in the related art cannot be uniformly dispersed and defoamed, and the batching efficiency and the quality of a final product are affected, the application provides a preparation process of an epoxy resin pouring sealant.
The preparation process of the epoxy resin pouring sealant is realized by the following technical scheme: a preparation process of epoxy resin pouring sealant comprises the following steps of (1) independently storing the component A and the component B, and mixing the component A and the component B according to the weight part ratio of 1 (0.4-0.7) when in use; the component A comprises the following raw material components in parts by weight: 25-40 parts of epoxy resin; 62-69 parts of a filler; 3-5 parts of a reactive diluent; 5-15 parts of a toughening agent; the component B comprises the following raw material components in parts by weight: 65-70 parts of a curing agent; 5-7 parts of a curing accelerator; the filler is prepared from 65-75 parts of alumina, 17-22 parts of aluminum nitride and 17-22 parts of boron nitride; the density of the alumina is 4.0g/ml, and the grain diameter D50 is 15-25 μm; the density of the boron nitride is 2.3g/ml, and the grain diameter D50 is 8-12 μm; the density of the aluminum nitride is 3.0g/ml, the grain diameter D50 is 2-5 μm, and the aluminum nitride is characterized in that: the epoxy resin pouring sealant is prepared by the following method,
step one, preparing a component A and a component B:
preparing the component A, namely measuring aluminum oxide, aluminum nitride and boron nitride according to the proportion, uniformly mixing, drying at the temperature of 110-125 ℃ for 1-2h, cooling to room temperature to obtain a filler, measuring epoxy resin, the filler, an active diluent and a toughening agent according to the proportion, adding the epoxy resin, the filler, the active diluent and the toughening agent into a high-speed dispersing device for high-speed dispersion and defoaming, controlling the rotating speed at 480rpm of 350-480, controlling the absolute vacuum degree at 50-100mbar and the defoaming time at 15-30min to obtain the component A;
preparing a component B, namely uniformly mixing a curing agent and a curing accelerator which are accurately metered to obtain the component B;
step two, adding the component B into a high-speed dispersing device to perform high-speed dispersion and deaeration with the component A, controlling the rotating speed at 350-480rpm, controlling the absolute vacuum degree at 50-200mbar and the deaeration time at 15-100min to obtain a finished product; the high-speed dispersing device comprises a dispersing kettle main body, a driving motor and a combined dispersing assembly, wherein the dispersing kettle main body is detachably connected with a sealing cover; the driving motor is fixedly connected with the sealing cover; the driving motor is fixedly connected with the combined dispersing assembly through a coupler; the combined dispersing component is positioned in the dispersing kettle main body and is used for dispersing and defoaming materials; the sealing cover is fixedly communicated with a feeding pipe communicated with the interior of the dispersion kettle main body; the center of the bottom of the dispersion kettle main body is fixedly communicated with a discharge pipe communicated with the inside of the dispersion kettle main body.
Through adopting above-mentioned technical scheme, to above-mentioned epoxy resin pouring sealant batching system, this application adopts the high-speed dispersion devices of independently research and development to carry out high-efficient dispersion deaeration to the material, can reduce ordinary dispersion impeller 4 h's dispersion time to 130min and below, can effectively shorten the time of preparation technology dispersion deaeration, promotes whole production efficiency, and can guarantee the accurate nature of batching, improves the quality of final products.
Preferably, the combined dispersing assembly comprises a flow guide piece and a combined stirrer, and the flow guide piece is detachably connected to the lower surface of the sealing cover; the flow guide piece is integrally formed with a flow passage which penetrates through the upper surface and the lower surface of the flow guide piece; one end of the combined stirrer is fixedly connected to an output shaft of the driving motor through a coupler, and the other end of the combined stirrer is close to the inner bottom surface of the dispersion kettle main body; the vertical distance between the other end surface of the combined stirrer and the inner bottom surface of the dispersion kettle main body is 1.0-50.0 mm; the combined stirrer is positioned in the flow passage, and a gap is reserved between the combined stirrer and the flow passage; in the rotation process of the combined stirrer, the material at the bottom in the dispersion kettle main body moves upwards in the flow channel along the axis of the flow channel.
By adopting the technical scheme, the combined stirrer rotates to enable the materials to move upwards along the axis of the flow channel, and the materials flow back into the dispersion kettle main body from the upper surface of the flow guide piece, so that the gas-liquid exchange area can be increased, the integral dispersion defoaming efficiency is improved, the integral process time is shortened, and the quality of the prepared product is ensured.
Preferably, the flow guide part comprises a flow guide main part, a liquid guide dispersible tablet and a mounting flange, and the geometric shape of the flow guide main part is a circular column; the liquid guiding dispersible tablet is fixedly connected to the outer side wall of the upper part of the flow guiding main part; the mounting flange is fixedly connected to the outer side wall of the top of the flow guide main part; the mounting flange is detachably connected to the lower surface of the sealing cover; the outer side wall of the flow guide main part is provided with a plurality of liquid guide circular holes communicated with the flow channel in a penetrating way; the liquid guide circular holes are uniformly arranged around the central axis of the flow guide main part; the distance between every two adjacent liquid guide circular holes is equal; the liquid guide circular hole is positioned between the liquid guide dispersible tablet and the mounting flange; and a gap for material backflow is reserved between one end of the liquid guiding dispersion tablet, which is back to the side wall of the flow guiding main part, and the inner wall of the dispersion kettle main body.
By adopting the technical scheme, the liquid-guiding dispersible tablet can increase the gas-liquid exchange area, further improve the integral dispersion defoaming efficiency, shorten the integral process time and ensure the quality of the prepared product
Preferably, the height of the relative ground at one end of the liquid guiding dispersion tablet, which is back to the side wall of the flow guiding main part, is lower than the height of the relative ground at the joint of the liquid guiding dispersion tablet and the side wall of the flow guiding main part.
Through adopting above-mentioned technical scheme, can increase the gas-liquid exchange area and be convenient for the material backward flow to the dispersion tank main part in, promote holistic deaeration efficiency and dispersion efficiency, shorten whole process time, guarantee the quality of the product of preparing.
Preferably, a connecting line of one end point of the liquid guiding dispersion tablet, which is back to the side wall of the main flow guiding component, and one point of the connecting part of the liquid guiding dispersion tablet and the side wall of the main flow guiding component is positioned in a vertical plane, and an acute angle formed by the connecting line and the horizontal plane is 10-40 degrees.
By optimizing the structure of the liquid guiding dispersible tablet, the integral defoaming efficiency and the integral dispersing efficiency can be further improved, the integral process time is shortened, and the quality of the prepared product is ensured.
Preferably, the combined stirrer comprises a spiral stirrer, and one end of the spiral stirrer is fixedly connected to an output shaft of the driving motor through a coupler; the vertical distance between the end face of the other end of the spiral stirrer and the inner bottom surface of the dispersion kettle main body is 1.0-50.0 mm; the length of a spiral belt on the spiral stirrer is 0.95-1.02 times of the vertical distance from the central axis of the liquid guide circular hole to the lower surface of the flow guide main part.
By adopting the technical scheme, the spiral stirrer can enable the materials to move upwards along the axis of the flow channel, the materials flow to the liquid guide dispersible tablets from the liquid guide circular holes of the flow guide pieces, and the materials flowing through the liquid guide dispersible tablets flow back to the dispersion kettle main body, so that the gas-liquid exchange area can be increased, the integral dispersion defoaming efficiency is improved, the integral process time is shortened, and the quality of the prepared product is ensured.
Preferably, the combined stirrer further comprises a dispersion disc, and the dispersion disc is fixedly connected to the periphery of the screw rod of the spiral stirrer; a gap is reserved between the dispersion disc and the flow channel; the dispersion disc is fixedly connected to the periphery of the screw of the spiral stirrer in a reverse direction; in the rotation process of the dispersion disc, materials in the flow channel move upwards in the flow channel along the axial direction of the flow channel; the vertical height of the upper surface of the dispersion disc relative to the ground is 0.95-1.02 times of the vertical distance height between the central axis of the liquid guide circular hole and the ground.
Through adopting above-mentioned technical scheme, the dispersion impeller rotates the in-process and makes liquid along the axis upward movement of runner in the runner, can slow down the time of material backward flow to bottom in the dispersion tank main part to be favorable to increasing the gas-liquid exchange area, further promote holistic dispersion homogeneity and dispersion efficiency, shorten whole process time, guarantee the quality of the product of preparing.
Preferably, the combined stirrer further comprises a speed reducing component, and the speed reducing component is connected to the periphery of the screw of the spiral stirrer; the dispersion disc is rotatably connected with the speed reducing assembly; the dispersion disc is reversely arranged on the speed reducing assembly, and in the rotating process of the dispersion disc, the materials in the flow channel move upwards in the flow channel along the axial direction of the flow channel; the height of the upper surface of the dispersion disc relative to the ground is 0.95-1.02 times of the height of the central axis of the liquid guide circular hole from the ground.
Through adopting above-mentioned technical scheme, the dispersion impeller rotates the in-process and makes liquid along the axis upward movement of runner in the runner, and the time of bottom in the dispersion tank main part can further be slowed down in the speed reduction subassembly to be favorable to increasing the gas-liquid exchange area, further promote holistic dispersion homogeneity and dispersion efficiency, shorten whole process time, guarantee the quality of the product of preparing.
Preferably, the speed reduction assembly comprises a driving gear, a transmission gear, a connecting rod and a connecting plate, and the driving gear is fixedly connected to the periphery of a screw of the spiral stirrer; the transmission gear is meshed with the driving gear; the transmission gear is fixedly connected to the circumferential direction of the connecting rod; the connecting plate is vertically and fixedly connected to the inner wall of the flow guide main part; the connecting rods rotate and are fixed between the two connecting plates; one end of the connecting rod penetrates through the upper surface and the lower surface of the connecting plate and is rotatably connected to the connecting plate; the dispersion impeller fixed connection wears to establish the rod end circumference on the upper and lower surface of connecting plate in the connecting rod, and the dispersion impeller is located the upper portion of connecting plate.
Through adopting above-mentioned technical scheme, the material that is located near drain round hole can carry out the predispersion deaeration under the effect of dispersion impeller in advance, is favorable to increasing the gas-liquid exchange area, further promotes holistic dispersion homogeneity and dispersion efficiency, shortens whole process time, guarantees the quality of the product of preparing.
In summary, the present application has the following advantages:
1. according to the method, the independently researched and developed high-speed dispersing device is adopted for dispersing and defoaming the ingredients, so that the overall process time can be shortened, and the quality of the prepared product can be ensured.
2. This application is through optimizing rotational speed, absolute vacuum and time, can effectively reduce the dispersion deaeration time of material, has promoted whole industrial production efficiency.
Drawings
Fig. 1 is a schematic view of a structure of a dispersion tray in the related art.
Fig. 2 is a schematic view of the overall structure of embodiment 1 in the present application.
Fig. 3 is a schematic structural view of the combination mixer of example 1 in this application.
Fig. 4 is a schematic structural view of the combination mixer of example 2 in this application.
Fig. 5 is a schematic view of the connection structure of the combination agitator and the speed reduction assembly in embodiment 2 of the present application.
In the figure, 1, a high-speed dispersing device; 10. a dispersion tank main body; 11. sealing the cover; 12. a feed pipe; 13. a discharge pipe; 2. a drive motor; 3. a modular dispersing assembly; 4. a flow guide member; 40. a flow channel; 41. a flow guide main part; 411. a liquid guiding round hole; 42. liquid guiding dispersing tablets; 43. installing a flange; 5. a combined agitator; 51. a helical agitator; 52. a dispersion tray; 53. a speed reduction assembly; 531. a driving gear; 5311. a through hole; 532. a transmission gear; 533. a connecting rod; 534. a connecting plate; 6. a cylinder; 7. and a vacuum pump set.
Detailed Description
The present application is described in further detail below with reference to figures 2-5 and examples.
Device
Equipment I
Referring to fig. 2, the high-speed dispersing apparatus 1 includes a dispersing main body 10, a cover 11, a driving motor 2 and a combined dispersing assembly 3, wherein the cover 11 is detachably connected to the dispersing main body 10 for sealing the dispersing main body 10, thereby facilitating the vacuum-pumping operation. The cover 11 is fixedly communicated with a vacuum pump set 7 communicated with the interior of the dispersion kettle main body 10, and the vacuum pump set 7 is used for evacuating the dispersion kettle main body 10. Driving motor 2 fixed connection is in the upper surface of closing cap 11, and driving motor 2's output shaft passes through shaft coupling and 3 fixed connection of combination formula dispersion subassembly, and combination formula dispersion subassembly 3 is located inside dispersion tank main part 10. The driving motor 2 drives the combined dispersing component 3 to rotate around the axial direction of the combined dispersing component, so that the aim of quickly dispersing and defoaming materials in the dispersing kettle main body 10 is fulfilled.
Referring to fig. 2, a feed pipe 12 communicating with the inside of the dispersion tank body 10 is fixedly connected to the upper surface of the cover 11. One end of the feeding pipe 12 is communicated with the inside of the dispersion kettle main body 10, the other end of the feeding pipe 12 is located on the upper portion of the sealing cover 11, one end of the feeding pipe 12 located on the upper portion of the sealing cover 11 is circumferentially threaded and is connected with the sealing cover in a sealing mode, and the sealing performance of the dispersion kettle main body 10 can be guaranteed due to the arrangement of the sealing cover. A discharge pipe 13 is fixedly communicated with the center of the bottom of the dispersion kettle main body 10. One end of the discharge pipe 13 is communicated with the inside of the dispersion tank main body 10, and the other end of the discharge pipe 13 is located below the bottom of the dispersion tank main body 10. In order to control the material outflow and canning, the discharge pipe 13 is fixedly communicated with an electromagnetic valve.
Referring to fig. 2, in order to facilitate cleaning of the inside of the dispersion tank body 10, a cylinder 6 is fixedly connected to an outer wall of the dispersion tank body 10. The number of the cylinders 6 is two, and the two cylinders 6 are symmetrically arranged about the central axis of the dispersion tank main body 10. The push rod of the cylinder 6 is fixedly connected to the lower surface of the cover 11. When the two cylinders 6 are started simultaneously, the sealing cover 11 is uncovered on the dispersion kettle main body 10 under the pushing of the cylinders 6, and an operator can clean and maintain the interior of the dispersion kettle main body 10.
Referring to fig. 3, the combined dispersing unit 3 is composed of a flow guide 4 and a combined stirrer 5, and a central axis of the combined stirrer 5 is vertical. Wherein the flow guide member 4 is detachably attached to the lower surface of the cover 11. The flow guide member 4 is integrally formed with a flow passage 40 through the upper and lower surfaces, and a central axis of the flow passage 40 is perpendicular to a horizontal plane. The diameter of the flow passage 40 is 0.8-0.9 times of the outer diameter of the flow guide part 4, and the diameter of the flow passage 40 in the device is 0.88 times of the outer diameter of the flow guide part 4.
Referring to fig. 3, one end of the combined stirrer 5 is fixedly connected to the output shaft of the driving motor 2 through a coupling, and the other end of the combined stirrer 5 is close to the inner bottom surface of the dispersion tank main body 10. The vertical distance between the other end surface of the combined stirrer 5 and the inner bottom surface of the dispersion kettle main body 10 is 5.0-10 mm. The combined stirrer 5 is positioned in the flow passage 40, and a gap for the material to flow is reserved between the combined stirrer 5 and the flow passage 40. During the rotation of the combined stirrer 5, the material located at the bottom of the dispersion tank main body 10 moves upward in the flow passage 40 along the axis of the flow passage 40.
Referring to fig. 3, the flow guiding member 4 includes a flow guiding main member 41, a liquid guiding dispersing tablet 42 and a mounting flange 43, the flow guiding main member 41 is a circular column in geometry, and mainly the flow guiding main member 41 is integrally formed with the flow channel 40. The liquid guiding dispersible tablets 42 are welded on the outer side wall of the upper part of the flow guiding main part 41 and are used for guiding materials, increasing the gas-liquid contact area of the materials, accelerating vacuum deaeration and removing water generated by reaction, facilitating uniform dispersion of fillers in a system, improving the overall production efficiency and ensuring the quality of final products. The mounting flange 43 is welded to the top outer side wall of the flow guide main part 41, and the upper surface of the mounting flange 43 is flush with the upper surface of the flow guide main part 41. The mounting flange 43 is bolted to the lower surface of the cover 11, so that the guide member 4 is detachably connected to the cover 11.
Referring to fig. 3, a plurality of liquid guiding circular holes 411 are vertically formed through the outer side wall of the flow guiding main part 41 and are communicated with the flow channel 40. The central axis of the circular liquid guiding hole 411 is perpendicular to the central axis of the main flow guiding element 41. The liquid guiding round hole 411 is located between the liquid guiding dispersion plate 42 and the mounting flange 43, and the central axes of the liquid guiding round holes 411 are all located in the same horizontal plane. The liquid guiding circular holes 411 are uniformly arranged around the central axis of the flow guiding main part 41, that is, the distance between the adjacent liquid guiding circular holes 411 is equal. A gap for material backflow is reserved between one end of the liquid guiding dispersion tablet 42, which is back to the side wall of the flow guiding main part 41, and the inner wall of the dispersion kettle main body 10.
Referring to fig. 3, in order to further increase the vacuum defoaming efficiency, the relative ground height of the end of the liquid guiding and dispersing tablet 42 facing away from the side wall of the main guiding component 41 is lower than the relative ground height of the joint of the liquid guiding and dispersing tablet 42 and the side wall of the main guiding component 41. Specifically, a connecting line between an end point of the liquid guiding dispersion tablet 42, which is back to the side wall of the main flow guiding component 41, and a point at the connecting position of the liquid guiding dispersion tablet 42 and the side wall of the main flow guiding component 41 is located in a vertical plane, and an acute angle formed by the connecting line and the horizontal plane is 10-40 degrees, and is preferably 15 degrees.
Referring to fig. 3, combination stirrer 5 includes a spiral stirrer 51 and a dispersion plate 52, one end of spiral stirrer 51 is fixedly connected to the output shaft of driving motor 2 through a coupling, and the vertical distance from the other end surface of spiral stirrer 51 to the inner bottom surface of dispersion tank body 10 is 5-10 mm. The length of the spiral belt on the spiral stirrer 51 is 1.0 time of the vertical distance from the central axis of the liquid guide circular hole 411 to the lower surface of the flow guide main part 41. The pitch of the helical agitator 51 is 1.0 or 1.25 diameters, preferably 1.0 diameter. During the rotation of the helical agitator 51, the liquid material at the bottom of the dispersion vessel main body 10 is introduced into the flow channel 40, the material in the flow channel 40 is conveyed to the upper part of the flow channel 40 along the axial direction of the flow channel 40, flows out of the flow guide main part 41 from the liquid guide circular hole 411, flows to the upper surface of the liquid guide dispersible tablet 42, and flows back to the bottom of the dispersion vessel main body 10 through the dispersion of the liquid guide dispersible tablet 42, so that the gas-liquid contact area of the material is increased, the vacuum deaeration is accelerated, the filler is uniformly dispersed in the system, the overall production efficiency is improved, and the quality of the final product is ensured.
Referring to fig. 3, the dispersion plate 52 is fixedly connected to the circumference of the screw of the helical agitator 51 in the opposite direction, so that the material in the flow path 40 moves upward in the flow path 40 in the axial direction of the flow path 40 during the rotation of the dispersion plate 52. A gap for a material flow passage is reserved between the dispersion plate 52 and the flow passage 40. The height of the upper surface of the dispersion plate 52 relative to the ground is 1.0 time of the vertical distance between the central axis of the liquid guide circular hole 411 and the ground.
Dispersion impeller 52 can rotate along with helical agitator 51 and take place synchronous rotation, pivoted dispersion impeller 52 drives the part and is located runner 40 and near liquid material along runner 40 axial upward movement in drain round hole 411, it flows water conservancy diversion main part 41 from drain round hole 411 to have realized partly material, partly material is transmitted to the purpose in the runner 40 that is located drain round hole 411 upper portion, the material in runner 40 is shunted and is handled, the velocity of flow of avoiding flowing out the material through drain round hole 411 is too fast, further increase the gas-liquid area of contact of material, accelerate vacuum defoamation, be convenient for pack homodisperse in the system, promote holistic production efficiency, guarantee the quality of final product. In addition, the rotating dispersion plate 52 can disperse the liquid material near the liquid guide circular hole 411, so that the vacuum defoaming efficiency can be further improved, and the overall production efficiency can be improved.
Device two
The difference between the second device and the first device is that: referring to fig. 4 and 5, the combination agitator 5 further includes a speed reduction assembly 53, the speed reduction assembly 53 includes a driving gear 531, a transmission gear 532, a connecting rod 533 and a connecting plate 534, and the driving gear 531 is welded to the screw circumference of the helical agitator 51. The driving gear 531 has a plurality of through holes 5311 penetrating the upper and lower surfaces. The straight-line distances between the central axes of the adjacent through holes 5311 are equal. The aperture ratio of the driving gear 531 is controlled to be 30-50%, and the aperture ratio of the driving gear 531 in the device is 40%. The transmission gear 532 is fixedly connected to the connecting rod 533 in the axial direction, and the transmission gear 532 is engaged with the driving gear 531. Two connecting plates 534 are vertically welded on the inner wall of the flow guiding main part 41. The connecting rod 533 is rotatably and fixedly connected between the two connecting plates 534.
Referring to fig. 4 and 5, the end of the connecting rod 533 higher than the ground is vertically inserted through the upper and lower surfaces of the connecting plate 534 and located on the upper surface of the connecting plate 534, and the connecting rod 533 is inserted through and rotatably connected to the connecting plate 534. The dispersion plate 52 is fixedly connected to the rod ends of the connecting rods 533 penetrating the upper and lower surfaces of the connecting plate 534 in the opposite directions. The purpose of the dispersion tray 52 being reversed is: some materials are transmitted to the runner 40 that is arranged in the upper portion of the liquid guide round hole 411, so that the shunting treatment of the materials is realized, the phenomenon that the flow speed of the materials flowing out through the liquid guide round hole 411 is too high is avoided, the gas-liquid contact area of the materials is further increased, the vacuum defoaming is accelerated, the fillers are conveniently and uniformly dispersed in a system, the overall production efficiency is improved, and the quality of final products is ensured.
Referring to fig. 4 and 5, the height of the upper surface of the dispersion board 52 relative to the ground is 1 time of the height of the vertical distance from the ground to the central axis of the liquid guiding circular hole 411. The diameter ratio of the driving gear 531 to the transmission gear 532 in the reduction assembly 53 is 3-5: 1. In the present embodiment, the ratio of the diameter of the driving gear 531 to the diameter of the transmission gear 532 is controlled to be 4:1, and therefore, the differential ratio between the helical agitator 51 and the dispersion plate 52 is 3.6: 1, namely the rotating speed of the driving motor 2 is 400rpm, and the rotating speed of the actual dispersion disc 52 is 1440rpm, so that the overall production efficiency can be improved, and the quality of the final product can be ensured.
Examples
Example 1
The epoxy resin pouring sealant in the embodiment comprises a component A and a component B, wherein the component A and the component B are separately stored and are mixed according to the weight part ratio of 1:0.4 when in use.
The component A is composed of the following raw materials in parts by weight: 25 parts of epoxy resin, 69 parts of filler and 3 parts of polyethylene glycol diglycidyl ether; 15 parts of carboxyl-terminated liquid nitrile rubber.
The filler comprises the following raw material components in parts by weight: 65 parts of aluminum oxide, 22 parts of boron nitride and 20 parts of aluminum nitride. The density of the alumina is 4.0g/ml, and the particle size D50 is 15 μm; the density of the boron nitride is 2.3g/ml, and the grain diameter D50 is 8 mu m; the density of the aluminum nitride was 3.0g/ml, and the particle diameter D50 was 3 μm.
The component B is composed of the following raw materials in parts by weight: 65 parts of liquid methyltetrahydrophthalic anhydride and 5 parts of benzyldiamine.
A preparation process of an epoxy resin pouring sealant comprises the following steps:
step one, preparing a component A and a component B:
preparing a component A, weighing alumina, boron nitride and aluminum nitride according to a mass ratio of 65:22:20, mixing and dispersing for 10min at 500rpm to obtain a filler, weighing 690g of the filler, drying for 2h at 120 ℃, cooling to room temperature, storing at a dry place for later use, then adding 250g of epoxy resin, 690g of the dried filler, 30g of polyethylene glycol diglycidyl ether and 150g of carboxyl-terminated liquid nitrile rubber into a dispersion kettle main body 10 in a first device through a feeding pipe 12, and performing high-speed dispersion and defoaming with an absolute vacuum degree of 100mbar, a rotating speed of 350rpm and a time of 30min to obtain the component A;
preparing a component B, namely mixing 650g of liquid methyl tetrahydrophthalic anhydride and 50g of benzyldiamine at 600rpm for 5min to obtain the component B;
and step two, adding the component B formed in the step one into the dispersion kettle main body 10 to perform high-speed dispersion and defoaming with the component A, controlling the rotating speed at 350rpm, controlling the absolute vacuum degree at 100mbar, and controlling the defoaming time at 30min to obtain a finished product.
Example 2
Example 2 differs from example 1 in that:
a preparation process of an epoxy resin pouring sealant comprises the following steps:
step one, preparing a component A and a component B:
preparing a component A, weighing alumina, boron nitride and aluminum nitride according to a mass ratio of 65:22:20, mixing and dispersing for 10min at 500rpm to obtain a filler, weighing 690g of the filler, drying for 2h at 120 ℃, cooling to room temperature, placing at a drying place for storage, then adding 250g of epoxy resin, 690g of the dried filler, 30g of polyethylene glycol diglycidyl ether and 150g of carboxyl-terminated liquid nitrile rubber into a dispersion kettle main body 10 in a first device through a feeding pipe 12, performing high-speed dispersion and defoaming, controlling an absolute vacuum degree at 100mbar, rotating speed at 400rpm, and time at 25min to obtain the component A;
preparing a component B, namely mixing 650g of liquid methyl tetrahydrophthalic anhydride and 50g of benzyldiamine at 600rpm for 5min to obtain the component B;
and step two, adding the component B formed in the step one into the dispersion kettle main body 10 to perform high-speed dispersion and defoaming with the component A, controlling the rotating speed at 400rpm, controlling the absolute vacuum degree at 100mbar, and controlling the defoaming time at 25min to obtain a finished product.
Example 3
Example 3 differs from example 1 in that:
a preparation process of an epoxy resin pouring sealant comprises the following steps:
step one, preparing a component A and a component B:
preparing a component A, weighing alumina, boron nitride and aluminum nitride according to a mass ratio of 65:22:20, mixing and dispersing for 10min at 500rpm to obtain a filler, weighing 690g of the filler, drying for 2h at 120 ℃, cooling to room temperature, placing at a drying place for storage, then adding 250g of epoxy resin, 690g of the dried filler, 30g of polyethylene glycol diglycidyl ether and 150g of carboxyl-terminated liquid nitrile rubber into a dispersion kettle main body 10 in a first device through a feeding pipe 12, performing high-speed dispersion and defoaming, controlling an absolute vacuum degree at 100mbar, rotating speed at 440rpm, and time at 20min to obtain the component A;
preparing a component B, namely mixing 650g of liquid methyl tetrahydrophthalic anhydride and 50g of benzyldiamine at 600rpm for 5min to obtain the component B;
and step two, adding the component B formed in the step one into the dispersion kettle main body 10 to perform high-speed dispersion and defoaming with the component A, controlling the rotating speed at 440rpm, controlling the absolute vacuum degree at 100mbar, and controlling the defoaming time at 25min to obtain a finished product.
Example 4
Example 4 differs from example 1 in that:
a preparation process of an epoxy resin pouring sealant comprises the following steps:
step one, preparing a component A and a component B:
preparing a component A, weighing alumina, boron nitride and aluminum nitride according to a mass ratio of 65:22:20, mixing and dispersing for 10min at 500rpm to obtain a filler, weighing 690g of the filler, drying for 2h at 120 ℃, cooling to room temperature, placing at a drying place for storage, then adding 250g of epoxy resin, 690g of the dried filler, 30g of polyethylene glycol diglycidyl ether and 150g of carboxyl-terminated liquid nitrile rubber into a dispersion kettle main body 10 in a first device through a feeding pipe 12, performing high-speed dispersion and defoaming, controlling an absolute vacuum degree at 100mbar, rotating speed at 480rpm, and time at 15min to obtain the component A;
preparing a component B, namely mixing 650g of liquid methyl tetrahydrophthalic anhydride and 50g of benzyldiamine at 600rpm for 5min to obtain the component B;
and step two, adding the component B formed in the step one into the dispersion kettle main body 10 to perform high-speed dispersion and defoaming with the component A, controlling the rotating speed at 480rpm, controlling the absolute vacuum degree at 100mbar and controlling the defoaming time at 20min to obtain a finished product.
Example 5
Example 5 differs from example 1 in that:
a preparation process of an epoxy resin pouring sealant comprises the following steps:
step one, preparing a component A and a component B:
preparing a component A, weighing alumina, boron nitride and aluminum nitride according to a mass ratio of 65:22:20, mixing and dispersing for 10min at 500rpm to obtain a filler, weighing 690g of the filler, drying for 2h at 120 ℃, cooling to room temperature, placing at a drying place for storage, then adding 250g of epoxy resin, 690g of the dried filler, 30g of polyethylene glycol diglycidyl ether and 150g of carboxyl-terminated liquid nitrile rubber into a dispersion kettle main body 10 in a second device through a feeding pipe 12, performing high-speed dispersion and defoaming, controlling an absolute vacuum degree at 100mbar, rotating speed at 350rpm, and time at 30min to obtain the component A;
preparing a component B, namely mixing 650g of liquid methyl tetrahydrophthalic anhydride and 50g of benzyldiamine at 600rpm for 5min to obtain the component B;
and step two, adding the component B formed in the step one into the dispersion kettle main body 10 to perform high-speed dispersion and defoaming with the component A, controlling the rotating speed at 350rpm, controlling the absolute vacuum degree at 100mbar, and controlling the defoaming time at 30min to obtain a finished product.
Example 6
Example 6 differs from example 1 in that:
a preparation process of an epoxy resin pouring sealant comprises the following steps:
step one, preparing a component A and a component B:
preparing a component A, weighing alumina, boron nitride and aluminum nitride according to a mass ratio of 65:22:20, mixing and dispersing for 10min at 500rpm to obtain a filler, weighing 690g of the filler, drying for 2h at 120 ℃, cooling to room temperature, placing in a drying place for storage, then adding 250g of epoxy resin, 690g of the dried filler, 30g of polyethylene glycol diglycidyl ether and 150g of carboxyl-terminated liquid nitrile rubber into a dispersion kettle main body 10 in a second device through a feeding pipe 12, performing high-speed dispersion and defoaming, controlling an absolute vacuum degree at 100mbar, rotating speed at 480rpm, and time at 15min to obtain the component A;
preparing a component B, namely mixing 650g of liquid methyl tetrahydrophthalic anhydride and 50g of benzyldiamine at 600rpm for 5min to obtain the component B;
and step two, adding the component B formed in the step one into the dispersion kettle main body 10 to perform high-speed dispersion and defoaming with the component A, controlling the rotating speed at 480rpm, controlling the absolute vacuum degree at 100mbar, and controlling the defoaming time at 15min to obtain a finished product.
Example 7
Example 7 differs from example 1 in that:
a preparation process of an epoxy resin pouring sealant comprises the following steps:
step one, preparing a component A and a component B:
preparing a component A, weighing alumina, boron nitride and aluminum nitride according to a mass ratio of 65:22:20, mixing and dispersing for 10min at 500rpm to obtain a filler, weighing 690g of the filler, drying for 2h at 120 ℃, cooling to room temperature, placing at a drying place for storage, then adding 250g of epoxy resin, 690g of the dried filler, 30g of polyethylene glycol diglycidyl ether and 150g of carboxyl-terminated liquid nitrile rubber into a dispersion kettle main body 10 in a second device through a feeding pipe 12, performing high-speed dispersion and defoaming, controlling an absolute vacuum degree at 100mbar, rotating speed at 400rpm, and time at 20min to obtain the component A;
preparing a component B, namely mixing 650g of liquid methyl tetrahydrophthalic anhydride and 50g of benzyldiamine at 600rpm for 5min to obtain the component B;
and step two, adding the component B formed in the step one into the dispersion kettle main body 10 to perform high-speed dispersion and defoaming with the component A, controlling the rotating speed at 480rpm, controlling the absolute vacuum degree at 100mbar, controlling the defoaming time at 60min, stopping stirring after defoaming for 60min, and continuously vacuumizing for 40min to obtain a finished product.
Example 8
Example 8 differs from example 1 in that: a preparation process of an epoxy resin pouring sealant comprises the following steps:
step one, preparing a component A and a component B:
preparing a component A, weighing alumina, boron nitride and aluminum nitride according to a mass ratio of 65:22:20, mixing and dispersing for 10min at 500rpm to obtain a filler, weighing 690g of the filler, drying for 2h at 120 ℃, cooling to room temperature, storing at a dry place for later use, then adding 250g of epoxy resin, 690g of the dried filler, 30g of polyethylene glycol diglycidyl ether and 150g of carboxyl-terminated liquid nitrile rubber into a dispersion kettle main body 10 in a first device through a feeding pipe 12, and performing high-speed dispersion and defoaming with an absolute vacuum degree of 50mbar, a rotating speed of 350rpm and a time of 30min to obtain the component A;
preparing a component B, namely mixing 650g of liquid methyl tetrahydrophthalic anhydride and 50g of benzyldiamine at 600rpm for 5min to obtain the component B;
and step two, adding the component B formed in the step one into the dispersion kettle main body 10 to perform high-speed dispersion and defoaming with the component A, controlling the rotating speed at 350rpm, controlling the absolute vacuum degree at 50mbar and controlling the defoaming time at 30min to obtain a finished product.
Example 9
Example 9 differs from example 1 in that: a preparation process of an epoxy resin pouring sealant comprises the following steps:
step one, preparing a component A and a component B:
preparing a component A, weighing alumina, boron nitride and aluminum nitride according to a mass ratio of 65:22:20, mixing and dispersing for 10min at 500rpm to obtain a filler, weighing 690g of the filler, drying for 2h at 120 ℃, cooling to room temperature, storing at a dry place for later use, then adding 250g of epoxy resin, 690g of the dried filler, 30g of polyethylene glycol diglycidyl ether and 150g of carboxyl-terminated liquid nitrile rubber into a dispersion kettle main body 10 in a first device through a feeding pipe 12, and performing high-speed dispersion and defoaming with an absolute vacuum degree of 50mbar, a rotating speed of 350rpm and a time of 30min to obtain the component A;
preparing a component B, namely mixing 650g of liquid methyl tetrahydrophthalic anhydride and 50g of benzyldiamine at 600rpm for 5min to obtain the component B;
and step two, adding the component B formed in the step one into the dispersion kettle main body 10 to perform high-speed dispersion and defoaming with the component A, controlling the rotating speed at 350rpm, controlling the absolute vacuum degree at 200mbar and controlling the defoaming time at 30min to obtain a finished product.
Example 10
Example 10 differs from example 1 in that: a preparation process of an epoxy resin pouring sealant comprises the following steps:
step one, preparing a component A and a component B:
preparing a component A, weighing alumina, boron nitride and aluminum nitride according to a mass ratio of 65:22:20, mixing and dispersing for 10min at 500rpm to obtain a filler, weighing 690g of the filler, drying for 2h at 120 ℃, cooling to room temperature, storing at a dry place for later use, then adding 250g of epoxy resin, 690g of the dried filler, 30g of polyethylene glycol diglycidyl ether and 150g of carboxyl-terminated liquid nitrile rubber into a dispersion kettle main body 10 in a first device through a feeding pipe 12, and performing high-speed dispersion and defoaming with an absolute vacuum degree of 50mbar, a rotating speed of 420rpm and a time of 30min to obtain the component A;
preparing a component B, namely mixing 650g of liquid methyl tetrahydrophthalic anhydride and 50g of benzyldiamine at 600rpm for 5min to obtain the component B;
and step two, adding the component B formed in the step one into the dispersion kettle main body 10 to perform high-speed dispersion and defoaming with the component A, controlling the rotating speed at 420rpm, controlling the absolute vacuum degree at 50mbar, controlling the defoaming time at 40min, stopping stirring after defoaming for 40min, and continuously vacuumizing for 40min to obtain a finished product.
Comparative example
Comparative example 1
A preparation process of an epoxy resin pouring sealant comprises the following steps:
step one, preparing a component A and a component B:
preparing a component A, weighing alumina, boron nitride and aluminum nitride according to a mass ratio of 65:22:20, mixing and dispersing for 10min at 500rpm to obtain a filler, weighing 690g of the filler, drying at 120 ℃ for 2h, cooling to room temperature, placing at a drying place for storage, adding 250g of epoxy resin, 690g of the dried filler, 30g of polyethylene glycol diglycidyl ether and 150g of carboxyl-terminated liquid nitrile rubber into a conventional high-speed dispersing kettle, and performing high-speed dispersion and defoaming in a conventional dispersing disc (see figure 1), wherein the absolute vacuum degree is controlled at 100mbar, the rotating speed is 2800rpm, and the time is 3h to obtain the component A;
preparing a component B, namely mixing 650g of liquid methyl tetrahydrophthalic anhydride and 50g of benzyldiamine at 600rpm for 5min to obtain the component B;
and step two, adding the component B formed in the step one into a conventional high-speed dispersion kettle to perform high-speed dispersion and defoaming with the component A, controlling the absolute vacuum degree to be 200mbar, controlling the rotating speed to be 2800rpm, and controlling the time to be 1h to obtain a finished product.
Comparative example 2
A preparation process of an epoxy resin pouring sealant comprises the following steps:
step one, preparing a component A and a component B:
preparing a component A, weighing alumina, boron nitride and aluminum nitride according to a mass ratio of 65:22:20, mixing and dispersing for 10min at 500rpm to obtain a filler, weighing 690g of the filler, drying at 120 ℃ for 2h, cooling to room temperature, placing at a drying place for storage, adding 250g of epoxy resin, 690g of the dried filler, 30g of polyethylene glycol diglycidyl ether and 150g of carboxyl-terminated liquid nitrile rubber into a conventional high-speed dispersing kettle, and performing high-speed dispersion and defoaming in a conventional dispersing disc (see figure 1) with an absolute vacuum degree of 100mbar, a rotating speed of 2800rpm and a time of 2.0h to obtain the component A;
preparing a component B, namely mixing 650g of liquid methyl tetrahydrophthalic anhydride and 50g of benzyldiamine at 600rpm for 5min to obtain the component B;
and step two, adding the component B formed in the step one into a conventional high-speed dispersion kettle to perform high-speed dispersion and defoaming with the component A, controlling the absolute vacuum degree to be 200mbar, controlling the rotating speed to be 2800rpm, and controlling the time to be 1.0h to obtain a finished product.
Comparative example 3
A preparation process of an epoxy resin pouring sealant comprises the following steps:
step one, preparing a component A and a component B:
preparing a component A, weighing alumina, boron nitride and aluminum nitride according to a mass ratio of 65:22:20, mixing and dispersing for 10min at 500rpm to obtain a filler, weighing 690g of the filler, drying for 2h at 120 ℃, cooling to room temperature, placing at a drying place for storage, then adding 250g of epoxy resin, 690g of the dried filler, 30g of polyethylene glycol diglycidyl ether and 150g of carboxyl-terminated liquid nitrile rubber into a dispersion kettle main body 10 in a first device through a feeding pipe 12, performing high-speed dispersion and defoaming, controlling an absolute vacuum degree at 100mbar, rotating speed at 250rpm, and time at 30min to obtain the component A;
preparing a component B, namely mixing 650g of liquid methyl tetrahydrophthalic anhydride and 50g of benzyldiamine at 600rpm for 5min to obtain the component B;
and step two, adding the component B formed in the step one into the dispersion kettle main body 10 to perform high-speed dispersion and defoaming with the component A, controlling the rotating speed at 250rpm, controlling the absolute vacuum degree at 100mbar, and controlling the defoaming time at 30min to obtain a finished product.
Comparative example 4
A preparation process of an epoxy resin pouring sealant comprises the following steps:
step one, preparing a component A and a component B:
preparing a component A, weighing alumina, boron nitride and aluminum nitride according to a mass ratio of 65:22:20, mixing and dispersing for 10min at 500rpm to obtain a filler, weighing 690g of the filler, drying for 2h at 120 ℃, cooling to room temperature, placing in a drying place for storage, then adding 250g of epoxy resin, 690g of the dried filler, 30g of polyethylene glycol diglycidyl ether and 150g of carboxyl-terminated liquid nitrile rubber into a dispersion kettle main body 10 in a first device through a feeding pipe 12, performing high-speed dispersion and defoaming, controlling an absolute vacuum degree at 100mbar, rotating speed at 520rpm, and time at 15min to obtain the component A;
preparing a component B, namely mixing 650g of liquid methyl tetrahydrophthalic anhydride and 50g of benzyldiamine at 600rpm for 5min to obtain the component B;
and step two, adding the component B formed in the step one into the dispersion kettle main body 10 to perform high-speed dispersion and defoaming with the component A, controlling the rotating speed at 520rpm, controlling the absolute vacuum degree at 100mbar, and controlling the defoaming time at 15min to obtain a finished product. Note: during the process of batching at 520rpm, the situation of material splashing is found, therefore, the rotating speed is controlled below 500rpm, and the upper limit of the rotating speed for avoiding the situation of material splashing is 480 rpm.
Comparative example 5
Comparative example 5 differs from example 1 in that: a preparation process of an epoxy resin pouring sealant comprises the following steps:
step one, preparing a component A and a component B:
preparing a component A, weighing alumina, boron nitride and aluminum nitride according to a mass ratio of 65:22:20, mixing and dispersing for 10min at 500rpm to obtain a filler, weighing 690g of the filler, drying for 2h at 120 ℃, cooling to room temperature, storing at a dry place for later use, then adding 250g of epoxy resin, 690g of the dried filler, 30g of polyethylene glycol diglycidyl ether and 150g of carboxyl-terminated liquid nitrile rubber into a dispersion kettle main body 10 in a first device through a feeding pipe 12, and performing high-speed dispersion and defoaming with an absolute vacuum degree of 30mbar, a rotating speed of 350rpm and time of 30min to obtain the component A;
preparing a component B, namely mixing 650g of liquid methyl tetrahydrophthalic anhydride and 50g of benzyldiamine at 600rpm for 5min to obtain the component B;
and step two, adding the component B formed in the step one into the dispersion kettle main body 10 to perform high-speed dispersion and defoaming with the component A, controlling the rotating speed at 350rpm, controlling the absolute vacuum degree at 30mbar and controlling the defoaming time at 30min to obtain a finished product.
Comparative example 6
Comparative example 6 differs from example 1 in that: a preparation process of an epoxy resin pouring sealant comprises the following steps:
step one, preparing a component A and a component B:
preparing a component A, weighing alumina, boron nitride and aluminum nitride according to a mass ratio of 65:22:20, mixing and dispersing for 10min at 500rpm to obtain a filler, weighing 690g of the filler, drying for 2h at 120 ℃, cooling to room temperature, storing at a dry place for later use, adding 250g of epoxy resin, 690g of the dried filler, 30g of polyethylene glycol diglycidyl ether and 150g of carboxyl-terminated liquid nitrile rubber into a dispersion kettle main body 10 in a first device through a feeding pipe 12, and performing high-speed dispersion and defoaming with an absolute vacuum degree of 300mbar, a rotating speed of 350rpm and a time of 30min to obtain the component A;
preparing a component B, namely mixing 650g of liquid methyl tetrahydrophthalic anhydride and 50g of benzyldiamine at 600rpm for 5min to obtain the component B;
and step two, adding the component B formed in the step one into the dispersion kettle main body 10 to perform high-speed dispersion and defoaming with the component A, controlling the rotating speed at 350rpm, controlling the absolute vacuum degree at 300mbar and controlling the defoaming time at 30min to obtain a finished product.
Performance test
Detection method/test method
1. Testing the material dispersion performance: and screening through a 100-mesh screen, and observing whether particulate matter residues exist on the screen, thereby judging the dispersion condition of the ingredients.
2. Testing the water content of the group A and the group B: the method is carried out according to the specification in GB/T6283-2008 'determination of the moisture content in chemical products, Karl Fischer method (general method)'.
3. Testing the insulating property of the condensate: according to GB/T15022.2-2007 part 2 of resin-based active compounds for electrical insulation: the test was carried out according to the protocol of test methods.
4. Specific gravity test: the method is carried out according to the regulations of GB/T12007.5-1989 pycnometer method for epoxy resin densitometry.
5. Testing of thermal conductivity coefficient: the measurement was carried out according to the specification of GB/T11205-2009 "Heat-ray method for measuring thermal conductivity of rubber".
Data analysis
Table 1 shows the dispersion test parameters of examples 1 to 10 and comparative examples 1 to 6
Test item Situation(s)
Example 1 Uniformly dispersed, and no particle residue is left after 100-mesh screening
Example 2 Uniformly dispersed, and no particle residue is left after 100-mesh screening
Example 3 Uniformly dispersed, and no particle residue is left after 100-mesh screening
Example 4 Uniformly dispersed, and no particle residue is left after 100-mesh screening
Example 5 Uniformly dispersed, and no particle residue is left after 100-mesh screening
Example 6 Uniformly dispersed, and no particle residue is left after 100-mesh screening
Example 7 Uniformly dispersed, and no particle residue is left after 100-mesh screening
Example 8 Uniformly dispersed, and no particle residue is left after 100-mesh screening
Example 9 Uniformly dispersed, and no particle residue is left after 100-mesh screening
Example 10 Uniformly dispersed, and no particle residue is left after 100-mesh screening
Comparative example 1 Uneven dispersion, residual particles on 100-mesh screen
Comparative example 2 Uneven dispersion, more particulate matter remains on a 100-mesh screen
Comparative example 3 Uneven dispersion, residual particles on 100-mesh screen
Comparative example 4 Uniformly dispersed, and no particle residue is left after 100-mesh screening
Comparative example 5 Uniformly dispersed, and no particle residue is left after 100-mesh screening
Comparative example 6 Uneven dispersion, residual particles on 100-mesh screen
Table 2 shows the test parameters of examples 1 to 10 and comparative examples 1 to 6
Specific gravity (g/ml) Coefficient of thermal conductivity w/(m k) Water content ppm Insulating property omega mm
Example 1 1.85 1.114 468 1.02*1016
Example 2 1.86 1.116 390 1.08*1016
Example 3 1.84 1.116 432 1.05*1016
Example 4 1.87 1.113 464 1.02*1016
Example 5 1.86 1.114 346 1.12*1016
Example 6 1.85 1.116 367 1.10*1016
Example 7 1.86 1.117 96 1.23*1016
Example 8 1.85 1.116 403 1.06*1016
Example 9 1.84 1.113 496 8.7*1015
Example 10 1.86 1.116 106 1.21*1016
Comparative example 1 1.78 1.058 1038 7.21*1014
Comparative example 2 1.79 1.064 1520 3.1*1014
Comparison ofExample 3 1.81 1.112 512 7.9*1015
Comparative example 4 1.85 1.115 401 1.02*1016
Comparative example 5 1.86 1.115 382 1.09*1016
Comparative example 6 1.84 1.112 682 2.1*1015
It can be seen from the combination of examples 1-10 and comparative examples 1-6 and the combination of Table 1-2 that the vacuum defoaming treatment is performed by using a high-speed dispersing device in the first equipment, the absolute vacuum degree is controlled to be 50-100mbar, the rotation speed is 350-480rpm, the time is 15-30min in the first step, the absolute vacuum degree is controlled to be 50-200mbar, the rotation speed is 350-480rpm, and the time is 15-100min in the second step, so that a finished product with lower water content and better insulating property can be prepared, the time of the whole process can be effectively shortened, and the whole production efficiency can be improved.
As can be seen by combining examples 1 to 10 and comparative examples 1 to 6 with tables 1 to 2, in example 5, as compared with example 1, the efficiency of the vacuum defoaming treatment using the high-speed dispersing device in the second apparatus is superior to that using the high-speed dispersing device in the first apparatus.
It can be seen from the combination of examples 1-10 and comparative examples 1-6 and the combination of tables 1-2 that the dispersion effect of the material in example 1 is better than that of the material in comparative example 3 and is similar to that of the material in comparative example 4, therefore, the vacuum defoaming treatment is performed by using a self-developed high-speed dispersing device, the absolute vacuum degree is controlled at 100mbar in the first step, the rotating speed is 350 and 480rpm, the time is 15-30min in the second step, the absolute vacuum degree is controlled at 100mbar, the rotating speed is 350 and 480rpm, and the time is 15-30min, so that a finished product with low water content and better insulating property can be prepared, the time of the whole process can be effectively shortened, and the whole production efficiency can be improved.
As can be seen by combining examples 1-10 and comparative examples 1-6 with tables 1-2, the prepared product in example 7 has the lowest water content and the best insulation, and therefore, in the second step of example 7, the rotating speed is controlled to 480rpm, the absolute vacuum degree is 100mbar, the defoaming time is 60min, after defoaming is 60min, stirring is stopped, and vacuum pumping is continued for 40min, so that the epoxy resin potting adhesive with low water content and excellent insulation can be obtained. Although the overall process time is prolonged compared with that of the embodiments 1 to 6, the finally prepared product has low water content and excellent insulating property, and compared with the comparative example 1, the overall process time is shortened, so that the accuracy of ingredients can be ensured, the quality of the product can be improved, the overall process time can be effectively shortened, and the overall production efficiency can be improved.
The present embodiment is only for explaining the present application, and it is not limited to the present application, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present application.

Claims (9)

1. A preparation process of epoxy resin pouring sealant comprises the following steps of (1) independently storing the component A and the component B, and mixing the component A and the component B according to the weight part ratio of 1 (0.4-0.7) when in use; the component A comprises the following raw material components in parts by weight: 25-40 parts of epoxy resin; 62-69 parts of a filler; 3-5 parts of a reactive diluent; 5-15 parts of a toughening agent; the component B comprises the following raw material components in parts by weight: 65-70 parts of a curing agent; 5-7 parts of a curing accelerator; the filler is prepared from 65-75 parts of alumina, 17-22 parts of aluminum nitride and 17-22 parts of boron nitride; the density of the alumina is 4.0g/ml, and the grain diameter D50 is 15-25 μm; the density of the boron nitride is 2.3g/ml, and the grain diameter D50 is 8-12 μm; the density of the aluminum nitride is 3.0g/ml, the grain diameter D50 is 2-5 μm, and the aluminum nitride is characterized in that: the epoxy resin pouring sealant is prepared by the following method,
step one, preparing a component A and a component B:
preparing a component A, namely measuring aluminum oxide, aluminum nitride and boron nitride according to a ratio, uniformly mixing, drying at the temperature of 110-125 ℃ for 1-2h, cooling to room temperature to obtain a filler, measuring epoxy resin, the filler, an active diluent and a toughening agent according to a ratio, adding the epoxy resin, the filler, the active diluent and the toughening agent into a high-speed dispersing device (1) for high-speed dispersion and defoaming, controlling the rotating speed at 350-480rpm, the absolute vacuum degree at 50-100mbar and the defoaming time at 15-30min to obtain the component A;
preparing a component B, namely uniformly mixing a curing agent and a curing accelerator which are accurately metered to obtain the component B;
step two, adding the component B into a high-speed dispersing device (1) to perform high-speed dispersion and defoaming with the component A, controlling the rotating speed at 350-480rpm, controlling the absolute vacuum degree at 50-200mbar and controlling the defoaming time at 15-100min to obtain a finished product; the high-speed dispersing device (1) comprises a dispersing kettle main body (10), a driving motor (2) and a combined dispersing assembly (3), wherein the dispersing kettle main body (10) is detachably connected with a sealing cover (11); the driving motor (2) is fixedly connected to the sealing cover (11); the driving motor (2) is fixedly connected with the combined dispersing component (3) through a coupler; the combined dispersing component (3) is positioned in the dispersing kettle main body (10) and is used for dispersing and defoaming materials; the sealing cover (11) is fixedly communicated with a feeding pipe (12) communicated with the interior of the dispersion kettle main body (10); the center of the bottom of the dispersion kettle main body (10) is fixedly communicated with a discharge pipe (13) communicated with the interior of the dispersion kettle main body (10).
2. The preparation process of the epoxy resin pouring sealant as claimed in claim 1, wherein: the combined dispersing assembly (3) comprises a flow guide part (4) and a combined stirrer (5), and the flow guide part (4) is detachably connected to the lower surface of the sealing cover (11); the flow guide piece (4) is integrally formed with a flow channel (40) penetrating through the upper surface and the lower surface of the flow guide piece (4); one end of the combined stirrer (5) is fixedly connected to an output shaft of the driving motor (2) through a coupler, and the other end of the combined stirrer (5) is close to the inner bottom surface of the dispersion kettle main body (10); the vertical distance between the other end surface of the combined stirrer (5) and the inner bottom surface of the dispersion kettle main body (10) is 1.0-50.0 mm; the combined stirrer (5) is positioned in the flow channel (40), and a gap is reserved between the combined stirrer (5) and the flow channel (40); during the rotation process of the combined stirrer (5), the material positioned at the bottom in the dispersion kettle main body (10) moves upwards in the flow channel (40) along the axis of the flow channel (40).
3. The preparation process of the epoxy resin pouring sealant as claimed in claim 2, wherein: the flow guide part (4) comprises a flow guide main part (41), a liquid guide dispersible tablet (42) and a mounting flange (43), and the geometric shape of the flow guide main part (41) is a circular ring column; the liquid guiding dispersible tablet (42) is fixedly connected to the outer side wall of the upper part of the flow guiding main part (41); the mounting flange (43) is fixedly connected to the outer side wall of the top of the flow guide main part (41); the mounting flange (43) is detachably connected to the lower surface of the sealing cover (11); a plurality of liquid guide circular holes (411) communicated with the flow channel (40) are formed in the outer side wall of the flow guide main part (41) in a penetrating mode; the liquid guide circular holes (411) are uniformly arranged around the central axis of the flow guide main part (41); the distance between the adjacent liquid guide circular holes (411) is equal; the liquid guide circular hole (411) is positioned between the liquid guide dispersible tablet (42) and the mounting flange (43); and a gap for material backflow is reserved between one end of the liquid guiding dispersion tablet (42), which is back to the side wall of the flow guiding main part (41), and the inner wall of the dispersion kettle main body (10).
4. The preparation process of the epoxy resin pouring sealant as claimed in claim 3, wherein: the relative ground height of one end of the liquid guiding dispersion tablet (42) back to the side wall of the flow guiding main part (41) is lower than the relative ground height of the joint of the liquid guiding dispersion tablet (42) and the side wall of the flow guiding main part (41).
5. The preparation process of the epoxy resin pouring sealant as claimed in claim 4, wherein: one end point of the liquid guiding dispersion tablet (42), which is back to the side wall of the flow guiding main part (41), and one point of the connection part of the liquid guiding dispersion tablet (42) and the side wall of the flow guiding main part (41) are connected and positioned in a vertical plane, and an acute angle formed by the connection part and the horizontal plane is 10-40 degrees.
6. The preparation process of the epoxy resin pouring sealant as claimed in claim 2, wherein: the combined stirrer (5) comprises a spiral stirrer (51), and one end of the spiral stirrer (51) is fixedly connected to an output shaft of the driving motor (2) through a coupler; the vertical distance between the end face of the other end of the spiral stirrer (51) and the inner bottom surface of the dispersion kettle main body (10) is 1.0-50.0 mm; the length of a spiral belt on the spiral stirrer (51) is 0.95-1.02 times of the vertical distance from the central axis of the liquid guide circular hole (411) to the lower surface of the flow guide main part (41).
7. The preparation process of the epoxy resin pouring sealant as claimed in claim 6, wherein: the combined stirrer (5) further comprises a dispersion disc (52), and the dispersion disc (52) is fixedly connected to the screw circumference of the spiral stirrer (51); a gap is reserved between the dispersion disc (52) and the flow channel (40); the dispersion disc (52) is fixedly connected to the periphery of a screw of the spiral stirrer (51) in a reverse direction; in the rotating process of the dispersion disc (52), the materials in the flow channel (40) move upwards in the flow channel (40) along the axial direction of the flow channel (40); the vertical height of the upper surface of the dispersion disc (52) relative to the ground is 0.95-1.02 times of the vertical distance height between the central axis of the liquid guide circular hole (411) and the ground.
8. The preparation process of the epoxy resin pouring sealant as claimed in claim 6, wherein: the combined stirrer (5) further comprises a speed reducing component (53), and the speed reducing component (53) is connected to the circumferential direction of a screw of the spiral stirrer (51); the dispersion disc (52) is rotatably connected with a speed reducing assembly (53); the dispersion disc (52) is reversely arranged on the speed reducing assembly (53), and in the rotating process of the dispersion disc (52), materials in the flow channel (40) move upwards in the flow channel (40) along the axial direction of the flow channel (40); the height of the upper surface of the dispersion disc (52) relative to the ground is 0.95-1.02 times of the height of the vertical distance from the central axis of the liquid guide circular hole (411) to the ground.
9. The preparation process of the epoxy resin pouring sealant as claimed in claim 8, wherein: the speed reduction assembly (53) comprises a driving gear (531), a transmission gear (532), a connecting rod (533) and a connecting plate (534), and the driving gear (531) is fixedly connected to the periphery of a screw of the spiral stirrer (51); the transmission gear (532) is meshed with the driving gear (531); the transmission gear (532) is fixedly connected to the circumferential direction of the connecting rod (533); the connecting plate (534) is vertically and fixedly connected to the inner wall of the flow guide main part (41); the connecting rod (533) rotates and is fixed between the two connecting plates (534); one end of the connecting rod (533) penetrates through the upper surface and the lower surface of the connecting plate (534), and the connecting rod (533) is rotatably connected to the connecting plate (534); the dispersion disc (52) is fixedly connected to the periphery of the rod end of the upper surface and the lower surface of the connecting rod (533) in a penetrating mode, and the dispersion disc (52) is located on the upper portion of the connecting rod (534).
CN202111407526.8A 2021-11-24 2021-11-24 Preparation process of epoxy resin pouring sealant Pending CN113913141A (en)

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CN110052191A (en) * 2019-04-15 2019-07-26 无锡市英波化工有限公司 Low VOC large arch dam anti-corrosion oil resistant coating process system, technique and its formula
CN212119108U (en) * 2020-04-23 2020-12-11 中山凯旋真空科技股份有限公司 Vacuum degassing tank

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CN104941493A (en) * 2015-06-02 2015-09-30 西安理工大学 Efficient defoaming solvent-free composite mixing unit cylinder
CN205435070U (en) * 2015-12-24 2016-08-10 深圳市欣音达科技有限公司 High -efficient vacuum defoamation device
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