A kind of detachable sealant and preparation method thereof

Abstract

The present invention relates to the technical field of sealants, in particular to a detachable sealant and a preparation method thereof. The sealant is mainly prepared from the following components in mass fractions: 20-30 parts of silane-modified polyether resin, 20-25 parts of plasticizer, 45-55 parts of flame retardant additive, 3-4 parts of coupling agent, and 0.1-1 parts of catalyst. By improving the formula and preparation method of the sealant, the detachable sealant of the present invention can reach V0 level of flame retardancy after encountering flame combustion (1200°C); the insulation effect volume resistance reaches 10 14 Ω*cm; Air tightness: Under 80℃ heating conditions, the water vapor transmission rate is less than 5*10 ‑3 cm 2 *min, which can ensure that the sealed battery pack shell or sealed pipe is not affected by water vapor. The shear strength is lower than 0.2MPa, which meets the detachable requirements. The elongation at break is higher than 100%, and the tensile strength is higher than 1MPa, which has good flexibility and toughness, ensuring that the battery pack can maintain the sealing of the shell under the destructive forces such as vibration, swing and impact.

Description

Technical Field

[0001] The present invention relates to the field of sealant technology, in particular to a detachable sealant and a preparation method thereof, which is suitable for bonding and sealing between the upper and lower shell (aluminum, stainless steel) structures of a power battery pack of a new energy vehicle. In addition, it can also be used for bonding and sealing of pipelines such as oil pipes and water pipes in an engine compartment, which is convenient for later maintenance and replacement. Background Art

[0002] Modified silane polyether glue (MS glue) is the most widely used glue product on the market. Due to its non-toxic and low VOC characteristics, it is considered to be the first choice for environmentally friendly, green and high-performance adhesives. Chinese invention patent CN 117986564A discloses a silane-modified polyether sealant to replace polyurethane sealant. It aims to reduce the high toxicity of traditional polyurethane sealants and improve the paintability through technologies such as no organic solvent addition and no toxic gas release. However, due to the low elongation at break of the product, the sealing performance is average, and the colloid does not have flame retardant, insulation and other properties. This type of sealant is only used as a conventional adhesive.

[0003] With the rapid development of the new energy vehicle industry, although the use of the above-mentioned traditional sealants to seal battery packs can achieve a certain sealing effect, it is often difficult to remove during maintenance and replacement of parts, which brings great difficulties to the maintenance of the battery pack. In addition, given the flammable characteristics of new energy battery packs, it is imperative to improve the flame retardancy of the sealant. Summary of the invention

[0004] In view of this, the present invention provides a detachable sealant and a preparation method thereof, which can improve the sealant's formula and process, thereby not only making it detachable, but also optimizing the air permeability, flame retardancy, insulation and other properties of the detachable sealant.

[0005] In order to achieve the above object, the present invention adopts the following technical solutions:

[0006] A removable sealant, characterized in that it is mainly prepared from the following components in the following mass fraction ratios:

[0007]

[0008] Specifically, the silane-modified polyether resin is an alkyl-terminated 107 resin, and its molecular formula is:

[0009]

[0010] Specifically, the plasticizer is diisononyl phthalate and polypropylene glycol, or a combination of the two in any proportion.

[0011] Specifically, the flame retardant auxiliary agent is aluminum hydroxide, melamine cyanurate, or a combination of the two in any proportion.

[0012] Specifically, the coupling agent is methyltrimethoxysilane and γ-aminopropyltriethoxysilane, or a combination of the two in any proportion.

[0013] Specifically, the catalyst is a chelated hybrid organic tin.

[0014] In order to achieve the above object, the present invention further provides a method for preparing a removable sealant as described in any one of the above, comprising the following steps:

[0015] At room temperature, add silane-modified polyether resin, plasticizer, and flame retardant additive into a reaction container, put the reaction container into a vacuum self-rotating revolution mixer, seal it and start the vacuum self-rotating revolution mixer, stir and mix for 60-90 seconds at a vacuum degree of 5-10KPa and a revolution speed of 1000-2000rpm;

[0016] Stop the vacuum auto-rotation and revolution mixer, wait for the sample to cool to room temperature, then start the vacuum auto-rotation and revolution mixer, and stir and mix for 60-90 seconds at a vacuum degree of 5-10 KPa and a revolution speed of 1000-2000 rpm;

[0017] Stop the vacuum auto-rotation stirrer, wait for the sample to cool to room temperature, add the coupling agent into the reaction vessel and seal it, start the vacuum auto-rotation stirrer, and stir and mix for 30-60 seconds at a vacuum degree of 5-10 KPa and a revolution speed of 1000-2000 rpm;

[0018] Stop the vacuum auto-rotating revolution mixer, wait for the sample to cool to room temperature, add the catalyst into the above reaction container and seal it, start the vacuum auto-rotating revolution mixer, and stir and mix for 15-30 seconds at a vacuum degree of 5-10KPa and a revolution speed of 1000-2000rpm.

[0019] Specifically, the flame retardant additive in step (1) needs to be dried in an oven at 100-110° C. for more than 24 hours to remove water before being added to the reaction container.

[0020] Specifically, during the stirring and mixing process of steps (1) to (4), the temperature in the reaction container does not exceed 60°C.

[0021] Compared with the prior art, the present invention has the following beneficial effects:

[0022] The detachable sealant of the present invention has good flame retardant performance. After encountering flame combustion (1200°C), it can achieve V0 grade flame retardant property; the volume resistance reaches 10 14Ω*cm, good insulation effect; and good air tightness, under 80℃ heating conditions, the water vapor transmission rate is less than 5*10 -3 cm 2 *min, which can ensure that the shell of the sealed battery pack or the sealed pipe is not affected by water vapor; the shear strength meets the detachable requirements and is lower than 0.2MPa; it has good flexibility and toughness, the elongation at break is higher than 100%, and the tensile strength is higher than 1MPa, which can ensure that the battery pack can still maintain the sealing of the shell under the destructive force of vibration, swing and impact. At the same time, the preparation method of the detachable sealant is simple, the production process has low energy consumption, and it can be placed for a long time without curing. Specific implementation methods

[0024] The exemplary embodiments disclosed in the present invention are described in more detail below, and these embodiments are for a more thorough understanding of the present invention and to fully convey the scope of the present invention to those skilled in the art. Although exemplary embodiments disclosed in the present invention are shown, it should be understood that the present invention should not be limited by the embodiments set forth herein.

[0025] Table 1 is a table showing the dosage of each component of the removable sealant of Examples 1-5.

[0026] Component dosage Example 1 Example 2 Example 3 Example 4 Example 5 Silane modified polyether 20 25 25 30 30 Plasticizers 21 20 25 20 25 Solid flame retardant additives 55 51 46 45 45 Coupling agent 3.9 3.5 3 4 4 catalyst 0.1 0.5 1 1 1

[0027] Example 1

[0028] The removable sealant of this embodiment is mainly composed of 20 parts of silane-modified polyether resin of brand OFT-200, 21 parts of plasticizer of brand DINP, 55 parts of flame retardant additive of brand APCC, 3.9 parts of coupling agent of brand MTMS, and 0.1 parts of catalyst of brand M-S211.

[0029] The flame retardant additive was dried in an oven at 100° C. for 26 hours to remove water before being added to the reaction vessel.

[0030] The preparation method of the removable sealant of this embodiment comprises the following steps:

[0031] At room temperature, add the modified silane polyether resin, plasticizer, and flame retardant additive after dehydration into a reaction vessel, put the reaction vessel into a vacuum self-rotating revolution mixer, seal it, start the vacuum pump of the vacuum self-rotating revolution mixer, and stir and mix for 90 seconds at a vacuum degree of 5 KPa and a revolution speed of 1000 rpm;

[0032] Stop the vacuum auto-rotation and revolving stirrer, wait for the sample to cool to room temperature, then start the vacuum auto-rotation and revolving stirrer, and stir and mix for 90 seconds at a vacuum degree of 5 KPa and a revolving speed of 1000 rpm;

[0033] Stop the vacuum auto-rotation stirrer, wait for the sample to cool to room temperature, then open the vacuum auto-rotation stirrer, add the coupling agent into the reaction vessel and seal it, start the vacuum auto-rotation stirrer, and stir and mix for 60 seconds at a vacuum degree of 5 KPa and a revolution speed of 1000 rpm;

[0034] Stop the vacuum auto-rotation stirrer, wait for the sample to cool to room temperature, then open the vacuum auto-rotation stirrer, add the catalyst into the reaction vessel and seal it, start the vacuum auto-rotation stirrer, and stir and mix for 30 seconds at a vacuum degree of 5 KPa and a revolution speed of 1000 rpm;

[0035] The temperature of the vacuum rotating and revolving mixer in the above steps is set to not exceed 60°C.

[0036] Example 2

[0037] The removable sealant of this embodiment is mainly composed of 25 parts of silane-modified polyether resin of brand OFT-200, 20 parts of plasticizer of brand DINP, 51 parts of flame retardant additive of brand APCC, 3.5 parts of coupling agent of brand MTMS, and 0.5 parts of catalyst of brand M-S211.

[0038] The flame retardant additive was dried in an oven at 110° C. for 24 hours to remove water before being added to the reaction vessel.

[0039] The preparation method of the removable sealant of this embodiment comprises the following steps:

[0040] At room temperature, add the modified silane polyether resin, plasticizer, and flame retardant additive after dehydration into a reaction container, put the reaction container into a vacuum self-rotating revolution mixer, seal it, start the vacuum pump of the vacuum self-rotating revolution mixer, and stir and mix for 60 seconds at a vacuum degree of 10 KPa and a revolution speed of 2000 rpm;

[0041] Stop the vacuum auto-rotation and revolution mixer, wait for the sample to cool to room temperature, then start the vacuum auto-rotation and revolution mixer, and stir and mix for 60 seconds at a vacuum degree of 10 KPa and a revolution speed of 2000 rpm;

[0042] Stop the vacuum auto-rotation stirrer, wait for the sample to cool to room temperature, then open the vacuum auto-rotation stirrer, add the coupling agent into the reaction vessel and seal it, start the vacuum auto-rotation stirrer, and stir and mix for 30 seconds at a vacuum degree of 10 KPa and a revolution speed of 2000 rpm;

[0043] Stop the vacuum auto-rotation stirrer, wait for the sample to cool to room temperature, then open the vacuum auto-rotation stirrer, add the catalyst into the reaction vessel and seal it, start the vacuum auto-rotation stirrer, and stir and mix for 15 seconds at a vacuum degree of 10 KPa and a revolution speed of 2000 rpm;

[0044] The temperature of the vacuum rotating and revolving mixer in the above steps is set to not exceed 60°C.

[0045] Example 3

[0046] The removable sealant of this embodiment is mainly composed of 25 parts of silane-modified polyether resin of brand OFT-200, 25 parts of plasticizer of brand PPG3000, 46 parts of flame retardant additive of brand MCA, 3 parts of coupling agent of brand KH550, and 1 part of catalyst of brand M-S211.

[0047] The flame retardant additive was dried in an oven at 105° C. for 25 hours to remove water before being added to the reaction vessel.

[0048] The preparation method of the removable sealant of this embodiment comprises the following steps:

[0049] At room temperature, add the modified silane polyether resin, plasticizer, and flame retardant additive after dehydration into a reaction container, put the reaction container into a vacuum self-rotating revolution mixer, seal it, start the vacuum pump of the vacuum self-rotating revolution mixer, and stir and mix for 60 seconds at a vacuum degree of 10 KPa and a revolution speed of 1000 rpm;

[0050] Stop the vacuum auto-rotation and revolving stirrer, wait for the sample to cool to room temperature, then start the vacuum auto-rotation and revolving stirrer, and stir and mix for 60 seconds at a vacuum degree of 10 KPa and a revolving speed of 1000 rpm;

[0051] Stop the vacuum auto-rotation stirrer, wait for the sample to cool to room temperature, then open the vacuum auto-rotation stirrer, add the coupling agent into the reaction vessel and seal it, start the vacuum auto-rotation stirrer, and stir and mix for 45 seconds at a vacuum degree of 10 KPa and a revolution speed of 1000 rpm;

[0052] Stop the vacuum auto-rotation stirrer, wait for the sample to cool to room temperature, open the vacuum auto-rotation stirrer, add the catalyst into the reaction vessel and seal it, start the vacuum auto-rotation stirrer, and stir and mix for 25 seconds at a vacuum degree of 10 KPa and a revolution speed of 1000 rpm;

[0053] The temperature of the vacuum rotating and revolving mixer in the above steps is set to not exceed 60°C.

[0054] Example 4

[0055] The preparation method of the new energy vehicle battery pack sealant of this embodiment is as follows: add 30 parts of silane-modified polyether resin of brand OFT-200, 20 parts of a plasticizer mixed with 10 parts of brand PPG3000 and 10 parts of DINP, 45 parts of a flame retardant additive mixed with 20 parts of brand AP22 and 25 parts of MCA, 4 parts of a coupling agent of brand KH550, and 1 part of a catalyst of brand M-S211.

[0056] The flame retardant additive was dried in an oven at 110° C. for 24 hours to remove water before being added to the reaction vessel.

[0057] The preparation method of the removable sealant of this embodiment comprises the following steps:

[0058] At room temperature, add the modified silane polyether resin, plasticizer, and flame retardant additive after dehydration into a reaction vessel, put the reaction vessel into a vacuum self-rotating revolution mixer, seal it, start the vacuum pump of the vacuum self-rotating revolution mixer, and stir and mix for 70 seconds at a vacuum degree of 7 KPa and a revolution speed of 1800 rpm;

[0059] Stop the vacuum auto-rotation and revolution mixer, wait for the sample to cool to room temperature, then start the vacuum auto-rotation and revolution mixer, and stir and mix for 80 seconds at a vacuum degree of 8 KPa and a revolution speed of 2000 rpm;

[0060] Stop the vacuum auto-rotation stirrer, wait for the sample to cool to room temperature, then open the vacuum auto-rotation stirrer, add the coupling agent into the reaction vessel and seal it, start the vacuum auto-rotation stirrer, and stir and mix for 50 seconds at a vacuum degree of 10 KPa and a revolution speed of 1500 rpm;

[0061] Stop the vacuum auto-rotation stirrer, wait for the sample to cool to room temperature, open the vacuum auto-rotation stirrer, add the catalyst into the above reaction vessel and seal it, start the vacuum auto-rotation stirrer, and stir and mix for 30 seconds at a vacuum degree of 6 KPa and a revolution speed of 1400 rpm;

[0062] The temperature of the vacuum rotating and revolving mixer in the above steps is set to not exceed 60°C.

[0063] Example 5

[0064] The preparation method of the new energy vehicle battery pack sealant of this embodiment is as follows: add 30 parts of silane-modified polyether resin of brand OFT-200, 25 parts of a mixed plasticizer of 5 parts of PPG3000 and 20 parts of DINP, 45 parts of a flame retardant additive of brand MCA, 4 parts of a coupling agent of 2 parts of MTMS and 2 parts of KH550, and 1 part of a catalyst of brand M-S211.

[0065] The flame retardant additive needs to be dried in an oven at 100° C. for 27 hours to remove water before being added to the reaction vessel.

[0066] The preparation method of the removable sealant of this embodiment comprises the following steps:

[0067] At room temperature, add the modified silane polyether resin, plasticizer, and flame retardant additive after dehydration into a reaction container, put the reaction container into a vacuum self-rotating revolution mixer, seal it, start the vacuum pump of the vacuum self-rotating revolution mixer, and stir and mix for 80 seconds at a vacuum degree of 8 KPa and a revolution speed of 1500 rpm;

[0068] Stop the vacuum auto-rotation and revolution mixer, wait for the sample to cool to room temperature, then start the vacuum auto-rotation and revolution mixer, and stir and mix for 75 seconds at a vacuum degree of 8 KPa and a revolution speed of 1400 rpm;

[0069] Stop the vacuum auto-rotation stirrer, wait for the sample to cool to room temperature, then open the vacuum auto-rotation stirrer, add the coupling agent into the reaction vessel and seal it, start the vacuum auto-rotation stirrer, and stir and mix for 40 seconds at a vacuum degree of 7 KPa and a revolution speed of 1500 rpm;

[0070] Stop the vacuum auto-rotation stirrer, wait for the sample to cool to room temperature, open the vacuum auto-rotation stirrer, add the catalyst into the above reaction vessel and seal it, start the vacuum auto-rotation stirrer, and stir and mix for 20 seconds at a vacuum degree of 7 KPa and a revolution speed of 1500 rpm;

[0071] The temperature of the vacuum rotating and revolving mixer in the above steps is set to not exceed 60°C.

[0072] The test results of the performance of the removable sealants prepared in the above Examples 1-5 are as follows:

[0073]

[0074] Among them, the removable sealant in the above embodiment,

[0075] Insulation test: Tested according to GB / T 1693-2007 standard.

[0076] Shear performance test: Tested according to GB / T 7124-2008 standard.

[0077] Among the above embodiments, Example 2 has the best raw material miscibility, best flame retardancy, best disassembly ability, best insulation performance, and best air tightness.

[0078] In the above embodiments,

[0079] The silane-modified polyether resin (brand name OFT-200) used was produced by Chengtian New Materials Co., Ltd.

[0080] The polypropylene glycol (brand name PPG3000) plasticizer used was produced by Jiangsu Haian Petrochemical Co., Ltd.;

[0081] The plasticizer used, diisononyl phthalate (brand name DINP), was produced by Shanghai Kunrui Chemical Co., Ltd.;

[0082] The aluminum hydroxide (brand name AP22) and melamine cyanurate (brand name MCA) flame retardant additives used are produced by Jiangsu Ruiyang Antai New Material Technology Co., Ltd.;

[0083] The methyltrimethoxysilane (brand name MTMS) and γ-aminopropyltriethoxysilane (brand name KH550) used were produced by Shandong Sike New Materials Co., Ltd.

[0084] The hybrid organotin (brand name M-S211) catalyst used was produced by Chengtian New Materials Co., Ltd.;

[0085] The detachable sealant of the present invention is a single-component silane-modified polyether adhesive, which is suitable for the upper and lower shell (aluminum, stainless steel) structures of the power battery pack of new energy vehicles. In addition, it can also be used for the bonding and sealing of pipelines such as oil pipes and water pipes in the engine compartment, which is convenient for later maintenance and replacement.

[0086] The preparation method adopted by the present invention can prepare a detachable sealant having the characteristics of air tightness, flame retardancy, insulation and detachability. In addition, the preparation method is simple, the production process has low energy consumption, and the solid and liquid raw materials can be mixed evenly with low energy consumption, and the prepared sealant can be placed for a long time without solidification.

[0087] The above description is only a preferred specific implementation manner of the present invention, but the protection scope of the present invention is not limited thereto. Any technician familiar with the technical field can make equivalent replacements or changes according to the technical scheme and inventive concept of the present invention within the technical scope disclosed by the present invention, which should be covered by the protection scope of the present invention.

Claims

1. A removable sealant, characterized in that: It is mainly prepared from the following components in the following mass ratios:

2. A removable sealant according to claim 1, characterized in that: The silane-modified polyether resin is alkyl-terminated 107 glue.

3. The removable sealant according to claim 1, characterized in that: The plasticizer is diisononyl phthalate and polypropylene glycol, or a combination of the two in any proportion.

4. The removable sealant according to claim 1, characterized in that: The flame retardant auxiliary agent is aluminum hydroxide and melamine cyanurate, or a combination of the two in any proportion.

5. The removable sealant according to claim 1, characterized in that: The coupling agent is methyltrimethoxysilane and gamma-aminopropyltriethoxysilane, or a combination of the two in any proportion.

6. The removable sealant according to claim 1, characterized in that: The catalyst is chelated hybrid organic tin.

7. A method for preparing a detachable sealant according to any one of claims 1 to 6, characterized in that: The steps include: (1) at room temperature, adding a silane-modified polyether resin, a plasticizer, and a flame retardant additive into a reaction vessel, placing the reaction vessel into a vacuum auto-rotation revolution mixer, sealing the reaction vessel, and starting the vacuum auto-rotation revolution mixer, stirring and mixing for 60-90 seconds at a vacuum degree of 5-10 KPa and a revolution speed of 1000-2000 rpm; (2) stopping the vacuum auto-rotation and revolution mixer, and after the sample cools to room temperature, starting the vacuum auto-rotation and revolution mixer, stirring and mixing for 60-90 seconds at a vacuum degree of 5-10 KPa and a revolution speed of 1000-2000 rpm; (3) stopping the vacuum auto-rotating revolution mixer, and after the sample is cooled to room temperature, adding the coupling agent into the above reaction container and sealing it, starting the vacuum auto-rotating revolution mixer, stirring and mixing for 30-60 seconds at a vacuum degree of 5-10 KPa and a revolution speed of 1000-2000 rpm; (4) Stop the vacuum auto-rotating revolution stirrer, wait for the sample to cool to room temperature, add the catalyst into the above reaction vessel and seal it, start the vacuum auto-rotating revolution stirrer, and stir and mix for 15-30 seconds at a vacuum degree of 5-10 KPa and a revolution speed of 1000-2000 rpm.

8. A method for preparing a detachable sealant according to claim 7, characterized in that: The flame retardant additive in step (1) needs to be dried in an oven at 100-110° C. for more than 24 hours to remove water before being added to the reaction vessel.

9. The method for preparing a detachable sealant according to claim 7, characterized in that: During the stirring and mixing process of steps (1) to (4), the temperature in the reaction container does not exceed 60°C.

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