CN110315814A - Glass engagement plural layers, laminated glass and its manufacturing method including it - Google Patents
Glass engagement plural layers, laminated glass and its manufacturing method including it Download PDFInfo
- Publication number
- CN110315814A CN110315814A CN201810904547.2A CN201810904547A CN110315814A CN 110315814 A CN110315814 A CN 110315814A CN 201810904547 A CN201810904547 A CN 201810904547A CN 110315814 A CN110315814 A CN 110315814A
- Authority
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- China
- Prior art keywords
- layer
- glass
- plural layers
- engagement
- engaging force
- Prior art date
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- Granted
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- 239000011521 glass Substances 0.000 title claims abstract description 186
- 239000005340 laminated glass Substances 0.000 title claims description 36
- 238000004519 manufacturing process Methods 0.000 title description 6
- 239000004014 plasticizer Substances 0.000 claims abstract description 61
- 229920006324 polyoxymethylene Polymers 0.000 claims abstract description 53
- 229920002554 vinyl polymer Polymers 0.000 claims abstract description 51
- 239000011354 acetal resin Substances 0.000 claims abstract description 48
- DHKHKXVYLBGOIT-UHFFFAOYSA-N 1,1-Diethoxyethane Chemical compound CCOC(C)OCC DHKHKXVYLBGOIT-UHFFFAOYSA-N 0.000 claims abstract description 45
- 238000009832 plasma treatment Methods 0.000 claims description 56
- 238000012360 testing method Methods 0.000 claims description 51
- 239000000203 mixture Substances 0.000 claims description 49
- 238000004381 surface treatment Methods 0.000 claims description 32
- 238000002360 preparation method Methods 0.000 claims description 29
- 238000000034 method Methods 0.000 claims description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 20
- 238000001125 extrusion Methods 0.000 claims description 19
- 238000003475 lamination Methods 0.000 claims description 13
- 230000015572 biosynthetic process Effects 0.000 claims description 11
- 230000008569 process Effects 0.000 claims description 11
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 10
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 10
- 229920001807 Urea-formaldehyde Polymers 0.000 claims description 3
- ODGAOXROABLFNM-UHFFFAOYSA-N polynoxylin Chemical compound O=C.NC(N)=O ODGAOXROABLFNM-UHFFFAOYSA-N 0.000 claims description 3
- 125000000218 acetic acid group Chemical group C(C)(=O)* 0.000 claims 2
- 239000010410 layer Substances 0.000 abstract description 557
- 238000009413 insulation Methods 0.000 abstract description 30
- 230000007547 defect Effects 0.000 abstract description 21
- 239000011229 interlayer Substances 0.000 abstract description 20
- 238000013016 damping Methods 0.000 abstract description 11
- 229920005989 resin Polymers 0.000 description 44
- 239000011347 resin Substances 0.000 description 44
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 description 28
- 230000000052 comparative effect Effects 0.000 description 19
- 150000001299 aldehydes Chemical class 0.000 description 15
- 239000000654 additive Substances 0.000 description 14
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 13
- 239000001301 oxygen Substances 0.000 description 13
- 229910052760 oxygen Inorganic materials 0.000 description 13
- 230000000694 effects Effects 0.000 description 12
- ZIBGPFATKBEMQZ-UHFFFAOYSA-N triethylene glycol Chemical compound OCCOCCOCCO ZIBGPFATKBEMQZ-UHFFFAOYSA-N 0.000 description 12
- ZTQSAGDEMFDKMZ-UHFFFAOYSA-N Butyraldehyde Chemical compound CCCC=O ZTQSAGDEMFDKMZ-UHFFFAOYSA-N 0.000 description 11
- -1 poly- Vinyl acetal resin Chemical compound 0.000 description 10
- 238000012545 processing Methods 0.000 description 9
- OXQGTIUCKGYOAA-UHFFFAOYSA-N 2-Ethylbutanoic acid Chemical class CCC(CC)C(O)=O OXQGTIUCKGYOAA-UHFFFAOYSA-N 0.000 description 8
- 238000005259 measurement Methods 0.000 description 7
- 238000006116 polymerization reaction Methods 0.000 description 7
- 239000002250 absorbent Substances 0.000 description 6
- 230000002745 absorbent Effects 0.000 description 6
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 description 6
- 239000003963 antioxidant agent Substances 0.000 description 6
- 235000006708 antioxidants Nutrition 0.000 description 6
- 238000012797 qualification Methods 0.000 description 6
- 239000002344 surface layer Substances 0.000 description 6
- 150000001241 acetals Chemical class 0.000 description 5
- 125000002777 acetyl group Chemical group [H]C([H])([H])C(*)=O 0.000 description 5
- 230000006872 improvement Effects 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 238000002156 mixing Methods 0.000 description 5
- OBETXYAYXDNJHR-SSDOTTSWSA-M (2r)-2-ethylhexanoate Chemical compound CCCC[C@@H](CC)C([O-])=O OBETXYAYXDNJHR-SSDOTTSWSA-M 0.000 description 4
- PYGXAGIECVVIOZ-UHFFFAOYSA-N Dibutyl decanedioate Chemical compound CCCCOC(=O)CCCCCCCCC(=O)OCCCC PYGXAGIECVVIOZ-UHFFFAOYSA-N 0.000 description 4
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 4
- 229930182556 Polyacetal Natural products 0.000 description 4
- 230000000996 additive effect Effects 0.000 description 4
- OBETXYAYXDNJHR-UHFFFAOYSA-N alpha-ethylcaproic acid Natural products CCCCC(CC)C(O)=O OBETXYAYXDNJHR-UHFFFAOYSA-N 0.000 description 4
- 230000003078 antioxidant effect Effects 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 4
- 230000005611 electricity Effects 0.000 description 4
- 150000002148 esters Chemical class 0.000 description 4
- CATSNJVOTSVZJV-UHFFFAOYSA-N heptan-2-one Chemical compound CCCCCC(C)=O CATSNJVOTSVZJV-UHFFFAOYSA-N 0.000 description 4
- 238000003780 insertion Methods 0.000 description 4
- 230000037431 insertion Effects 0.000 description 4
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 4
- 238000002844 melting Methods 0.000 description 4
- 230000008018 melting Effects 0.000 description 4
- 229910000831 Steel Inorganic materials 0.000 description 3
- 239000012963 UV stabilizer Substances 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 239000005357 flat glass Substances 0.000 description 3
- 239000012760 heat stabilizer Substances 0.000 description 3
- 230000000704 physical effect Effects 0.000 description 3
- 239000010959 steel Substances 0.000 description 3
- UNNGUFMVYQJGTD-UHFFFAOYSA-N 2-Ethylbutanal Chemical compound CCC(CC)C=O UNNGUFMVYQJGTD-UHFFFAOYSA-N 0.000 description 2
- SSKNCQWPZQCABD-UHFFFAOYSA-N 2-[2-[2-(2-heptanoyloxyethoxy)ethoxy]ethoxy]ethyl heptanoate Chemical compound CCCCCCC(=O)OCCOCCOCCOCCOC(=O)CCCCCC SSKNCQWPZQCABD-UHFFFAOYSA-N 0.000 description 2
- KEOUIRVJRXECRC-UHFFFAOYSA-N 6-[2-(2-butoxyethoxy)ethoxy]-6-oxohexanoic acid Chemical compound CCCCOCCOCCOC(=O)CCCCC(O)=O KEOUIRVJRXECRC-UHFFFAOYSA-N 0.000 description 2
- AMIMRNSIRUDHCM-UHFFFAOYSA-N Isopropylaldehyde Chemical compound CC(C)C=O AMIMRNSIRUDHCM-UHFFFAOYSA-N 0.000 description 2
- 241000533950 Leucojum Species 0.000 description 2
- JKIJEFPNVSHHEI-UHFFFAOYSA-N Phenol, 2,4-bis(1,1-dimethylethyl)-, phosphite (3:1) Chemical compound CC(C)(C)C1=CC(C(C)(C)C)=CC=C1OP(OC=1C(=CC(=CC=1)C(C)(C)C)C(C)(C)C)OC1=CC=C(C(C)(C)C)C=C1C(C)(C)C JKIJEFPNVSHHEI-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 230000004913 activation Effects 0.000 description 2
- 235000011037 adipic acid Nutrition 0.000 description 2
- 239000001361 adipic acid Substances 0.000 description 2
- 150000001412 amines Chemical class 0.000 description 2
- 239000000470 constituent Substances 0.000 description 2
- 238000010276 construction Methods 0.000 description 2
- 150000002085 enols Chemical class 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 125000000524 functional group Chemical group 0.000 description 2
- JARKCYVAAOWBJS-UHFFFAOYSA-N hexanal Chemical compound CCCCCC=O JARKCYVAAOWBJS-UHFFFAOYSA-N 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 230000035699 permeability Effects 0.000 description 2
- SCVFZCLFOSHCOH-UHFFFAOYSA-M potassium acetate Chemical compound [K+].CC([O-])=O SCVFZCLFOSHCOH-UHFFFAOYSA-M 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- IYAZLDLPUNDVAG-UHFFFAOYSA-N 2-(benzotriazol-2-yl)-4-(2,4,4-trimethylpentan-2-yl)phenol Chemical compound CC(C)(C)CC(C)(C)C1=CC=C(O)C(N2N=C3C=CC=CC3=N2)=C1 IYAZLDLPUNDVAG-UHFFFAOYSA-N 0.000 description 1
- 229920002799 BoPET Polymers 0.000 description 1
- 239000004593 Epoxy Substances 0.000 description 1
- BGYHLZZASRKEJE-UHFFFAOYSA-N [3-[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxy]-2,2-bis[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxymethyl]propyl] 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoate Chemical compound CC(C)(C)C1=C(O)C(C(C)(C)C)=CC(CCC(=O)OCC(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)=C1 BGYHLZZASRKEJE-UHFFFAOYSA-N 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- OCWYEMOEOGEQAN-UHFFFAOYSA-N bumetrizole Chemical compound CC(C)(C)C1=CC(C)=CC(N2N=C3C=C(Cl)C=CC3=N2)=C1O OCWYEMOEOGEQAN-UHFFFAOYSA-N 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000007872 degassing Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000012634 fragment Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000002847 impedance measurement Methods 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 239000005001 laminate film Substances 0.000 description 1
- 238000010030 laminating Methods 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- UEGPKNKPLBYCNK-UHFFFAOYSA-L magnesium acetate Chemical compound [Mg+2].CC([O-])=O.CC([O-])=O UEGPKNKPLBYCNK-UHFFFAOYSA-L 0.000 description 1
- 229940069446 magnesium acetate Drugs 0.000 description 1
- 235000011285 magnesium acetate Nutrition 0.000 description 1
- 239000011654 magnesium acetate Substances 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000008301 phosphite esters Chemical class 0.000 description 1
- OJMIONKXNSYLSR-UHFFFAOYSA-N phosphorous acid Chemical class OP(O)O OJMIONKXNSYLSR-UHFFFAOYSA-N 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 235000011056 potassium acetate Nutrition 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 229920003002 synthetic resin Polymers 0.000 description 1
- 239000000057 synthetic resin Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B17/00—Layered products essentially comprising sheet glass, or glass, slag, or like fibres
- B32B17/06—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material
- B32B17/10—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin
- B32B17/10005—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing
- B32B17/1055—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing characterized by the resin layer, i.e. interlayer
- B32B17/10761—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing characterized by the resin layer, i.e. interlayer containing vinyl acetal
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B17/00—Layered products essentially comprising sheet glass, or glass, slag, or like fibres
- B32B17/06—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material
- B32B17/10—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin
- B32B17/10005—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing
- B32B17/10009—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing characterized by the number, the constitution or treatment of glass sheets
- B32B17/10036—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing characterized by the number, the constitution or treatment of glass sheets comprising two outer glass sheets
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B17/00—Layered products essentially comprising sheet glass, or glass, slag, or like fibres
- B32B17/06—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material
- B32B17/10—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin
- B32B17/10005—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing
- B32B17/1055—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing characterized by the resin layer, i.e. interlayer
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B17/00—Layered products essentially comprising sheet glass, or glass, slag, or like fibres
- B32B17/06—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material
- B32B17/10—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin
- B32B17/10005—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing
- B32B17/1055—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing characterized by the resin layer, i.e. interlayer
- B32B17/10605—Type of plasticiser
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B17/00—Layered products essentially comprising sheet glass, or glass, slag, or like fibres
- B32B17/06—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material
- B32B17/10—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin
- B32B17/10005—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing
- B32B17/10807—Making laminated safety glass or glazing; Apparatus therefor
- B32B17/10889—Making laminated safety glass or glazing; Apparatus therefor shaping the sheets, e.g. by using a mould
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B17/00—Layered products essentially comprising sheet glass, or glass, slag, or like fibres
- B32B17/06—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material
- B32B17/10—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin
- B32B17/10005—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing
- B32B17/10807—Making laminated safety glass or glazing; Apparatus therefor
- B32B17/10981—Pre-treatment of the layers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/18—Layered products comprising a layer of synthetic resin characterised by the use of special additives
- B32B27/22—Layered products comprising a layer of synthetic resin characterised by the use of special additives using plasticisers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/42—Layered products comprising a layer of synthetic resin comprising condensation resins of aldehydes, e.g. with phenols, ureas or melamines
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B3/00—Layered products comprising a layer with external or internal discontinuities or unevennesses, or a layer of non-planar shape; Layered products comprising a layer having particular features of form
- B32B3/02—Layered products comprising a layer with external or internal discontinuities or unevennesses, or a layer of non-planar shape; Layered products comprising a layer having particular features of form characterised by features of form at particular places, e.g. in edge regions
- B32B3/06—Layered products comprising a layer with external or internal discontinuities or unevennesses, or a layer of non-planar shape; Layered products comprising a layer having particular features of form characterised by features of form at particular places, e.g. in edge regions for securing layers together; for attaching the product to another member, e.g. to a support, or to another product, e.g. groove/tongue, interlocking
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2307/00—Properties of the layers or laminate
- B32B2307/10—Properties of the layers or laminate having particular acoustical properties
- B32B2307/102—Insulating
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2307/00—Properties of the layers or laminate
- B32B2307/50—Properties of the layers or laminate having particular mechanical properties
- B32B2307/558—Impact strength, toughness
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2310/00—Treatment by energy or chemical effects
- B32B2310/14—Corona, ionisation, electrical discharge, plasma treatment
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2315/00—Other materials containing non-metallic inorganic compounds not provided for in groups B32B2311/00 - B32B2313/04
- B32B2315/08—Glass
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2605/00—Vehicles
- B32B2605/003—Interior finishings
Landscapes
- Joining Of Glass To Other Materials (AREA)
Abstract
The present invention provides a kind of glass engagement plural layers etc., and the glass engagement plural layers include: first layer, includes the first polyvinyl acetal resin and the first plasticizer, the first layer with the first glass while directly connect；And the second layer, the one side of the second layer directly connects with the another side of the first layer, it and include the second polyvinyl acetal resin and the second plasticizer, thus, the glass engagement plural layers improve the inter-layer bonding force of plural layers while impact resistance, resistance to connectivity, sound damping etc. are maintained at certain level or more, and the difference between the engaging force at the interface between the interface between plural layers and glass and each layer of plural layers is reduced, thus minimizes the defect of such as frost flower phenomenon sound insulation intermediate coat.
Description
Technical field
The present invention relates to the glass engagement plural layers of reduction defect generation, including the glass engagement plural layers
Laminated glass and its manufacturing method (Multilayer Film For Laminating Glasses, Laminated Glasses
Comprising Of The Same,Manufacturing Method For The Same)。
Background technique
In general, the laminated glass being made of a pair of of glass panel and the film of synthetic resin being inserted between these panels is i.e.
Make its glass fragment when broken that will not disperse, therefore there is excellent safety, to be widely used in such as automobile road
The glass for vehicle window of vehicle and the window-glass of building.
This laminated glass is needed with sound insulation value.The sound insulation value indicates the loss that penetrates based on frequency, and
Sound insulation value is assessed through method of loss etc. by the frequency range assessment in 500Hz or more.But sound insulation value exists
There are many case where frequency field near 2000Hz significantly reduces.In order to minimize this phenomenon, it has been proposed that
Various measures, for example, the increase of the quality of laminated glass, multilaminated glass structure, the division of laminated glass area and interlayer
The improvement etc. of glass support structure.However, not only effect is not so good for these methods, but also the cost in business application, work
The unreasonable situation of property etc. is more, therefore, usually using three layers or more of plural layers as acoustic film application.
Although the existing multilayered structure polyacetals intermediate coat with sound insulation value has excellent sound insulation value, need
Compensate the durability of such as low interlayer engaging force.
Existing technical literature
Patent document
Patent document 0001: (grant date: 2015.02.06 " improves resistance to pass through to Korean granted patent the 10-1492971st
The Polyvinyl acetal film of the general character ")；
Patent document 0002: Korean Patent Publication bulletin the 10-2014-0138860th (publication date: 2014.12.04,
" defect inhibits sound insulation intermediate middle layer ").
Summary of the invention
Technical problem
The purpose of the present invention is to provide the glass of a kind of raising inter-layer bonding force and reduction acoustic film defect generation to connect
Share plural layers, laminated glass and its manufacturing method including the glass engagement plural layers.
Solution to problem
In order to reach purpose described above, the glass engagement of an embodiment according to the present invention can wrap with plural layers
Include: first layer includes the first polyvinyl acetal resin and the first plasticizer, the one side of the first layer and the one of the first glass
Face directly connects；And the second layer, the one side of the second layer directly connect with the another side of the first layer, and include second poly-
Vinyl acetal resin and the second plasticizer, wherein first glass and described first assessed by 180 degree peel test
The difference between the engaging force between engaging force and the first layer and the second layer between layer can be equal to or less than 7Kgf/
10mm。
Glass engagement plural layers according to another embodiment of the present invention may include: first layer, poly- comprising first
Vinyl acetal resin and the first plasticizer, the first layer with the first glass while directly connect；And the second layer,
The one side of the second layer directly connects with the another side of the first layer, and includes the second polyvinyl acetal resin and second
Plasticizer, wherein the one side of the first layer for the glass engagement plural layers assessed by 180 degree peel test with
Engaging force between the second layer can have the engaging force increase rate value equal to or more than 20%, the engaging force increase rate
Value expression is improved compared with the engaging force between the second layer with the one side of the first layer engaged without plasma treatment
The degree of engaging force.
Glass engagement plural layers according to still another embodiment of the invention may include: first layer, poly- comprising first
Vinyl acetal resin and the first plasticizer, the first layer with the first glass while directly connect；And the second layer,
The one side of the second layer directly connects with the another side of the first layer, and includes the second polyvinyl acetal resin and second
Plasticizer, wherein by engaging force between 180 degree peel test first glass assessed and the first layer and described
The difference of engaging force between first layer and the second layer can be equal to or less than 20%.
The second layer can contain more plasticizer compared with the first layer.
The hydroxy radical content of first polyvinyl acetal resin can be equal to or more than 30mol%, and acetyl content
2mol% can be less than.
After the glass engagement plural layers are placed 24 hours at 50 DEG C of temperature and 20% relative humidities,
It forms the hole 8mm and forms laminated glass, then, after being placed 24 hours in 85 DEG C of baking ovens, observe raw on the hole periphery
The size of long bubble, result can satisfy bubble with the condition of the 200% of hole range growth below.
Interface between the first layer and the second layer can be by described to connect with the second layer
One layer or with engage after the while carry out plasma treatment of the second layer that connects of the first layer made of.
The bonding force value between the first layer and the second layer assessed by 180 degree peel test can for 25 to
40Kgf/10mm。
The glass engagement plural layers may also include third layer, and the one side of the third layer and the second layer are direct
Connect and its another side directly connects with the second glass, and the third layer includes that third polyvinyl acetal resin and third increase
Mould agent.
Pass through the engaging force and described second between 180 degree peel test second glass assessed and the third layer
The difference between engaging force between layer and the third layer can be equal to or less than 7Kgf/10mm.
The one side of the third layer for the glass engagement plural layers assessed by 180 degree peel test with it is described
Connecing between the one side and the second layer of the third layer that the engaging force between the second layer can be engaged with without plasma treatment
Resultant force is compared and improves 20% or more.
The second layer can contain more plasticizer compared with the third layer.
The hydroxy radical content of the third polyvinyl acetal resin can be equal to or more than 30mol%, and acetyl content
2mol% can be less than.
Interface between the third layer and the second layer can be by described to connect with the third layer
Two layers or with engage after the while carry out plasma treatment of third layer that connects of the second layer made of.
Bonding force value between the second layer assessed by 180 degree peel test and the third layer can for 25 to
40Kgf/10mm。
The preparation method of plural layers according to still another embodiment of the invention includes: extrusion step, will be gathered comprising first
The first layer formation of vinyl acetal resin and the first plasticizer puts into the first extruder with composition, will include the second poly- second
The second layer formation of enol acetal resin and the second plasticizer puts into the second extruder with composition, thus squeeze out first layer and
The second layer；Surface treatment step, to the first layer or the while carry out plasma treatment of the second layer formed
Surface treated one side；And Stacking steps, extrusion lamination is carried out, so as to pass through in the first layer and the second layer
One layer of the surface treatment step it is surface treated with another layer without surface treatment while connect.
To prepare first glass assessed by 180 degree peel test and described the using the preparation method
The difference between the engaging force between engaging force and the first layer and the second layer between one layer is equal to or less than 7Kgf/
Plural layers are used in the glass engagement of 10mm.
Glass engagement plural layers can be prepared using the preparation method, are assessed by 180 degree peel test
Engaging force between the one side and the second layer of the first layer of the glass engagement plural layers with without etc. from
Subprocessing and the one side of first layer engaged improves 20% or more compared with the engaging force between the second layer.
The plasma treatment of the surface treatment step can under the conditions of 30 to 50 DEG C of temperature with 5 to 10m/min into
Roll-to-roll process go to complete.
Laminated glass according to still another embodiment of the invention includes above-mentioned glass engagement plural layers and glass
Laminated body.Specifically, the laminated body may include the first glass and the second glass, first glass in the glass
In the two sides of engagement plural layers with first layer share the plural layers outside it while connect, described
Two glass connect with the another side of the plural layers.
The effect of invention
Glass engagement plural layers according to the present invention, the laminated glass including the glass engagement plural layers and its
Manufacturing method is capable of providing glass engagement plural layers of following characteristic etc., these characteristics refer to: can by impact resistance,
Resistance to connectivity, sound damping etc. are maintained at certain level or more and improve the inter-layer bonding force of plural layers, and can pass through
Between the engaging force for reducing the interface between each layer in the engaging force and plural layers at the interface between plural layers and glass
Difference come make sound insulation intermediate coat as the defects of frost flower phenomenon minimizes.
Detailed description of the invention
(a) of Fig. 1 is partially and the part (b) is respectively the layer for laminated glass for illustrating an embodiment according to the present invention
The schematic diagram in the section of the specific embodiment of laminate film.
Fig. 2 and Fig. 3 is the schematic diagram for illustrating the method for the peel test executed in an embodiment of the present invention.
(a) of Fig. 4 partially just prepares laminated glass in the bubble test of the embodiment of the present invention to schematically show
The case where figure of sample later, left side is schematically shows after bubble test qualified (Pass) in part (b) of Fig. 4
And right side is figure the case where schematically showing unqualified (Fail).
The explanation of appended drawing reference
100: plural layers are used in glass engagement
200: the first glass
300: first layer
400: the second layer
500: third layer
600: the second glass
700: laminated glass
800: attachment release film
850: insertion release film
Interface between A: the first glass and first layer
B: the interface between first layer and the second layer
C: the interface between the second layer and third layer
D: the interface between third layer and the second glass
Specific embodiment
In the following, the embodiment of the present invention is described in detail, so that those skilled in the art can be easily real
Apply the present invention.But the present invention can be realized by various ways, however it is not limited to embodiment described herein.
About " about " and " actually " etc. used in all specifications as term relevant to degree, referring to
Meaning in when proposing intrinsic foozle and material allowable error, with its error value or close to the meaning of its error value
It uses, also, to prevent by helping to understand related accurate or absolute numerical value of the invention without improper use of good infringer
Disclosure and use.
In all specifications, " a combination thereof " as the term for including in the description of Markush type refers to, from by Markush
The more than one mixing or combination selected in the group of multiple constituent elements composition of type description, to indicate to include from by above-mentioned
More than one selected in the group of multiple constituent element compositions.
In all specifications, the record of " A and/or B " refers to " A, B or A and B ".
In all specifications, unless otherwise indicated, such as " first ", " second " or " A ", " B " term are for will be identical
Term be distinguished from each other.
In the present specification, " B is located on A " refers to that B is located on A in a manner of directly contacting with A, or refers to B in A and B
Between clip and be located on A in the state of other layers, and be not limited to the meaning that B is located on A in such a way that the surface with A directly contacts
Think.
In the present specification, unless otherwise indicated, singular expression may be interpreted as including the odd number interpreted from context or multiple
Several meanings.
The inventors found that: glass engagement is configured to intermediate coat with more when in order to ensure sound insulation functionality
When the glass engagement intermediate coat that layer is formed, surface (skin) layer and intermediate (core) layer generate difference on its engaging force, by
There are problems that separating between the relatively low middle layer of engaging force and superficial layer when engaging glass in above-mentioned difference.
To which the present inventor recognizes needs and compensates the defect as caused by the above problem (interlaminar separation, frost flower (ice
)) etc. flower the necessity of the physical property for needing to be improved plural layers, and the present invention is completed by research repeatedly.
According to the present invention, by for being had differences in terms of the resin of polyacetal resin is copolymerized composition and plasticising dosage
Superficial layer and middle layer using the hydroxy radical content for adjusting polyacetal resin and carry out additional surface treatment (oxygen plasma etc.)
Deng method, increase the engaging force between superficial layer and middle layer to prevent interlaminar separation, to improve multilayer polyacetal films
Durability.
In the present invention, reportedly in the sound insulation polyvinyl butyral film as representative multilayer polyacetal films
Showing for air blister defect (the bubble defect) that is known as frost flower (ice flower, snowflake) occurs after engaging glass
As this phenomenon is identified as produced nuclei of bubbles at any time by being grown into and expanding to wide region and generate more
The layer distinctive defect of structural membrane confirmed that this defect more mostly occurs in table compared between glass and superficial layer by research
Between surface layer and middle layer.
The present inventor is the reason of this phenomenon occurs for judgement: in the heterogeneous biggish feelings of the interlayer of multilayered structure
Under condition, in the biggish situation of heterogeneity especially between interface, that is to say, that the engaging force between glass and superficial layer is big
In the case where engaging force between superficial layer and surface layer, above-mentioned multilayered structure, which becomes, is easy to that heterogeneous structure occurs, by
This nuclei of bubbles is generated and is grown in above-mentioned interface.Therefore, the present inventor following completes this hair by solving the problems, such as
Bright, which refers to: viscosity is lower due to the characteristic of the middle layer with sound insulation value, therefore has there are nuclei of bubbles and once produce
The problem of characteristic of growth is easy to after raw.
(a) of Fig. 1 is partially and the part (b) is to illustrate being used for for one embodiment of the invention for a part with section respectively
The schematic diagram of the illustrative knot for the laminated glass that the plural layers of laminated glass are engaged with glass.Referring to Fig.1, to the present invention into
Row is described in more detail.
The glass engagement plural layers 100 of an embodiment according to the present invention include: first layer 300, poly- comprising first
Vinyl acetal resin and the first plasticizer, the first layer with the first glass 200 while directly connect；And second
Layer 400, the one side of the second layer directly connects with the another side of the first layer, and includes the second polyvinyl acetal resin
With the second plasticizer, wherein by between 180 degree peel test first glass 200 assessed and the first layer 300
The difference between engaging force between engaging force and the first layer 300 and the second layer 400 is equal to or less than 7Kgf/10mm.
Glass engagement plural layers 100 according to another embodiment of the present invention include: first layer 300, include first
Polyvinyl acetal resin and the first plasticizer, the first layer with the first glass 200 while directly connect；And the
Two layer 400, the one side of the second layer directly connects with the another side of the first layer, and includes the second Pioloform, polyvinyl acetal tree
Rouge and the second plasticizer, wherein by between 180 degree peel test first glass 200 assessed and the first layer 300
Engaging force and the first layer 300 and the second layer 400 between engaging force between difference be equal to or less than 20%.
A feature of the present invention is, as follows in order to solve the problems, such as in the glass engagement in plural layers 100,
The engaging force reduced between the A and the B is poor, wherein described problem refers to, by sound insulation plural layers included first
The engaging force of interface A between glass 200 and first layer 300 is abundant, but in contrast to this between first layer 300 and the second layer 400
Interface B engaging force it is relatively low, so as to cause the problem of the part is easy to happen defect.
Specifically, the difference of the engaging force can be 0.1 to 7Kgf/10mm, 1 to 6Kgf/10mm, 2 to 5Kgf/10mm
Or 4 to 5Kgf/10mm.The engaging force difference be equal to or less than 7Kgf/10mm when, due to interlayer engaging force difference relatively
Defect that is small and can reducing multiple sound insulation film occurs, and is equal to or less than the feelings of 5Kgf/10mm with the difference of the engaging force
Condition is more excellent compared to the effect for inhibiting defect to occur.
Specifically, the difference of the engaging force can be 20%, 0.01 to 20% or 1 to 15%.Such to have
When characteristic mode forms plural layers, less plural layers that defect occurs can be prepared.
It carries out assessing the engagement on the basis of the end value of the 180 degree glass test illustrated in the following embodiments
Power.Also, the difference refers to the absolute value for the value that A-B is obtained, and is worth situation more in general, A value is greater than B, but in the present invention
Specific embodiment in the case where being not excluded in contrast.
The second layer 400 can contain more plasticizer compared with the first layer 300.
The first layer 300 can be used as the layer directly to connect with glass as surface layer.The second layer 400 is used as puigging
Or sandwich layer can be used as glass engagement together with one or more surface layer and play sound damping with intermediate coat, and therefore, institute
It states first layer 300 and the second layer 400 and uses the polyvinyl acetal resin with different characteristics, and the content of plasticizer respectively
It is different from each other.
Specifically, include the plasticizer in the first layer 300 content by the first layer it is all on the basis of can
Think and is less than 30wt%, 20 to 30wt% or 25 to 30wt%.Specifically, including the plasticizer in the second layer 400
Content can be for equal to or more than 32wt%, 32 to 40wt% or 34 to 38wt% on the basis of the second layer.When comprising
When plasticizer in above-mentioned content range, it can provide and the machine performance of resistance to connectivity, resistance to permeability etc. is maintained at certain water
Film flat above and with sound damping.
The plasticizer can selected from by the double 2 ethyl hexanoic acid ester (3G8) of triethylene glycol, tetraethylene glycol diheptanoate (4G7),
The double 2 Ethylbutanoic acid esters (3GH) of triethylene glycol, triethylene glycol double 2- heptanoates (3G7), di butoxyethoxyethyl adipate
(DBEA), butyl carbitol adipate ester (DBEEA), dibutyl sebacate (DBS), the own ester of two 2- of adipic acid (DHA) and its mixed
In the group for closing object composition, specifically, compatibility between resin, keep film in terms of it is preferable to use
Selected from by the double 2 ethyl hexanoic acid ester (3G8) of triethylene glycol, the double 2 Ethylbutanoic acid esters (3GH) of triethylene glycol, triethylene glycol double 2- heptan
One of the group of acid esters (3G7) and combinations thereof composition.
The hydroxy radical content of first polyvinyl acetal resin can be equal to or more than 30mol%, and acetyl content
2mol% can be less than.Specifically, the hydroxy radical content of first polyvinyl acetal resin can be 30 to 50mol%.
When resin with the above characteristics is used as first polyvinyl acetal resin, the engagement between glass can be prepared
The first layer that power is good and machine performance is excellent.
The hydroxy radical content of second polyvinyl acetal resin can be equal to or less than 40mol%, be equal to or less than
30mol% or 1 to 30mol% can also be equal to or less than 10mol%.Also, the second of second polyvinyl acetal resin
Acyl group content can be equal to or more than 8mol%.When by resin with the above characteristics be used as the second Pioloform, polyvinyl acetal tree
When rouge, it can prepare and machine performance is maintained at certain level or more and with the second layer of excellent sound damping.
The hydroxyl of the hydroxy radical content of second polyvinyl acetal resin and first polyvinyl acetal resin contains
Difference between amount can be for equal to or more than 2mol%, 1 to 15mol% or 5 to 15mol%.In this case, it is possible to glass
Engagement assigns more good sound insulation value with plural layers.
The polyvinyl acetal resin can be to be carried out by the polyvinyl alcohol that is 1600 to 3000 to the degree of polymerization with aldehyde
Polyvinyl acetal resin obtained from acetalation.The aldehyde is not particularly limited.For example, the aldehyde can be selected from by positive fourth
In the group that aldehyde, isobutylaldehyde, positive bucket aldehyde, 2- ethyl butyraldehyde, n-hexyl aldehyde and its hybrid resin form.Specifically, due to n-butanal
It is excellent come the small and engaging force with glass of the refringence between the resin and glass that prepare, therefore it is preferable to use n-butanals to make
Standby resin.
Interface B between the first layer 300 and the second layer 400 can be by with 400 phase of the second layer
The first layer 300 connect or with after the while carry out plasma treatment of the second layer 400 that connects of the first layer 300
Made of engagement.The plasma treatment can make the first layer 300 or the second layer 400 while surface
Functional group's activation, thus, with without being surface-treated the case where differently can sufficiently improve interlayer engaging force.
Normal-pressure plasma device can be used to carry out in the plasma treatment, specifically, can by with
During the composition for preparing each layer carries out melting extrusion respectively and squeezes out lamination can to each layer carry out on one side etc. from
The method of the normal-pressure plasma device of daughter surface treatment carries out.
Specifically, the plasma treatment can use atmospheric plasma, oxygen plasma can also be used.
The plasma treatment can carry out roll-to-roll process under the conditions of 30 to 50 DEG C of temperature with 5 to 10m/min
(Roll to Roll) is completed.Pressure condition can be condition of normal pressure.When carrying out the plasma treatment by above-mentioned condition
When, the mechanical strength of each layer itself can be maintained at certain level or more and sound insulation value is maintained at certain level or more,
Interlayer engaging force can be improved simultaneously.
The plasma treatment can carry out under 10 to 15Kv application voltage conditions.Applying the electricity in above range
When pressure, inter-layer bonding force improvement effect is not only obtained, while being conducive to keep the mechanical strength characteristic of each layer and improving processing effect
Rate.
The bonding force value between the first layer 300 and the second layer 400 assessed by 180 degree peel test can be with
It is 25 to 40Kgf/10mm, 25 to 33Kgf/10mm or 34 to 40Kgf/10mm.Preferably, the engaging force can for 32 to
38Kgf/10mm。
When the engaging force between the first layer 300 and the second layer 400 within the above range when, with without it is equal from
Daughter surface treatment etc. is described come compared with not improving the first layer 300 with the engaging force between the second layer 400 the case where
Engaging force improves about 20% or more, specifically, improving 20 to 120%, therefore, sound insulation multi-layer thin can be significantly reduced
The defects of air bubble growth of film, occurs.
It can by the bonding force value between 180 degree peel test first glass 200 assessed and the first layer 300
Think 30 to 45Kgf/10mm or 30 to 40Kgf/10mm.
The glass engagement is placed at 50 DEG C of temperature and 20% relative humidities with plural layers 100 24 hours it
Afterwards, it forms the hole 8mm and forms laminated glass 700, then, after being placed 24 hours in 85 DEG C of baking ovens, observe in the hole
The size of the bubble of periphery growth, result can satisfy bubble with the condition of the 200% of hole range growth below.By
This, can sufficiently inhibit the phenomenon that the generation of the frost flower phenomenon of one of reported defect of sound insulation plural layers, so as to
Plural layers are used in the glass engagement for providing more better quality.
The glass engagement plural layers 100 may also include third layer, the one side of the third layer and the second layer
400 directly connect and its another side directly connects with the second glass 600, and the third layer includes third Pioloform, polyvinyl acetal tree
Rouge and third plasticizer.
Pass through engaging force between 180 degree peel test second glass 600 assessed and the third layer 500 and institute
7Kgf/10mm can be equal to or less than by stating the difference between the engaging force between the second layer 400 and the third layer 500.
The third layer 500 can have composition actually identical with the first layer 300 and characteristic.Therefore, because
Its record is omitted with about the illustrating to repeat of first layer 300 about illustrating for the third layer 500.Also, about institute
State the interface C between the second layer 400 and third layer 500 and the interface between the third layer 500 and second glass 600
The explanation of D, also with as described above about the explanation of the interface A between first glass 200 and first layer 300 and about
Interface B's between the first layer 300 and the second layer 400 illustrates to repeat respectively, therefore omits its record.
The loss coefficient (L/F) of glass engagement plural layers 100 measured under 20 DEG C and 2000Hz can wait
In or greater than 0.35.
The glass engagement plural layers 100 can satisfy the impact resistance characteristic based on KS L 2007:2008.
The glass engagement plural layers 100 can satisfy the resistance to connectivity characteristic based on KS L 2007.
The glass engagement plural layers can further include selected from by antioxidant, heat stabilizer, UV absorbent,
Additive in the group of UV stabilizer, IR absorbent, glass engaging force regulator and combinations thereof composition.
The additive may be embodied in the first layer, the second layer, at least one layer of in third layer and the 4th layer.Pass through packet
The long durabilities such as thermal stability, the photostability of film, which can be improved, and disperse containing the additive prevents performance.
Hindered amine (hindered amine) class or hindered phenol (hindered phenol) can be used in the antioxidant
Class.Specifically, from the perspective of polyvinyl butyral (PVB) preparation section for the process temperature for needing 150 DEG C or more,
More preferably use hindered phenol anti-oxidants.For example, BASF (BASF) company can be used in hindered phenol anti-oxidants
IRGANOX 1076,1010 etc..
In view of the compatibility with antioxidant, phosphite ester (phosphite) class heat is can be used in the heat stabilizer
Stabilizer.It is, for example, possible to use the IRGAFOS 168 of BASF AG.
The UV absorbent can be used CHEMIPRO be melted into the Chemisorb 12 of Co., Ltd., Chemisolve 79,
Tinuvin 328, Tinuvin 329, the Tinuvin 326 of Chemisolve 74, Chemisolve 102 and BASF AG
Deng.The Tinuvin etc. of BASF AG can be used in the UV stabilizer.ITO, ATO, AZO can be used in the IR absorbent
Or mixtures thereof the metal salts such as Mg, K, Na, epoxy modified polysiloxane etc., but the present invention can be used Deng, glass engaging force regulator
It is without being limited thereto.
Glass engagement plural layers 100 according to another embodiment of the present invention may include: first layer 300, include
First polyvinyl acetal resin and the first plasticizer, the first layer with the first glass 200 while directly connect；
And the second layer 400, the one side of the second layer directly connect with the another side of the first layer, and include the contracting of the second polyvinyl alcohol
Urea formaldehyde and the second plasticizer, wherein pass through described the of the glass engagement plural layers that 180 degree peel test is assessed
The engaging force of B has the engaging force increase rate value equal to or more than 20% between one layer of one side and the second layer, described to connect
Resultant force increase rate value indicates the engaging force phase between the one side and the second layer of the first layer engaged with without plasma treatment
Degree than the engaging force improved.
Specifically, the engaging force increase rate can be calculated by following formula 1.
[formula 1]
Engaging force increase rate (%)=100 × [| P1-2-N1-2|/N1-2]
In the formula 1, P1-2Refer to the engaging force between the first layer and the second layer by plasma treatment, and N1-2It is
Refer to without the engaging force between the first layer and the second layer of plasma treatment.
The engaging force is on the basis of the value (unit, Kgf/10mm) that is obtained in the present invention by 180 degree peel test
It is assessed.
A feature of the present invention is, as follows in order to solve the problems, such as in the glass engagement in plural layers 100,
Further increase the engaging force between the A and the B, wherein described problem refers to, since sound insulation plural layers are included
The engaging force of interface A between first glass 200 and first layer 300 is abundant, but first layer 300 and the second layer 400 in contrast to this
Between interface B engaging force it is relatively low, so as to cause the part defect frequent occurrence the problem of,.
Specifically, the engaging force increase rate value can be 20 to 120%, 20 to 90% or 25 to 80%.To have
When having the film of the engaging force increase rate value in above range to be used as the intermediate coat for laminated glass, can provide will be resistance to
The characteristics such as connectivity, impact resistance and sound damping are maintained at certain level or more and reduce the generation such as the defects of frost flower phenomenon
Plural layers.
The second layer 400 can have more plasticizer compared with the first layer 300.
The first layer 300 can be used as the layer directly to connect with glass as surface layer.The second layer 400 is used as puigging
Or sandwich layer can be used as glass engagement together with one or more surface layer and play sound damping with intermediate coat, and therefore, institute
It states first layer 300 and the second layer 400 and uses the polyvinyl acetal resin with different characteristics, and the content of plasticizer respectively
It is different from each other.
Specifically, including that the content of the plasticizer in the first layer 300 can on the basis of the first layer premise
Think and is less than 30wt%, 20 to 30wt% or 25 to 30wt%.Specifically, including the plasticizer in the second layer 400
Content can be for equal to or more than 32wt%, 32 to 40wt% or 34 to 38wt% on the basis of the second layer.When comprising
When plasticizer in above-mentioned content range, it can provide and the machine performance of resistance to connectivity, resistance to permeability etc. is maintained at certain water
Film flat above and with sound damping.
The plasticizer can selected from by the double 2 ethyl hexanoic acid ester (3G8) of triethylene glycol, tetraethylene glycol diheptanoate (4G7),
The double 2 Ethylbutanoic acid esters (3GH) of triethylene glycol, triethylene glycol double 2- heptanoates (3G7), di butoxyethoxyethyl adipate
(DBEA), butyl carbitol adipate ester (DBEEA), dibutyl sebacate (DBS), the own ester of two 2- of adipic acid (DHA) and its mixed
In the group for closing object composition, specifically, compatibility between resin, keep film in terms of it is preferable to use
Selected from by the double 2 ethyl hexanoic acid ester (3G8) of triethylene glycol, the double 2 Ethylbutanoic acid esters (3GH) of triethylene glycol, triethylene glycol double 2- heptan
One of the group of acid esters (3G7) and combinations thereof composition.
The hydroxy radical content of first polyvinyl acetal resin can be equal to or more than 30mol%, and acetyl content
2mol% can be less than.When resin with the above characteristics is used as first polyvinyl acetal resin, can prepare
The first layer that engaging force between glass is good and machine performance is excellent.
The hydroxy radical content of second polyvinyl acetal resin can be equal to or less than 10mol%, and acetyl content
8mol% can be less than.When resin with the above characteristics is used as second polyvinyl acetal resin, can prepare
Machine performance is maintained at certain level or more and the good second layer of sound insulation value.
The polyvinyl acetal resin can be to be carried out by the polyvinyl alcohol that is 1600 to 3000 to the degree of polymerization with aldehyde
Polyvinyl acetal resin obtained from acetalation.The aldehyde is not particularly limited.For example, the aldehyde can be selected from by positive fourth
In the group that aldehyde, isobutylaldehyde, positive bucket aldehyde, 2- ethyl butyraldehyde, n-hexyl aldehyde and its hybrid resin form.Specifically, due to n-butanal
It is excellent come the smaller and engaging force with glass of the refringence between the resin and glass that prepare, therefore it is preferable to use n-butanals to come
The resin of preparation.
Interface B between the first layer 300 and the second layer 400 can be by with 400 phase of the second layer
The first layer 300 connect or with after the while carry out plasma treatment of the second layer 400 that connects of the first layer 300
Made of engagement.The plasma treatment can make the first layer 300 or the second layer 400 while surface
Functional group's activation, thus, with without being surface-treated the case where differently can sufficiently improve interlayer engaging force.
Normal-pressure plasma device can be used to carry out in the plasma treatment, specifically, can by with
During the composition for preparing each layer carries out melting extrusion respectively and squeezes out lamination can to each layer carry out on one side etc. from
The method of the normal-pressure plasma device of daughter surface treatment carries out.
Specifically, the plasma treatment can use atmospheric plasma, oxygen plasma can also be used.
The plasma treatment can carry out roll-to-roll process under the conditions of 30 to 50 DEG C of temperature with 5 to 10m/min and come
It completes.Pressure condition can be condition of normal pressure.It, can be by each layer itself when carrying out the plasma treatment by above-mentioned condition
Mechanical strength be maintained at certain level or more and sound insulation value be maintained at certain level or more, while interlayer can be improved and connect
With joint efforts.
The plasma treatment can carry out under 10 to 15Kv application voltage conditions.Applying the electricity in above range
When pressure, inter-layer bonding force improvement effect is not only obtained, while being conducive to keep the mechanical strength characteristic of each layer and improving processing effect
Rate.
The bonding force value between the first layer 300 and the second layer 400 assessed by 180 degree peel test can be with
It is 25 to 40Kgf/10mm, 25 to 33Kgf/10mm or 34 to 40Kgf/10mm.Preferably, the engaging force can for 32 to
38Kgf/10mm。
When the engaging force between the first layer 300 and the second layer 400 within the above range when, shelled by 180 degree
Between the engaging force and the first layer and the second layer between first glass and the first layer from test assessment
Engaging force between difference can be equal to or less than 7Kgf/10mm, 0.1 to 7Kgf/10mm, 1 to 6Kgf/10mm or 2 to 5Kgf/
10mm.When difference in this way between interlayer engaging force is reduced, the defects of air bubble growth of sound insulation plural layers can be significantly reduced
Generation.
It can by the bonding force value between 180 degree peel test first glass 200 assessed and the first layer 300
Think 30 to 45Kgf/10mm or 30 to 40Kgf/10mm.
The glass engagement is placed at 50 DEG C of temperature and 20% relative humidities with plural layers 100 24 hours it
Afterwards, it forms the hole 8mm and forms laminated glass, then, after being placed 24 hours in 85 DEG C of baking ovens, observe on the hole periphery
The size of the bubble of growth, result can satisfy bubble with the condition of the 200% of hole range growth below.As a result,
It can inhibit the phenomenon that the generation of the frost flower phenomenon of one of reported defect of sound insulation plural layers, sufficiently so as to provide
Plural layers are used in the glass engagement of more better quality.
The glass engagement plural layers 100 may also include third layer, the one side of the third layer and the second layer
400 directly connect and its another side directly connects with the second glass 600, and the third layer includes third Pioloform, polyvinyl acetal tree
Rouge and third plasticizer.
Pass through engaging force between 180 degree peel test second glass 600 assessed and the third layer 500 and institute
7Kgf/10mm can be equal to or less than by stating the difference between the engaging force between the second layer 400 and the third layer 500.
The third layer 500 can have composition actually identical with the first layer 300 and characteristic.Therefore, because
Its record is omitted with about the illustrating to repeat of first layer 300 about illustrating for the third layer 500.Also, about institute
State the interface C between the second layer 400 and third layer 500 and the interface between the third layer 500 and second glass 600
The explanation of D, also with as described above about the explanation of the interface A between first glass 200 and first layer 300 and about
Interface B's between the first layer 300 and the second layer 400 illustrates to repeat respectively, therefore omits its record.
The loss coefficient (L/F) of glass engagement plural layers 100 measured under 20 DEG C and 2000Hz can wait
In or greater than 0.35.
The glass engagement plural layers 100 can satisfy the impact resistance characteristic based on KS L 2007:2008.
The glass engagement plural layers 100 can satisfy the resistance to connectivity characteristic based on KS L 2007.
The glass engagement plural layers can further include selected from by antioxidant, heat stabilizer, UV absorbent,
Additive in the group of UV stabilizer, IR absorbent, glass engaging force regulator and combinations thereof composition.Due to about each addition
Illustrating for agent illustrates to repeat with above, therefore omits its record.
The preparation method of plural layers according to still another embodiment of the invention includes: extrusion step, will be gathered comprising first
The first layer formation of vinyl acetal resin and the first plasticizer puts into the first extruder with composition, will include the second poly- second
The second layer formation of enol acetal resin and the second plasticizer puts into the second extruder with composition, to squeeze out first layer
300 and the second layer 400；Surface treatment step, to the first layer 300 or the second layer 400 while carry out etc.
Ion processing forms surface treated one side；And Stacking steps, extrusion lamination is carried out, so that in the first layer 300
With Jing Guo the surface treatment step in the second layer 400 one layer of surface treated one side with another layer without
Spend connecting on one side for surface treatment.
By the preparation method can prepare first glass 200 assessed by 180 degree peel test with it is described
The difference between the engaging force between engaging force and the first layer 300 and the second layer 400 between first layer 300 be equal to or
Glass engagement plural layers less than 7Kgf/10mm.
Normal-pressure plasma device can be used to carry out in the plasma treatment, specifically, can by with
During the composition for preparing each layer carries out melting extrusion respectively and squeezes out lamination can to each layer carry out on one side etc. from
The method of the normal-pressure plasma device of daughter surface treatment carries out.
Specifically, the plasma treatment can use atmospheric plasma, oxygen plasma can also be used.
The plasma treatment can carry out roll-to-roll process under the conditions of 30 to 50 DEG C of temperature with 5 to 10m/min and come
It completes.Pressure condition can be condition of normal pressure.It, can be by each layer itself when carrying out the plasma treatment by above-mentioned condition
Mechanical strength be maintained at certain level or more and sound insulation value be maintained at certain level or more, while interlayer can be improved and connect
With joint efforts.
The plasma treatment can carry out under 10 to 15Kv application voltage conditions.Applying the electricity in above range
When pressure, inter-layer bonding force improvement effect is not only obtained, while being conducive to keep the mechanical strength characteristic of each layer and improving processing effect
Rate.
About glass engagement plural layers 100, first layer 300, the second layer 400, additional third layer 500, each layer
The particular content of ingredient, the characteristic at interface, the characteristic of the plural layers etc. illustrates to repeat with above, therefore omits its note
It carries.
Also, about the interface C and the third layer 500 and described between the second layer 400 and third layer 500
The explanation of interface D between two glass 600, also and as described above about between first glass 200 and first layer 300
The explanation of interface A and illustrate to repeat respectively about the interface B between the first layer 300 and the second layer 400, therefore
Omit its record.
The preparation method of plural layers 100 according to still another embodiment of the invention includes: extrusion step, will include first
The first layer formation of polyvinyl acetal resin and the first plasticizer puts into the first extruder with composition, will gather comprising second
The second layer formation of vinyl acetal resin and the second plasticizer puts into the second extruder with composition, to squeeze out first layer
300 and the second layer 400；Surface treatment step, to the first layer 300 or the second layer 400 while carry out etc.
Ion processing forms surface treated one side；And Stacking steps, extrusion lamination is carried out, so that in the first layer 300
With Jing Guo the surface treatment step in the second layer 400 one layer of surface treated one side with another layer without
Spend connecting on one side for surface treatment.
Following glass engagement plural layers can be prepared by the preparation method, that is, pass through 180 degree peel test
Engagement between the one side and the second layer 400 of the first layer 300 of the glass engagement plural layers 100 of assessment
Power has the engaging force increase rate value equal to or more than 20%, and the engaging force increase rate value indicates and without plasma treatment
And the degree for the engaging force that the one side of the first layer 300 engaged is improved compared with the engaging force between the second layer 400.
Normal-pressure plasma device can be used to carry out in the plasma treatment, specifically, can by with
During the composition for preparing each layer carries out melting extrusion respectively and squeezes out lamination can to each layer carry out on one side etc. from
The method of the normal-pressure plasma device of daughter surface treatment carries out.
Specifically, the plasma treatment can use atmospheric plasma, oxygen plasma can also be used.
The plasma treatment can carry out roll-to-roll process under the conditions of 30 to 50 DEG C of temperature with 5 to 10m/min and come
It completes.Pressure condition can be condition of normal pressure.It, can be by each layer itself when carrying out the plasma treatment by above-mentioned condition
Mechanical strength be maintained at certain level or more and sound insulation value be maintained at certain level or more, while interlayer can be improved and connect
With joint efforts.
The plasma treatment can carry out under 10 to 15Kv application voltage conditions.Applying the electricity in above range
When pressure, inter-layer bonding force improvement effect is not only obtained, while being conducive to keep the mechanical strength characteristic of each layer and improving processing effect
Rate.
Due to about glass engagement plural layers 100, first layer 300, the second layer 400, additional third layer 500, each
The ingredient of layer, the particular content of characteristic, the characteristic of the plural layers etc. at interface illustrate to repeat, therefore omit it with above
It records.
Laminated glass 700 according to still another embodiment of the invention includes that plural layers are used in glass as described above engagement
100 with the laminated body of glass 200,600.Specifically, the laminated body may include the first glass 200 and the second glass 600,
First glass 200 with shared outside it in the glass engagement with the one side in the two sides of plural layers 100 with first layer 300
The plural layers on surface connect on one side, and second glass 600 connects with the another side of the plural layers.
In the following, a specific embodiment of the invention is described in more detail.
Preparation example
(preparation of polyvinyl butyral resin)
The preparation of polyvinyl butyral resin (a): the polyvinyl alcohol resin for being 1700 to average degree of polymerization synthesizes positive fourth
Aldehyde, obtain butyral base content be 69.1mol%, the polyvinyl butyral resin (a) that hydroxy radical content is 30.1mol%.
The preparation of polyvinyl butyral resin (b): the polyvinyl alcohol resin for being 2400 to average degree of polymerization synthesizes positive fourth
Aldehyde, obtain butyral base content be 59.2mol%, the polyvinyl butyral resin (b) that hydroxy radical content is 28.8mol%.
The preparation of polyvinyl butyral resin (c): the polyvinyl alcohol resin for being 1700 to average degree of polymerization synthesizes positive fourth
Aldehyde, obtain butyral base content be 58.7mol%, the polyvinyl butyral resin (c) that hydroxy radical content is 40.5mol%.
The preparation of polyvinyl butyral resin (d): the polyvinyl alcohol resin for being 2400 to average degree of polymerization synthesizes positive fourth
Aldehyde, obtain butyral base content be 65.2mol%, the polyvinyl butyral resin (d) that hydroxy radical content is 20.4mol%.
The preparation of polyvinyl butyral resin (e): the polyvinyl alcohol resin for being 2400 to average degree of polymerization synthesizes positive fourth
Aldehyde, obtain butyral base content be 48.9mol%, the polyvinyl butyral resin (e) that hydroxy radical content is 39.1mol%.
(compositions of additives)
Mix the irganox1010 of 0.1 parts by weight, the irgafos168 of 0.1 parts by weight, 0.3 parts by weight TINUVIN
P, the potassium acetate of 0.022 parts by weight and the magnesium acetate of 0.028 parts by weight prepare the compositions of additives of 0.55 parts by weight.
(prepared by the plural layers of embodiment 1)
Put into the polyvinyl butyral resin (a) of 72.45 parts by weight, the plasticizer 3G8 of 27 parts by weight and 0.55 weight
Part compositions of additives and mixing, then by double screw extruder extrude prepare with a thickness of 0.33mm first layer.It is logical
It crosses roll-to-roll normal-pressure plasma device and carries out oxygen plasma treatment on the side of prepared first layer to prepare process
The first layer of surface treatment.The plasma device condition is using 40 DEG C of temperature, the application of the speed of 10m/min and 14kV
Voltage.
The plasticizer 3G8 of the polyvinyl butyral resin (b) and 35 parts by weight that mix 65 parts by weight throws mixture
Enter to double screw extruder, to prepare the second layer with a thickness of 0.12mm, so that the second layer is located at the warp of the first layer
The mode crossed in the one side of plasma treatment carries out extrusion lamination, so that preparation has first layer/second layer double-layer structure
Plural layers (part (a) referring to Fig.1).
Volume pair is used to the one side of the exposure of the second layer in the plural layers with first layer/second layer double-layer structure
It rolls up normal-pressure plasma device and carries out oxygen plasma treatment, the one side to prepare the second layer is surface treated to have first
The plural layers (part (b) referring to Fig.1) of the double-layer structure of the layer/second layer.At this point, the plasma device condition uses
The application voltage of 40 DEG C of temperature, the speed of 10m/min and 14kV.
Mix the polyvinyl butyral resin (a) of 72.45 parts by weight, the plasticizer 3G8 of 27 parts by weight and 0.55 weight
Then the compositions of additives of part squeezes out the third layer being laminated into a thickness of 0.33mm by double screw extruder, to prepare
With the first layer/second layer/third layer three-decker plural layers.The multilayer with three-decker prepared as described above
The overall thickness of film is 0.78mm.
(prepared by the plural layers of comparative example 1)
Other than without plasma surface treatment, with the embodiment 1 it is identical form and method preparation
With the first layer/second layer/third layer three-decker plural layers.At this point, the thickness of each layer is as follows, that is, first layer
With a thickness of 0.33mm, third layer with a thickness of 0.33mm, the second layer with a thickness of 0.12mm, and the overall thickness of plural layers is
0.78mm。
(prepared by the plural layers of embodiment 2)
Put into the polyvinyl butyral resin (c) of 72.45 parts by weight, the plasticizer 3G8 of 27 parts by weight and 0.55 weight
Part compositions of additives and mixing, then by double screw extruder extrude prepare with a thickness of 0.33mm the first film.
Oxygen plasma treatment is carried out on the side of prepared the first film by roll-to-roll normal-pressure plasma device to prepare
Surface treated first layer.The plasma device condition is using 40 DEG C of temperature, the speed of 10m/min and 14kV
Apply voltage.
The plasticizer 3G8 of the polyvinyl butyral resin (d) and 35 parts by weight that mix 65 parts by weight throws mixture
Enter to double screw extruder, to prepare the second layer with a thickness of 0.12mm, so that the second layer is located at the warp of the first layer
The mode crossed in the one side of plasma treatment carries out extrusion lamination, so that preparation has first layer/second layer double-layer structure
Plural layers.
To the one side of the exposure of the second layer in the plural layers with first layer/second layer double-layer structure with roll-to-roll
Normal-pressure plasma device carries out oxygen plasma treatment, and the one side to prepare the second layer is surface treated to have first
The plural layers of the double-layer structure of the layer/second layer.At this point, the plasma device condition uses 40 DEG C of temperature, 10m/min
Speed and 14kV application voltage.
Mix the polyvinyl butyral resin (c) of 72.45 parts by weight, the plasticizer 3G8 of 27 parts by weight and 0.55 weight
Then the compositions of additives of part squeezes out the third layer being laminated into a thickness of 0.33mm by double screw extruder, to prepare
With the first layer/second layer/third layer three-decker plural layers.The multilayer with three-decker prepared as described above
The overall thickness of film is 0.78mm.
(prepared by the plural layers of comparative example 2)
Other than without plasma surface treatment, with the embodiment 2 it is identical form and method preparation
With the first layer/second layer/third layer three-decker plural layers.At this point, the thickness of each layer is as follows, that is, first layer
With a thickness of 0.33mm, third layer with a thickness of 0.33mm, the second layer with a thickness of 0.12mm, and the overall thickness of plural layers is
0.78mm。
(prepared by the plural layers of embodiment 3)
Put into the polyvinyl butyral resin (a) of 72.45 parts by weight, the plasticizer 3G8 of 27 parts by weight and 0.55 weight
Part compositions of additives and mixing, then by double screw extruder extrude prepare with a thickness of 0.33mm first layer.It is logical
It crosses roll-to-roll normal-pressure plasma device and carries out oxygen plasma treatment on the side of prepared first layer to prepare process
The first layer of surface treatment.The plasma device condition is using 40 DEG C of temperature, the application of the speed of 10m/min and 14kV
Voltage.
The plasticizer 3G8 of the polyvinyl butyral resin (d) and 35 parts by weight that mix 65 parts by weight throws mixture
Enter to double screw extruder, to prepare the second layer with a thickness of 0.12mm, so that the second layer is located at the warp of the first layer
The mode crossed in the one side of plasma treatment carries out extrusion lamination, so that preparation has first layer/second layer double-layer structure
Plural layers.
Volume pair is utilized to the one side of the exposure of the second layer in the plural layers with first layer/second layer double-layer structure
It rolls up normal-pressure plasma device and carries out oxygen plasma treatment, the one side to prepare the second layer is surface treated to have first
The plural layers of the double-layer structure of the layer/second layer.At this point, the plasma device condition uses 40 DEG C of temperature, 10m/min
Speed and 14kV application voltage.
Mix the polyvinyl butyral resin (a) of 72.45 parts by weight, the plasticizer 3G8 of 27 parts by weight and 0.55 weight
Then the compositions of additives of part squeezes out the third layer being laminated into a thickness of 0.33mm by double screw extruder, to prepare
With the first layer/second layer/third layer three-decker plural layers.The multilayer with three-decker prepared as described above
The overall thickness of film is 0.78mm.
(prepared by the plural layers of comparative example 3)
Other than without plasma surface treatment, with the embodiment 3 it is identical form and method preparation
With the first layer/second layer/third layer three-decker plural layers.At this point, the thickness of each layer is as follows, that is, first layer
With a thickness of 0.33mm, third layer with a thickness of 0.33mm, the second layer with a thickness of 0.12mm, and the overall thickness of plural layers is
0.78mm。
(prepared by the plural layers of embodiment 4)
Put into the polyvinyl butyral resin (c) of 72.45 parts by weight, the plasticizer 3G8 of 27 parts by weight and 0.55 weight
Part compositions of additives and mixing, then by double screw extruder extrude prepare with a thickness of 0.33mm first layer.It is logical
It crosses roll-to-roll normal-pressure plasma device and carries out oxygen plasma treatment on the side of prepared first layer to prepare process
The first layer of surface treatment.The plasma device condition is using 40 DEG C of temperature, the application of the speed of 10m/min and 14kV
Voltage.
The plasticizer 3G8 of the polyvinyl butyral resin (e) and 35 parts by weight that mix 65 parts by weight throws mixture
Enter to double screw extruder, to prepare the second layer with a thickness of 0.12mm, so that the second layer is located at the warp of the first layer
The mode crossed in the one side of plasma treatment carries out extrusion lamination, so that preparation has first layer/second layer double-layer structure
Plural layers.
Volume pair is utilized to the one side of the exposure of the second layer in the plural layers with first layer/second layer double-layer structure
It rolls up normal-pressure plasma device and carries out oxygen plasma treatment, the one side to prepare the second layer is surface treated to have first
The plural layers of the double-layer structure of the layer/second layer.At this point, the plasma device condition uses 40 DEG C of temperature, 10m/min
Speed and 14kV application voltage.
Mix the polyvinyl butyral resin (c) of 72.45 parts by weight, the plasticizer 3G8 of 27 parts by weight and 0.55 weight
Then the compositions of additives of part squeezes out the third layer being laminated into a thickness of 0.33mm by double screw extruder, to prepare
With the first layer/second layer/third layer three-decker plural layers.The multilayer with three-decker prepared as described above
The overall thickness of film is 0.78mm.
(prepared by the plural layers of embodiment 5)
Other than without plasma surface treatment, with the embodiment 4 it is identical form and method preparation
With the first layer/second layer/third layer three-decker plural layers.At this point, the thickness of each layer is as follows, that is, first layer
With a thickness of 0.33mm, third layer with a thickness of 0.33mm, the second layer with a thickness of 0.12mm, and the overall thickness of plural layers is
0.78mm。
The type and content of polyvinyl butyral (PVB) resin applied to each layer, plasticizer are summarized in the following table 1
Content, thickness of each layer etc..
[table 1]
Physical property appraisal procedure
Engaging force measures (180 degree peel test (peel test))
Illustrate engaging force measuring method referring to Fig. 2 and Fig. 3.
The plural layers of the embodiment and comparative example are placed 24 hours in the environment of 50 DEG C and 20% relative humidity
Afterwards, plural layers are cut to make width × length × thickness become 150 × 100 × 2.1mm, thus sample of the preparation for assessment
Product.The sample so prepared is placed on width × length × with a thickness of on the first glass plate of 150 × 100 × 2.1mm, and
And as measurement auxiliary substrate, on first glass plate place as adhere to release film 800 primary coat width ×
Length × with a thickness of the PET film (being manufactured by SKC Co., Ltd) of 150 × 250 × 0.188mm.
1) the engagement force estimation at the interface (A) of the first glass-first layer
It is between the first glass and first layer, the longitudinal direction of 50 μm of insertion release film 850 from first glass is last
End is inserted into the position at 20mm, and is applicable in as the starting point for making peel test.
The test being laminated as described above is put into vacuum laminator with sample, is engaged in advance under 150 DEG C and 1 atmospheric pressure
20 seconds, main engagement is then carried out in autoclave.The condition of main engagement is the heating until rising to 140 DEG C from room temperature
Time is 25 minutes, and the retention time is 25 minutes at 140 DEG C.Peeling tester uses the universal test of QMESYS joint-stock company
The QM100S model of machine (UTM, universal testing machine).
As above the test sample engaged is cut with 10mm width interval to longitudinal from the point of 15mm from both-side ends
It cuts, test sample is thus made.Hereafter, the insertion release film 850 is removed.
By the first glass end of prepared test sample and the plural layers for being bonded to attachment release film 800
The angle that end keeps that it is made to keep 180 degree respectively using UTM retainer, and with the load of 50kgf with 300mm/min's
Rate carries out peel test.Measurement is removed after separating plural layers and the first glass to 70mm, is then terminated.
It is measuring in this way the result is that will terminate from measurement starting point by the point of 20mm as starting point and as described above
Point is terminal come the average interface (A) as the first glass-first layer of the engaging force measured in the range of calculating during this period
Engaging force indicate.Such measurement repeats more than three times, and its average value is expressed as end value.
2) the engagement force estimation of first layer-second layer interface (B)
The interface between the first layer and the second layer of prepared plural layers is grasped and separated to ensure for making
50 μm of insertion release film 850, is then inserted by the area that release film enters from the longitudinal end of first glass
Position at 20mm, and be applicable in as the starting point for making peel test.
By with above 1) in it is identical in a manner of assess the engaging force of sample produced above.
Bubble test
The plural layers of the embodiment and comparative example are placed 24 hours in the environment of 50 DEG C and 20% relative humidity
Afterwards, plural layers are cut to make width × length become 100 × 100mm, then in the hole that one diameter of centre drill is 8mm.
Above-mentioned film is placed between the glass for the two panels 2.1mm thickness for being cut into identical size, and with same as described above
Mode is engaged in advance and main engagement is come to prepare laminated glass.
The laminated glass prepared as described above is placed in 85 DEG C of baking ovens after 24 hours, whether observation bubble grows.It will
In addition to its external periphery of the 8mm as initial aperture is the same as to be equal to or less than 200% dimensional growth bubble compared with original
The case where be expressed as qualification, will be to be expressed as unqualified (figure with to be greater than 200% dimensional growth bubble compared with original the case where
Left side shows qualification in 4 part (b), and right side shows unqualified).
Sound-proofing assessment
Each plural layers of embodiment and comparative example are cut into the size that length is 30cm, width is 2.5cm, by cutting
Plural layers are clipped in two transparency glass plates (length 30cm, width 2.5cm, with a thickness of 2.1cm), to obtain laminated glass
Glass.Laminated glass is placed in rubber bag, and at the deaerated under vacuum of 2.6KPa 20 minutes, it then, will in the state of degassing
Laminated glass is transferred in baking oven, is further kept for laminated glass 30 minutes at 90 DEG C, with vacuum press to laminated glass into
Row pre-extrusion.By precompressed laminated glass squeezes at 140 DEG C of temperature and the pressure condition of 1.2MPa in autoclave
Pressure 20 minutes, to obtain the laminated glass for measuring sound-proofing.
In order to obtain stable sound insulation value, curing (aging) 72 hours in the chamber of 20 DEG C and 20% relative humidity
More than, then assess the sound insulation value of laminated glass.
Laminated glass is applied by the vibration machine for toppling over test and is vibrated, thus obtained vibrant characteristic is made
Amplified with impedance measurement device, rumble spectrum is analyzed by FFT spectrum analyzer, obtains L/F (loss factor) value, it will be
The situation that value at 20 DEG C is 0.35 or more is expressed as qualification, and by the value at 20 DEG C less than 0.35 the case where is expressed as not conforming to
Lattice.
Resistance to connectivity assessment
The resistance to connectivity of laminated glass is assessed based on KS L 2007.
It is made respectively using the glass of 300mm × 300mm with a thickness of 2.1cm and each plural layers of Examples and Comparative Examples
It is standby at glass-plural layers-glass stepped construction, then pre-terminated merging is de-gassed and edge seal under vacuum conditions.
Then, main at 150 DEG C using autoclave to engage 2 hours, so that sample be made.Then, the steel ball of 2.26kg is fallen
In the height (MBH) that on the sample, thus measurement sample is pierced.At this point, by being pierced at position of the height less than 4m
The case where be expressed as it is unqualified, and will height equal to or more than 4m position at be pierced the case where be expressed as qualification.
Impact resistance assessment
It is whether notch based on the KS L 2007:2008 laminated glass for assessing embodiment and comparative example.
By with above-mentioned resistance to connectivity assess it is identical in a manner of carry out glass and Examples and Comparative Examples using 2.1cm thickness
Each plural layers prepare respectively and are bonded into glass-plural layers-glass stepped construction process.
Low temperature evaluation in, by 227g steel ball subzero 20 DEG C at a temperature of keep 4 hours, then from the height of 9m throw
Under, by by the sample broke impacted and glass disperses or the amount of glass that falls off from sheet material is 15g or more situation is expressed as
It is unqualified, by by the sample impacted it is broken or glass does not disperse and the case where the sheet glass amount that falls off from sheet material is less than 15g
It is expressed as qualification.
Room temperature evaluation in, by 227g steel ball subzero 40 DEG C at a temperature of keep 4 hours, then from the height of 10m throw
Under, by by the sample broke impacted and glass disperses or the amount of glass that falls off from sheet material is 15g or more situation is expressed as
It is unqualified, by by the sample impacted it is broken or glass does not disperse and the case where the sheet glass amount that falls off from sheet material is less than 15g
It is expressed as qualification.
Physical property assessment result
The assessment result of resistance to connectivity etc.
For the resistance to connectivity of the above embodiments 1 to 3 and comparative example 1 to 3, impact resistance, sound damping, bubble test
As a result it is shown in the following table 2.
[table 2]
Referring to upper table 2, the sample of embodiment and comparative example be evaluated as having excellent resistance to connectivity, impact resistance and every
Sound characteristic.
In particular, in the case where sound damping, even if being made as in the present invention by carrying out surface plasma processing
When making plural layers, sound insulation value is also maintained at certain level or more, it can thus be assumed that surface plasma processing greatly mentions
High bonding force but big influence is not brought on sound insulation value.In addition, all samples of the embodiment and comparative example all meet machine
Tool performance condition may thereby determine that also there is sample the resistance to of certain level or more to pass through even if carrying out surface plasma processing
The general character and impact resistance.
In particular, there are sizable differences between embodiment and comparative sample in bubble test result, in embodiment
In the case where, it confirms and significantly suppresses air bubble growth.What this species diversity was considered as generating due to interlayer engaging force is improved,
And embodiment is assessed as the machine performance of plural layers and sound damping being maintained at certain level or more and inhibits bubble raw
It is long, to inhibit the effect of the formation of the snowflake (frost flower) illustrated in an embodiment of the present invention as the defect of sound insulation intermediate coat
It is brilliant.
Each interlayer engaging force measurement result
The engaging force and first layer and second at the interface between the first glass that assessment is engaged with first layer in the above described manner
Engaging force between layer, and the difference between these values is also had evaluated, its result is summarised in the following table 3.
[table 3]
| Unit: Kgf/10mm | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 |
| The engaging force (1) of the-the first glass interface of first layer (A) | 30 | 40 | 30 | 40 |
| The engaging force (2) of the-the second bed boundary of first layer (B) | 32 | 36 | 25 | 43 |
| The difference [difference of (1) and (2)] of engaging force | 2 | 4 | 5 | 3 |
| (1) and the engaging force difference * * (%) of (2) | 6.7 | 10.0 | 16.7 | 7.5 |
| Engaging force measurement result | Comparative example 1 | Comparative example 2 | Comparative example 3 | Embodiment 5 |
| The engaging force (1) of the-the first glass interface of first layer (A) | 30 | 39 | 30 | 40 |
| The engaging force (2) of the-the second bed boundary of first layer (B) | 22 | 28 | 15 | 35 |
| The difference [difference of (1) and (2)] of engaging force | 8 | 11 | 8 | 5 |
| (1) and the engaging force difference * * (%) of (2) | 26.7 | 28.2 | 50.0 | 12.5 |
| (2) engaging force increase rate * (%) | 45.5 | 28.6 | 66.7 | 22.9 |
* engaging force poor (%) will be in each embodiment or comparative example | [the engagement of the-the first glass interface of first layer (A)
Power (1)]-[engaging force (2) of the-the second bed boundary of first layer (B)] |/[engaging force (1) of the-the first glass interface of first layer (A)]
Value is as a percentage.
* engaging force increase rate will be formed when being constituted film with identical | (the-the second bed boundary of first layer of embodiment
Engaging force)-(engaging force of the-the second bed boundary of first layer of comparative example) | the/(engagement of the-the second bed boundary of first layer of comparative example
Power) value is as a percentage.
It can determine that in the sample of embodiment, especially the engaging force of first layer-second layer interface (B) is substantially by upper table 3
It improves.And it is possible to determine between the engaging force and surface-core interface engaging force at the interface (A) of the-the first glass of first layer
Difference is greatly decreased.
Although as described above, the preferred embodiment of the present invention is described in detail, although it will be appreciated that of the invention
Range is not limited to the above embodiments, but uses the art technology for the basic conception of the invention being defined in the claims
The various changes or deformation of personnel all belong to the scope of the present invention.
Claims (21)
1. a kind of glass engagement plural layers, comprising:
First layer, comprising the first polyvinyl acetal resin and the first plasticizer, the one side of the first layer and the first glass
Directly connect on one side；And
The second layer, the one side of the second layer directly connect with the another side of the first layer, and include the contracting of the second polyvinyl alcohol
Urea formaldehyde and the second plasticizer,
Wherein, pass through the engaging force and described between 180 degree peel test first glass assessed and the first layer
The difference between engaging force between one layer and the second layer is equal to or less than 7Kgf/10mm.
2. glass engagement plural layers according to claim 1, wherein
The second layer contains more plasticizer compared with the first layer.
3. glass engagement plural layers according to claim 1, wherein
The hydroxy radical content of first polyvinyl acetal resin is equal to or more than 30mol%, and acetyl content is less than
2mol%.
4. glass engagement plural layers according to claim 1, wherein
Interface between the first layer and the second layer is by one to the first layer to connect with the second layer
Made of being engaged after the one side of face or the second layer to connect with the first layer progress plasma treatment.
5. glass engagement plural layers according to claim 1, wherein
The bonding force value between the first layer and the second layer assessed by 180 degree peel test is 25 to 40Kgf/
10mm。
6. glass engagement plural layers according to claim 1, further includes:
Third layer, the one side of the third layer directly connects with the second layer and its another side directly connects with the second glass,
And the third layer includes third polyvinyl acetal resin and third plasticizer,
Wherein, pass through the engaging force and described between 180 degree peel test second glass assessed and the third layer
The difference between engaging force between two layers and the third layer is equal to or less than 7Kgf/10mm.
7. glass engagement plural layers according to claim 6, wherein
The second layer contains more plasticizer compared with the third layer.
8. glass engagement plural layers according to claim 6, wherein
The hydroxy radical content of the third polyvinyl acetal resin is equal to or more than 30mol%, and acetyl content is less than
2mol%.
9. glass engagement plural layers according to claim 6, wherein
Interface between the third layer and the second layer is by one to the second layer to connect with the third layer
Made of being engaged after the one side of face or the third layer to connect with the second layer progress plasma treatment.
10. glass engagement plural layers according to claim 6, wherein
Bonding force value between the second layer assessed by 180 degree peel test and the third layer is 25 to 40Kgf/
10mm。
11. a kind of preparation method of plural layers, comprising:
Extrusion step puts into the first layer formation comprising the first polyvinyl acetal resin and the first plasticizer with composition
Second layer formation comprising the second polyvinyl acetal resin and the second plasticizer is put into composition by the first extruder
Two extruders, to squeeze out first layer and the second layer；
Surface treatment step, to the first layer or the second layer while carry out plasma treatment come formed by
The one side of surface treatment；And
Stacking steps carry out extrusion lamination, so as to pass through the surface treatment step in the first layer and the second layer
One layer it is surface treated with another layer without surface treatment while connect,
Wherein, connecing between the first glass and the first layer assessed using the method preparation by 180 degree peel test
Glass of the difference equal to or less than 7Kgf/10mm between resultant force and the engaging force between the first layer and the second layer engages
Use plural layers.
12. the preparation method of plural layers according to claim 11, wherein
The plasma treatment of the surface treatment step carries out under the conditions of 30 to 50 DEG C of temperature with 5 to 10m/min roll-to-roll
Process is completed.
13. a kind of laminated glass, including stack gradually the first glass, glass engagement multi-layer thin according to claim 1
Laminated body made of film and the second glass.
14. a kind of glass engagement plural layers, comprising:
First layer, comprising the first polyvinyl acetal resin and the first plasticizer, the one side of the first layer and the first glass
Directly connect on one side；And
The second layer, the one side of the second layer directly connect with the another side of the first layer, and include the contracting of the second polyvinyl alcohol
Urea formaldehyde and the second plasticizer,
Wherein, the one side of the first layer for the glass engagement plural layers assessed by 180 degree peel test and institute
Stating the engaging force between the second layer has the engaging force increase rate value for being equal to or more than 20%, and the engaging force increase rate value indicates
With the engaging force that the one side of the first layer engaged without plasma treatment is improved compared with the engaging force between the second layer
Degree.
15. glass engagement plural layers according to claim 14, wherein
Interface between the first layer and the second layer is by one to the first layer to connect with the second layer
Made of being engaged after the one side of face or the second layer to connect with the first layer progress plasma treatment.
16. glass engagement plural layers according to claim 14, wherein
The bonding force value between the first layer and the second layer assessed by 180 degree peel test is 25 to 40Kgf/
10mm。
17. glass engagement plural layers according to claim 14, further includes:
Third layer, the one side of the third layer directly connects with the second layer and its another side directly connects with the second glass,
And the third layer includes third polyvinyl acetal resin and third plasticizer,
Wherein, the one side of the third layer for the glass engagement plural layers assessed by 180 degree peel test and institute
State the engagement between the one side and the second layer for the third layer that the engaging force between the second layer is engaged with without plasma treatment
Power is compared and improves 20% or more.
18. glass engagement plural layers according to claim 17, wherein
Interface between the third layer and the second layer is by one to the second layer to connect with the third layer
Made of being engaged after the one side of face or the third layer to connect with the second layer progress plasma treatment.
19. glass engagement plural layers according to claim 17, wherein
Bonding force value between the second layer assessed by 180 degree peel test and the third layer is 25 to 40Kgf/
10mm。
20. a kind of preparation method of plural layers, comprising:
Extrusion step puts into the first layer formation comprising the first polyvinyl acetal resin and the first plasticizer with composition
Second layer formation comprising the second polyvinyl acetal resin and the second plasticizer is put into composition by the first extruder
Two extruders, to squeeze out first layer and the second layer；
Surface treatment step, to the first layer or the second layer while carry out plasma treatment come formed by
The one side of surface treatment；And
Stacking steps carry out extrusion lamination, so that passing through the surface treatment step in the first layer and the second layer
One layer it is surface treated with another layer without surface treatment while connect,
Wherein, glass engagement plural layers are prepared using the method, is connect by the glass that 180 degree peel test is assessed
The engaging force shared between the one side and the second layer of the first layer of plural layers connects with without plasma treatment
The one side of the first layer of conjunction improves compared with the engaging force between the second layer 20% or more.
21. a kind of laminated glass, including stack gradually the first glass, glass engagement multi-layer thin according to claim 14
Laminated body made of film and the second glass.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| KR1020180037733A KR102004091B1 (en) | 2018-03-30 | 2018-03-30 | Multilayer film for laminating glasses, laminated glasses comprising of the same, manudacturing method for the same |
| KR10-2018-0037733 | 2018-03-30 |
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| Publication Number | Publication Date |
|---|---|
| CN110315814A true CN110315814A (en) | 2019-10-11 |
| CN110315814B CN110315814B (en) | 2022-03-22 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810904547.2A Active CN110315814B (en) | 2018-03-30 | 2018-08-09 | Multilayer film for glass bonding, laminated glass including the same, and method for producing the same |
Country Status (2)
| Country | Link |
|---|---|
| KR (1) | KR102004091B1 (en) |
| CN (1) | CN110315814B (en) |
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| CN114096407A (en) * | 2019-11-13 | 2022-02-25 | Skc株式会社 | Laminated film for bonding and light-transmitting laminate comprising same |
| CN114103311A (en) * | 2020-09-01 | 2022-03-01 | Skc株式会社 | Resin layer, intermediate film for bonding, light-transmitting laminate, and vehicle |
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Also Published As
| Publication number | Publication date |
|---|---|
| KR102004091B1 (en) | 2019-07-25 |
| CN110315814B (en) | 2022-03-22 |
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