CN114163967A - Double-component pouring sealant and preparation method and application thereof - Google Patents

Double-component pouring sealant and preparation method and application thereof Download PDF

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CN114163967A
CN114163967A CN202210051172.6A CN202210051172A CN114163967A CN 114163967 A CN114163967 A CN 114163967A CN 202210051172 A CN202210051172 A CN 202210051172A CN 114163967 A CN114163967 A CN 114163967A
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component
preparation
diisocyanate
pouring sealant
potting adhesive
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CN114163967B (en
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区炜
刘保华
艾娇艳
宋丽娜
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Guangdong University of Technology
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J175/00Adhesives based on polyureas or polyurethanes; Adhesives based on derivatives of such polymers
    • C09J175/04Polyurethanes
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02Non-macromolecular additives
    • C09J11/06Non-macromolecular additives organic
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E10/00Energy generation through renewable energy sources
    • Y02E10/50Photovoltaic [PV] energy

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  • Organic Chemistry (AREA)
  • Sealing Material Composition (AREA)
  • Polyurethanes Or Polyureas (AREA)

Abstract

The application belongs to the technical field of pouring sealant, and particularly relates to a two-component pouring sealant as well as a preparation method and application thereof. The application provides a two ingredient casting glue soak in weakly alkaline solution such as ethanolamine, the hydrone in the solution can adsorb on the casting glue molecular chain, take place hydrolysis reaction with the ester on the casting glue molecular chain, generate the short molecular chain, the short molecular chain continues to hydrolyze into the small molecular chain, thereby make two ingredient casting glue lose intensity, can remove, and, the casting glue that removes can pass through compost degradation, can not cause environmental pollution, thereby solve among the prior art electronic components unable maintenance behind the embedment electronic glue, retrieve, cause environmental pollution's technical problem easily.

Description

Double-component pouring sealant and preparation method and application thereof
Technical Field
The application belongs to the technical field of pouring sealant, and particularly relates to a two-component pouring sealant as well as a preparation method and application thereof.
Background
The pouring sealant is used for bonding and sealing electronic components, and achieves the effects of dust prevention, moisture prevention, shock resistance, corrosion resistance and the like, and the commonly used pouring sealant at present comprises epoxy pouring sealant, organic silicon pouring sealant and polyurethane pouring sealant; and the polyurethane contains a unique soft-segment phase separation structure, so that after the polyurethane pouring sealant is poured and sealed, the colloid part has good elasticity, wear resistance and impact resistance, the work of components in severe environment can be ensured, the stability of the components is improved, and the service life of the components is prolonged.
However, when the electronic components after the polyurethane potting adhesive have a local problem, the currently used potting adhesive cannot be degraded, the electronic components lose the maintenance value, and only the electronic components can be discarded, which causes huge waste.
Disclosure of Invention
In view of the above, the application provides a two-component pouring sealant and a preparation method and application thereof, the two-component pouring sealant is stable in the using process after electronic components are poured and sealed, the contained PPC can be degraded into small molecular compounds in a weak alkaline environment, and can be degraded through compost, so that the technical problems that in the prior art, the electronic components cannot be maintained and recovered after the electronic components are poured and sealed with the electronic sealant, and the environmental pollution is easily caused are solved.
The application provides a two-component pouring sealant in a first aspect, which comprises a component A and a component B;
the component A comprises polypropylene carbonate polyol, diisocyanate, an organic metal catalyst and an anti-aging agent;
the component B comprises a chain extension crosslinking agent, a catalyst, a defoaming agent and an ultraviolet absorber.
Preferably, the poly (propylene carbonate) polyol comprises 2 or more than 2 PPCs with the molecular weight of 500-3000 g/mol.
It is noted that PPC is referred to herein as polypropylene carbonate polyol.
Preferably, the component A comprises the following components in parts by mass:
100 parts of polypropylene carbonate polyol;
20-60 parts of diisocyanate;
0.01-0.1 part of organic metal catalyst;
0.1-5 parts of an anti-aging agent;
the component B comprises:
1-15 parts of a chain extension crosslinking agent;
0.01-0.1 part of a crosslinking agent;
0.1-1 part of defoaming agent;
0.1-1 part of ultraviolet absorbent.
Preferably, the diisocyanate includes one or more of toluene diisocyanate, diphenylmethane diisocyanate, liquefied diphenylmethane diisocyanate, polymeric isocyanate, isophorone diisocyanate, hexamethylene diisocyanate, and hydrogenated diphenylmethane diisocyanate.
Preferably, the organometallic catalyst comprises one or more of stannous octoate, stannous isooctanoate, dibutyltin dilaurate and organic bismuth.
Preferably, the aging inhibitor includes 2, 6-di-tert-butyl-4-methylphenol and/or pentaerythritol tetrakis [ β - (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ].
Preferably, the chain-extending crosslinking agent comprises one or more of ethylene glycol, butylene glycol, diethylene glycol, dipropylene glycol, 1, 6-hexanediol, 1, 3-propanediol, 1, 2-propanediol, trimethylolpropane, 1, 4-hydroxymethylcyclohexane, trimethylpentanediol, di-n-butylamine, ethylenediamine, trimethylhexamethylenediamine, tetraethylenepentamine, diethylenetriamine and isophorone diamine.
Preferably, the crosslinking agent comprises trimethylolpropane.
Preferably, the ultraviolet absorber comprises 2-hydroxy-4-n-octoxybenzophenone and/or 2-hydroxy-4-methoxybenzophenone.
Preferably, the defoaming agent comprises a silicone-based defoaming agent.
The second aspect of the application provides a preparation method of the two-component pouring sealant, wherein the preparation method of the component A comprises the following steps: in a nitrogen atmosphere, reacting the dehydrated polypropylene carbonate polyol with organic metal catalyst, diisocyanate and an anti-aging agent at 75-85 ℃ to obtain a component A;
the preparation method of the component B comprises the following steps: and reacting the chain extension crosslinking agent, the defoaming agent and the ultraviolet absorbent at 75-85 ℃ to obtain the component B.
The third aspect of the application provides an application of the pouring sealant in the field of electronic components.
The pouring sealant provided by the application has the characteristics of easy removal and easy degradation, so that the electronic components can be maintained and recovered, and the pouring sealant can be widely applied to the field of various electronic components.
In summary, the application provides a two-component pouring sealant and a preparation method and application thereof; the two-component pouring sealant comprises a component A and a component B, wherein the component A comprises polypropylene carbonate polyol, diisocyanate, an organic metal catalyst and an anti-aging agent, and the component B comprises a chain extension cross-linking agent, a catalyst, a defoaming agent and an ultraviolet absorber; when the two-component pouring sealant is used, the component A and the component B are mixed and stirred according to a certain proportion, then the mixture is quickly poured into an electronic component, and finally the mixture is solidified to realize the potting of the electronic component Recycling and easily causing environmental pollution.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without inventive exercise.
Fig. 1 is a degradation schematic diagram of a two-component pouring sealant provided in the embodiment of the present application.
Detailed Description
The application provides a two-component pouring sealant and a preparation method and application thereof, the two-component pouring sealant is stable in the using process after electronic components are poured and sealed, contained PPC can be degraded into small molecular compounds in a weak alkaline environment, the pouring sealant can be degraded through compost after being abandoned, and the technical problem that in the prior art, the electronic components cannot be maintained and recovered after the electronic components are poured and sealed, and environmental pollution is easily caused is solved.
The technical solutions in the embodiments of the present application will be described clearly and completely below, and it should be understood that the described embodiments are only a part of the embodiments of the present application, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present application.
The reagents or raw materials used in the following examples are commercially available or self-made.
Example 1
The application embodiment 1 provides a first preparation method of a two-component pouring sealant, which comprises the preparation of a component A and the preparation of a component B.
(1) Preparation of component A
According to the mass parts, 60 parts of polypropylene carbonate with the molecular weight of 1000g/mol and 40 parts of polypropylene carbonate with the molecular weight of 2000g/mol are dehydrated for 2-3 hours in vacuum at 110-120 ℃, then the temperature is reduced to 60-70 ℃, 0.08 part of organic metal catalyst stannous octoate is added, 25 parts of isophorone diisocyanate is added, the temperature is gradually increased to 75-85 ℃ within 30min for reaction, nitrogen protection is conducted in the reaction process, the NCO% value is tested, the reaction is stopped when the NCO% value reaches a set value, and anti-aging agent 2, 6-di-tert-butyl-4-methylphenol is added to obtain component A, wherein the set value is in the range of 5% -15%.
(2) Preparation of component B
Adding 3 parts of chain extender butanediol and 0.1 part of cross-linking agent trimethylolpropane into a reaction kettle, stirring and mixing, preheating to 50-80 ℃, adding 0.1 part of organic silicon defoamer and 0.2 part of ultraviolet absorber catalyst 2-hydroxy-4-n-octoxy benzophenone, stirring uniformly, and defoaming to obtain the component B.
Example 2
The second preparation method of the two-component pouring sealant is provided in the application example 2, and comprises the preparation of the component A and the preparation of the component B.
The difference from the embodiment 1 is that the preparation raw material ratio of the component A and the component B is as follows:
Figure BDA0003474350290000041
Figure BDA0003474350290000051
example 3
The application embodiment 3 provides a third preparation method of the two-component pouring sealant, which comprises the preparation of the component A and the preparation of the component B.
The difference from the example 1 is that the preparation raw materials of the component A and the component B are as follows:
raw materials Component A
Polypropylene carbonate polyol (Mn ═ 2000) 60
Polypropylene carbonate polyol (Mn 3000) 40
Toluene diisocyanate (MDI) 20
Catalyst (stannous octoate) 0.08
Anti-aging agent (2, 6-di-tert-butyl-4-methylphenol) 0.1
Raw materials Component B
Chain extender (butanediol) 3
Crosslinking agent (trimethylolpropane) 0.5
Defoaming agent BYK-A530 0.1
Ultraviolet ray absorbent (2-hydroxy-4-n-octoxy benzophenone) 0.2
The mass mixing ratio of the component A and the component B 100:15
Example 4
The application embodiment 4 provides a fourth preparation method of the two-component pouring sealant, which comprises the preparation of the component A and the preparation of the component B.
The difference from the example 1 is that the preparation raw materials of the component A and the component B are as follows:
raw materials Component A
Polypropylene carbonate polyol (Mn ═ 2000) 60
Polypropylene carbonate polyol (Mn 3000) 40
Toluene diisocyanate (MDI) 20
Catalyst (stannous octoate) 0.08
Anti-aging agent (2, 6-di-tert-butyl-4-methylphenol) 0.15
Raw materials Component B
Chain extender (dipropylene glycol) 3
Crosslinking agent (trihydroxy)Methyl propane) 0.5
Defoaming agent BYK-392 0.1
Ultraviolet ray absorbent (2-hydroxy-4-methoxybenzophenone) 0.2
The mass mixing ratio of the component A and the component B 100:10
Comparative example 1
The application and the comparative example 1 provide a fifth preparation method of the two-component pouring sealant, which comprises the preparation of the component A and the preparation of the component B.
The difference from the example 1 is that the preparation raw materials of the component A and the component B are as follows:
Figure BDA0003474350290000061
Figure BDA0003474350290000071
comparative example 2
The application and the comparative example 2 provide a sixth preparation method of the two-component pouring sealant, which comprises the preparation of the component A and the preparation of the component B.
The difference from the example 1 is that the preparation raw materials of the component A and the component B are as follows:
raw materials Component A
Polytetrahydrofuran (Mn 3000) 40
Isophorone diisocyanate (IPDI) 25
Catalyst (stannous octoate) 0.08
Anti-aging agent (2, 6-di-tert-butyl-4-methylphenol) 0.15
Raw materials Component B
Chain extender (dipropylene glycol) 3
Crosslinking agent (trimethylolpropane) 0.5
Defoaming agent BYK-088 0.1
Ultraviolet ray absorbent (2-hydroxy-4-methoxybenzophenone) 0.2
The mass mixing ratio of the component A and the component B 100:12
Example 5
In this example 5, the performance of the potting compound prepared in examples 1-2 and comparative examples 1-2 was tested, and the testing procedure included: the pouring sealant prepared in the examples 1-2 and the comparative examples 1-2 is mixed and stirred for 3min according to the mass ratio, then the mixture is quickly poured into a mold preheated at 60 ℃, the mixture is cured at 60 ℃ for 24h and at 100 ℃ for 24h to obtain a sample strip, and then the hardness, the strength and the degradation removal performance of the sample strip are tested in sequence, and the results are shown in the table 1:
Figure BDA0003474350290000081
TABLE 1
In table 1, the degradation agent is diethanolamine and triethanolamine, and the solvent is tetrahydrofuran, ethyl acetate, butyl acetate, and the like.
As can be seen from table 1, compared with the pouring sealant prepared in comparative example 1, the pouring sealant provided in the embodiment of the present application can be degraded in a mixed solvent of diethanolamine and tetrahydrofuran, because the pouring sealant is soaked in a weakly alkaline solution such as ethanolamine, water molecules in the solution can be adsorbed onto the molecular chain of the pouring sealant, and undergo a hydrolysis reaction with ester groups on the molecular chain of the pouring sealant to generate a short molecular chain, and the short molecular chain is continuously hydrolyzed into small molecular chains, so that the two-component pouring sealant loses strength and can be removed; the degradation principle is shown in the attached figure 1.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.

Claims (10)

1. The two-component pouring sealant is characterized by comprising a component A and a component B;
the component A comprises polypropylene carbonate polyol, diisocyanate, an organic metal catalyst and an anti-aging agent;
the component B comprises a chain extension crosslinking agent, a catalyst, a defoaming agent and an ultraviolet absorber.
2. The two-component potting adhesive of claim 1, wherein the polypropylene carbonate polyol comprises 2 or more than 2 PPCs with molecular weights of 500-3000 g/mol.
3. The two-component potting adhesive of claim 1, wherein the component a comprises, in parts by mass:
100 parts of polypropylene carbonate polyol;
20-60 parts of diisocyanate;
0.01-0.1 part of organic metal catalyst;
0.1-5 parts of an anti-aging agent;
the component B comprises:
1-15 parts of a chain extension crosslinking agent;
0.01-0.1 part of a crosslinking agent;
0.1-1 part of defoaming agent;
0.1-1 part of ultraviolet absorbent.
4. The two-component potting adhesive of claim 1, wherein the diisocyanate comprises one or more of toluene diisocyanate, diphenylmethane diisocyanate, liquefied diphenylmethane diisocyanate, polymeric isocyanate, isophorone diisocyanate, hexamethylene diisocyanate, and hydrogenated diphenylmethane diisocyanate.
5. The two-component potting adhesive of claim 1, wherein the organometallic catalyst comprises one or more of stannous octoate, stannous iso-octoate, dibutyltin dilaurate, and organobismuth.
6. The two-component potting adhesive of claim 1, wherein the aging inhibitors comprise 2, 6-di-tert-butyl-4-methylphenol and/or pentaerythrityl tetrakis [ β - (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ].
7. The two-component potting adhesive of claim 1, wherein the chain extending crosslinker comprises one or more of ethylene glycol, butylene glycol, diethylene glycol, dipropylene glycol, 1, 6-hexanediol, 1, 3-propanediol, 1, 2-propanediol, trimethylolpropane, 1, 4-hydroxymethylcyclohexane, trimethylpentanediol, di-n-butylamine, ethylenediamine, trimethylhexamethylenediamine, tetraethylenepentamine, diethylenetriamine, and isophorone diamine.
8. The two-component potting adhesive of claim 1, wherein the uv absorber comprises 2-hydroxy-4-n-octoxybenzophenone and/or 2-hydroxy-4-methoxybenzophenone.
9. The preparation method of the two-component pouring sealant according to any one of claims 1 to 8, characterized in that the preparation method of the component A comprises the following steps: in a nitrogen atmosphere, reacting the dehydrated polypropylene carbonate polyol with organic metal catalyst, diisocyanate and an anti-aging agent at 75-85 ℃ to obtain a component A;
the preparation method of the component B comprises the following steps: and reacting the chain extension crosslinking agent, the defoaming agent and the ultraviolet absorbent at 75-85 ℃ to obtain the component B.
10. The two-component potting adhesive according to any of claims 1 to 8 or the two-component potting adhesive prepared by the preparation method according to claim 9 is applied to the field of electronic components.
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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101597376A (en) * 2009-07-10 2009-12-09 中山大学 A kind of polyurethane propylene carbonate material and preparation method thereof
CN106928895A (en) * 2017-03-09 2017-07-07 宜兴市普利泰电子材料有限公司 Flexible LED lamp bar polyurethane electronic casting glue and preparation method thereof
CN107033829A (en) * 2017-04-28 2017-08-11 东华大学 A kind of polytrimethylene carbonate moisture-curable polyurethane hot melt adhesive and preparation method thereof
CN112175566A (en) * 2020-09-28 2021-01-05 杭州应星新材料有限公司 Room-temperature curing bi-component polyurethane heat-conducting composition and preparation method thereof
CN112724909A (en) * 2020-12-30 2021-04-30 广州集泰化工股份有限公司 High-shear-strength two-component polyurethane corner adhesive and preparation method thereof

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101597376A (en) * 2009-07-10 2009-12-09 中山大学 A kind of polyurethane propylene carbonate material and preparation method thereof
CN106928895A (en) * 2017-03-09 2017-07-07 宜兴市普利泰电子材料有限公司 Flexible LED lamp bar polyurethane electronic casting glue and preparation method thereof
CN107033829A (en) * 2017-04-28 2017-08-11 东华大学 A kind of polytrimethylene carbonate moisture-curable polyurethane hot melt adhesive and preparation method thereof
CN112175566A (en) * 2020-09-28 2021-01-05 杭州应星新材料有限公司 Room-temperature curing bi-component polyurethane heat-conducting composition and preparation method thereof
CN112724909A (en) * 2020-12-30 2021-04-30 广州集泰化工股份有限公司 High-shear-strength two-component polyurethane corner adhesive and preparation method thereof

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