CN118076571A - 乙烯-乙烯醇缩醛类作为陶瓷坯片中的粘结剂的用途 - Google Patents
乙烯-乙烯醇缩醛类作为陶瓷坯片中的粘结剂的用途 Download PDFInfo
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- CN118076571A CN118076571A CN202280068098.7A CN202280068098A CN118076571A CN 118076571 A CN118076571 A CN 118076571A CN 202280068098 A CN202280068098 A CN 202280068098A CN 118076571 A CN118076571 A CN 118076571A
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- Prior art keywords
- ethylene
- vinyl
- binders
- acetal
- ceramic green
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 229920002554 vinyl polymer Polymers 0.000 title claims abstract description 36
- 239000000919 ceramic Substances 0.000 title claims abstract description 26
- 239000011230 binding agent Substances 0.000 title claims abstract description 24
- 239000005977 Ethylene Substances 0.000 claims abstract description 21
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical group C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 13
- 239000000203 mixture Substances 0.000 claims abstract description 13
- 239000000725 suspension Substances 0.000 claims abstract description 13
- 239000002270 dispersing agent Substances 0.000 claims abstract description 10
- DHKHKXVYLBGOIT-UHFFFAOYSA-N acetaldehyde Diethyl Acetal Natural products CCOC(C)OCC DHKHKXVYLBGOIT-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000004014 plasticizer Substances 0.000 claims abstract description 8
- 239000001023 inorganic pigment Substances 0.000 claims abstract description 6
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- ZTQSAGDEMFDKMZ-UHFFFAOYSA-N butyric aldehyde Natural products CCCC=O ZTQSAGDEMFDKMZ-UHFFFAOYSA-N 0.000 claims description 16
- 238000004519 manufacturing process Methods 0.000 claims description 10
- 125000004036 acetal group Chemical group 0.000 claims description 8
- AMIMRNSIRUDHCM-UHFFFAOYSA-N isobutyric aldehyde Natural products CC(C)C=O AMIMRNSIRUDHCM-UHFFFAOYSA-N 0.000 claims description 7
- IMROMDMJAWUWLK-UHFFFAOYSA-N Ethenol Chemical compound OC=C IMROMDMJAWUWLK-UHFFFAOYSA-N 0.000 claims description 5
- 125000004432 carbon atom Chemical group C* 0.000 claims description 5
- WDLUEZJSSHTKAP-UHFFFAOYSA-N acetaldehyde;1,1-diethoxyethane Chemical group CC=O.CCOC(C)OCC WDLUEZJSSHTKAP-UHFFFAOYSA-N 0.000 claims description 2
- 239000000976 ink Substances 0.000 abstract 1
- 229920000219 Ethylene vinyl alcohol Polymers 0.000 description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 12
- 238000006359 acetalization reaction Methods 0.000 description 11
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 9
- 150000001299 aldehydes Chemical class 0.000 description 9
- 229920005989 resin Polymers 0.000 description 8
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- 239000006185 dispersion Substances 0.000 description 7
- 239000004715 ethylene vinyl alcohol Substances 0.000 description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 6
- RZXDTJIXPSCHCI-UHFFFAOYSA-N hexa-1,5-diene-2,5-diol Chemical compound OC(=C)CCC(O)=C RZXDTJIXPSCHCI-UHFFFAOYSA-N 0.000 description 6
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 6
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- 238000005266 casting Methods 0.000 description 5
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- 229920006324 polyoxymethylene Polymers 0.000 description 5
- IKHGUXGNUITLKF-UHFFFAOYSA-N Acetaldehyde Chemical compound CC=O IKHGUXGNUITLKF-UHFFFAOYSA-N 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 4
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- NBBJYMSMWIIQGU-UHFFFAOYSA-N Propionic aldehyde Chemical compound CCC=O NBBJYMSMWIIQGU-UHFFFAOYSA-N 0.000 description 4
- 239000003054 catalyst Substances 0.000 description 4
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- HGBOYTHUEUWSSQ-UHFFFAOYSA-N valeric aldehyde Natural products CCCCC=O HGBOYTHUEUWSSQ-UHFFFAOYSA-N 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 3
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- YGHRJJRRZDOVPD-UHFFFAOYSA-N 3-methylbutanal Chemical compound CC(C)CC=O YGHRJJRRZDOVPD-UHFFFAOYSA-N 0.000 description 2
- IAZDPXIOMUYVGZ-WFGJKAKNSA-N Dimethyl sulfoxide Chemical compound [2H]C([2H])([2H])S(=O)C([2H])([2H])[2H] IAZDPXIOMUYVGZ-WFGJKAKNSA-N 0.000 description 2
- WTDHULULXKLSOZ-UHFFFAOYSA-N Hydroxylamine hydrochloride Chemical compound Cl.ON WTDHULULXKLSOZ-UHFFFAOYSA-N 0.000 description 2
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- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 2
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- 230000002378 acidificating effect Effects 0.000 description 2
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 description 2
- 229910002113 barium titanate Inorganic materials 0.000 description 2
- HUMNYLRZRPPJDN-UHFFFAOYSA-N benzaldehyde Chemical compound O=CC1=CC=CC=C1 HUMNYLRZRPPJDN-UHFFFAOYSA-N 0.000 description 2
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- 229910010293 ceramic material Inorganic materials 0.000 description 2
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- 238000007127 saponification reaction Methods 0.000 description 2
- 235000011121 sodium hydroxide Nutrition 0.000 description 2
- 238000009864 tensile test Methods 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- JOXIMZWYDAKGHI-UHFFFAOYSA-N toluene-4-sulfonic acid Chemical compound CC1=CC=C(S(O)(=O)=O)C=C1 JOXIMZWYDAKGHI-UHFFFAOYSA-N 0.000 description 2
- BHVGMUDWABJNRC-UHFFFAOYSA-N (±)-2-methylhexanal Chemical compound CCCCC(C)C=O BHVGMUDWABJNRC-UHFFFAOYSA-N 0.000 description 1
- 238000005160 1H NMR spectroscopy Methods 0.000 description 1
- FJJYHTVHBVXEEQ-UHFFFAOYSA-N 2,2-dimethylpropanal Chemical compound CC(C)(C)C=O FJJYHTVHBVXEEQ-UHFFFAOYSA-N 0.000 description 1
- GPTMCJMLSOIYGU-UHFFFAOYSA-N 2,4-dimethylpentanal Chemical compound CC(C)CC(C)C=O GPTMCJMLSOIYGU-UHFFFAOYSA-N 0.000 description 1
- UNNGUFMVYQJGTD-UHFFFAOYSA-N 2-Ethylbutanal Chemical compound CCC(CC)C=O UNNGUFMVYQJGTD-UHFFFAOYSA-N 0.000 description 1
- BFKSYXOOFDWKFF-UHFFFAOYSA-N 2-ethyl-2-methylbutanal Chemical compound CCC(C)(CC)C=O BFKSYXOOFDWKFF-UHFFFAOYSA-N 0.000 description 1
- SHGPBDQRELYPLO-UHFFFAOYSA-N 2-ethyl-3-methylbutanal Chemical compound CCC(C=O)C(C)C SHGPBDQRELYPLO-UHFFFAOYSA-N 0.000 description 1
- LTNUSYNQZJZUSY-UHFFFAOYSA-N 3,3-dimethylbutanal Chemical compound CC(C)(C)CC=O LTNUSYNQZJZUSY-UHFFFAOYSA-N 0.000 description 1
- SZBNDYYJXRXQHA-UHFFFAOYSA-N 3,4-dimethylpentanal Chemical compound CC(C)C(C)CC=O SZBNDYYJXRXQHA-UHFFFAOYSA-N 0.000 description 1
- ZSJUABCTGCNBPF-UHFFFAOYSA-N 3-Methylhexanal Chemical compound CCCC(C)CC=O ZSJUABCTGCNBPF-UHFFFAOYSA-N 0.000 description 1
- VHYFNPMBLIVWCW-UHFFFAOYSA-N 4-Dimethylaminopyridine Chemical compound CN(C)C1=CC=NC=C1 VHYFNPMBLIVWCW-UHFFFAOYSA-N 0.000 description 1
- GIGNTOMJQYNUNL-UHFFFAOYSA-N 4-methylhexanal Chemical compound CCC(C)CCC=O GIGNTOMJQYNUNL-UHFFFAOYSA-N 0.000 description 1
- JGEGJYXHCFUMJF-UHFFFAOYSA-N 4-methylpentanal Chemical compound CC(C)CCC=O JGEGJYXHCFUMJF-UHFFFAOYSA-N 0.000 description 1
- GEKRISJWBAIIAA-UHFFFAOYSA-N 5-methylhexanal Chemical compound CC(C)CCCC=O GEKRISJWBAIIAA-UHFFFAOYSA-N 0.000 description 1
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 1
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- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
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- 229910010252 TiO3 Inorganic materials 0.000 description 1
- 229910003080 TiO4 Inorganic materials 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 235000010724 Wisteria floribunda Nutrition 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
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- IKHGUXGNUITLKF-XPULMUKRSA-N acetaldehyde Chemical compound [14CH]([14CH3])=O IKHGUXGNUITLKF-XPULMUKRSA-N 0.000 description 1
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- 150000001298 alcohols Chemical class 0.000 description 1
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- 150000004706 metal oxides Chemical class 0.000 description 1
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 1
- 125000001434 methanylylidene group Chemical group [H]C#[*] 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 150000007522 mineralic acids Chemical class 0.000 description 1
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- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
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- 239000003973 paint Substances 0.000 description 1
- QNGNSVIICDLXHT-UHFFFAOYSA-N para-ethylbenzaldehyde Natural products CCC1=CC=C(C=O)C=C1 QNGNSVIICDLXHT-UHFFFAOYSA-N 0.000 description 1
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- 235000017557 sodium bicarbonate Nutrition 0.000 description 1
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 229910052712 strontium Inorganic materials 0.000 description 1
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
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- 239000011701 zinc Substances 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
- C04B35/632—Organic additives
- C04B35/634—Polymers
- C04B35/63404—Polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C04B35/6342—Polyvinylacetals, e.g. polyvinylbutyral [PVB]
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/46—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates
- C04B35/462—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates based on titanates
- C04B35/465—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates based on titanates based on alkaline earth metal titanates
- C04B35/468—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates based on titanates based on alkaline earth metal titanates based on barium titanates
- C04B35/4682—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates based on titanates based on alkaline earth metal titanates based on barium titanates based on BaTiO3 perovskite phase
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/62605—Treating the starting powders individually or as mixtures
- C04B35/6261—Milling
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
- C04B35/632—Organic additives
- C04B35/634—Polymers
- C04B35/63448—Polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- C04B35/63488—Polyethers, e.g. alkylphenol polyglycolether, polyethylene glycol [PEG], polyethylene oxide [PEO]
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
- C04B2235/602—Making the green bodies or pre-forms by moulding
- C04B2235/6025—Tape casting, e.g. with a doctor blade
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Abstract
本发明涉及某些乙烯‑乙烯醇缩醛类在印刷墨中作为粘结剂的用途。公开了一种悬浮液组合物，其包含一种或多种无机颜料、一种或多种有机溶剂、一种或多种粘结剂、一种或多种增塑剂和一种或多种分散剂，其中所述粘结剂是包含在25～60mol％范围内的乙烯单元的乙烯‑乙烯醇缩醛类。还公开了使用所述悬浮液生产陶瓷坯片或陶瓷模塑体的方法。
Description
技术领域
本发明涉及乙烯-乙烯醇缩醛类(ethylene vinyl acetals)作为陶瓷坯片中的粘结剂的用途。
背景技术
像用于电子工业的陶瓷电容器的陶瓷材料通常通过烧结包含陶瓷材料的所谓坯片即膜状薄模塑体来生产。为了生产这些坯片，生产金属氧化物、增塑剂、分散剂和粘结剂在有机溶剂中的悬浮液。随后将悬浮液借助于合适的工艺(即刮刀工艺)以所需厚度施加到载体膜上，并且除去溶剂。由此获得的坯片必然没有裂纹，显示平滑的表面，并且仍然具有一定的弹性。
如聚乙烯醇丁醛的聚乙烯醇缩醛类经常用作生产陶瓷坯片的粘结剂。为此，DE4003 198 A1描述了用于陶瓷坯膜的流延浆料(casting slip)的生产，所述陶瓷坯膜中具有0～2重量％的残余聚乙酸乙烯酯含量的聚乙烯醇缩丁醛用作粘结剂。
近年来，多层陶瓷电容器(MLCC)在电子工业中变得越来越重要。MLCC由许多并联堆叠在一起并通过端子表面接触的独立电容器构成。由于电子组件的小型化推进，粉末颗粒的尺寸可以小到10nm。因此，生产要求其中使用的陶瓷片的精度增加。此外，在生产工艺中，陶瓷坯片的多层堆叠通常被卷绕成卷。为了避免分层，单个坯片必须在粘合和断裂伸长率方面具有优异的性能。为此，工业上需要在悬浮液中使用进一步改进的粘结剂。
因此，本发明的一个目的是提供用于陶瓷坯片的粘结剂，其导致改善的粘合性、改善的断裂伸长率、改善的分散效果、改善的环境和安全影响和/或在陶瓷坯片的生产和使用中具有更好的经济性。
已经发现这些和其他某些乙烯-乙烯醇缩醛类非常适合于作为用于陶瓷悬浮液的生产并且因此用于陶瓷坯片的生产的粘结剂。
因此，本发明涉及乙烯-乙烯醇缩醛类作为粘结剂用于生产陶瓷坯片或陶瓷模塑体的用途，其中乙烯-乙烯醇缩醛类包含在25～60mol％范围内的乙烯单元。
本发明的乙烯-乙烯醇缩醛类可以通过使醛与乙烯-乙烯醇(EVOH)进行缩醛化反应来获得。这种乙烯-乙烯醇是本领域已知的，并且可以通过在酸性催化剂存在下使乙烯共聚来获得。此外，乙烯-乙烯醇是市售可得的。
优选地，乙烯-乙烯醇是通过使乙烯和乙酸乙烯酯共聚并将所获得的共聚物水解而获得的。在水解反应中，可以使用常规已知的碱催化剂或酸催化剂，其中，使用甲醇作为溶剂和苛性钠(NaOH)催化剂的水解反应是方便的。
优选地，乙烯-乙烯醇中的乙烯单元的百分比为25～60mol％，更优选30～55mol％，并且还更优选35～50mol％。
将缩醛反应后获得的反应产物用碱中和，然后用水洗涤，获得乙烯-乙烯醇缩醛类。
对用于进行缩醛化反应的催化剂没有特别限制，并且可以使用任何有机酸或无机酸。其实例包括乙酸、对甲苯磺酸、硝酸、硫酸、盐酸、碳酸等。
虽然对乙酸酯基团的皂化度没有特别的限制，但优选为95mol％以上，更优选98mol％以上，还更优选99mol％以上，最优选99.9mol％以上。
优选地，乙烯-乙烯醇缩醛类中的乙烯单元的百分比为30～55mol％，更优选35～50mol％。还优选地，乙烯-乙烯醇缩醛类中的乙烯单元的百分比为50～60mol％。
优选地，缩醛基团单独具有1～7个碳原子，即它们来源于与具有1～7个碳原子的醛的缩合反应。更优选地，它们来源于下述组成的列表中：甲醛，乙醛，正丙醛(丙醛)，正丁醛(丁醛)，异丁醛(2-甲基-1-丙醛、异丁醛)，正戊醛(戊醛)，异戊醛(3-甲基-1-丁醛)，仲戊醛(2-甲基-1-丁醛)，叔戊醛(2,2-二甲基-1-丙醛)，正己醛(己醛)，异己醛(2-甲基-1-戊醛，3-甲基-1-戊醛，4-甲基-1-戊醛)，2,2-二甲基-1-丁醛，2,3-二甲基-1-丁醛，3,3-二甲基-1-丁醛，2-乙基-1-丁醛，正庚醛，2-甲基-1-己醛，3-甲基-1-己醛，4-甲基-1-己醛，5-甲基-1-己醛，2,2-二甲基-1-戊醛，3,3-二甲基-1-戊醛，4,4-二甲基-1-戊醛，2,3-二甲基-1-戊醛，2,4-二甲基-1-戊醛，3,4-二甲基-1-戊醛，2-乙基-1-戊醛，2-乙基-2-甲基-1-丁醛，2-乙基-3-甲基-1-丁醛，3-乙基-2-甲基-1-丁醛，环己醛和苯甲醛。最优选地，它们来源于与异丁醛、乙醛和/或正丁醛的缩合反应。
还优选地，根据本发明的乙烯-乙烯醇缩醛类是混合缩醛，即它们包含至少两种不同的缩醛基团。换句话说，本发明中使用的乙烯-乙烯醇缩醛类包括来源于相应的乙烯乙烯醇的两个羟基与第一醛的反应的第一缩醛基团和至少来源于相应的乙烯乙烯醇的另外两个羟基与第二醛的反应的第二缩醛基团，其中第一醛不同于第二醛。优选的醛与上面列出的具有一个缩醛基团的缩醛中使用的相同；最优选的组合为来源于乙醛和正丁醛的缩醛的混合物。
虽然对本发明的本实施方案中使用的乙烯-乙烯醇缩醛类的生产方法没有特别限制，但它们可以通过在酸性条件下将醛添加到乙烯乙烯醇溶液并且进行缩醛化反应的方法来生产。
优选地，本发明中使用的乙烯-乙烯醇缩醛类的缩醛化程度为5mol％以上且小于40mol％，更优选缩醛化程度的下限为大于6mol％、大于7mol％、大于8mol％、大于9mol％，最优选大于10mol％。此外，缩醛化程度的上限更优选依次为38mol％以下、36mol％以下、34mol％以下、32mol％以下，最优选小于30mol％。
优选地，本发明的乙烯-乙烯醇缩醛类树脂中的乙烯醇单元基于构成树脂的总单体单元的百分比为24～71mol％。
根据DIN ISO 3681(乙酸酯含量)和DIN ISO 53240(PVA含量)确定乙烯-乙烯醇缩醛类的乙烯醇含量和乙酸乙烯酯含量。乙烯醇缩醛类含量可以计算为根据DIN ISO 53401/53240确定的乙烯醇含量和乙酸乙烯酯含量之和以及成为100所需的乙烯的剩余部分。缩醛化程度可以通过乙烯醇缩醛类含量除以乙烯醇含量、乙烯醇缩醛类含量和乙酸乙烯酯含量之和来计算。通过本领域技术人员已知的公式实现从重量％换算为mol％。
通过NMR光谱测量乙烯-乙酸乙烯酯共聚物的乙烯含量。首先，将乙烯-乙烯醇缩醛类树脂溶解在乙醇中，加入2N盐酸盐羟胺溶液和盐酸，并且在水浴中在用冷凝器回流下搅拌混合物4小时，冷却后，加入氨水。然后，加入甲醇，将聚合物沉淀、洗涤和干燥，获得乙酰化的乙烯-乙烯醇共聚物。然后，在120℃下将乙酰化的乙烯-乙烯醇共聚物溶解在DMSO(二甲基亚砜)中，冷却至室温，然后向其中加入N,N-二甲基-4-氨基吡啶和乙酸酐，接着搅拌1小时，接着用离子交换水和丙酮沉淀，并且干燥，获得乙烯-乙酸乙烯酯共聚物。将聚合物溶解在DMSO-d6中，并通过400MHz的质子NMR光谱仪进行测量。将获得的光谱积分256次。乙烯-乙烯醇共聚物的乙烯单元的摩尔比由源自乙烯单元和乙酸乙烯酯单元的次甲基质子(1.1～1.9ppm的峰)和源自乙酸乙烯酯单元的末端甲基质子(2.0ppm的峰)的强度比计算出。注意，由于乙烯单元不受缩醛化反应的影响，所以缩醛化反应前的乙烯-乙烯醇共聚物的乙烯单元的摩尔比(n)等于缩醛化反应后获得的乙烯-乙烯醇缩醛类树脂的乙烯单元的摩尔比(n)。
在第二方面，本发明涉及包含一种或多种无机颜料、一种或多种有机溶剂、一种或多种粘结剂、一种或多种增塑剂和一种或多种分散剂的悬浮液组合物，其中粘结剂是包含在25～60mol％范围内的乙烯单元的乙烯-乙烯醇缩醛类。
优选地，缩醛基团具有2～7个碳原子并且来源于与上述相同的醛。最优选地，乙烯-乙烯醇缩醛类包含正丁醛缩醛基团和/或乙醛缩醛基团。
无机颜料可以选自顺电或铁电原料的精细研磨的颗粒，并且包括二氧化钛(金红石)，优选通过锌、锆、铌、镁、钽、钴和/或锶的添加剂以及选自MgNb2O6、ZnNb2O6、MgTa2O6、ZnTa2O6、(ZnMg)TiO3、(ZrSn)TiO4和Ba2Ti9O20或BaTiO3(钛酸钡)的化合物改性。无机颜料的平均粒径优选为约0.01～1μm。
有机溶剂可以选自芳香族化合物，如甲苯和二甲苯；和醇化合物，如乙醇、异丙醇和丁醇，更优选其混合物。
适合的分散剂包括鱼油、磷酸酯和在侧链上包含聚氧亚烷基的功能聚合物，如从NOF America Cooperation商购可得的MALIALIMTM系列。
除了根据本发明的粘结剂，悬浮液还可以包含尤其选自其它粘结剂、如聚乙二醇或邻苯二甲酸酯的增塑剂、和/或消泡剂的其它组分，所述其它粘结剂如纤维素树脂、丙烯酸类树脂、乙酸乙烯酯树脂、聚乙烯醇树脂。
悬浮液组合物的生产方法没有特别限制。可以使用各种分散方法，例如，使用介质型研磨机如珠磨机、球磨机、磨碎机、油漆摇拌器和砂磨机的方法，；捏合粉状陶瓷、分散介质、分散剂、粘结剂、增塑剂等的方法；和使用三辊研磨机的方法。使用三辊研磨机，该方法包括将粉状无机颜料和分散剂、粘结剂、增塑剂等一起分散在有机溶剂(混合物)中。
优选地，将粉状陶瓷、分散剂和溶剂(混合物)预混合并分散，使得分散剂吸附在粉状陶瓷上。在第二步骤中，向这样形成的混合物中添加粘结剂，随后，再次进行混合和分散。
通过这些工艺生产的涂布膜的厚度可为0.25～25μm，并且通常为0.5～10μm。
实施例
实施例1乙烯-乙烯醇缩醛类
将根据日本专利申请特开No.2016-28139中描述的工艺合成的100重量份含有44mol％乙烯单元的(皂化度：99％)的乙烯乙烯醇共聚物分散在315重量份1-丙醇中，并在搅拌下将溶液温度升高至60℃。然后，添加40重量份1M盐酸，接着加入34.2重量份正丁醛，同时保持温度在60℃下。随着反应进行，乙烯-乙烯醇共聚物溶解，并且反应混合物变成均相溶液。36小时后，加入6.4重量份碳酸氢钠以停止反应。在向反应溶液中加入500重量份1-丙醇以使其均匀后，将其滴加到2000重量份水中以沉淀树脂。此后，过滤和水洗的操作重复三次，所得固体在60℃下真空干燥8小时。这样获得的乙烯-乙烯醇缩醛类具有44mol％的乙烯单元含量和46mol％的缩醛化程度。
比较例1正丁基缩醛类
使用从Kuraray Europe GmbH获得的包含由正丁醛和聚合物链中没有乙烯单元的聚乙烯醇制备的缩醛单元的聚乙烯醇缩醛树脂B 75H制备PVB溶液。将该PVB溶液用作粘结剂溶液来制备陶瓷坯片。坯片制备的描述细节在下节中。
无机分散体的制备
将1.3g聚氧亚烷基分散剂(MALIALIMTM系列，名称：SC-0505K，供应商：NOF)添加到25g甲苯和25g乙醇的混合溶剂中并且通过搅拌溶解。接下来，将130g钛酸钡粉末(由FujiTitanium Industry制造，UQBT-20)和500gZrO2珠(直径：2mm)添加到获得的溶液中。将有机分散体在辊式混合器上混合6-8小时。
树脂溶液的制备
通过将10.4g(聚乙烯醇)缩醛树脂和3.95g增塑剂3G8添加到59.8g乙醇和59.8g甲苯的混合溶剂中来制备树脂溶液。搅拌混合物以溶解树脂。
陶瓷坯片的生产
将树脂溶液添加到获得的无机分散体中并且使用辊式坯料(block)混合器混合10h以获得用于陶瓷坯片的组合物。
使用尼龙筛网/过滤器将ZrO2珠从分散体中分离。
将获得的分散体脱气，并使用自动膜涂机根据刮刀工艺流延(casted)。硅化PET(RN 2 SLK，厚度75μm)用作流延支承体。流延后，将膜在空气中干燥24小时(温度：23℃，相对湿度：50％)，随后抽出。
获得的膜的厚度为15μm并且在光学评估期间出现裂纹、起泡或缺陷。
从涉及的坯片中，冲压出所谓“狗骨”形式的适合的拉伸试样。与流延方向交叉冲压出每种类型的膜的8个拉伸试样并且通过人眼检查。对于实施例1和比较例1二者，选择看起来具有来自冲压工艺的最少缺陷的4个试样用于测量。将万能拉伸试验机用于拉伸力测量。根据DIN EN ISO 527-1和DIN EN ISO 527-3，在23℃和50％相对湿度的受控条件下进行测量。
表1：拉伸试验的结果
拉伸试验的结果显示用乙烯-乙烯醇缩醛类获得的陶瓷坯片的断裂伸长率值大于用PVB标准获得的两倍。
Claims (8)
1.乙烯-乙烯醇缩醛类作为粘结剂用于生产陶瓷坯片或陶瓷模塑体的用途，其中所述乙烯-乙烯醇缩醛类包含在25～60mol％范围内的乙烯单元。
2.根据权利要求1所述的用途，其中所述缩醛基团具有2至7个碳原子。
3.根据权利要求1或2所述的用途，其中所述乙烯-乙烯醇缩醛类包含正丁醛缩醛基团和/或异丁醛缩醛基团。
4.根据权利要求1至3中任一项所述的用途，其中所述乙烯-乙烯醇缩醛类中的残余乙烯醇为15～40mol％。
5.一种悬浮液组合物，其包含一种或多种无机颜料、一种或多种有机溶剂、一种或多种粘结剂、一种或多种增塑剂和一种或多种分散剂，其中所述粘结剂是包含在25～60mol％范围内的乙烯单元的乙烯-乙烯醇缩醛类。
6.根据权利要求5所述的悬浮液，其中所述缩醛基团具有2至7个碳原子。
7.根据权利要求5或6所述的悬浮液，其中所述乙烯-乙烯醇缩醛类包含正丁醛缩醛基团和/或乙醛缩醛基团。
8.一种使用根据权利要求5至7中任一项所述的悬浮液生产陶瓷坯片或陶瓷模塑体的方法。
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| EP21201836.0A EP4163265A1 (en) | 2021-10-11 | 2021-10-11 | Use of ethylene vinyl acetals as binder in ceramic green sheets |
| EP21201836.0 | 2021-10-11 | ||
| PCT/EP2022/076702 WO2023061741A1 (en) | 2021-10-11 | 2022-09-26 | Use of ethylene vinyl acetals as binder in ceramic green sheets |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN118076571A true CN118076571A (zh) | 2024-05-24 |
Family
ID=78402038
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202280068098.7A Pending CN118076571A (zh) | 2021-10-11 | 2022-09-26 | 乙烯-乙烯醇缩醛类作为陶瓷坯片中的粘结剂的用途 |
Country Status (3)
| Country | Link |
|---|---|
| EP (1) | EP4163265A1 (zh) |
| CN (1) | CN118076571A (zh) |
| WO (1) | WO2023061741A1 (zh) |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE4003198A1 (de) | 1990-02-03 | 1991-08-08 | Hoechst Ceram Tec Ag | Giessmasse zur herstellung keramischer gruenfolien und ihre verwendung |
| JP6239841B2 (ja) * | 2013-03-27 | 2017-11-29 | 積水化学工業株式会社 | セラミックグリーンシート用スラリー組成物 |
| JP6178093B2 (ja) * | 2013-03-29 | 2017-08-09 | 積水化学工業株式会社 | 変性ポリビニルアセタール樹脂 |
| EP2963496B1 (en) * | 2014-06-30 | 2017-04-05 | Agfa Graphics NV | A lithographic printing plate precursor including ( ethylene, vinyl acetal ) copolymers |
| JP6704688B2 (ja) | 2014-07-11 | 2020-06-03 | 株式会社クラレ | 樹脂組成物及び多層構造体 |
-
2021
- 2021-10-11 EP EP21201836.0A patent/EP4163265A1/en not_active Withdrawn
-
2022
- 2022-09-26 WO PCT/EP2022/076702 patent/WO2023061741A1/en unknown
- 2022-09-26 CN CN202280068098.7A patent/CN118076571A/zh active Pending
Also Published As
| Publication number | Publication date |
|---|---|
| EP4163265A1 (en) | 2023-04-12 |
| WO2023061741A1 (en) | 2023-04-20 |
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