CN103743889A - Kit for rapidly detecting hydrocarbons plasticizer in silicone sealant and application thereof - Google Patents

Kit for rapidly detecting hydrocarbons plasticizer in silicone sealant and application thereof Download PDF

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Publication number
CN103743889A
CN103743889A CN201310727179.6A CN201310727179A CN103743889A CN 103743889 A CN103743889 A CN 103743889A CN 201310727179 A CN201310727179 A CN 201310727179A CN 103743889 A CN103743889 A CN 103743889A
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test paper
butyl rubber
paper
box body
silicone sealant
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CN103743889B (en
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齐文
许嘉龙
郑怡
敖光智
张轶楠
戚丁文
耿彦威
刘泽华
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Liaoning Institute Of Product Quality Supervision & Inspection
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Abstract

The invention relates to a kit for rapidly detecting a hydrocarbons plasticizer in a silicone sealant and an application thereof. The kit comprises a box body, butyl rubber test paper, a test paper fixing device, testing paper, a pressing module and a box cover, wherein the box body is a through cavity with unsealed two sides; the test paper fixing device is arranged outside the box body; the butyl rubber test paper is flatly fixedly arranged at the bottom of the box body by the test paper fixing device; an ungummed face of the test paper faces to the inner part of the box body; and a gumming face faces to the test paper fixing device and the box cover covers. The testing paper and the pressing module are arranged between the box cover and the test paper fixing device; and the butyl rubber test paper is composed of butyl rubber and a supporting material. In the detection process, a silicone sealant sample to be detected is injected to the box body of the kit filled with the butyl rubber test paper so that the sample and the ungummed face of the test paper are sufficiently contacted to be tested. The disposable kit prepared by the invention can be used for rapidly detecting the hydrocarbons plasticizer in the uncured silicone sealant; and the method is simple and can be used for rapidly judging whether the uncured silicone sealant contains the hydrocarbons plasticizer or not within two hours.

Description

Kit and application thereof for hydrocarbon plasticizer in fast detecting silicone sealant
Technical field
The present invention relates to a kind of kit for silicone sealant hydrocarbon plasticizer fast detecting and its preparation method and application, belong to building sealant detection technique field.
Background technology
Silicone sealant, as double glazing Yong Er road fluid sealant, structure sealant and filleting weather proofing sealant, has been widely used in full implied or half concealed frame glass curtain wall at present, and the quality of its performance is directly connected to the security performance of glass curtain wall entirety.In recent years, because silicone sealant market competition is day by day fierce, the prices of raw and semifnished materials sharp rise, part silicone adhesive manufacturing enterprise starts to adopt the alternative organopolysiloxanes such as the cheap hydrocarbon plasticizer of White Mineral Oil, whiteruss, causes having occurred on market that a class mixes the silicone sealant inferior of hydrocarbon ils.Along with increasing and the increase of Years Of Service of glass curtain wall use amount, silicone sealant inferior also manifests day by day on the impact of glass curtain wall system.Some fluid sealants start to occur the phenomenons such as efflorescence, cracking, some even cause that hollow glass unit part oil impregnate lost efficacy, there is the phenomenon that glass is shed tears, this not only has influence on the attractive in appearance of buildings, making to build sealing property declines, more have a strong impact on the serviceable life of glass curtain wall system, threatened the people's lives and property safety.
At present, although the domestic existing correlative study for harmful plastifier detection method in silicone sealant, the detection method of reporting is time-consuming, effort not only, and mainly depends on laboratory testing equipment, cannot realize field quick detection.Patent CN101887014A discloses a kind of authentication method of white oil-doped silicone sealant.The method adopts organic solvent to carry out swelling or extracting to curing silicone sealant sample, adopts infra-red sepectrometry to qualitatively judge in silicone sealant whether contain white oil composition, then measures the white oil content in silicone sealant by thermal weight loss method.Although the method provides a kind of relatively accurate white oil authentication method, but the method is the check based on silicone sealant after solidifying mainly, swelling or extractive process is loaded down with trivial details, test period long (sample curing time needs more than 14 days), and depend on laboratory testing equipment, cannot realize field quick detection.In addition,, after Zhou Fuwei etc. have proposed that silicone sealant sample is dried to 2 hours under 250 ℃ of conditions, the method for measuring the weightless quality of sample detects white oil component in silicone sealant sample.Although the method has obviously shortened detection time, its testing process still needs to rely on laboratory condition, cannot realize field quick detection.
Summary of the invention
The present invention aims to provide hydrocarbon plasticizer kit and application thereof in a kind of fast detecting silicone sealant, for judging whether silicone sealant for building contains the detection technique of excessive hydrocarbon plasticizer fast.This kit, comprises box body (1), butyl rubber test paper (2), test paper stationary installation (3), test paper (4), by die block (5) and lid (6).Above-mentioned box body (1) is the cavity of both sides open-ended, the outer test paper stationary installation (3) that is provided with of box body (1), butyl rubber test paper (2) is entirely fixed on the bottom of box body (1) by test paper stationary installation (3), wherein the back-adhesive surface of test paper (8) is towards box body inside; Coated face (7) is towards test paper stationary installation (3), and adds a cover lid (6).Between above-mentioned lid (6) and test paper stationary installation (3), be provided with test paper (4) and by die block (5).
The butyl rubber test paper that in the present invention, kit adopts is comprised of butyl rubber and propping material, its preparation technology is by butyl rubber melt or solution, through rolling process, casting, scrape one or more mixed methods in embrane method and spraying process, be coated on propping material surface, it through cooling or dry aftershaping thickness, is the even butyl rubber film test paper of 3 μ m~2000 μ m, a side that wherein scribbles butyl rubber on propping material is coated face, and its dorsal part is back-adhesive surface.
Above-mentioned butyl rubber is butyl rubber, hot melt butyl rubber and the potpourri that contains butyl rubber composition; Above-mentioned propping material is filter paper, chromatographic paper, industrial oil-Absorbing Sheets, face cleaning oil-absorbing paper, kraft capacitor paper, wrapping paper, liquid chromatography paper, rice paper, lens paper, gauze, the nonwoven fabrics of thickness 2 μ m~500 μ m or porous or the Web materials with the organic and inorganic and metal of supporting role.
Its concrete preparation process is as follows:
(1) take butyl rubber, by butyl rubber heating and melting or be dissolved in suitable solvent, form the butyl rubber solution that butyl rubber melt or massfraction are 1%~60%;
(2) one or more mixed methods of adopt rolling process, casting, scraping in embrane method and spraying process suppress, pour into a mould, apply or spray butyl rubber melt or solution one or many in propping material surface, form the body paper that is covered with butyl rubber melt or solution;
(3) to being covered with the body paper of butyl rubber melt or solution, carry out coolingly or dry, final molding thickness is the even butyl rubber film test paper of 3 μ m~2000 μ m.
In the present invention, for dissolving the suitable solvent of butyl rubber, be C 1-C 32liquid alkane, naphthenic hydrocarbon, alkene, halogenated alkane, and benzene,toluene,xylene, styrene, whiteruss, white oil, mineral oil, sherwood oil, acetone, N, the mixed solvent of one or more solvents in dinethylformamide, DMA, 1-METHYLPYRROLIDONE or tetrahydrofuran.
The application process of kit of the present invention is: butyl rubber test paper is entirely fixed on to box body bottom by test paper stationary installation, make its back-adhesive surface towards box body inside, coated face is towards test paper stationary installation, and add a cover lid in box body bottom, silicone sealant sample to be measured is injected into box body inside by box body top, testing sample is fully contacted with butyl rubber test paper back-adhesive surface, after standing 2 hours, take off bottom lid, test paper is placed in to butyl rubber test paper coated face, and will be placed in test paper surface by die block, lid is covered again, then take out and press die block, test paper is taken off gently from butyl rubber test paper surface, whether observe has butyl rubber adhesion thing (9) to be as shown in Figure 3 transferred to test paper surface from test paper surface, if have butyl rubber adhesion thing on test paper surface, illustrate in silicone sealant sample and contain hydrocarbon plasticizer.
Beneficial effect of the present invention and feature: can directly for uncured sealant specimen, detect, adopt the kit of gained of the present invention within 2 hours, to judge fast and in uncured silicone fluid sealant, whether contain excessive hydro carbons plasticiser (as: white oil, whiteruss etc.), with respect to the detection technique of organic hydrocarbon plasticiser in existing silicone sealant, save the curing time of silicone sealant, greatly improved detection efficiency.And gained kit method of operating of the present invention is simple, is convenient for carrying, detect and do not rely on laboratory equipment, be applicable to Site Detection.
Accompanying drawing explanation
Fig. 1 is the structural representation of kit in the present invention.
Fig. 2 is the structural representation of butyl rubber test paper in the present invention.
Fig. 3 is kit testing result schematic diagram in actual applications in the present invention.
Shown in figure: 1, box body; 2, butyl rubber test paper; 3, test paper stationary installation; 4, test paper; 5, press die block; 6, lid; 7, coated face; 8, back-adhesive surface; 9, butyl rubber adhesion thing.
Embodiment
Embodiment 1
See figures.1.and.2, hydrocarbon plasticizer kit in fast detecting silicone sealant, this kit, comprises box body 1, butyl rubber test paper 2, test paper stationary installation 3, test paper 4, by die block 5 and lid 6.Above-mentioned box body 1 is the cavity of both sides open-ended, and box body 1 is outer is provided with test paper stationary installation 3, and butyl rubber test paper 2 is entirely fixed on the bottom of box body 1 by test paper stationary installation 3, and wherein the back-adhesive surface 8 of test paper is towards box body inside; Coated face 7 is towards test paper stationary installation 3, and adds a cover lid 6.Between above-mentioned lid 6 and test paper stationary installation 3, be provided with test paper 4 and by die block 5.The top inner plane of lid 6 is apart from least 5mm distance of box body base plane of fixing butyl rubber test paper 2.
Above-mentioned test paper 4 is clean industrial oil-Absorbing Sheets, face cleaning oil-absorbing paper, kraft capacitor paper, wrapping paper, liquid chromatography paper, rice paper or lens paper of surface; Above-mentioned by die block 5 for thering is flat surface, and thickness is not less than the porous elastic materials such as the sponge, Ethylene Propylene Terpolymer bipeltate, foamed silica gel, polyurathamc, polyethylene foamed ethyl acetate of 6mm.
Embodiment 2
According to the described method of embodiment 1, prepare and assemble hydrocarbon plasticizer kit in fast detecting silicone sealant.
The preparation of butyl rubber test paper: get massfraction and be butyl rubber/triclene solution of 20%, the filter paper that is 25 μ m by thickness is laid in the glass pane surface of surfacing fixing.Adopt at ambient temperature blade applicator that butyl rubber/triclene solution of 20% is coated on to filter paper surface, acquisition one side is covered with the body paper of 20% butyl rubber/triclene solution.This body paper is positioned over to 24h under natural ventilation condition, after naturally drying, obtains even butyl rubber film test paper.
Butyl rubber test paper is entirely fixed on to box body bottom by test paper stationary installation, and the back-adhesive surface of test paper is towards box body inside, and adds a cover lid, and lid top inner plane is 5mm apart from the box body base plane distance of having fixed test paper.Uncured silicone sealant sample A to be measured is injected into box body inside by box body top, sample butyl rubber test paper back-adhesive surface is fully contacted, after standing 2 hours, take off bottom lid, the industrial oil-Absorbing Sheets that surface is clean are placed in butyl rubber test paper coated face, and the Ethylene Propylene Terpolymer foam that is 6mm by thickness is placed in another surface of industrial oil-Absorbing Sheets, lid is covered again, then take off, take out Ethylene Propylene Terpolymer foam, industrial oil-Absorbing Sheets are taken off gently from a side on butyl rubber test paper surface, observe oil-Absorbing Sheets and butyl rubber test paper surface in contact, define butyl rubber adhesion thing and be transferred to oil-Absorbing Sheets surface from butyl rubber test paper surface, as shown in Figure 3, illustrate in this silicone sealant sample A and contain hydrocarbon plasticizer.
After adopting Oven Method that this silicone sealant sample A is dried to 2 hours in the air dry oven of 250 ℃ of conditions, measuring the weightless quality of sample is 12%, illustrates in this silicone sealant sample A and contains hydrocarbon plasticizer.
Embodiment 3
According to the described method of embodiment 1, prepare and assemble hydrocarbon plasticizer kit in fast detecting silicone sealant.
The preparation of butyl rubber test paper: get massfraction and be butyl rubber/triclene solution of 20%, the filter paper that is 25 μ m by thickness is laid in the glass pane surface of surfacing fixing.Adopt at ambient temperature blade applicator that butyl rubber/triclene solution of 20% is coated on to filter paper surface, acquisition one side is covered with the body paper of 20% butyl rubber/triclene solution.This body paper is positioned over to 24h under natural ventilation condition, after naturally drying, obtains even butyl rubber film test paper.
This butyl rubber test paper is entirely fixed on to box body bottom by test paper stationary installation, and the back-adhesive surface of test paper is towards box body inside, and adds a cover lid, and lid top inner plane is 5mm apart from the box body base plane distance of having fixed test paper.To determine that the silicone sealant sample B containing white oil is not injected into box body inside by box body top, sample butyl rubber test paper back-adhesive surface is fully contacted, after standing 2 hours, take off bottom lid, the face cleaning oil-absorbing paper that surface is clean is placed in butyl rubber test paper coated face, and the Ethylene Propylene Terpolymer foam that is 6mm by thickness is placed in another surface of face cleaning oil-absorbing paper, lid is covered again, then take off, take out Ethylene Propylene Terpolymer foam, face cleaning oil-absorbing paper is taken off gently from a side on butyl rubber test paper surface, observe oil-Absorbing Sheets and butyl rubber test paper surface in contact, determining does not have butyl rubber adhesion thing to be as shown in Figure 3 transferred to oil-Absorbing Sheets surface from butyl rubber test paper surface, illustrate in this silicone sealant sample B and do not contain hydrocarbon plasticizer.
Embodiment 4
According to the described method of embodiment 1, prepare and assemble hydrocarbon plasticizer kit in fast detecting silicone sealant.
The preparation of butyl rubber test paper: take 50g butyl hot-melt glue, be heated to melting under 160 ℃ of conditions.The industrial oil-Absorbing Sheets that are 25 μ m by thickness are laid in the smooth surface of steel plate of surfacing fixing.Adopt blade applicator that the butyl hot-melt glue of melting is evenly coated on to industrial oil-Absorbing Sheets surface, acquisition one side is covered with the industrial oil-Absorbing Sheets of butyl hot-melt glue.These oil-Absorbing Sheets are naturally cooled to room temperature, obtain even butyl rubber film test paper.
This butyl rubber test paper is entirely fixed on to box body bottom by test paper stationary installation, and the back-adhesive surface of test paper is towards box body inside, and adds a cover lid, and lid top inner plane is 5mm apart from the box body base plane distance of having fixed test paper.Silicone sealant sample C to be measured is injected into box body inside by box body top, sample butyl rubber test paper back-adhesive surface is fully contacted, after standing 2 hours, take off bottom lid, the face cleaning oil-absorbing paper that surface is clean is placed in butyl rubber test paper coated face, and the sponge that is 7mm by thickness is placed in another surface of face cleaning oil-absorbing paper, lid is covered again, then take off, take out sponge, face cleaning oil-absorbing paper is taken off gently from a side on butyl rubber test paper surface, observe oil-Absorbing Sheets and butyl rubber test paper surface in contact, found that butyl rubber adhesion thing is transferred to oil-Absorbing Sheets surface from butyl rubber test paper surface, as shown in Figure 3, illustrate in this silicone sealant sample C and contain hydrocarbon plasticizer.
Embodiment 5
According to the described method of embodiment 1, prepare and assemble hydrocarbon plasticizer kit in fast detecting silicone sealant.
The preparation of butyl rubber test paper: get massfraction and be butyl hot-melt glue/(methylene chloride and DMF) solution (mixed solvent mass ratio is 2:1) of 10%.The face cleaning oil-absorbing paper that is 20 μ m by thickness is laid in the glass pane surface of surfacing and fixes.The mould that is 5cm × 5cm by inside casing area is placed in face cleaning oil-absorbing paper central authorities, is poured into therein butyl hot-melt glue/(methylene chloride and DMF) solution of 10% of 2ml, makes its natural levelling.These oil-Absorbing Sheets are positioned under natural ventilation condition after 24h, put into the dry 24h of baking oven of 60 ℃, obtain uniform butyl rubber film test paper.
This butyl rubber test paper is entirely fixed on to box body bottom by test paper stationary installation, and the back-adhesive surface of test paper is towards box body inside, and adds a cover lid, and lid top inner plane is 8mm apart from the box body base plane distance of having fixed test paper.Silicone sealant sample D to be measured is injected into box body inside by box body top, sample butyl rubber test paper back-adhesive surface is fully contacted, after standing 2 hours, take off bottom lid, the paper of showing on trial that surface is clean is placed in butyl rubber test paper coated face, and the sponge that is 10mm by thickness is placed in another surface of paper of showing on trial, lid is covered again, then take off, take out sponge, by showing on trial, paper is taken off gently from a side on butyl rubber test paper surface, observation show on trial paper and butyl rubber test paper surface in contact, found that butyl rubber adhesion thing is as shown in Figure 3 transferred to from butyl rubber test paper surface the paper surface of showing on trial, illustrate in this silicone sealant sample D and contain hydrocarbon plasticizer.
The foregoing is only preferred embodiment of the present invention, be not limited to the present invention, all within the present invention spirit and principle, any modification of making, be equal to replacement, improvement etc., within all should being included in protection scope of the present invention.

Claims (7)

1. hydrocarbon plasticizer kit in a fast detecting silicone sealant, it is characterized in that this kit, comprise box body, butyl rubber test paper, test paper stationary installation, test paper, by die block and lid, above-mentioned box body is the cavity of both sides open-ended, box body is provided with test paper stationary installation outward, butyl rubber test paper is entirely fixed on the bottom of box body by test paper stationary installation, wherein the back-adhesive surface of test paper is towards box body inside; Coated face is towards test paper stationary installation, and adds a cover lid, is provided with test paper and by die block between above-mentioned lid and test paper stationary installation.
2. hydrocarbon plasticizer kit in fast detecting silicone sealant as claimed in claim 1, is characterized in that: the top inner plane of described lid is apart from least 5mm distance of box body base plane of fixing butyl rubber test paper.
3. hydrocarbon plasticizer kit in fast detecting silicone sealant as claimed in claim 1, is characterized in that: described test paper is clean industrial oil-Absorbing Sheets, face cleaning oil-absorbing paper, kraft capacitor paper, wrapping paper, liquid chromatography paper, rice paper or lens paper of surface.
4. hydrocarbon plasticizer kit in fast detecting silicone sealant as claimed in claim 1, it is characterized in that: above-mentioned by die block for thering is flat surface, and thickness is not less than sponge, Ethylene Propylene Terpolymer bipeltate, foamed silica gel, the polyurathamc of 6mm, the porous elastic material of polyethylene foamed ethyl acetate.
5. hydrocarbon plasticizer kit in fast detecting silicone sealant as claimed in claim 1, it is characterized in that: described butyl rubber test paper is comprised of butyl rubber and propping material, its preparation method is by butyl rubber melt or solution, through rolling process, casting, scrape one or more mixed methods in embrane method and spraying process, be coated on propping material surface, it through cooling or dry aftershaping thickness, is the even butyl rubber film test paper of 3 μ m~2000 μ m, a side that wherein scribbles butyl rubber on propping material is coated face, and its dorsal part is back-adhesive surface.
6. hydrocarbon plasticizer kit in fast detecting silicone sealant as claimed in claim 5, is characterized in that: in described butyl rubber test paper preparation process, butyl rubber is butyl rubber, hot melt butyl rubber and the potpourri that contains butyl rubber composition; The thickness of described propping material is filter paper, chromatographic paper, industrial oil-Absorbing Sheets, face cleaning oil-absorbing paper, kraft capacitor paper, wrapping paper, liquid chromatography paper, rice paper, lens paper, gauze, the nonwoven fabrics of 2 μ m~500 μ m and porous or the Web materials with the organic and inorganic and metal of supporting role; Butyl rubber solution is for adopting C 1-C 32liquid alkane, naphthenic hydrocarbon, alkene, halogenated alkane, and benzene, toluene, styrene, whiteruss, white oil, mineral oil, sherwood oil, acetone, N, the butyl rubber solution that the massfraction of the mixed solvent preparation of one or more solvents in dinethylformamide, DMA, 1-METHYLPYRROLIDONE or tetrahydrofuran is 1%~60%.
7. the application of kit for hydrocarbon plasticizer in a fast detecting silicone sealant, it is characterized in that: butyl rubber test paper is entirely fixed on to box body bottom by test paper stationary installation, make its back-adhesive surface towards box body inside, coated face is towards test paper stationary installation, and add a cover lid in box body bottom, silicone sealant sample to be measured is injected into box body inside by box body top, testing sample butyl rubber test paper back-adhesive surface is fully contacted, after standing 2 hours, take off bottom lid, test paper is placed in to butyl rubber test paper coated face, and will press material and be placed in test paper surface, lid is covered again, then take off, material is pressed in taking-up, test paper is taken off gently from butyl rubber test paper surface, observations, result judgement: have butyl rubber adhesion thing to be transferred to test paper surface from test paper surface, illustrate in silicone sealant sample and contain hydrocarbon plasticizer.
CN201310727179.6A 2013-12-25 2013-12-25 Hydrocarbon plasticizer kit and application thereof in quick detection silicone sealant Active CN103743889B (en)

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CN107722305A (en) * 2017-10-17 2018-02-23 辽宁省产品质量监督检验院(辽宁省建筑材料监督检验院) A kind of standard butyl rubber solution
CN107796931A (en) * 2017-10-17 2018-03-13 辽宁省产品质量监督检验院(辽宁省建筑材料监督检验院) A kind of green test method of the silicone sealant of plasticizer containing alkane

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Publication number Priority date Publication date Assignee Title
CN107722305A (en) * 2017-10-17 2018-02-23 辽宁省产品质量监督检验院(辽宁省建筑材料监督检验院) A kind of standard butyl rubber solution
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CN107796931B (en) * 2017-10-17 2020-12-08 辽宁省产品质量监督检验院(辽宁省建筑材料监督检验院) Green detection method for silicone sealant containing alkane plasticizer

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