CN109880578A - A kind of two-component soft thermal polyurethane casting glue and preparation method thereof - Google Patents
A kind of two-component soft thermal polyurethane casting glue and preparation method thereof Download PDFInfo
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- CN109880578A CN109880578A CN201910148774.1A CN201910148774A CN109880578A CN 109880578 A CN109880578 A CN 109880578A CN 201910148774 A CN201910148774 A CN 201910148774A CN 109880578 A CN109880578 A CN 109880578A
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Abstract
The present invention relates to a kind of two-component soft thermal polyurethane casting glue, including component A and B component, the component A includes the raw material of following parts by weight: 30~60 parts of isocyanates, 20~40 parts of plasticizer, 10~30 parts of fire retardant；The B component includes the raw material of following parts by weight: 20~40 parts of macromolecular polyol, 20~40 parts of polyolefin polyhydric alcohol, 30~70 parts of inorganic filler, 0.1~1 part of heat stabilizer, 0.1~1 part of antioxidant, 0.01~0.1 part of catalyst, 0.1~1 part of defoaming agent.Polyurethane pouring sealant of the invention has the characteristics that hardness is low, Good Heat-resistance；In addition, the preparation method of two-component soft thermal polyurethane casting glue of the present invention, simple process, are not necessarily to extra-high voltage ultrahigh-temperature equipment, it is highly-safe.
Description
Technical field
The present invention relates to dual-component polyurethane casting glue field, in particular to a kind of two-component soft thermal polyurethane fills
Sealing and preparation method thereof.
Background technique
Casting glue mainly has this three categories of epoxy pouring sealant, organic silicon potting adhesive, polyurethane pouring sealant.Epoxy pouring sealant is exhausted
Edge resistance is high, but it is more crisp, be also easy to produce the modified toughening of micro-crack after high/low temperature recycles after, the production cost increases, and performance is not up to
To best, often good toughness, intensity is with regard to low, and intensity is high, and toughness is with regard to poor.Organic silicon potting adhesive insulation resistance is high, but and is glued
Object adhesive strength is low.Polyurethane pouring sealant insulation resistance and adhesive strength are all higher, are comparatively ideal casting glues.Encapsulating polyurethane
Glue is mechanical strength with higher, excellent toughness, impact resistance, wearability, anti-as a kind of high performance high molecular material
Lancinating etc., be very suitable for connector assembly, circuit board etc. sealing, the production of the pouring pieces such as bowling, also can be used as adhesive and
Coating uses.Ambient temperature curable, also heating curable, solidification temperature and time are adjustable.
With the development of national economy, electronics industry achieves rapid progress, also increasingly to the demand of casting glue
Greatly, meanwhile, increasingly higher demands are proposed to the performance of casting glue.
Polyurethane pouring sealant is as a kind of high performance high molecular material, in physical mechanical property, weatherability, electrical property etc.
Aspect has unique advantage.But there is the defects of excessive high hardness, poor heat resistance in use, these defects are to casting glue
It properties of product and is caused greatly to damage by the performance of pot electronics component.The excessive high hardness of polyurethane pouring sealant, be easy to cause
Stress is concentrated, and electronic component is damaged；And common polyurethane pouring sealant is during military service, it is heated for a long time that heat drop easily occurs
Solution loses the encapsulating protective effect to electronic component.These defects limit the application field of polyurethane pouring sealant, also unfavorable
In the development of electronics industry.
Summary of the invention
It is an object of the invention to: in view of the above drawbacks of the prior art, provide a kind of two-component soft ammonia of resistance to hot polymerization
Ester casting glue and preparation method thereof has the characteristics that hardness is low, Good Heat-resistance.
To achieve the goals above, the invention provides the following technical scheme:
A kind of two-component soft thermal polyurethane casting glue, including component A and B component, the component A include following heavy
Measure the raw material of part: 30~60 parts of isocyanates, 20~40 parts of plasticizer, 10~30 parts of fire retardant；The B component includes following heavy
Measure the raw material of part: 20~40 parts of macromolecular polyol, 20~40 parts of polyolefin polyhydric alcohol, 30~70 parts of inorganic filler, thermostabilization
0.1~1 part of agent, 0.1~1 part of antioxidant, 0.01~0.1 part of catalyst, 0.1~1 part of defoaming agent.
Preferably, the isocyanates is toluene di-isocyanate(TDI), methyl diphenylene diisocyanate, liquefaction hexichol first
Any one or a few in methane diisocyanate, poly methylene poly phenyl poly isocyanate；The plasticizer is containing benzene
Di-2-ethylhexyl terephthalate, diisooctyl phthalate, the different monooctyl ester of trimellitic acid three, trimellitic acid three of ring structure
Isodecyl ester, dipropylene glycol dibenzoate, any one or a few in diethylene glycol dibenzoate；The fire retardant is to increase
Plastotype fire retardant.
Preferably, the fire retardant is trimethyl phosphate, triethyl phosphate, tributyl phosphate, trioctyl phosphate, phosphoric acid
Any one or a few in triphenylmethyl methacrylate.
Preferably, the macromolecular polyol is polypropylene oxide alcohol, the castor oil, soybean of molecular weight 500~5000
Any one or a few in oil polyalcohol, palm oil polyalcohol；The polyolefin polyhydric alcohol is the end hydroxyl of molecular weight 2600
Base polybutadiene；The inorganic filler is powdered whiting, precipitated calcium carbonate, activated wollastonite powder, common aluminium hydroxide, general
Any one or a few in logical magnesium hydroxide, common talcum powder；The heat stabilizer is metal soap, organic tin, organic
One or more of antimony class；The antioxidant be Hinered phenols, amine, phosphorous acid esters, in thioether class any one or
It is several；The catalyst is dibutyl tin dilaurate, stannous octoate, dibutyltin diacetate, triethylene diamine, bis- (diformazans
Amino-ethyl) any one or a few in ether；The defoaming agent be organic silicon defoamer, Polyether Modified Polysiloxanes Defoaming Agent,
Any one or a few in antifoaming agent of non-silicone.
Preferably, the heat stabilizer is magnesium stearate, calcium stearate, barium stearate, aluminum stearate, calcium benzoate, horse
Come sour dibutyl tin, Dibutyltin oxide, any one or a few in three mercaptans types；The antioxidant is 2,4,6- tri- tertiary fourths
Base phenol, styrenated phenol, 1,2,3- benzotriazole, triphenyl phosphite, tributyl phosphite, thiodipropionic acid dilauryl
Any one or a few in osmanthus ester, thio-2 acid polyester.
A kind of preparation method of two-component soft thermal polyurethane casting glue, comprises the following steps:
(1) plasticizer, fire retardant: being uniformly mixed by the preparation of component A first, and vacuum is de- under the conditions of 120~130 DEG C
Water；Next is cooled to 50~60 DEG C, and isocyanates is added, and 0.5~1h is mixed under the conditions of 70~80 DEG C, leads to nitrogen in reaction process
Gas shielded；Then sampling and measuring NCO%, NCO%, which reach 10~20%, can stop heating；Finally, being down to room temperature up to A group
Point；
(2) preparation of B component: macromolecular polyol, polyolefin polyhydric alcohol, inorganic filler are uniformly mixed 120 first
2~3h of vacuum dehydration under the conditions of~130 DEG C；Next is cooled to 70~90 DEG C of addition heat stabilizers, antioxidant, catalyst, defoaming
Agent is stirred 0.5~1h；It is down to room temperature finally up to B component；
(3) the resulting component A of (1) step and the resulting B component of (2) step are mixed by weight 10~50:100 equal
It is even to get two-component soft thermal polyurethane casting glue.
The beneficial effects of the present invention are:
(1) plasticizer in component A of the invention and fire retardant are not involved in the curing reaction of dual-component polyurethane casting glue,
It is free to be present in inside polyurethane, the internal stress of casting glue can be weakened, reduce hardness.
(2) contain big component polyalcohol in B component of the invention, strand is submissive, can weaken internal stress, the drop of casting glue
Soft.
(3) contain polyolefin polyhydric alcohol in B component of the invention, polyolefin polyhydric alcohol polarity is low, degree of functionality is low, can weaken
The internal stress of casting glue reduces hardness.
(4) plasticizer in component A of the invention is the plasticizer containing benzene ring structure, and benzene ring structure thermal stability is excellent
It is different, the resistance to thermal degradation performance of casting glue can be improved.
(5) the polyolefin polyhydric alcohol host molecule chain in B component of the invention is polybutadiene alkyl chain, and heat resistance is excellent
It is different, the resistance to thermal degradation performance of casting glue can be improved.
(6) B component of the invention contains heat stabilizer and antioxidant, the correct selection of heat stabilizer and antioxidant and rationally
Resistance to thermal degradation performance of the casting glue under aerobic, few complex environments such as oxygen or anaerobic can be improved in collocation.
(7) preparation method of two-component soft thermal polyurethane casting glue of the present invention, simple process, without spy
High pressure ultrahigh-temperature equipment, it is highly-safe.
Specific embodiment
Embodiment 1
A kind of preparation method of two-component soft thermal polyurethane casting glue, comprises the following steps:
(1) component A: 30.0g Di-2-ethylhexyl terephthalate, 20.0g triethyl phosphate are uniformly mixed first, 120
Vacuum dehydration under the conditions of DEG C；Next is cooled to 60 DEG C, and 50.0g toluene di-isocyanate(TDI) is added, mixes 0.5h under the conditions of 80 DEG C,
Lead to nitrogen protection in reaction process；Then sampling and measuring NCO%, NCO% reach 24.0% and stop heating；Finally, being down to room
Temperature is up to component A.
(2) preparation of B component: first by 25.0g soybean oil polyol (Mn1000), 20.0g end hydroxy butadiene
(Mn2600), 55.0g general industry grade magnesium hydroxide is uniformly mixed vacuum dehydration 2h under the conditions of 120 DEG C；Next is down to 90 DEG C
0.3g magnesium stearate, 0.3g dilauryl thiodipropionate, 0.02g stannous octoate, 0.5g organic silicon defoamer is added, stirring mixes
Close 0.5h；It is down to room temperature finally up to B component.
(3) the resulting component A of (1) step and the resulting B component of (2) step are uniformly mixed by weight 20:100, i.e.,
Obtain two-component soft thermal polyurethane casting glue.
Embodiment 2
A kind of preparation method of two-component soft thermal polyurethane casting glue, comprises the following steps:
(1) component A: the different monooctyl ester of 35.0g trimellitic acid three, 15.0 tributyl phosphates are uniformly mixed first, at 120 DEG C
Under the conditions of vacuum dehydration；Next is cooled to 60 DEG C, 50.0g poly methylene poly phenyl poly isocyanate is added, under the conditions of 80 DEG C
0.5h is mixed, leads to nitrogen protection in reaction process；Then sampling and measuring NCO%, NCO% reach 15.0% and stop heating；Most
Afterwards, room temperature is down to up to component A.
(2) preparation of B component: first by 26.0g castor oil, 24.0g end hydroxy butadiene, 50.0g powdered whiting
It is uniformly mixed vacuum dehydration 2h under the conditions of 120 DEG C；Next is down to 90 DEG C of addition 0.3g calcium benzoates, 0.3g phosphorous triphenyl phosphates
Ester, 0.02g dibutyl tin dilaurate, 0.5g organic silicon defoamer, is stirred 0.5h；It is down to room temperature finally up to B component.
(3) the resulting component A of (1) step and the resulting B component of (2) step are uniformly mixed by weight 20:100, i.e.,
Obtain two-component soft thermal polyurethane casting glue.
Embodiment 3
A kind of preparation method of two-component soft thermal polyurethane casting glue, comprises the following steps:
(1) component A: three isodecyl ester of 35.0g trimellitic acid, 20.0g triethyl phosphate are uniformly mixed first, 120
Vacuum dehydration under the conditions of DEG C；Next is cooled to 60 DEG C, 45.0g liquefaction methyl diphenylene diisocyanate is added, in 80 DEG C of conditions
Lower mixing 0.5h leads to nitrogen protection in reaction process；Then sampling and measuring NCO%, NCO% reach 14.0% and stop heating；
Finally, being down to room temperature up to component A.
(2) preparation of B component: first by 30.0g castor oil, 25.0g end hydroxy butadiene, 45.0g general industry grade
Magnesium hydroxide is uniformly mixed vacuum dehydration 2h under the conditions of 120 DEG C；Next is down to 90 DEG C of addition 0.3g barium stearates, 0.3g 2,
4,6- tri-butyl-phenols, 0.05g triethylenediamine, 0.3g organic silicon defoamer, are stirred 0.5h；Finally it is down to room temperature
Up to B component.
(3) the resulting component A of (1) step and the resulting B component of (2) step are uniformly mixed by weight 20:100, i.e.,
Obtain two-component soft thermal polyurethane casting glue.
Comparative example 1
The common competing product 6624 of a encapsulating polyurethane sealing in the market are labeled as comparative example 1.
The performance test of the polyurethane pouring sealant of the casting glue and comparative example 1 of Examples 1 to 3 preparation is more as shown in table 1.
The performance of 1 casting glue of table compares
By performance parameter in table 1, the hardness of the casting glue of embodiment 1,2,3 be lower than with comparative example 1, casting glue can be met
Soft requirement.By test, the military service duration (h, 100 DEG C and h, 120 DEG C) under the conditions of fixed temperature is compared its heat resistance,
Military service duration of the embodiment 1,2,3 under the conditions of 100 DEG C and 120 DEG C is all better than comparative example 1, illustrates the heat-resisting of embodiment 1,2,3
Performance is better than comparative example.
In conclusion the performances such as the soft of the polyurethane pouring sealant of the embodiment of the present invention, heat resistance are better than Vehicles Collected from Market
Existing product.
Claims (6)
1. a kind of two-component soft thermal polyurethane casting glue, it is characterised in that: including component A and B component, the component A
Raw material comprising following parts by weight: 30~60 parts of isocyanates, 20~40 parts of plasticizer, 10~30 parts of fire retardant；The B component
Raw material comprising following parts by weight: 20~40 parts of macromolecular polyol, 20~40 parts of polyolefin polyhydric alcohol, inorganic filler 30~70
Part, 0.1~1 part of heat stabilizer, 0.1~1 part of antioxidant, 0.01~0.1 part of catalyst, 0.1~1 part of defoaming agent.
2. a kind of two-component soft thermal polyurethane casting glue according to claim 1, it is characterised in that: described is different
Cyanate is toluene di-isocyanate(TDI), methyl diphenylene diisocyanate, liquefaction hexichol methyl hydride diisocyanate, polymethylene
Any one or a few in polyphenyl polyisocyanate；The plasticizer is that the terephthalic acid (TPA) two containing benzene ring structure is different pungent
Ester, diisooctyl phthalate, the different monooctyl ester of trimellitic acid three, three isodecyl ester of trimellitic acid, dipropylene glycol dibenzoic acid
Any one or a few in ester, diethylene glycol dibenzoate；The fire retardant is plasticising type fire retardant.
3. a kind of two-component soft thermal polyurethane casting glue according to claim 1, it is characterised in that: the resistance
Combustion agent be trimethyl phosphate, triethyl phosphate, tributyl phosphate, trioctyl phosphate, in triphenyl phosphate any one or it is several
Kind.
4. a kind of two-component soft thermal polyurethane casting glue according to claim 1, it is characterised in that: described is big
Molecular polylol is in the polypropylene oxide alcohol of molecular weight 500~5000, castor oil, soybean oil polyol, palm oil polyalcohol
Any one or a few；The polyolefin polyhydric alcohol is the end hydroxy butadiene of molecular weight 2600；It is described inorganic to fill out
Material is powdered whiting, in precipitated calcium carbonate, activated wollastonite powder, common aluminium hydroxide, common magnesium hydroxide, common talcum powder
Any one or a few；The heat stabilizer is one or more of metal soap, organic tin, antimony organic class；It is described
Antioxidant is Hinered phenols, amine, phosphorous acid esters, any one or a few in thioether class；The catalyst is two laurels
Sour dibutyl tin, stannous octoate, dibutyltin diacetate, triethylene diamine, any one in bis- (dimethylaminoethyl) ethers
Or it is several；The defoaming agent is organic silicon defoamer, Polyether Modified Polysiloxanes Defoaming Agent, any one in antifoaming agent of non-silicone
Kind is several.
5. a kind of two-component soft thermal polyurethane casting glue according to claim 1, it is characterised in that: the heat is steady
Determining agent is magnesium stearate, calcium stearate, barium stearate, aluminum stearate, calcium benzoate, dibutyitin maleate, dibutyl oxidation
Any one or a few in tin, three mercaptans types；The antioxidant be 2,4,6- tri-butyl-phenols, styrenated phenol, 1,
2,3- benzotriazole, triphenyl phosphite, tributyl phosphite, dilauryl thiodipropionate, in thio-2 acid polyester
Any one or a few.
6. a kind of preparation method of the two-component soft thermal polyurethane casting glue as described in claim 1-5 any one,
It is characterized by: comprising the following steps:
(1) plasticizer, fire retardant: being uniformly mixed by the preparation of component A first, vacuum dehydration under the conditions of 120~130 DEG C；Its
It is secondary to be cooled to 50~60 DEG C, isocyanates is added, 0.5~1h is mixed under the conditions of 70~80 DEG C, leads to nitrogen in reaction process and protects
Shield；Then sampling and measuring NCO%, NCO%, which reach 10~20%, can stop heating；Finally, being down to room temperature up to component A；
(2) preparation of B component: macromolecular polyol, polyolefin polyhydric alcohol, inorganic filler are uniformly mixed 120~130 first
2~3h of vacuum dehydration under the conditions of DEG C；Next is cooled to 70~90 DEG C of addition heat stabilizers, antioxidant, catalyst, defoaming agent, stirs
Mix 0.5~1h of mixing；It is down to room temperature finally up to B component；
(3) the resulting component A of (1) step and the resulting B component of (2) step are uniformly mixed by weight 10~50:100, i.e.,
Obtain two-component soft thermal polyurethane casting glue.
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Cited By (5)
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| CN110964311A (en) * | 2018-09-30 | 2020-04-07 | 天津市橡胶工业研究所有限公司 | Low-density polyurethane encapsulating material and preparation method thereof |
| CN110982472A (en) * | 2019-11-19 | 2020-04-10 | 天津利锋新能源科技有限公司 | Flame-retardant adhesive for lithium battery pack and preparation method thereof |
| CN113136162A (en) * | 2021-04-23 | 2021-07-20 | 杭州之江新材料有限公司 | High-temperature-resistant high-humidity-resistant double-component polyurethane flame-retardant pouring sealant and preparation method thereof |
| CN114316878A (en) * | 2021-12-07 | 2022-04-12 | 黎明化工研究设计院有限责任公司 | Polyurethane pouring sealant and preparation method and application thereof |
| CN115595108A (en) * | 2022-10-31 | 2023-01-13 | 上海富铭密封材料有限公司（Cn） | Polyurethane pouring sealant and preparation method thereof |
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| CN110964311A (en) * | 2018-09-30 | 2020-04-07 | 天津市橡胶工业研究所有限公司 | Low-density polyurethane encapsulating material and preparation method thereof |
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Application publication date: 20190614 |