CN105218714A - A kind of flame retardant microcapsule and its preparation method and application - Google Patents
A kind of flame retardant microcapsule and its preparation method and application Download PDFInfo
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Abstract
The invention discloses a kind of flame retardant microcapsule and its preparation method and application, described flame retardant microcapsule comprises core and is coated on the coating layer outside core; Described core is liquid heptafluoro-propane or liquid HFC-236fa; Described coating layer is polymethacrylate polymkeric substance, by suspension polymerization polymerization preparation.Described flame retardant microcapsule can separately as fire-retardant filler, also can combine the preparation for electron pouring sealant as fire-retardant filler with magnesium hydroxide/aluminium hydroxide jointly.Product thermostability of the present invention is high, permeability resistance good, and the leakage of core can not occur in normal state; Only when being subject to high hot burning, the softening liquid core vaporization simultaneously of coating layer makes internal pressure increase cause coating layer swelling fracture, and final core is discharged, quick flame-retarding fire-extinguishing, has wide prospect of the application in electron pouring sealant preparation field.<!-- 2 -->
Description
Technical field
The present invention relates to a kind of flame retardant microcapsule, be specifically related to a kind ofly be applicable to the flame retardant microcapsule in electron pouring sealant field and its preparation method and application.
Background technology
Macromolecular material, general oxygen index such as such as plastics, coating, fiber and rubber etc. is low, belongs to inflammable material, easily produces fire safety evaluating hidden danger, and therefore in macromolecular material, normal needs is considered to add fire retardant to improve its flame retardant resistance.Along with the development of electronic industry, electronic component is more tending towards densification and miniaturization, and significantly improving of electronic device power also it is also proposed higher requirement to the flame retardant properties of joint sealant.Normally prepare flame-retarded heat-conducting joint sealant by adding fire-retardant filler at present.
The Halogen according to whether, can be divided into halogen containing flame-retardant and halogen-free flame retardants by fire retardant.Wherein, halogen containing flame-retardant generally refers to fire retardant that is brominated, chlorine element, this based flame retardant can produce a large amount of smog and toxic and harmful in combustion, severe contamination is produced to environment, there is huge destruction to atmospheric ozone layer, do not used by promotion in electronic product and even prohibit the use.Halogen-free flame retardants can be divided into again metal hydroxide combustion inhibitor and nitrogen phosphorus compound flame redundant, wherein conventional in electron pouring sealant field with metal hydroxide combustion inhibitor.Metal hydroxide combustion inhibitor itself have good stability, the amount of being fuming little, do not produce toxic gas, abundance, the advantage such as cheap, but, the poor compatibility of metal hydroxide combustion inhibitor and macromolecule organic material, easy moisture absorption conglomeration, bad dispersibility, often cause processing fluidity to be deteriorated when addition is large in use procedure, reduce the physical and mechanical properties of material.When aluminium hydroxide or magnesium hydroxide join in joint sealant as fire retardant, often sacrificing the flowing property of joint sealant in order to obtain more excellent flame retardant properties, putting down and dropping down embedding difficulty, the cohesiveness of joint sealant reduces, thus affects the life-span of electronic component.
Microcapsulary with natural or synthesis polymer continuous film forming material, solid, liquid, gas material (core or interior phase) is rolled into diameter and is about 1 ~ 500 μm; the thickness of wall is the capsule of 0.5 ~ 150 μm; the original chemical property of such guarantee core material at all can't harm; rely on the shielding effect of cyst wall to play the effect of protection core, then little by little by some outside stimulus or slow releasing function, the function of object is presented in outside again.At present, the microcapsule preparation of fire retardant is all widely used in reasonable offer, weaving, building, paint field.
Summary of the invention
For solving the problems referred to above that prior art exists, the object of the present invention is to provide a kind of with liquid heptafluoro-propane or liquid HFC-236fa be core, the flame retardant microcapsule that is coating layer with polymethacrylate polymkeric substance, this flame retardant microcapsule thermostability and permeability resistance good, flame-retarding fire-extinguishing effect is strong, and the fire-retardant filler be specially adapted to as electron pouring sealant uses.
For achieving the above object, the technical solution adopted in the present invention is:
A kind of flame retardant microcapsule, comprises core and is coated on the coating layer outside core.Described core is liquid flame-proof fire-fighting medium, is preferably liquid heptafluoro-propane or liquid HFC-236fa.Described coating layer is organic polymer, overlays on core skin by monomer aggregate packet under the initiation of initiator; Be preferably polymethacrylate polymkeric substance, by suspension polymerization polymerization preparation.
The preparation method of described flame retardant microcapsule, comprises following steps:
A, transfer core to liquid state by gaseous state by pressurization, moulding pressure control 3MPa ~ 8Mpa, preferred pressure is 4 ~ 6MPa;
B, in liquid core, add water, dispersion agent and emulsifying agent, be heated with stirring to 50 DEG C ~ 70 DEG C;
C, initiator is joined monomer room-temperature dissolution, then join in the reaction solution of step b, dropwising rear adjustment stirring velocity is 100 ~ 300rmp/min, after constant agitation speed, intensification is heated to 60 DEG C ~ 100 DEG C (preferably 65 ~ 85 DEG C), carry out suspension polymerization, reaction times 1 ~ 3h; Draw a small amount of pearl, if hardening after cooling, then stop stirring, terminating reaction;
After d, reaction terminate, lay down reactor pressure, reaction solution is down to room temperature, after filtration, washing, after drying, namely obtain flame retardant microcapsule.
In above-mentioned preparation method, the ratio of quality and the number of copies of described monomer, core, water, dispersion agent, emulsifying agent, initiator is 100:400 ~ 1500:200 ~ 600:100 ~ 250:5 ~ 12:0.4 ~ 2, and preferred proportion is 100:500 ~ 1200:300 ~ 500:150 ~ 200:8 ~ 10:0.5 ~ 1.
In above-mentioned preparation method:
Described monomer is any one in methyl methacrylate, isobornyl methacrylate, methacrylic acid;
Described dispersion agent is polyvinyl alcohol, and being preferably massfraction is the polyvinyl alcohol solution of 1%;
Described initiator is oil-soluble initiator, specifically refers to any one in benzoyl peroxide (BPO), dilauroyl peroxide (LPO), dicumyl peroxide, di-tert-butyl peroxide, dicumyl peroxide, Diisopropyl azodicarboxylate;
Described emulsifying agent is any one or a few the mixing in OP series, sodium laurylsulfonate, sodium lauryl sulphate, and wherein, polyoxyethylene nonylphenol ether series comprises OP-10, OP-4, OP-7, OP-15;
Described flame retardant microcapsule can be used as fire-retardant filler in the preparation of electron pouring sealant.Can use as fire-retardant filler separately during application, also can with magnesium hydroxide/aluminium hydroxide jointly as fire-retardant filler conbined usage.
The invention has the beneficial effects as follows:
The invention provides a kind of flame retardant microcapsule and its preparation method and application, with liquid heptafluoro-propane or liquid HFC-236fa be core, with polymethacrylate polymkeric substance for coating layer, thermostability is high, permeability resistance good, and the leakage of core can not occur in normal state; Only when being subject to high hot burning, coating layer is softening, liquid core vaporization simultaneously makes internal pressure increase cause coating layer swelling fracture, and final core is discharged, quick flame-retarding fire-extinguishing, has wide prospect of the application in electron pouring sealant preparation field.
Product core of the present invention adopts liquid heptafluoro-propane or liquid HFC-236fa, these two kinds of alkane be all colorless and odorless can the gas of low-pressure liquefied storage, have that critical temperature is high, boiling point is low, critically to force down, feature that saturation steam forces down, can long storage periods at normal temperatures.And these two kinds alkane is non-conductive, toxicity is low, non-secondary pollution, do not have solid liquid phase residue after fire extinguishing, be zero to the loss latent energy value (ODP value) of ozonosphere, do not have destruction, Greenhouse effect negligible to atmospheric ozone layer, environmental protection, particularly corrosion failure effect be there is no to electrical equipment, electronics, be therefore particularly suitable as core and use.
The coating layer of product of the present invention is polymethacrylate polymkeric substance, coating layer has good thermoplasticity and thermostability, certain high moderate pressure can be tolerated, not easily break, covered effect is good, and other raw materials of its polarity and electron pouring sealant are close, thus have good consistency; And core can not produce the water vapour of etching electronic element after being subject to high temperature, therefore, use product of the present invention as electron pouring sealant fire-retardant filler, to replace or part replaces magnesium hydroxide/aluminium hydroxide to use completely, good dispersiveness and consistency can be obtained, reduce and the loss of matrix physical and mechanical properties, adhesive property are protected, extend its sedimentation time simultaneously, reduce joint sealant viscosity and make trickling easy, flatly drop down embedding and be achieved.
The preparation of product of the present invention adopts suspension polymerization, without the need to core and coating layer are separately prepared, core is liquefied as liquid state in autoclave, then direct polymerization reaction balling-up in autoclave, monomer selects methacrylic acid/methyl acrylic ester, oil-soluble initiator selected by initiator, preparation process only needs to add water, dispersion agent and emulsifying agent, reaction process is simple, system is single, temperature of reaction is low, polymerization time is short, transformation efficiency is high, and following process treatment process is simple, reaction cost is low, it is useless that reaction process does not produce danger, environmental protection, dangerous low, very be applicable to industrial amplification production, have broad application prospects.
Preparation method of the present invention selects the polyvinyl alcohol of applicable system of the present invention to be dispersion agent, using sodium laurylsulfonate, sodium lauryl sulphate, OP series as emulsifying agent, and give rational add-on, effectively prevent the reunion of microcapsule in reaction process, obtained flame retardant microcapsule product is complete spheroidal particle, dispersing property is good, coating layer is complete, granularity reaches micron order, effectively ensure that the stability of flame retardant microcapsule product under normal temperature and pressure conditions, can standing storage, security is high.
Embodiment
Below by specific embodiment, the present invention is described in further detail, but embodiment is not the restriction of scope.
Embodiment 1
A kind of flame retardant microcapsule, its core is liquid heptafluoro-propane, and its coating layer is poly methyl methacrylate polymer.Its preparation method is as follows:
A, at room temperature 600g gaseous state heptafluoro-propane is passed into compressive reaction still, moulding pressure control 4Mpa, makes heptafluoro-propane transfer liquid state to;
B, in the liquid heptafluoro-propane in compressive reaction still, add 300g water, 150g massfraction be 1% polyvinyl alcohol solution, 8g sodium laurylsulfonate, be heated with stirring to 50 DEG C ~ 55 DEG C;
C, 0.6g initiator B PO added in 100g methyl methacrylate and dissolves, then slowly instill in the reaction solution of step b; Dropwising rear adjustment stirring velocity is 200rmp/min, after constant agitation speed, controls suspension polymerization temperature 78 ± 2 DEG C, polymerization reaction time 2h; Then a small amount of pearl is drawn, hardening after cooling, confirm that reaction terminates; Stop stirring, terminating reaction;
D, reaction terminate rear release, and reaction solution is down to room temperature, and distilled water wash 4 times after filtering, 60 DEG C are dried to constant weight, obtain flame retardant microcapsule 658g.
Embodiment 2
A kind of flame retardant microcapsule, its core is liquid HFC-236fa, and its coating layer is poly methyl methacrylate polymer.Its preparation method is as follows:
A, at room temperature 800g gaseous state HFC-236fa is passed into compressive reaction still, moulding pressure control 5Mpa, makes heptafluoro-propane transfer liquid state to;
B, in the liquid HFC-236fa in compressive reaction still, add 400g water, 160g massfraction be 1% polyvinyl alcohol solution, 9gOP-10 emulsifying agent, be heated with stirring to 50 DEG C ~ 55 DEG C;
C, 0.8g initiator B PO added in 100g methyl methacrylate and dissolves, then slowly instill in the reaction solution of step b; Dropwising rear adjustment stirring velocity is 200rmp/min, after constant agitation speed, controls suspension polymerization temperature 78 ± 2 DEG C, polymerization reaction time 2h; Then a small amount of pearl is drawn, hardening after cooling, confirm that reaction terminates; Stop stirring, terminating reaction;
D, reaction terminate rear release, and reaction solution is down to room temperature, and use distilled water wash 5 times after filtering, 60 DEG C are dried to constant weight, obtain flame retardant microcapsule 760g.
Embodiment 3
A kind of flame retardant microcapsule, its core is liquid heptafluoro-propane, and its coating layer is polymethacrylic acid polymer.Its preparation method is as follows:
A, at room temperature 700g gaseous state heptafluoro-propane is passed into compressive reaction still, moulding pressure control 5Mpa, makes heptafluoro-propane transfer liquid state to;
B, in the liquid HFC-236fa in compressive reaction still, add 500g water, 180g massfraction be 1% polyvinyl alcohol solution, 8g sodium lauryl sulphate, be heated with stirring to 60 DEG C ~ 65 DEG C;
C, 0.6g initiator Diisopropyl azodicarboxylate added in 100g methacrylic acid and dissolves, then slowly instill in the reaction solution of step b; Dropwising rear adjustment stirring velocity is 250rmp/min, after constant agitation speed, controls suspension polymerization temperature 85 ± 2 DEG C, polymerization reaction time 3h; Then a small amount of pearl is drawn, hardening after cooling, confirm that reaction terminates; Stop stirring, terminating reaction;
D, reaction terminate rear release, and reaction solution is down to room temperature, and use distilled water wash 4 times after filtering, 70 DEG C are dried to constant weight, obtain flame retardant microcapsule 695g.
Embodiment 4
A kind of flame retardant microcapsule, its core is liquid heptafluoro-propane, and its coating layer is polyisobornyl methacrylate polymkeric substance.Its preparation method is as follows:
A, at room temperature 1000g gaseous state heptafluoro-propane is passed into compressive reaction still, moulding pressure control 7Mpa, makes heptafluoro-propane transfer liquid state to;
B, in the liquid heptafluoro-propane in compressive reaction still, add 500g water, 200g massfraction be 1% polyvinyl alcohol solution, 8g sodium laurylsulfonate, be heated with stirring to 60 DEG C ~ 65 DEG C;
C, 0.8g initiator Diisopropyl azodicarboxylate added in 100g methyl methacrylate and dissolves, then slowly instill in the reaction solution of step b; Dropwising rear adjustment stirring velocity is 250rmp/min, after constant agitation speed, controls suspension polymerization temperature 90 ± 2 DEG C, polymerization reaction time 2h; Then a small amount of pearl is drawn, hardening after cooling, confirm that reaction terminates; Stop stirring, terminating reaction;
D, reaction terminate rear release, and reaction solution is down to room temperature, and use distilled water wash 5 times after filtering, 80 DEG C are dried to constant weight, obtain flame retardant microcapsule 880g.
Below, flame retardant microcapsule prepared by embodiment 1 ~ embodiment 4 is mixed with aluminium hydroxide and prepares bi-component organic silicon fire-proof potting compound as fire-retardant filler, and be used alone the bi-component organic silicon fire-proof potting compound of aluminium hydroxide as fire-retardant filler and carry out performance test comparison.
One, the preparation of the bi-component organic silicon fire-proof potting compound of mixing fire-retardant filler is added
(1) base-material preparation: 100g vinyl silicone oil, 20g aluminium hydroxide, 20g flame retardant microcapsule and 150g aluminum oxide are joined vacuum kneader and mixes, obtain base-material; Base-material prepares two parts altogether;
(2) component A preparation: under normal temperature, add 0.35g Karst catalyzer wherein in a base-material, uses high speed dispersor fully to stir 0.5h;
(3) B component preparation: under normal temperature, add 0.06g alkynyl hexalin, 12g containing hydrogen silicone oil to another part of base-material, uses high speed dispersor fully to stir 0.5h;
(4) joint sealant preparation: by etc. the component A of quality and B component high speed dispersor mix, vacuum defoamation 10min, pours mould self cure 24h into, i.e. obtained bi-component organic silicon fire-proof potting compound product.
The joint sealant adopting embodiment 1, embodiment 2, embodiment 3, embodiment 4 product to prepare is labeled as S-1, S-2, S-3, S-4 respectively.
Two, the preparation of the bi-component organic silicon fire-proof potting compound of aluminium hydroxide fire retardant is added
The preparation process mixing the bi-component organic silicon fire-proof potting compound of fire retardant is substantially identical with adding, and its difference is: do not use flame retardant microcapsule, adds separately 40g aluminium hydroxide and prepares as fire-retardant filler.Gained joint sealant product labelling is D-1.
Get above-mentioned obtained bi-component organic silicon fire-proof potting compound product S-1, S-2, S-3, S-4, D-1, measure its viscosity, tensile strength, limiting oxygen index(LOI) and flame retardant rating respectively.Wherein, viscosity test, according to GB/T2794-1995 standard, adopts rotary viscosity design determining; Tensile strength test, according to GB/T528-2009, adopts electronic universal tester to measure; Limiting oxygen index(LOI) test, according to GB/T10707-2008, adopts oxygen index measurer to measure; Flame retardant rating test, according to GB/T10707-2008, adopts horizontal vertical combustion testing machine to measure.
Test result sees the following form.
The different fire-retardant filler of table 1 is on the impact of organic silicon flame-retardant joint sealant
In table 1, data can be found out, the flame retardant rating of D-1 joint sealant product only can reach V1 level, and oxygen index is low, and tensile strength is low, viscosity is larger; And use four joint sealant products of flame retardant microcapsule of the present invention and aluminium hydroxide compositional flame-retardant, its flame retardant rating all can reach V0 level, oxygen index is high, nonflammable, and its tensile strength and D-1 joint sealant have significant lifting, lower suitable the putting down of viscosity drops down embedding, the overall performance of electron pouring sealant is significantly superior, and be more applicable to the trend of present electronic component densification, superpower, safety coefficient is high.
Above-described embodiment is used for explaining and the present invention is described, instead of limits the invention, and in the protection domain of the claims in the present invention, any amendment make the present invention and change, all fall into protection scope of the present invention.
Claims (10)
1. a flame retardant microcapsule, is characterized in that: described flame retardant microcapsule comprises core and is coated on the coating layer outside core; Described core is liquid flame-proof fire-fighting medium, and described coating layer is organic polymer, overlays on core skin by monomer aggregate packet under the initiation of initiator.
2. a kind of flame retardant microcapsule as claimed in claim 1, is characterized in that: described core is liquid heptafluoro-propane or liquid HFC-236fa; Described coating layer is polymethacrylate polymkeric substance, by suspension polymerization polymerization preparation.
3. the preparation method of a kind of flame retardant microcapsule as described in any one of claim 1 or 2, is characterized in that comprising following steps:
A, transfer core to liquid state by gaseous state by pressurization, moulding pressure control 3MPa ~ 8Mpa;
B, in liquid core, add water, dispersion agent and emulsifying agent, be heated with stirring to 50 DEG C ~ 70 DEG C;
C, initiator is joined monomer room-temperature dissolution, then join in the reaction solution of step b, dropwising rear adjustment stirring velocity is 100 ~ 300rmp/min, after constant agitation speed, intensification is heated to 60 DEG C ~ 100 DEG C, carries out suspension polymerization, reaction times 1 ~ 3h; Draw a small amount of pearl, if hardening after cooling, then stop stirring, terminating reaction;
After d, reaction terminate, lay down reactor pressure, reaction solution is down to room temperature, after filtration, washing, after drying, namely obtain flame retardant microcapsule.
4. the preparation method of a kind of flame retardant microcapsule as claimed in claim 3, is characterized in that: the ratio of quality and the number of copies of described monomer, core, water, dispersion agent, emulsifying agent, initiator is 100:400 ~ 1500:200 ~ 600:100 ~ 250:5 ~ 12:0.4 ~ 2.
5. the preparation method of a kind of flame retardant microcapsule as claimed in claim 4, is characterized in that: the ratio of quality and the number of copies of described monomer, core, water, dispersion agent, emulsifying agent, initiator is 100:500 ~ 1200:300 ~ 500:150 ~ 200:8 ~ 10:0.5 ~ 1.
6. the preparation method of a kind of flame retardant microcapsule as described in any one of claim 3 ~ 5, is characterized in that: described monomer is any one in methyl methacrylate, isobornyl methacrylate, methacrylic acid; Described dispersion agent is polyvinyl alcohol; Described initiator is oil-soluble initiator.
7. the preparation method of a kind of flame retardant microcapsule as claimed in claim 6, is characterized in that: described dispersion agent to be massfraction be 1% polyvinyl alcohol solution; Described initiator is any one in benzoyl peroxide, dilauroyl peroxide, dicumyl peroxide, di-tert-butyl peroxide, dicumyl peroxide, Diisopropyl azodicarboxylate.
8. the preparation method of a kind of flame retardant microcapsule as described in any one of claim 3 ~ 5, is characterized in that: described emulsifying agent is any one or a few the mixing in OP series, sodium laurylsulfonate, sodium lauryl sulphate.
9. the preparation method of a kind of flame retardant microcapsule as claimed in claim 8, is characterized in that: described polyoxyethylene nonylphenol ether series comprises OP-10, OP-4, OP-7, OP-15.
10. the application of a kind of flame retardant microcapsule as described in any one of claim 1 or 2, it is characterized in that: when described flame retardant microcapsule is used for the preparation of electron pouring sealant as fire-retardant filler, use as fire-retardant filler separately or with magnesium hydroxide/aluminium hydroxide jointly as fire-retardant filler conbined usage.
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