CN1916098A - Flame resisting agent with no halogen in series of crylic acid in use for pressure sensitive adhesive tape, and prepartion method - Google Patents
Flame resisting agent with no halogen in series of crylic acid in use for pressure sensitive adhesive tape, and prepartion method Download PDFInfo
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- CN1916098A CN1916098A CN 200510028764 CN200510028764A CN1916098A CN 1916098 A CN1916098 A CN 1916098A CN 200510028764 CN200510028764 CN 200510028764 CN 200510028764 A CN200510028764 A CN 200510028764A CN 1916098 A CN1916098 A CN 1916098A
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- sensitive adhesive
- acrylic acid
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- retardant agent
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Abstract
This invention relates to a method for preparing halogen-free flame retardant for acrylic acid pressure-sensitive adhesive tape. The halogen-free flame retardant comprises: organic halogen-free flame phosphate 0-50 wt.%, inorganic matters 20-90 wt.%, and nitrogen-containing compounds 5-50 wt.%. The method comprises: (1) mixing the components with organic solvent at a weight ratio of 1: 1 to obtain a slurry, and milling in a ball mill for 2-4 h; (2) sieving by 120 mesh sieve, pouring the liquid into acrylic acid pressure-sensitive adhesive, and stirring evenly to obtain acrylic acid pressure-sensitive adhesive containing the halogen-free flame retardant; (3) coating onto a matrix material to obtain acrylic acid pressure-sensitive adhesive tape. The acrylic acid pressure-sensitive adhesive tape added with the halogen-free flame retardant has good flame retardancy without damage to its adhesiveness and electric properties.
Description
Technical field
The present invention relates to a kind of incombustible agent, relate in particular to the non-halogen fire-retardant agent and preparation method thereof of a kind of acrylic acid series pressure-sensitive adhesive tape.
Background technology
In recent years, in order to improve pressure-sensitive adhesive tape, particularly the flame retardancy of acrylic acid series pressure-sensitive adhesive tape is generally added Halogen incombustible agent and insalubrious antimonous oxide.When but the pressure-sensitive adhesive tape of Halogen incombustible agent is used for household electrical appliances, precision instrument, because Working environment is in certain high temperature, and be heated through long duration of action and produce the problem of halide-ions corroding metal component, especially the corrosion situation is even more serious under high humidity, and the Pressuresensitive Tape that contains the halogen incombustible agent also can generate mordant hydrogen halide when discarded burning disposal.For this reason, for environmental protection, produce obnoxious flavour and avoid the etching problem equal angles to consider, people have proposed the method for the fire-retardant pressure-sensitive adhesive tape of various use halogen-free flame retardantss.
Adopt as Japanese Patent H 08-193187 and to come flame-proof acrylic series pressure-sensitive adhesive tape with red phosphorus and nitrogenous phosphorus compound are composite.It is tackiness agent and obtain difficult combustion protection sealing tape that JP2002-69400 has proposed with nitrogenous compound flame-proof acrylics such as melamine cyanurate (be called for short MC), melamines.JP2002-69403 then proposes with silicon dioxide compound, metal oxide, phosphorus compound, nitrogenous compound, metal hydroxides, borate etc. non-woven fabrics base material and acrylate glue adhesion coating to be carried out fire-retardant and obtain difficulty firing sealing tape.It is tackiness agent and obtain the difficult sealing tape that fires that JP 2002-338906 proposes phosphonitrile, aluminium hydroxide, APP compositional flame-retardant light-cured acrylic.JP 2003-160768 and JP2003-160776 propose aluminium hydroxide, nitrogenous phosphorus compound and the aliphatic polyol fire retardant as the thermal conduction pressure-sensitive adhesive tape.
Though above-mentioned existent technique has good flame-retardant effect, but in actual fabrication, there is unsatisfactory part, as separating out, cause the sealing tape tackiness poor owing to low-molecular-weight inorganic incombustible agent or organo phosphorous compounds and pressure-sensitive adhesive tape matrix resin acrylic ester adhesive consistency difference; And for example, the sealing tape that contains red phosphorus combustion inhibitor easy coloring not.
Summary of the invention
The object of the present invention is to provide a kind of acrylic acid series pressure-sensitive adhesive tape with non-halogen fire-retardant agent and preparation method thereof, it can not only satisfy fire-retardant requirement but also not influence sealing tape adhesiveproperties and electrical property.
The object of the present invention is achieved like this:
A kind of acrylic acid series pressure-sensitive adhesive tape non-halogen fire-retardant agent is characterized in that this incombustible agent comprises following component and weight percent thereof:
Organic non-halogen phosphoric acid ester 0～50%,
Inorganics 20～90%,
Nitrogenous compound 5～50%.
A kind of acrylic acid series pressure-sensitive adhesive tape preparation method of non-halogen fire-retardant agent, it is characterized in that may further comprise the steps: the mix that at first carries out the non-halogen fire-retardant agent, this incombustible agent comprises that following component and weight percent thereof are: organic non-halogen phosphoric acid ester 0～50%, inorganics 20～90%, nitrogenous compound 5～50%; The granularity of these three kinds of components is less than 100 μ m; Then by 1: (0.5～2) weight ratio is with the incombustible agent mixture and organic solvent is mixed into slurries and through ball mill grinding, add in the required fire-retardant acrylate pressure sensitive adhesive by the slurries that will sieve behind 120 mesh sieves and to stir, obtain containing the acrylic acid series pressure sensitive adhesive of non-halogen fire-retardant agent, the weight percent of this pressure sensitive adhesive is 100 parts of acrylate pressure sensitive adhesives, and the total addition level of non-halogen fire-retardant agent is 10～25 parts; The acrylic acid series pressure sensitive adhesive that at last this is contained the non-halogen fire-retardant agent is coated on and makes the acrylic acid series pressure-sensitive adhesive tape on the base material.
The present invention, a kind of acrylic acid series pressure-sensitive adhesive tape, makes it compared with prior art owing to adopted above-mentioned technical scheme with non-halogen fire-retardant agent and preparation method thereof, has tangible advantage and positively effect.
The non-halogen fire-retardant agent that component among the present invention and preparation method thereof obtains, owing to do not contain red phosphorus, therefore can make light acrylic pressure sensitive amine goods, in pressure sensitive adhesive, add an amount of fire retardant, not only can reach UL94 testing vertical flammability method VTM-0 grade, and not influence the adhesiveproperties and the electrical property of sealing tape.
Embodiment
The present invention, a kind of acrylic acid series pressure-sensitive adhesive tape non-halogen fire-retardant agent, this incombustible agent comprises following component and weight percent thereof: organic non-halogen phosphoric acid ester 0～50%, inorganics 20～90%, nitrogenous compound 5～50%; Component that this incombustible agent is preferable and weight percent thereof are: organic non-halogen phosphoric acid ester 0～30%, inorganics 50～90%, nitrogenous compound 5～30%.
Use in the non-halogen fire-retardant agent, wherein at above-mentioned acrylic acid series pressure-sensitive adhesive tape:
Described organic non-halogen phosphoric acid ester is selected from one or more in dimethyl methyl phosphonate, diethyl ethylphosphate, annular phosphonate DMPP, tributyl phosphate, trioctylphosphine phosphoric acid ester, trimethylphenyl phosphoric acid ester, tolyl diphenyl phosphoester, three (xylyl) phosphoric acid ester, phenylbenzene isooctyl phosphoric acid ester, propyloxy phenyl phenyl phosphate ester, phenyl diisooctyl phosphorous acid ester, triphenylphosphate, triphenyl phosphite, the tritolyl phosphate;
Described inorganics is selected from one or more in magnesium hydroxide, aluminium hydroxide, brucite, magnesiumcarbonate, antimonous oxide, boron trioxide, ammonium borate, zinc borate, the boric acid;
Described nitrogenous compound is selected from one or more in melamine, cyanuric acid, melamine cyanurate, polyphosphoric acid melamine, ammonium polyphosphate, Dyhard RU 100, benzo trimeric cyanamide, melamine resin, the urea;
The granularity of described organic non-halogen phosphoric acid ester, inorganics, three kinds of components of nitrogenous compound is less than 100 μ m.
The present invention, a kind of acrylic acid series pressure-sensitive adhesive tape preparation method of non-halogen fire-retardant agent is characterized in may further comprise the steps:
At first carry out the mix of non-halogen fire-retardant agent, this incombustible agent comprises that following component and weight percent thereof are: organic non-halogen phosphoric acid ester 0～50%, inorganics 20～90%, nitrogenous compound 5～50%; The granularity of these three kinds of components is less than 100 μ m; Then by 1: (0.5～2) weight ratio is with the incombustible agent mixture and organic solvent is mixed into slurries and through ball mill grinding, add in the required fire-retardant acrylate pressure sensitive adhesive by the slurries that will sieve behind 120 mesh sieves and to stir, obtain containing the acrylic acid series pressure sensitive adhesive of non-halogen fire-retardant agent, the weight percent of this pressure sensitive adhesive is 100 parts of acrylate pressure sensitive adhesives, and the total addition level of non-halogen fire-retardant agent is 10～25 parts; The acrylic acid series pressure sensitive adhesive that at last this is contained the non-halogen fire-retardant agent is coated on and makes the acrylic acid series pressure-sensitive adhesive tape on the base material.
In the above-mentioned preparation method of a kind of acrylic acid series pressure-sensitive adhesive tape with the non-halogen fire-retardant agent, wherein,
Described acrylic acid series pressure sensitive adhesive is the solvent-borne type pressure-sensitive adhesive;
Described base material is selected from a kind of in dry goods, plastics film class, porous plastics, paper tape and the tinsel;
Described dry goods comprises cotton, synthetic fiber cloth, woven fiber glass and non-woven fabrics, described plastics film class comprises soft and semi-rigid polyvinyl chloride, polyethylene, polypropylene, polyester, polyamide elastomer, EEA, described paper tape comprises flaxen fiber paper, kraft paper, goffered paper, glass transparent paper, and described tinsel comprises aluminium foil, Copper Foil.
The present invention, a kind of acrylic acid series pressure-sensitive adhesive tape preparation method of non-halogen fire-retardant agent, further comprising the steps of:
Described inorganics can adopt coupling agent and/or tensio-active agent that it is handled;
Described coupling agent and/or tensio-active agent are selected from one or more in silane coupling agent, titanate coupling agent, aluminate coupling agent, nonionogenic tenside, cats product, the fluorochemical surfactant;
Relative 100 parts of (wt) acrylate pressure sensitive adhesives, in the acrylate pressure sensitive adhesive halogen-free flame retardants of the present invention, the total addition level of organic non-halogen phosphoric acid ester, inorganics, nitrogenous compound is 10～25wt%, total addition level is 15～20wt% preferably.The fire retardant addition is crossed the major general influences flame retardant effect, the excessive adhesiveproperties variation that then can make sealing tape of fire retardant addition.The coat-thickness of fire-retardant pressure sensitive adhesive be 0.02mm to 0.04mm, when this can guarantee the existing certain flame retardancy of fire-retardant pressure-sensitive adhesive tape, can also lessly influence the adhesiveproperties and the electrical property of Pressuresensitive Tape.
Constituent of the present invention can be allocated additives such as copper(greening)inhibitor, tackifier, tinting material and filler into according to actual needs.
The invention will be further described below in conjunction with specific embodiment and comparative example, but therefore protection scope of the present invention is not subjected to the restriction of embodiment.
Embodiment
Mix by 15 parts of fire retardants described in each example of table 1, by 1: 1 weight ratio flame-retardant mixture and ethyl acetate are mixed into slurries, and through ball mill grinding after 2～4 hours, behind 120 mesh sieves, magnificent 97 glue (the solvent-type acrylic tackiness agent in homemade Asia that the slurries that sieve is added 85 parts, solid content is 45%) in, the flame-proof acrylic tackiness agent that viscosity is about 2000cp obtained after stirring.
Table 1
| Melamine cyanurate | 0.75 | 1.5 | 4.5 | 4 | 4 | ||||||
| Aluminium hydroxide | 6.0 | 8.9 | 3.5 | 8.25 | 6 | 3.5 | 6 | ||||
| Zinc borate | 13.5 | 13.5 | 2 | 3 | |||||||
| Boric acid | 4 | ||||||||||
| Dimethyl methyl phosphonate | 4.5 | 6 | 4 | ||||||||
| Tritolyl phosphate | 0.75 | - | 0 | 7.5 | 4.5 | 1.5 | |||||
| Three (2,3-two chloropropyls) phosphoric acid ester | 7 | 10 | 8 | ||||||||
| Sb2O3 | 5 | 3 |
Then this flame-proof acrylic pressure-sensitive adhesive evenly is coated in polyester film (50 μ m are thick), institute's rubberised layer thickness is 0.02mm, and oven dry back reel cuts off and obtains fire-retardant pressure-sensitive adhesive tape.
Performance evaluation:
For comparing the performance of flame-proof acrylic series pressure-sensitive adhesive tape, adopt following testing method such as UL94 testing vertical flammability, 180 ° of stripping strengths (claiming clinging power again), insulation paste adhesive tape power frequency proof voltage and voltage breakdown, adhesive tape disruptive strength to be estimated.
UL94 testing vertical flammability: carry out the VTM test by UL94 " the plastic material inflammability test of equipment and device component " standard.Be divided into VTM-0, VTM-1, VTM-2 Three Estate.
180 ° of peeling strength tests of pressure-sensitive adhesive tape: undertaken by GB/T 2792-1998 standard.
With 20mm wide * the long sealing tape sample of 200mm is bonded on the PE test board, comes the rollback pressure three times on sample with 2 kilograms pressure rollers.Place after 30 minutes, the 180 ° of directions in 23 ℃ of lower edges are peeled off with 300mm/min speed, measure stripping strength.
Insulation paste adhesive tape disruptive strength testing experiment: the sample of getting gluing bandwidth 12mm, long 300mm is tested by the GB7752-87 standard.
Insulation paste adhesive tape power frequency proof voltage and breakdown voltage test: the sample of getting gluing bandwidth 12mm, long 300mm is tested by GB/T 14517-93 standard.
The results are shown in Table 2 by above-mentioned testing method gained.
Table 2
| Numbering | Embodiment | Comparative example | |||||||||
| 1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 | 9 | 10 | 11 | |
| Base material | PET | PET | PET | PET | PET | PET | PET | PET | PET | PET | PET |
| UL94 | VT M-0 | VT M-0 | VT M-0 | VT M-0 | VT M-0 | VT M-0 | VT M-0 | VT M-0 | VT M-0 | VT M-1 | VT M-1 |
| Stripping strength (N/m) | 562 | 563 | 558 | 568 | 580 | 565 | 580 | 560 | 560 | 568 | 575 |
| Disruptive strength/V/m | 1.7 | 6.6 | 6.5 | 6.7 | 6.8 | 6.9 | 6.7 | 6.5 | 6.7 | 6.9 | 6.5 |
| Voltage breakdown/V | 6400 | 6400 | 6500 | 6400 | 6500 | 6500 | 6400 | 6400 | 6300 | 6200 | 6200 |
| Withstand voltage KV/15 second | 4.3 | 4.2 | 4.4 | 4.3 | 4.4 | 4.4 | 4.3 | 4.6 | 4.5 | 4.1 | 4.1 |
Claims (10)
1. acrylic acid series pressure-sensitive adhesive tape non-halogen fire-retardant agent, it is characterized in that: this incombustible agent comprises following component and weight percent thereof:
Organic non-halogen phosphoric acid ester 0～50%,
Inorganics 20～90%,
Nitrogenous compound 5～50%.
2. acrylic acid series pressure-sensitive adhesive tape non-halogen fire-retardant agent as claimed in claim 1, it is characterized in that: this incombustible agent comprises following component and weight percent thereof:
Organic non-halogen phosphoric acid ester 0～30%,
Inorganics 50～90%,
Nitrogenous compound 5～30%.
3. acrylic acid series pressure-sensitive adhesive tape non-halogen fire-retardant agent as claimed in claim 1 or 2 is characterized in that: described organic non-halogen phosphoric acid ester is selected from one or more in dimethyl methyl phosphonate, diethyl ethylphosphate, annular phosphonate DMPP, tributyl phosphate, trioctylphosphine phosphoric acid ester, trimethylphenyl phosphoric acid ester, tolyl diphenyl phosphoester, three (xylyl) phosphoric acid ester, phenylbenzene isooctyl phosphoric acid ester, propyloxy phenyl phenyl phosphate ester, phenyl diisooctyl phosphorous acid ester, triphenylphosphate, triphenyl phosphite, the tritolyl phosphate.
4. acrylic acid series pressure-sensitive adhesive tape non-halogen fire-retardant agent as claimed in claim 1 or 2, it is characterized in that: described inorganics is selected from one or more in magnesium hydroxide, aluminium hydroxide, brucite, magnesiumcarbonate, antimonous oxide, boron trioxide, ammonium borate, zinc borate, the boric acid.
5. acrylic acid series pressure-sensitive adhesive tape non-halogen fire-retardant agent as claimed in claim 1 or 2 is characterized in that: described nitrogenous compound is selected from one or more in melamine, cyanuric acid, melamine cyanurate, polyphosphoric acid melamine, ammonium polyphosphate, Dyhard RU 100, benzo trimeric cyanamide, melamine resin, the urea.
6. acrylic acid series pressure-sensitive adhesive tape non-halogen fire-retardant agent as claimed in claim 1 or 2 is characterized in that: the granularity of described three kinds of components is less than 100 μ m.
7. an acrylic acid series pressure-sensitive adhesive tape is with the preparation method of non-halogen fire-retardant agent, it is characterized in that may further comprise the steps: the mix that at first carries out the non-halogen fire-retardant agent, this incombustible agent comprises that following component and weight percent thereof are: organic non-halogen phosphoric acid ester 0～50%, inorganics 20～90%, nitrogenous compound 5～50%; The granularity of these three kinds of components is less than 100 μ m; Then by 1: (0.5～2) weight ratio is with the incombustible agent mixture and organic solvent is mixed into slurries and through ball mill grinding, add in the required fire-retardant acrylate pressure sensitive adhesive by the slurries that will sieve behind 120 mesh sieves and to stir, obtain containing the acrylic acid series pressure sensitive adhesive of non-halogen fire-retardant agent, the weight percent of this pressure sensitive adhesive is 100 parts of acrylate pressure sensitive adhesives, and the total addition level of non-halogen fire-retardant agent is 10～25 parts; The acrylic acid series pressure sensitive adhesive that at last this is contained the non-halogen fire-retardant agent is coated on and makes the acrylic acid series pressure-sensitive adhesive tape on the base material.
8. a kind of acrylic acid series pressure-sensitive adhesive tape as claimed in claim 7 preparation method of non-halogen fire-retardant agent, it is characterized in that: described acrylic acid series pressure sensitive adhesive is the solvent-borne type pressure-sensitive adhesive.
9. a kind of acrylic acid series pressure-sensitive adhesive tape as claimed in claim 7 is characterized in that with the preparation method of non-halogen fire-retardant agent: described base material is selected from a kind of in dry goods, plastics film class, porous plastics, paper tape and the tinsel.
10. a kind of acrylic acid series pressure-sensitive adhesive tape as claimed in claim 9 preparation method of non-halogen fire-retardant agent, it is characterized in that: described dry goods comprises cotton, synthetic fiber cloth, woven fiber glass and non-woven fabrics, described plastics film class comprises soft and semi-rigid polyvinyl chloride, polyethylene, polypropylene, polyester, polyamide elastomer, EEA, described paper tape comprises flaxen fiber paper, kraft paper, goffered paper, glass transparent paper, and described tinsel comprises aluminium foil, Copper Foil.
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