CN111286299A - Bi-component condensed type encapsulating material convenient for construction and preparation method thereof - Google Patents
Bi-component condensed type encapsulating material convenient for construction and preparation method thereof Download PDFInfo
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- CN111286299A CN111286299A CN201811544654.5A CN201811544654A CN111286299A CN 111286299 A CN111286299 A CN 111286299A CN 201811544654 A CN201811544654 A CN 201811544654A CN 111286299 A CN111286299 A CN 111286299A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J183/00—Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Adhesives based on derivatives of such polymers
- C09J183/04—Polysiloxanes
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/06—Non-macromolecular additives organic
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08L2203/00—Applications
- C08L2203/20—Applications use in electrical or conductive gadgets
- C08L2203/206—Applications use in electrical or conductive gadgets use in coating or encapsulating of electronic parts
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Abstract
The invention provides a two-component condensation type encapsulating material convenient for construction, which comprises a component A and a component B, wherein the mixing ratio of the component A to the component B is 4-6: 1, the main raw materials of the component A comprise, by mass, α parts of omega-dihydroxy polydimethylsiloxane, 100 parts of plasticizer, 0-50 parts of flame retardant, 50-150 parts of heat-conducting filler, 10-150 parts of other filler and 10-100 parts of flame retardant, the main raw materials of the component B comprise, by mass, 0.1-5 parts of catalyst, 100 parts of polyether and 20-100 parts of cross-linking agent composition, and the component B does not contain linear dimethyl silicone oil or branched dimethyl silicone oil.
Description
Technical Field
The invention belongs to the technical field of organic silicon materials, and particularly relates to a two-component condensed type encapsulating material convenient for construction and a preparation method thereof.
Background
With the rapid development of science and technology, electronic components tend to be miniaturized and integrated, and the heating power during the operation of the electronic components is also remarkably increased, so that higher requirements on the performance of the pouring sealant are provided. The currently used pouring sealant includes epoxy resin and organosilicon material, but epoxy resin has poor high temperature resistance and moisture resistance, which results in shortened service life of the element, or moisture enters into the element to easily cause short circuit. The organosilicon material has good performances of shock resistance, moisture resistance, high and low temperature resistance, electrical insulation and the like, and is widely applied to coating or encapsulating of electronic products. The existing organosilicon material pouring sealant is generally divided into addition type and condensation type, wherein the addition type product is easy to be oxidized, so that the stability of long-term use is difficult to be ensured. In addition, the adhesion of the addition type pouring sealant to the electronic components is poor, so that the waterproof performance of the product is influenced. The two-component condensed pouring sealant has the advantages of fast curing, good adhesion, difficult poisoning of catalyst and the like. However, the two-component condensed pouring sealant on the market at present has the technical problems of poor storage stability, complex construction, low qualified rate of sealant application and the like.
Patent 200910248012.5, patent 201310288227.6, patent 201510420454.9 and patent 201510511625.9 respectively disclose a two-component condensed type organic silicon pouring sealant. The above patents relate to the use of the two-component condensation type pouring sealant for the pouring protection of electronic products or solar energy industry, which can meet the basic requirements of the market on the two-component condensation type pouring sealant, but in the face of the increasingly complex trend of the current electronic products, there are still many technical problems to be solved, such as: 1) the viscosity difference of two components of the condensed type bi-component pouring sealant in the market is generally large, and the bi-component gluing machine needs to be subjected to complicated debugging in use, so that the difficulty of a user in construction is increased, the matching stability between the pouring sealant and gluing equipment is reduced, the fluctuation range of the mixing proportion of the user in the gluing process is increased, and the quality after curing is unstable; 2) the storage stability of the B component is not high, and the curing speed of the B component can be reduced to half of the initial value within less than two months; 3) the common pouring sealant pursues higher fluidity, but gaps exist in the design of a plurality of electronic components or shells of equipment on the market, and the use of the common pouring sealant with higher fluidity leads to easy glue leakage and low gluing qualified rate.
Disclosure of Invention
In view of the technical defects in the prior art, the present invention aims to: the two-component condensed type encapsulating material convenient for construction is provided, wherein the component A and the component B are mixed according to the mass ratio of 4: 1-6: 1; the viscosity difference between the component A and the component B is not more than 5 times, which is beneficial to uniform mixing by hand or in equipment and ensures the stable quality of the glue after curing.
It is a further object of the present invention how to improve the storage stability of component B.
Still another object of the present invention is to provide a component A and a component B having a significant thickening effect at the initial stage of mixing, which is not liable to cause a bleed-out when applied to a component having a gap in the case.
The invention also provides a preparation method of the double-component condensed type encapsulating material convenient for construction.
The purpose of the invention is realized by the following technical scheme:
the two-component condensed type encapsulating material comprises the following components in percentage by mass: the component A is a component B which is 4: 1-6: 1;
the component A comprises the following main raw materials in parts by weight:
the component B comprises the following main raw materials in parts by weight:
10.1-5 parts of catalyst
Polyether 100 parts
20-100 parts of a cross-linking agent composition,
the component B does not contain linear dimethyl silicone oil or branched chain type dimethyl silicone oil.
In the similar two-component condensed type heat-conducting flame-retardant pouring sealant products in the market at present, the mixing ratio of the component A and the component B is generally 10:1, if the mixing ratio is 5:1 to meet the customer requirements, linear dimethyl silicone oil (201 silicone oil) is often added into the component B, and if no dimethyl silicone oil plasticizer is added, the gel after curing is too brittle, deep curing is incomplete and other unfavorable results occur due to the excessive amount of a cross-linking agent.
The inventor of the invention finds out through experiments that when the linear dimethyl silicone oil or the branched chain type dimethyl silicone oil is added into the component B, the storage stability of the component B is obviously reduced, so that in the invention, the polyether is used for replacing the non-linear dimethyl silicone oil or the branched chain type dimethyl silicone oil in the component B, and due to the fact, the storage stability of the component B is obviously improved compared with the similar products in the market.
According to the preferred technical scheme of the component A, the viscosity of the α omega-dihydroxy polydimethylsiloxane is 100-5000 mPa & s, and the preferred viscosity is 300-3000 mPa & s;
the plasticizer is at least one of dimethyl silicone oil and methyl phenyl silicone oil; the viscosity of the plasticizer is 50 to 350 mPas, preferably 50 to 200 mPas.
In practical application, the viscosity of α, omega-dihydroxy polydimethylsiloxane and the plasticizer is selected according to practical requirements, if the viscosity is too low, the fluidity is too good, glue leakage is easy to occur after encapsulation, otherwise, if the viscosity is too high, partial gaps in parts are not easy to fill.
The flame retardant is at least one of zinc borate, aluminum hydroxide, magnesium hydroxide, expanded graphite, melamine cyanurate and a platinum (0) -1, 3-divinyl tetramethyl disiloxane complex;
the heat-conducting filler is at least one of aluminum oxide, zinc oxide, boron nitride and aluminum nitride;
the other fillers are at least one of ground limestone, silica micropowder, mica powder, diatomite, attapulgite, organic bentonite, carbon black and white carbon black;
the white carbon black is preferably gas-phase white carbon black or precipitated white carbon black.
Dimethicone may be added to component a as a plasticizer, where dimethicone does not affect the storage stability of component a.
In the preferable technical scheme of the component B, the polyether has the following structure:
wherein R is1is-H, an alkoxysilane containing an imido group (-CONH-) and an alkoxysilane containing an alkylene group (- (CH)2)nAn alkoxy-silanoalkenyl group or an alkenyl group.
The alkoxysilane containing an imide group-CONH-is preferably-OCNH (CH)2)3Si(OCH3)3、-OCNH(CH2)3Si(OC2H5)3、-OCNH(CH2)3SiCH3(OCH3)2(ii) a Said alkylene group (- (CH)2)nThe alkoxysilane alkenyl group of (E-O) is preferably- (CH)2)3Si(OCH3)3、-(CH2)3Si(O C2H5)3Or- (CH)2)3Si CH3(OCH3)2(ii) a The alkenyl group is preferably-CH2CH＝CH2、-CH2CH2CH＝CH2。
m is an integer of 0 to 12, preferably an integer of 0 to 6;
n is an integer of 0 to 400, preferably 100 to 300.
The values of m and n are reasonably controlled with the aim of achieving the final ideal viscosity, if the values of m and n are too small, the overall molecular weight is small, the viscosity of the material is low, the overall viscosity is low after the component B is prepared, and the difference between the overall viscosity and the viscosity of the component A is not within 5 times; if the values of m and n are too large, the substance may be in a crystalline state at normal temperature, and the preparation of the B component is inconvenient.
The viscosity of the polyether is 500-50000 mPa & s; preferably 5000 to 50000 mPas; further preferably 10000 to 50000 mPas. The viscosity of the polyether is reasonably controlled, so that the difference between the viscosity of the component A and the viscosity of the component B is not too large, and the difference multiple is preferably controlled within 5 times, so that the good matching property of the pouring sealant and equipment is ensured, the ratio fluctuation of materials during sealant application is reduced, and the yield is improved.
The polyether can be prepared and synthesized by self or purchased from other manufacturers, such as the following manufacturers: the trade manufacturer is chemical industry of Huangma, Zhejiang, and Japanese Brillouin chemical industry with a trade mark of SAX 400; the commercial manufacturer is Shanghai Dongda chemical Co., Ltd under the designation STP polymeric resin Donseal S250.
The catalyst 1 is at least one of dibutyltin dilaurate, dioctyltin dilaurate, dibutyltin dioctoate, isopropyl titanate, n-butyl titanate, diisopropyl bis (ethyl acetoacetate) titanate and organic tin chelate.
The cross-linking agent composition comprises the following main raw materials in parts by weight: 200-300 parts of multifunctional silane and 0.1-5 parts of catalyst 2; the multifunctional silane is trifunctional silane and oligomer thereof, tetrafunctional silane and oligomer thereof and a silane coupling agent, wherein the mass ratio of the trifunctional silane to the oligomer thereof, the tetrafunctional silane to the oligomer thereof and the silane coupling agent is (1: 1) - (2): 0.1 to 0.6; the catalyst 2 is a compound of an organic tin catalyst and a titanate catalyst, wherein the mass ratio of organic tin to titanate is 1: 0.8-1.2, and preferably 1: 1. The mass parts of the raw materials of the cross-linking agent composition and the mass parts of the cross-linking agent composition in the component B are independently and respectively calculated, and are not contradictory.
Further preferably, the tri-functional silane is selected from at least one of methyltrimethoxysilane, phenyltrimethoxysilane, vinyltrimethoxysilane, propyltrimethoxysilane, methyltriethoxysilane, diethylaminomethyltriethoxysilane, anilinomethyltrimethoxysilane; the tetrafunctional silane is selected from at least one of tetramethoxy silane and tetraethoxy silane (Si-28); the oligomer of trifunctional silane and tetrafunctional silane is selected from the group consisting of polymethyltriethoxysilane, polyethyl silicate (Si-40); the silane coupling agent is selected from a silane coupling agent KH-550, a silane coupling agent KH-560, a silane coupling agent KH-792 and a silane coupling agent KH-910; the organic tin catalyst is at least one of dibutyltin dilaurate, dioctyltin dilaurate and dibutyltin dioctoate; the titanate catalyst is selected from at least one of n-butyl titanate and isopropyl titanate.
The preparation method of the cross-linking agent composition comprises the following steps:
1) adding the required components into a three-mouth bottle;
2) isolating water vapor and stirring for 10 minutes;
3) and (3) under the condition of keeping water vapor isolated and stirring, heating to 50-150 ℃, refluxing for 2 hours, and naturally cooling to room temperature.
The invention heats and reflows the cross-linking agent composition, and then adds the cross-linking agent composition into the component B, so that the encapsulating material has wide adhesiveness.
The common double-component condensed type organic silicon pouring sealant on the market has good fluidity due to slow viscosity increase in the initial stage of mixing, and is easy to leak glue when being used for parts (such as junction boxes, connectors and the like) with gaps outside, so that the waste of glue is caused, the qualified rate of glue application is reduced, and the use of users is seriously influenced.
The potting material has low viscosity under the condition that the component A and the component B exist independently, and keeps good construction performance, when the component A and the component B are mixed and beaten glue, α and omega-dihydroxy polydimethylsiloxane in the component A and polyether in the component B generate hydrogen bonds, so that the acting force among polymer chains is increased, the system is thickened immediately, glue leakage is not easy to occur after beating glue, the potting qualification rate of parts with gaps outside is greatly improved, and meanwhile, the range of viscosity increase can be controlled within certain reasonable construction conditions, and construction is not influenced.
In a further preferable technical scheme of the invention, the median particle size (D50) of the zinc borate, the aluminum hydroxide, the magnesium hydroxide and the expanded graphite is 0.1-20 μm, and is preferably 3-10 μm;
the median particle diameter (D50) of the aluminum oxide, the zinc oxide, the boron nitride and the aluminum nitride is 0.1-20 μm, preferably 1-10 μm;
the median particle diameter (D50) of the heavy calcium carbonate, the silicon micropowder, the mica powder, the diatomite, the attapulgite and the organic bentonite is 0.1-20 μm, preferably 1-10 μm;
the median filler particle size (D50) is the particle size corresponding to the cumulative percent particle size distribution of a sample at 50%. The selection of the median particle size is determined according to the actual demand, and if the median particle size is too large, the potting material is easy to settle before curing, and is rough after curing, and the flame retardance and the heat conductivity are also negatively affected; if the median particle size is too small, the viscosity of the encapsulating material under the same formula is too high, which is not beneficial to gluing.
The invention also provides a preparation method of the double-component condensed type encapsulating material, which comprises the following specific steps:
the component A is prepared by the steps of adding α, omega-dihydroxy polydimethylsiloxane, a plasticizer, a flame retardant, a heat-conducting filler and other fillers into a planetary stirrer or a high-speed stirrer in proportion, stirring for 20-60 minutes, vacuumizing and stirring for 5-30 minutes, and adding α, omega-dihydroxy polydimethylsiloxane, the plasticizer, the flame retardant, the heat-conducting filler and other fillers into a double-screw extruder in proportion, fully dispersing various materials of the component A through the dispersing and shearing action of a screw, and vacuumizing at a proper position of the double-screw extruder to ensure that no obvious bubbles are generated in the component A.
And (B) component: and adding the catalyst 1, polyether and the cross-linking agent composition into a reaction kettle in proportion, insulating water vapor, stirring for 5-60 minutes, and then insulating water vapor and storing.
And (3) uniformly mixing the component A and the component B at room temperature according to the mass ratio of 4-6: 1 to obtain the double-component condensed type flame-retardant heat-conducting encapsulating material.
The invention provides a bi-component condensed type encapsulating material and a preparation method thereof. Compared with the prior art, the invention has the following beneficial effects:
1) compared with similar products, the polyether with a specific structure does not contain linear dimethyl silicone oil or branched chain type dimethyl silicone oil, and the storage stability of the component B is improved.
2) When the component A and the component B are mixed and beaten, hydrogen bonds are formed among α, omega-dihydroxy polydimethylsiloxane in the component A and polyether in the component B, the system is thickened immediately, glue leakage is not easy to cause after beating, and the encapsulation qualification rate of parts with gaps outside is greatly improved.
3) The difference multiple of the viscosity of the component A and the viscosity of the component B is preferably controlled within a range of 5 times, so that the good matching of the pouring sealant and equipment is ensured, the proportion fluctuation of materials during sealant application is reduced, and the filling and sealing qualification rate of parts is further improved.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to specific embodiments.
Example 1
Adding α parts, omega-dihydroxy polydimethylsiloxane (with the viscosity of 400 mPas), 30 parts of dimethyl silicone oil (with the viscosity of 50 mPas), 150 parts of flame retardant, 10 parts of heat-conducting filler and 10 parts of ground calcium carbonate into a planetary stirrer in proportion, stirring for 20 minutes, and then vacuumizing and stirring for 5 minutes to obtain a component A of the two-component pouring sealant, wherein the flame retardant comprises zinc borate and aluminum hydroxide in a mass part ratio of 1:3, the heat-conducting filler comprises aluminum oxide and zinc oxide in a mass part ratio of 3:1, the median particle sizes (D50) of the zinc borate and the aluminum hydroxide are 7 microns, the median particle size (D50) of the aluminum oxide is 5 microns, the median particle size (D50) of the zinc oxide is 1 micron, and the median particle size (D50) of the ground calcium carbonate is 1 micron.
Will be describedAnd adding 1 part of dibutyltin dilaurate, 100 parts of polyether and 30 parts of cross-linking agent composition into a reaction kettle in proportion, insulating water vapor, stirring for 5 minutes, and then insulating water vapor and storing to obtain a component B of the bi-component pouring sealant. Wherein the polyether has the following structure:
wherein R is1is-H, m is about 4, n is about 200, and the viscosity is 10000 mPas.
The preparation method of the cross-linking agent composition comprises the following steps: 1) adding 50 parts of methyltrimethoxysilane, 50 parts of vinyltrimethoxysilane, 50 parts of tetramethoxysilane, 100 parts of tetraethoxysilane (Si-28), 20 parts of silane coupling agent KH-550, 20 parts of silane coupling agent KH-560, 0.1 part of dibutyltin dilaurate and 0.1 part of n-butyl titanate into a three-mouth bottle; 2) isolating water vapor and stirring for 10 minutes; 3) keeping the stirring condition without water vapor, heating to 50 ℃, refluxing for 2 hours, and naturally cooling to room temperature.
And (3) uniformly mixing the component A and the component B according to the mass ratio of 5:1 at room temperature to obtain the bi-component condensed type encapsulating material.
Example 2
The same procedure as in example 1 was repeated, except that the A component and the B component were mixed at a mass ratio of 4: 1.
Example 3
The same procedure as in example 1 was repeated, except that the A component and the B component were mixed at a mass ratio of 6: 1.
Example 4
The viscosity of the polyether was 2000 mPas, m was about 4 and n was about 80, as in example 1.
Example 5
The viscosity of the polyether was 80000 mPas, m was about 4 and n was about 480, as in example 1.
Example 6
Adding α parts, omega-dihydroxy polydimethylsiloxane (with the viscosity of 750mPa & s), 20 parts of methyl phenyl silicone oil (with the viscosity of 100mPa & s), 50 parts of flame retardant, 50 parts of heat-conducting filler and 20 parts of ground limestone into a planetary stirrer in proportion, stirring for 20 minutes, and then vacuumizing and stirring for 5 minutes to obtain a component A of the bi-component pouring sealant, wherein the flame retardant is aluminum hydroxide, melamine cyanurate and a platinum (0) -1, 3-divinyl tetramethyl disiloxane complex in a mass ratio of 10:5:1, the heat-conducting filler is aluminum oxide and boron nitride in a mass ratio of 1:1, and the other fillers are silicon micropowder and precipitated silica in a mass ratio of 5:1, the aluminum hydroxide and the melamine cyanurate are 3 μm, the median particle size (D50) of the aluminum oxide and the boron nitride is 5 μm, and the median particle size (D50) of the silicon micropowder is 2 μm.
And adding the 3 parts of catalyst, 100 parts of polyether and 40 parts of cross-linking agent composition into a reaction kettle in proportion, insulating water vapor, stirring for 60 minutes, and then insulating water vapor and storing to obtain a component B of the bi-component pouring sealant. Wherein the catalyst is dioctyltin dilaurate and dibutyltin dilaurate, and the mass ratio is 1: 1; the polyether has the following structure:
R1is- (CH)2)3SiCH3(OCH3)2M is about 5 and n is about 300. The viscosity was 24000 mPas.
The preparation method of the cross-linking agent composition comprises the following steps: 1) adding 20 parts of methyltrimethoxysilane, 10 parts of vinyltrimethoxysilane, 10 parts of phenyltrimethoxysilane, 10 parts of propyltrimethoxysilane, 10 parts of methyltriethoxysilane, 10 parts of tetramethoxysilane, 50 parts of tetraethoxysilane (Si-28), 50 parts of polyethyl silicate (Si-40), 10 parts of silane coupling agent KH-550, 20 parts of silane coupling agent KH-560, 5 parts of silane coupling agent KH-792, 5 parts of diethylamino methyl triethoxy silane, 2 parts of dibutyltin dilaurate and 2 parts of n-butyl titanate into a three-mouth bottle; 2) isolating water vapor and stirring for 10 minutes; 3) keeping the stirring condition without water vapor, heating to 70 ℃, refluxing for 2 hours, and naturally cooling to room temperature.
And (3) uniformly mixing the component A and the component B according to the mass ratio of 5:1 at room temperature to obtain the double-component condensed pouring sealant material.
Example 7
The preparation method comprises the steps of adding α parts of omega-dihydroxy polydimethylsiloxane (with the viscosity of 2000mPa & s), 50 parts of plasticizer (with the viscosity of 100mPa & s), 50 parts of flame retardant, 100 parts of heat-conducting filler and 20 parts of other fillers into a high-speed stirrer in proportion, stirring for 30 minutes, and then vacuumizing and stirring for 20 minutes to obtain a component A of the bi-component pouring sealant, wherein the flame retardant comprises magnesium hydroxide and expanded graphite in a mass part ratio of 1:1, the heat-conducting filler comprises aluminum nitride, aluminum oxide and boron nitride in a mass part ratio of 1:5:1, the other fillers comprise ground calcium carbonate, silicon micropowder, mica powder and organic bentonite in a mass part ratio of 1:1:1, the catalyst comprises dibutyltin dilaurate and n-butyl titanate in a mass part ratio of 10:1, the median particle sizes (D50) of the magnesium hydroxide and the expanded graphite are 4 μm, the median particle sizes (D50) of the aluminum nitride and the boron nitride are 3 μm, the median particle sizes (D50) of the aluminum oxide are 6 μm, the median particle sizes (D50) of the silicon micropowder and the heavy calcium carbonate (D50) of the bentonite are 3 μm, and the organic bentonite is 50 μm.
And adding the 0.5 part of catalyst, 100 parts of polyether and 50 parts of cross-linking agent composition into a reaction kettle, insulating water vapor, stirring for 30 minutes, and then insulating water vapor and storing to obtain a component B of the bi-component pouring sealant. Wherein the polyether has the following structure:
wherein R is1is-OCNH (CH)2)3Si(OCH3)3M is about 6 and n is about 400. The viscosity was 50000 mPas. The preparation method of the cross-linking agent composition comprises the following steps: 1) 50 parts of vinyltrimethoxysilane, 30 parts of polymethyltriethoxysilane, 10 parts of tetramethoxysilane, 50 parts of tetraethoxysilane (Si-28), 50 parts of polyethyl silicate (Si-40), 10 parts of silane coupling agent KH-910, 20 parts of phenylaminomethyltrimethoxysilane, 0.1 part of dibutyltin dilaurate and 0.1 part of n-butyl titanate are added into a three-necked flask; 2) isolating water vapor and stirring for 10 minutes; 3) keeping the stirring condition of isolating water vapor, heating to 120 ℃, refluxing for 2 hours, and naturally cooling to room temperature.
And (3) uniformly mixing the component A and the component B according to the mass ratio of 5:1 at room temperature to obtain the double-component condensed pouring sealant material.
Comparative example 1
Adding α parts, omega-dihydroxy polydimethylsiloxane (with the viscosity of 400 mPas), 30 parts of dimethyl silicone oil (with the viscosity of 50 mPas), 10 parts of flame retardant, 10 parts of heat-conducting filler and 10 parts of ground calcium carbonate into a planetary stirrer in proportion, stirring for 20 minutes, and then vacuumizing and stirring for 5 minutes to obtain a component A of the bi-component pouring sealant, wherein the flame retardant comprises zinc borate and aluminum hydroxide in a mass part ratio of 1:3, the heat-conducting filler comprises aluminum oxide and zinc oxide in a mass part ratio of 3:1, the median particle sizes (D50) of the zinc borate and the aluminum hydroxide are 7 microns, the median particle size of the aluminum oxide is 5 microns, the median particle size (D50) of the zinc oxide is 1 micron, and the median particle size (D50) of the ground calcium carbonate is 1 micron.
Adding 1 part of dibutyltin dilaurate, 100 parts of dimethyl silicone oil (with the viscosity of 10000) and 30 parts of a cross-linking agent composition into a reaction kettle in proportion, insulating water vapor, stirring for 5 minutes, and then insulating water vapor for storage to obtain a component B of the bi-component pouring sealant. The preparation method of the cross-linking agent composition comprises the following steps: 1) adding 50 parts of methyltrimethoxysilane, 50 parts of vinyltrimethoxysilane, 50 parts of tetramethoxysilane, 100 parts of tetraethoxysilane (Si-28), 20 parts of silane coupling agent KH-550, 20 parts of silane coupling agent KH-560, 0.1 part of dibutyltin dilaurate and 0.1 part of n-butyl titanate into a three-mouth bottle; 2) isolating water vapor and stirring for 10 minutes; 3) keeping the stirring condition without water vapor, heating to 50 ℃, refluxing for 2 hours, and naturally cooling to room temperature.
And (3) uniformly mixing the component A and the component B according to the mass ratio of 5:1 at room temperature to obtain the double-component condensed pouring sealant material.
Comparative example 2
The component A is prepared by adding α parts, omega-dihydroxy polydimethylsiloxane (with the viscosity of 750mPa & s), 20 parts of methyl phenyl silicone oil (with the viscosity of 100mPa & s), 50 parts of flame retardant, 50 parts of heat-conducting filler and 20 parts of other fillers into a double-screw extruder in proportion, fully dispersing various materials of the component A through the dispersing and shearing action of a screw, and vacuumizing the double-screw extruder at a proper position to ensure that no obvious bubbles are generated in the component A, wherein the flame retardant is aluminum hydroxide, melamine cyanurate and a platinum (0) -1, 3-divinyl tetramethyl disiloxane complex in a mass ratio of 10:5:1, the heat-conducting filler is aluminum oxide and boron nitride in a mass ratio of 1:1, the other fillers are silicon micropowder and precipitated white carbon black in a mass ratio of 5:1, the median particle size (D50) of the aluminum hydroxide is 3 μm, the median particle size (D50) of the aluminum oxide and the median particle size (D50) of the silicon micropowder is 4 μm.
And (B) component: adding the 1 part of catalyst and 100 parts of cross-linking agent composition into a reaction kettle in proportion, insulating water vapor, stirring for 60 minutes, and then insulating water vapor and storing. Wherein the catalyst is dioctyltin dilaurate and dibutyltin dilaurate, and the mass ratio is 1: 1; the preparation method of the cross-linking agent composition comprises the following steps: 1) adding 20 parts of methyltrimethoxysilane, 10 parts of phenyltrimethoxysilane, 10 parts of vinyltrimethoxysilane, 10 parts of propyltrimethoxysilane, 10 parts of methyltriethoxysilane, 10 parts of tetramethoxysilane, 50 parts of tetraethoxysilane (Si-28), 50 parts of polyethyl silicate (Si-40), 10 parts of silane coupling agent KH-550, 20 parts of silane coupling agent KH-560, 5 parts of silane coupling agent KH-792, 5 parts of diethylamino methyl triethoxy silane, 2 parts of dibutyltin dilaurate and 2 parts of n-butyl titanate into a three-mouth bottle; 2) isolating water vapor and stirring for 10 minutes; 3) keeping the stirring condition without water vapor, heating to 70 ℃, refluxing for 2 hours, and naturally cooling to room temperature.
And (3) uniformly mixing the component A and the component B according to the mass ratio of 10:1 at room temperature to obtain the double-component condensed pouring sealant material.
The results of the tests on the product properties of examples 1 to 5 and comparative examples 1 to 2 are shown in Table 1.
The performance test method of the encapsulating material comprises the following steps:
and testing the flame retardant grade of the encapsulating material according to GB 2409-84.
And testing the Shore hardness of the encapsulating material according to GB/T531.
The thermal conductivity of the potting material was tested according to ISO 22007-2.
The viscosity of the potting material was tested according to GB/T2794.
TABLE 1 Performance test results of two-component condensed type pouring sealant materials
As can be seen from the comparison of the results of the embodiment and the comparative example, the flame retardant property and the heat conducting property of the two-component condensed pouring sealant provided by the invention can meet the actual requirements. Examples 1-3 through reasonable formulation design, the viscosity difference between component a and component B was controlled within 4.31 times, while ensuring a significant increase in initial viscosity after mixing, rather than simple mechanical mixing, thereby increasing the user's qualification rate of gluing. In examples 6 and 7, the difference times of the viscosities of the component A and the component B are reduced to be 2.50 and 3.14, and the qualified rate of glue application is further improved. The inventor also unexpectedly finds that, in addition to controlling the difference multiple of the viscosities of the component a and the component B within a certain range preferably to further improve the yield of the glue application, the viscosity of the polyether also affects the performance of the finished two-component pouring sealant, in example 5, although the difference multiple of the viscosities of the component a and the component B is not large and is 2.41, the yield of the glue application is limited due to the large viscosity of the polyether in the component B. In practical use, the component A and the component B can be mixed according to the mass ratio of 4: 1-6: 1 as required, different mixing ratios can lead to different performances of the solidified potting material, but when the two-component condensed type potting material is used within the mixing ratio range specified by the invention, higher gluing qualified rate can be ensured; if the actual mixing ratio deviates from 4:1 to 6:1, the use requirement can not be met according to the original formula, and the product formula needs to be adjusted, which is not discussed herein.
If the polyether in the embodiment 1 is replaced by the dimethyl silicone oil with the same viscosity in the comparative example 1, the storage stability of the component B in the comparative example is greatly reduced, and the gel time is slowed to be more than 2 times of the initial gel time when the two-component condensed pouring sealant material is stored at room temperature for 2 months, but the gel time is only slightly increased when the two-component condensed pouring sealant material provided by the invention is stored at room temperature for 6 months; in the product of comparative example 1, the initial viscosity of component A and component B after mixing does not increase significantly as in example 1; the result is that the yield of the comparative example 1 is much lower than that of the example 1 when the glue is actually applied.
Comparative example 2, the mixing ratio was changed to 10:1 which is common in the market, and the storage stability of component B was ensured by removing the plasticizer from component B; however, since the mixing ratio of the component a and the component B is 10:1, the equipment compatibility is deteriorated, and the ratio of the viscosity difference between the component a and the component B is inevitably increased, resulting in a lower yield of actual gluing.
In conclusion, compared with similar 4: 1-6: 1 products, the heat-conducting encapsulating material has the advantages that the storage stability of the component B is improved; when the glue is mixed and applied, the system is immediately thickened, glue leakage is not easy to cause, and the encapsulation qualification rate of parts with gaps outside is greatly improved. The difference multiple of the viscosity of the component A and the viscosity of the component B can be controlled within a range of 5 times, so that the good matching of the pouring sealant and equipment is ensured, the proportion fluctuation of materials during sealant application is reduced, and the filling and sealing qualification rate of parts is improved.
Although the present invention has been described herein with reference to the illustrated embodiments thereof, which are intended to be preferred embodiments of the present invention, it is to be understood that the invention is not limited thereto, and that numerous other modifications and embodiments can be devised by those skilled in the art that will fall within the spirit and scope of the principles of this disclosure.
Claims (10)
1. The two-component condensed type flame-retardant heat-conducting encapsulating material is characterized by comprising the following components in parts by mass: the component A is a component B which is 4-6: 1;
the component A comprises the following main raw materials in parts by weight:
the component B comprises the following main raw materials in parts by weight:
10.1-5 parts of catalyst
Polyether 100 parts
20-100 parts of a cross-linking agent composition,
the component B does not contain linear dimethyl silicone oil or branched chain type dimethyl silicone oil.
2. The two-component condensed-type flame-retardant heat-conductive potting material of claim 1, wherein the polyether has the following structure:
wherein R is1is-H, an alkoxysilane containing an imido group (-CONH-) and an alkoxysilane containing an alkylene group (- (CH)2)n-an alkoxy-silanoalkenyl group, an alkenyl group; m is an integer of 0 to 12, preferably an integer of 0 to 6; n is an integer of 0 to 400, preferably an integer of 100 to 300; the viscosity of the polyether is 500-50000 mPa & s; preferably 5000 to 50000 mPas; further preferably 10000 to 50000 mPas.
3. The two-component condensed type flame retardant heat conductive potting material of claim 2, wherein the imido-CONH-containing alkoxysilane is selected from the group consisting of-OCNH (CH)2)3Si(OCH3)3、-OCNH(CH2)3Si(OC2H5)3、-OCNH(CH2)3SiCH3(OCH3)2(ii) a Said alkylene group- (CH)2)nThe alkoxysilane alkenyl of (A) is selected from- (CH)2)3Si(OCH3)3、-(CH2)3Si(O C2H5)3Or- (CH)2)3Si CH3(OCH3)2(ii) a The alkenyl is selected from-CH2CH＝CH2、-CH2CH2CH＝CH2。
4. The two-component condensed type flame-retardant heat-conducting potting material as claimed in any one of claims 1 to 3, wherein the viscosity of the α omega-dihydroxy polydimethylsiloxane is 100 to 5000 mPas, preferably 300 to 3000 mPas, the plasticizer is at least one of simethicone and methyl phenyl silicone oil, and the viscosity of the plasticizer is 50 to 350 mPas, preferably 50 to 200 mPas.
5. The two-component condensed-type flame-retardant, heat-conductive potting material of any one of claims 1 to 3, wherein the flame retardant is at least one of zinc borate, aluminum hydroxide, magnesium hydroxide, expanded graphite, melamine cyanurate, platinum (0) -1, 3-divinyltetramethyldisiloxane complex; the heat-conducting filler is at least one of aluminum oxide, zinc oxide, boron nitride and aluminum nitride; the other fillers are at least one of ground limestone, silica micropowder, mica powder, diatomite, attapulgite, organic bentonite, carbon black and white carbon black; the white carbon black is preferably fumed silica or precipitated white carbon black, and the catalyst 1 is at least one of dibutyltin dilaurate, dioctyltin dilaurate, dibutyltin dioctoate, isopropyl titanate, n-butyl titanate, diisopropyl bis (ethyl acetoacetate) titanate and organic tin chelate.
6. The two-component condensed type flame-retardant heat-conductive potting material of claim 5, wherein the zinc borate, the aluminum hydroxide, the magnesium hydroxide, the expanded graphite, the melamine cyanurate have a median particle size (D50) of 0.1 to 20 μm, preferably 2 to 10 μm;
the median particle diameter (D50) of the aluminum oxide, the zinc oxide, the boron nitride and the aluminum nitride is 0.1-20 μm, preferably 1-10 μm;
the median particle diameter (D50) of the heavy calcium carbonate, the silicon micropowder, the mica powder, the diatomite, the attapulgite and the organic bentonite is 0.1-20 μm, preferably 1-10 μm.
7. The two-component condensed type flame-retardant heat-conducting potting material according to any one of claims 1 to 3, wherein the cross-linking agent composition comprises the following main raw materials in parts by mass: 200-300 parts of multifunctional silane and 0.1-5 parts of catalyst 2; the multifunctional silane is trifunctional silane and oligomer thereof, tetrafunctional silane and oligomer thereof and a silane coupling agent, wherein the mass ratio of the trifunctional silane to the oligomer thereof, the tetrafunctional silane to the oligomer thereof and the silane coupling agent is (1: 1) - (2): 0.1 to 0.6; the catalyst 2 is a compound of an organic tin catalyst and a titanate catalyst, wherein the mass ratio of organic tin to titanate is 1: 0.8-1.2, and preferably 1: 1.
8. The two-component condensed-type flame-retardant heat-conductive potting material of claim 7, wherein the tri-functional silane is selected from at least one of methyltrimethoxysilane, phenyltrimethoxysilane, vinyltrimethoxysilane, propyltrimethoxysilane, methyltriethoxysilane, diethylaminomethyltriethoxysilane, anilinomethyltrimethoxysilane; the tetrafunctional silane is selected from at least one of tetramethoxy silane and tetraethoxy silane (Si-28); the oligomer of trifunctional silane and tetrafunctional silane is selected from the group consisting of polymethyltriethoxysilane, polyethyl silicate (Si-40); the silane coupling agent is selected from a silane coupling agent KH-550, a silane coupling agent KH-560, a silane coupling agent KH-792 and a silane coupling agent KH-910; the organic tin catalyst is at least one of dibutyltin dilaurate, dioctyltin dilaurate and dibutyltin dioctoate; the titanate catalyst is selected from at least one of n-butyl titanate and isopropyl titanate.
9. The method for preparing the two-component condensed-type potting material according to any one of claims 1 to 8, wherein the specific steps are as follows:
the component A is prepared by the steps of adding α, omega-dihydroxy polydimethylsiloxane, a plasticizer, a flame retardant, a heat-conducting filler and other fillers into a planetary stirrer or a high-speed stirrer in proportion, stirring for 20-60 minutes, vacuumizing and stirring for 5-30 minutes, and adding α, omega-dihydroxy polydimethylsiloxane, the plasticizer, the flame retardant, the heat-conducting filler and other fillers into a double-screw extruder in proportion, fully dispersing various materials of the component A through the dispersing and shearing action of a screw, and vacuumizing at a proper position of the double-screw extruder to ensure that no obvious bubbles are generated in the component A;
and (B) component: adding the catalyst 1, polyether and cross-linking agent composition into a reaction kettle in proportion, insulating water vapor, stirring for 5-60 minutes, and then insulating water vapor and storing;
and (3) uniformly mixing the component A and the component B at room temperature according to the mass ratio of 4-6: 1 to obtain the double-component condensed type flame-retardant heat-conducting encapsulating material.
10. The method of claim 9, wherein the crosslinker composition is prepared by:
1) adding the required components into a three-mouth bottle;
2) isolating water vapor and stirring for 10 minutes;
3) and (3) under the condition of keeping water vapor isolated and stirring, heating to 50-150 ℃, refluxing for 2 hours, and naturally cooling to room temperature.
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