CN115975566A - Single-component pouring sealant suitable for automobile radar and preparation method thereof - Google Patents
Single-component pouring sealant suitable for automobile radar and preparation method thereof Download PDFInfo
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- CN115975566A CN115975566A CN202211734058.XA CN202211734058A CN115975566A CN 115975566 A CN115975566 A CN 115975566A CN 202211734058 A CN202211734058 A CN 202211734058A CN 115975566 A CN115975566 A CN 115975566A
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- 239000000565 sealant Substances 0.000 title claims abstract description 39
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000003063 flame retardant Substances 0.000 claims abstract description 23
- 229920005989 resin Polymers 0.000 claims abstract description 22
- 239000011347 resin Substances 0.000 claims abstract description 22
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 21
- 238000003756 stirring Methods 0.000 claims description 21
- 229920000642 polymer Polymers 0.000 claims description 20
- 150000001875 compounds Chemical class 0.000 claims description 16
- 239000002245 particle Substances 0.000 claims description 11
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims description 9
- 239000007788 liquid Substances 0.000 claims description 9
- 238000007710 freezing Methods 0.000 claims description 8
- 230000008014 freezing Effects 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 8
- 150000002460 imidazoles Chemical group 0.000 claims description 7
- VYKXQOYUCMREIS-UHFFFAOYSA-N methylhexahydrophthalic anhydride Chemical compound C1CCCC2C(=O)OC(=O)C21C VYKXQOYUCMREIS-UHFFFAOYSA-N 0.000 claims description 7
- RAXXELZNTBOGNW-UHFFFAOYSA-N imidazole Natural products C1=CNC=N1 RAXXELZNTBOGNW-UHFFFAOYSA-N 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 claims description 3
- 229910001862 magnesium hydroxide Inorganic materials 0.000 claims description 3
- 239000000347 magnesium hydroxide Substances 0.000 claims description 3
- 238000005303 weighing Methods 0.000 claims description 3
- 150000008064 anhydrides Chemical group 0.000 claims description 2
- 239000003822 epoxy resin Substances 0.000 claims description 2
- 229920000647 polyepoxide Polymers 0.000 claims description 2
- 229920001661 Chitosan Polymers 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 9
- 238000005538 encapsulation Methods 0.000 description 9
- 230000006698 induction Effects 0.000 description 4
- 239000000853 adhesive Substances 0.000 description 3
- 230000001070 adhesive effect Effects 0.000 description 3
- 230000004888 barrier function Effects 0.000 description 3
- 239000003292 glue Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 239000000523 sample Substances 0.000 description 3
- 238000001816 cooling Methods 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 238000009472 formulation Methods 0.000 description 2
- 238000004806 packaging method and process Methods 0.000 description 2
- 238000010008 shearing Methods 0.000 description 2
- 239000004593 Epoxy Substances 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005674 electromagnetic induction Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000004382 potting Methods 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 229920001187 thermosetting polymer Polymers 0.000 description 1
- 239000004634 thermosetting polymer Substances 0.000 description 1
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- Sealing Material Composition (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a single-component pouring sealant suitable for an automobile radar and a preparation method thereof, wherein the single-component pouring sealant comprises the following components in parts by mass: 35-55 parts of temperature-resistant resin, 35-40 parts of curing agent, 13-20 parts of flame retardant, 3-5 parts of chitosan rubber and 1-2 parts of accelerator. The invention also provides the single-component pouring sealant suitable for the automobile radar and a preparation method thereof. The single-component pouring sealant suitable for the automobile radar has excellent flame retardance and heat conduction performance, easy curing condition, normal-temperature operability, low thermal expansion coefficient, higher insulating property and mechanical property. Compared with the prior art, the single-component pouring sealant provided by the invention has remarkable progress in passing a cold and hot impact cycle test at-50 ℃ to 125 ℃ and a double 85 test.
Description
Technical Field
The invention belongs to the technical field of epoxy pouring sealants, and particularly relates to a single-component high-pouring sealant applied to an automobile radar and a preparation method thereof.
Background
The encapsulation is to inject liquid encapsulation glue into a device provided with electronic components and a PCB circuit in a mechanical or manual mode, and the liquid encapsulation glue is cured into a thermosetting polymer insulating material at normal temperature or in a heating state, so that the purposes of bonding, sealing, encapsulation, coating protection and the like are achieved; the integrity and the insulativity of the electronic device can be enhanced, elements and lines are prevented from being directly exposed, and the waterproof, dustproof and moistureproof performances are achieved.
The automobile radar sensor transmits signals through the induction coil, an echo signal can be generated when the automobile radar sensor touches a barrier, the sensor can process the received echo signal through the host to judge the position of the barrier, and the front of a driver can be warned of the barrier, so that driving is safer. The induction coil is packaged in a narrow cavity, the metal coil is wound in the cavity and is connected to the coil in the cavity through two metal wires, and the metal coil generates current, electromagnetic induction and the like in the cavity and needs an insulating environment in the cavity, so that glue is required to be filled and sealed in the packaged induction coil part to enable the packaged induction coil part to be a whole, and the resistance to external impact and vibration is improved; meanwhile, the coil is prevented from being directly exposed, and the waterproof, dustproof and damp-proof performance of the whole device is improved.
The automobile industry in China is in a high-speed development stage, the automobile configuration is gradually improved, and the radar sensor with a higher proportion is also the same, so that the method has higher requirements on the development of the encapsulation technology of the radar sensor component. Because the narrow cavity containing the coil is encapsulated and the coil and the cavity are prevented from falling off, the encapsulating material is required to have higher insulating property, mechanical property and lower thermal expansion coefficient; meanwhile, the reliability of the sensor can be ensured by considering flame retardance, moisture resistance and low viscosity. The patent No. CN1150288804A discloses a semiconductor pouring sealant which has complex specific synthesis method, high curing conditions and high production requirements.
Therefore, it is necessary to provide a potting adhesive for radar sensors for vehicles, which has high insulation and flame retardancy, low viscosity, moisture resistance and aging resistance.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: the problem that the coil cannot be tightly bonded with the shell due to the fact that the coil is easy to crack or fall off when the temperature is increased because the cold and hot expansion coefficient is too large is solved; the problems of high viscosity and incapability of high-efficiency encapsulation in the process are solved; the low shearing force is overcome, and the resistance of the packaging device to external impact is improved.
In order to solve the technical problems, the invention provides the following technical scheme:
the single-component pouring sealant suitable for the automobile radar comprises temperature-resistant resin, a curing agent, a flame retardant, shell polymer rubber and an accelerant, and is characterized in that the temperature-resistant resin, the curing agent, the flame retardant, the shell polymer rubber and the accelerant are prepared from the following components in parts by weight:
as a further scheme of the invention, the temperature-resistant resin selected by the pouring sealant is one or more of polyfunctional epoxy resin AFG-90, EPM-420 and AG-80, preferably EPM-420.
As a further scheme of the invention, the shell polymer rubber particles selected by the pouring sealant are XP-425 and/or EPX-125, preferably XP-425.
As a further scheme of the invention, the flame retardant selected by the pouring sealant is one or two of aluminum hydroxide and magnesium hydroxide, and preferably, the aluminum hydroxide.
As a further scheme of the invention, the curing agent selected by the pouring sealant is an anhydride curing agent, preferably methyl hexahydrophthalic anhydride.
As a further proposal of the invention, the accelerator used by the pouring sealant is a modified imidazole accelerator, preferably 2101 CN-liquid imidazole is used as the accelerator.
The invention also provides a preparation method of the single-component pouring sealant suitable for the automobile radar, which is characterized by comprising the following steps of:
the method comprises the following steps: weighing 35-55 parts of temperature-resistant resin, 35-40 parts of curing agent, 13-20 parts of flame retardant, 3-5 parts of shell polymer rubber and 1-2 parts of accelerator according to the mass parts;
step two: putting the temperature-resistant resin and the shell polymer rubber particles into a stirrer, and stirring for 15 minutes in vacuum at the rotating speed of 250rpm;
step three: adding the flame retardant into the compound stirred in the second step, and stirring for 30 minutes at the rotating speed of 500rpm in a vacuum environment;
step four: freezing the compound stirred in the step three to 10-15 ℃ at low temperature, adding a curing agent into the frozen compound, and stirring at the rotating speed of 250rpm in vacuum for 15 minutes;
step five: freezing the compound stirred in the step four to 10-15 ℃ at low temperature, adding the accelerant into the frozen compound, stirring, and stirring for 30 minutes in vacuum at the rotating speed of 500 rpm;
step six: and 5, freezing the mixture stirred in the fifth step at a low temperature to obtain the single-component pouring sealant suitable for the automobile radar.
The invention has the following beneficial effects:
1. the single-component pouring sealant suitable for the automobile radar is low in viscosity, good in flowability and high in pouring efficiency.
2. The single-component pouring sealant applicable to the automobile radar is filled with the shell polymer rubber particles, so that the mechanical and thermal stability of the pouring sealant can be improved.
3. The invention provides a single-component pouring sealant suitable for automobile radars, which adopts a temperature-resistant resin and a flame retardant which can pass a UL94V-0 flame retardant test and 10 cycle tests of impact at a temperature of between 50 ℃ below zero and 125 ℃.
Detailed Description
The invention provides a single-component high-heat-conductivity adhesive, which aims to solve the problems that: the coil is easy to crack or fall off when the temperature is increased due to overlarge cold and hot expansion coefficient, so that the coil cannot be tightly bonded with the shell; the viscosity is high, and the efficient encapsulation cannot be realized in the process; the shearing force is small, and the problem that the whole resistance to external force impact cannot be ensured.
The following technical scheme is proposed for the problems: a single-component pouring sealant suitable for automobile radars and a preparation method thereof are disclosed, the general idea is as follows:
the method comprises the following steps: weighing 35-55 parts of temperature-resistant resin, 35-40 parts of curing agent, 13-20 parts of flame retardant, 3-5 parts of shell polymer rubber and 1-2 parts of accelerator according to the mass parts;
step two: putting the temperature-resistant resin and the shell polymer rubber particles into a stirrer, and stirring for 15 minutes in vacuum at the rotating speed of 250rpm;
step three: adding the flame retardant into the compound stirred in the second step, and stirring for 30 minutes at the rotating speed of 500rpm in a vacuum environment;
step four: putting the compound stirred in the step three into a low temperature freezer to 10-15 ℃, adding a curing agent into the frozen compound, and stirring at the rotating speed of 250rpm for 15 minutes in vacuum;
step five: freezing the compound stirred in the step four to 10-15 ℃ at low temperature, adding the accelerant into the frozen compound, stirring, and stirring for 30 minutes in vacuum at the rotating speed of 500 rpm;
step six: freezing the mixture stirred in the fifth step at low temperature to obtain the single-component pouring sealant suitable for the automobile radar
In order to better understand the technical scheme, the technical scheme is described in detail in the following with reference to the description tables 1-1 and 1-2 and specific embodiments.
Example one
The pouring sealant in the embodiment of the invention comprises 35 parts of temperature-resistant resin, preferably EPM-420, 38 parts of curing agent, preferably methyl hexahydrophthalic anhydride, 20 parts of flame retardant, preferably aluminum hydroxide, 5 parts of shell polymer rubber particles, preferably XP-425, 2 parts of accelerator, preferably 2101 CN-liquid modified imidazole; the operation steps are as follows: stirring temperature-resistant resin EPM-420 and shell polymer rubber particles XP-425 for 15 minutes at the rotating speed of 250rpm in vacuum, adding flame retardant aluminum hydroxide for stirring for 30 minutes at the rotating speed of 500rpm in vacuum, freezing the stirred compound at low temperature to 10 ℃, adding curing agent methyl hexahydrophthalic anhydride, stirring for 15 minutes at the rotating speed of 250rpm in vacuum, cooling at low temperature to 12 ℃ after stirring, adding accelerator 2101 CN-liquid modified imidazole, stirring for 30 minutes at the rotating speed of 500rpm in vacuum, and cooling at low temperature after stirring to obtain the adhesive pouring sealant of the embodiment.
Example two
The pouring sealant in the embodiment of the invention comprises 40 parts of temperature-resistant resin, preferably EPM-420, 37 parts of curing agent, preferably methyl hexahydrophthalic anhydride, 16 parts of flame retardant, preferably aluminum hydroxide, 5 parts of shell polymer rubber particles, preferably XP-425, 2 parts of accelerator, preferably 2101 CN-liquid modified imidazole; the operation steps are consistent with the first example.
EXAMPLE III
The pouring sealant in the embodiment of the invention comprises 45 parts of temperature-resistant resin, preferably EPM-420, 35 parts of curing agent, preferably methyl hexahydrophthalic anhydride, 15 parts of flame retardant, preferably aluminum hydroxide, 4 parts of shell polymer rubber particles, preferably XP-425, 1 part of accelerator, preferably 2101 CN-liquid modified imidazole; the operation steps are consistent with example one.
Example four
The pouring sealant in the embodiment of the invention is prepared from 55 parts of temperature-resistant resin, preferably EPM-420, 28 parts of curing agent, preferably methyl hexahydrophthalic anhydride, 13 parts of flame retardant, preferably aluminum hydroxide, 3 parts of shell polymer rubber particles, preferably XP-425, 1 part of accelerator, preferably 2101 CN-liquid modified imidazole; the operation steps are consistent with the first example.
Comparative example 1
The difference between the formula of the pouring sealant in the comparative example of the invention and the second example is as follows: the temperature-resistant resin is AFG-90, the shell polymer rubber is EPX-125, and the flame retardant is magnesium hydroxide; the remaining parts by mass and procedure were identical to example two.
Comparative example No. two
The difference between the formula of the pouring sealant in the embodiment of the invention and the first comparative example is as follows: the temperature-resistant resin is AG-80; the remaining parts by mass and steps were identical to those of comparative example two.
Each set of formulations for examples 1-4 and comparative examples 1-2 is shown in Table 1-1, and each set of formulations for examples 1-4 and comparative examples 1-2 corresponds to properties shown in Table 1-2, where the viscosity test method: taking 200ml of a test sample at 25 ℃ in a standard environment by using a Brookfield HBDV-2T viscometer, placing a probe in the test sample, and reading after data are stable; the thermal expansion coefficient is tested by adopting the ASTM E831-14 standard, the temperature is-40 ℃ to 280 ℃, and the unit is mum/(m DEG C); hardness standard ISO 868 shore D200 degree C4 hours; the shear strength test adopts ISO 4857 standard, steel is ground the sand surface; the cold and hot impact temperature range is-50 ℃ to 125 ℃; the volume resistivity is tested by adopting the IEC 60093 standard; the curing conditions were 100 ℃ and 3mm thick.
Tables 1 to 1:
| example one | Example two | Example three | Example four | Comparative example 1 | Comparative example No. two | |
| Temperature resistant resin | 35 | 40 | 45 | 55 | 40 | 40 |
| Curing agent | 38 | 37 | 35 | 28 | 37 | 37 |
| Flame retardant | 20 | 16 | 15 | 13 | 16 | 16 |
| Chitosan polymer | 5 | 5 | 4 | 3 | 5 | 5 |
| Accelerator | 2 | 2 | 1 | 1 | 2 | 2 |
(Note: the mixture ratio of the components in the table is mass fraction)
Tables 1-2:
(Note: the above example data is available from the laboratory)
The technical scheme in the embodiment of the invention has the following technical effects:
1. the viscosity is low, the encapsulation is convenient, and the encapsulation efficiency in production can be improved by 15%;
2. the curing time is short, the curing can be completely carried out within 22 minutes at the fastest speed of 100 ℃ and 3mm, the subsequent packaging time is effectively shortened, and the overall production efficiency is improved;
3. the thermal shock resistance is circulated for 10 times, the flame retardant grade reaches UL94V-0 grade, and the stability and reliability of the encapsulated device can be effectively ensured.
Claims (7)
1. The single-component pouring sealant suitable for the automobile radar comprises temperature-resistant resin, a curing agent, a flame retardant, shell polymer rubber and an accelerant, and is characterized in that the temperature-resistant resin, the curing agent, the flame retardant, the shell polymer rubber and the accelerant are prepared from the following components in parts by weight:
2. the single-component pouring sealant suitable for the automotive radar as claimed in claim 1, wherein: the temperature-resistant resin is one or more of polyfunctional epoxy resin AFG-90, EPM-420 and AG-80, preferably EPM-420.
3. The one-component pouring sealant suitable for the automotive radar as claimed in claim 1, wherein: the shell polymer rubber particles are one or two of XP-425 and EPX-125, preferably XP-425.
4. The single-component pouring sealant suitable for the automotive radar as claimed in claim 1, wherein: the flame retardant is one or two of aluminum hydroxide and magnesium hydroxide, and preferably is aluminum hydroxide.
5. The single-component pouring sealant suitable for the automotive radar as claimed in claim 1, wherein: the curing agent is an anhydride curing agent, preferably methyl hexahydrophthalic anhydride.
6. The one-component pouring sealant suitable for the automotive radar as claimed in claim 1, wherein: the accelerator is a modified imidazole accelerator, preferably 2101 CN-liquid imidazole as the accelerator.
7. The preparation method of the single-component pouring sealant suitable for the automobile radar is characterized by comprising the following steps of:
the method comprises the following steps: weighing 35-55 parts of temperature-resistant resin, 35-40 parts of curing agent, 13-20 parts of flame retardant, 3-5 parts of shell polymer rubber and 1-2 parts of accelerator according to the mass parts;
step two: putting the temperature-resistant resin and the shell polymer rubber particles into a stirrer, and stirring for 15 minutes in vacuum at the rotating speed of 250rpm;
step three: adding the flame retardant into the compound stirred in the second step, and stirring for 30 minutes at the rotating speed of 500rpm in a vacuum environment;
step four: putting the compound stirred in the step three into a low temperature freezer to 10-15 ℃, adding a curing agent into the frozen compound, and stirring at the rotating speed of 250rpm for 15 minutes in vacuum;
step five: freezing the compound stirred in the step four to 10-15 ℃ at low temperature, adding the accelerant into the frozen compound, stirring, and stirring for 30 minutes in vacuum at the rotating speed of 500 rpm;
step six: and 5, freezing the mixture stirred in the fifth step at a low temperature to obtain the single-component pouring sealant suitable for the automobile radar.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211734058.XA CN115975566A (en) | 2022-12-30 | 2022-12-30 | Single-component pouring sealant suitable for automobile radar and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211734058.XA CN115975566A (en) | 2022-12-30 | 2022-12-30 | Single-component pouring sealant suitable for automobile radar and preparation method thereof |
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| Publication Number | Publication Date |
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| CN115975566A true CN115975566A (en) | 2023-04-18 |
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| CN202211734058.XA Pending CN115975566A (en) | 2022-12-30 | 2022-12-30 | Single-component pouring sealant suitable for automobile radar and preparation method thereof |
Country Status (1)
| Country | Link |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20130115442A1 (en) * | 2011-11-09 | 2013-05-09 | Cytec Technology Corp. | Structural adhesive and bonding application thereof |
| CN110467896A (en) * | 2019-08-13 | 2019-11-19 | 上海闰龙电子材料有限公司 | A kind of high heat resistance & low temperature resistant epoxy resin casting glue and preparation method thereof |
| CN113913142A (en) * | 2021-11-26 | 2022-01-11 | 铠博新材料(天津)有限公司 | High-thermal-conductivity epoxy resin adhesive for energy storage battery |
-
2022
- 2022-12-30 CN CN202211734058.XA patent/CN115975566A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20130115442A1 (en) * | 2011-11-09 | 2013-05-09 | Cytec Technology Corp. | Structural adhesive and bonding application thereof |
| CN110467896A (en) * | 2019-08-13 | 2019-11-19 | 上海闰龙电子材料有限公司 | A kind of high heat resistance & low temperature resistant epoxy resin casting glue and preparation method thereof |
| CN113913142A (en) * | 2021-11-26 | 2022-01-11 | 铠博新材料(天津)有限公司 | High-thermal-conductivity epoxy resin adhesive for energy storage battery |
Non-Patent Citations (1)
| Title |
|---|
| 张敏;饶保林;田华杰;李小萍;: "混合动力汽车引擎用高导热环氧灌封胶的研制", 绝缘材料, no. 01, 20 February 2011 (2011-02-20) * |
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