JPS6363568B2 - - Google Patents
Info
- Publication number
- JPS6363568B2 JPS6363568B2 JP869278A JP869278A JPS6363568B2 JP S6363568 B2 JPS6363568 B2 JP S6363568B2 JP 869278 A JP869278 A JP 869278A JP 869278 A JP869278 A JP 869278A JP S6363568 B2 JPS6363568 B2 JP S6363568B2
- Authority
- JP
- Japan
- Prior art keywords
- vinyl acetate
- acetate copolymer
- mol
- ethylene
- saponified ethylene
- 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.)
- Expired
Links
- 239000005038 ethylene vinyl acetate Substances 0.000 claims description 30
- 229920001200 poly(ethylene-vinyl acetate) Polymers 0.000 claims description 30
- 239000006185 dispersion Substances 0.000 claims description 21
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 18
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 claims description 15
- 239000005977 Ethylene Substances 0.000 claims description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- 239000000839 emulsion Substances 0.000 claims description 13
- 238000007127 saponification reaction Methods 0.000 claims description 12
- 239000004094 surface-active agent Substances 0.000 claims description 12
- 238000009775 high-speed stirring Methods 0.000 claims description 11
- 238000010438 heat treatment Methods 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 7
- 238000004519 manufacturing process Methods 0.000 claims description 5
- 150000001298 alcohols Chemical class 0.000 claims description 4
- 125000004432 carbon atom Chemical group C* 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 2
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 30
- 235000019441 ethanol Nutrition 0.000 description 19
- 238000000034 method Methods 0.000 description 10
- 239000002245 particle Substances 0.000 description 5
- -1 plastic moldings Substances 0.000 description 5
- 238000000576 coating method Methods 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 229920005989 resin Polymers 0.000 description 4
- 239000011347 resin Substances 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 3
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 3
- 229920001577 copolymer Polymers 0.000 description 3
- 239000011253 protective coating Substances 0.000 description 3
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 2
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 description 2
- DKGAVHZHDRPRBM-UHFFFAOYSA-N Tert-Butanol Chemical compound CC(C)(C)O DKGAVHZHDRPRBM-UHFFFAOYSA-N 0.000 description 2
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical compound CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 description 2
- 239000003945 anionic surfactant Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- ZXEKIIBDNHEJCQ-UHFFFAOYSA-N isobutanol Chemical compound CC(C)CO ZXEKIIBDNHEJCQ-UHFFFAOYSA-N 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000012046 mixed solvent Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 238000010137 moulding (plastic) Methods 0.000 description 2
- 239000000123 paper Substances 0.000 description 2
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 2
- 235000019333 sodium laurylsulphate Nutrition 0.000 description 2
- 239000002023 wood Substances 0.000 description 2
- JHPBZFOKBAGZBL-UHFFFAOYSA-N (3-hydroxy-2,2,4-trimethylpentyl) 2-methylprop-2-enoate Chemical compound CC(C)C(O)C(C)(C)COC(=O)C(C)=C JHPBZFOKBAGZBL-UHFFFAOYSA-N 0.000 description 1
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- RNMDNPCBIKJCQP-UHFFFAOYSA-N 5-nonyl-7-oxabicyclo[4.1.0]hepta-1,3,5-trien-2-ol Chemical compound C(CCCCCCCC)C1=C2C(=C(C=C1)O)O2 RNMDNPCBIKJCQP-UHFFFAOYSA-N 0.000 description 1
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 description 1
- 239000004925 Acrylic resin Substances 0.000 description 1
- 229920000178 Acrylic resin Polymers 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 description 1
- AMQJEAYHLZJPGS-UHFFFAOYSA-N N-Pentanol Chemical compound CCCCCO AMQJEAYHLZJPGS-UHFFFAOYSA-N 0.000 description 1
- 229920001214 Polysorbate 60 Polymers 0.000 description 1
- 125000003158 alcohol group Chemical group 0.000 description 1
- 150000001449 anionic compounds Chemical class 0.000 description 1
- 125000000129 anionic group Chemical group 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 229940105990 diglycerin Drugs 0.000 description 1
- GPLRAVKSCUXZTP-UHFFFAOYSA-N diglycerol Chemical compound OCC(O)COCC(O)CO GPLRAVKSCUXZTP-UHFFFAOYSA-N 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 description 1
- 238000004945 emulsification Methods 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 235000011187 glycerol Nutrition 0.000 description 1
- 230000001771 impaired effect Effects 0.000 description 1
- 229940035429 isobutyl alcohol Drugs 0.000 description 1
- 229960004592 isopropanol Drugs 0.000 description 1
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 239000002736 nonionic surfactant Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000005022 packaging material Substances 0.000 description 1
- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical compound OCC(CO)(CO)CO WXZMFSXDPGVJKK-UHFFFAOYSA-N 0.000 description 1
- 229920005862 polyol Polymers 0.000 description 1
- 150000003077 polyols Chemical class 0.000 description 1
- 229920000259 polyoxyethylene lauryl ether Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 description 1
- DAJSVUQLFFJUSX-UHFFFAOYSA-M sodium;dodecane-1-sulfonate Chemical compound [Na+].CCCCCCCCCCCCS([O-])(=O)=O DAJSVUQLFFJUSX-UHFFFAOYSA-M 0.000 description 1
- BWYYYTVSBPRQCN-UHFFFAOYSA-M sodium;ethenesulfonate Chemical compound [Na+].[O-]S(=O)(=O)C=C BWYYYTVSBPRQCN-UHFFFAOYSA-M 0.000 description 1
- 230000003381 solubilizing effect Effects 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 229920001897 terpolymer Polymers 0.000 description 1
- 239000011882 ultra-fine particle Substances 0.000 description 1
- 238000009834 vaporization Methods 0.000 description 1
- 230000008016 vaporization Effects 0.000 description 1
Landscapes
- Processes Of Treating Macromolecular Substances (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Description
【発明の詳細な説明】
本発明はエチレン−酢酸ビニル系共重合体けん
化物乳化分散液の製造法に関するものである。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for producing an emulsified dispersion of a saponified ethylene-vinyl acetate copolymer.
エチレン−酢酸ビニル共重合体けん化物は、酸
素バリヤー性や耐薬品性に優れているため包装材
料素材や、プラスチツクス成型物、金属表面、
紙、木材などの保護被覆用樹脂として極めて優れ
たものである。 Saponified ethylene-vinyl acetate copolymer has excellent oxygen barrier properties and chemical resistance, so it can be used as packaging materials, plastic moldings, metal surfaces,
It is an extremely excellent resin for the protective coating of paper, wood, etc.
かかる保護被覆用樹脂としては、特公昭47−
48489号に開示されている方法、即ちアルコール
−水混合溶媒に溶解した溶液状のものがある。し
かしながら上記方法に於ける溶液状のものには、
多量のアルコールが存在しているため、被膜形成
過程に於いてアルコールの気散による作業環境の
悪化及びアルコール回収のための装置を要するな
どの経済的不利な条件を有しているものである。 As such a resin for protective coating, Japanese Patent Publication No. 47-
There is a method disclosed in No. 48489, that is, a method in which the solution is dissolved in an alcohol-water mixed solvent. However, for the solution in the above method,
Since a large amount of alcohol is present, it has disadvantageous economic conditions, such as deterioration of the working environment due to the vaporization of alcohol during the film formation process and the need for equipment for alcohol recovery.
また、エチレン−酢酸ビニル共重合体けん化物
を水と界面活性剤に可溶化又は、分散する方法が
開示されている。特公昭50−33697号では陰イオ
ン界面活性剤を多量に使用し、エチレン−酢酸ビ
ニル共重合体けん化物を可溶化しているが、かか
る方法では、界面活性剤が多量に存在しているた
め形成被膜がもろく、表面保護被膜として不適で
あり、エチレン−酢酸ビニル系共重合体けん化物
の特性を損なうものである。 Also disclosed is a method of solubilizing or dispersing a saponified ethylene-vinyl acetate copolymer in water and a surfactant. In Japanese Patent Publication No. 50-33697, a large amount of anionic surfactant is used to solubilize the saponified ethylene-vinyl acetate copolymer. The film formed is brittle and unsuitable as a surface protective film, and the properties of the saponified ethylene-vinyl acetate copolymer are impaired.
さらに、特開昭50−63275号に於ける方法は、
単にエチレン−酢酸ビニル共重合体けん化物の微
粉末を分散し、水サスペンジヨンとしたものにす
ぎず、表面保護被覆用として不適なものである。 Furthermore, the method in JP-A No. 50-63275 is
This is merely a suspension of water by dispersing fine powder of a saponified ethylene-vinyl acetate copolymer, and is therefore unsuitable for use as a surface protective coating.
本発明者は、上記従来方法の諸欠点を解決し、
表面被覆用及び中間被覆用として有用なエチレン
−酢酸ビニル系共重合体けん化物乳化分散液を製
造する方法について、検討を重ねた結果、エチレ
ン−酢酸ビニル系共重合体けん化物を炭素数１〜
５のアルコール群から選ばれた１種又は、２種以
上の混合物と水及び界面活性剤存在下に加温溶解
し、強制高速撹拌下に於いて、該アルコールを除
去しながら乳化分散することによつて、均一な乳
化分散液が得られることを見い出し、本発明を完
成するにいたつたのである。 The present inventor solved the various drawbacks of the above conventional methods,
As a result of repeated studies on a method for producing an emulsified dispersion of a saponified ethylene-vinyl acetate copolymer useful for surface coatings and intermediate coatings, we found that a saponified ethylene-vinyl acetate copolymer having a carbon number of 1 to
One type or a mixture of two or more selected from the alcohol group No. 5 is dissolved by heating in the presence of water and a surfactant, and emulsified and dispersed while removing the alcohol under forced high-speed stirring. Therefore, they discovered that a uniform emulsified dispersion can be obtained and completed the present invention.
本発明では、特に加温溶解後に強制高速撹拌
下、アルコールを除去しながら乳化分散する点に
特徴があり、かかる方法以外では本発明で得られ
る分散液ほど優れた均一性を達成することはでき
ない。 The present invention is particularly characterized in that it emulsifies and disperses while removing alcohol under forced high-speed stirring after heating and dissolving, and it is not possible to achieve uniformity as excellent as the dispersion obtained by the present invention by any method other than this method. .
本発明によつて得られたエチレン−酢酸ビニル
系共重合体けん化物乳化分散液は、溶媒が水単独
又は水と極少量のアルコールであるから、被膜形
成時に於いて作業環境を悪化することはなく安全
に使用出来るものであり、またエチレン−酢酸ビ
ニル系共重合体けん化物の特性を生かしてプラス
チツクス成型物、金属、紙、木材など表面被覆用
や中間被膜用として有用なものである。 Since the ethylene-vinyl acetate copolymer saponified emulsion dispersion obtained by the present invention uses water alone or water and a very small amount of alcohol as a solvent, the working environment will not be deteriorated during film formation. It is safe to use, and by taking advantage of the properties of the saponified ethylene-vinyl acetate copolymer, it is useful as a surface coating or intermediate coating for plastic moldings, metals, paper, wood, etc.
さらにまた本発明によつて得られたエチレン−
酢酸ビニル系共重合体けん化物乳化分散液は、通
常のエマルジヨン、例えば酢酸ビニル樹脂エマル
ジヨン、アクリル樹脂エマルジヨン、エチレン−
酢酸ビニル系共重合体エマルジヨンなどとブレン
ドして、用途に応じた使用が可能であり、特にエ
チレン−酢酸ビニル系共重合体エマルジヨンとの
配合物は、造膜性、密着性の向上をもたらすもの
である。 Furthermore, ethylene obtained according to the present invention
The saponified vinyl acetate copolymer emulsion dispersion can be prepared using ordinary emulsions such as vinyl acetate resin emulsion, acrylic resin emulsion, and ethylene-based emulsion.
It can be used depending on the application by blending with vinyl acetate copolymer emulsion etc. In particular, blending with ethylene-vinyl acetate copolymer emulsion improves film forming properties and adhesion. It is.
本発明で用いられるエチレン−酢酸ビニル系共
重合体けん化物は、エチレン、酢酸ビニル成分の
ほかに、共重合性単量体、例えばアクリル酸、メ
タアクリル酸、アクリル酸エステル、メタアクリ
ル酸エステル、無水マレイン酸、アクリル酸アミ
ド、などの第三成分との三元共重合体をも使用し
うるものであつて、その量としては10モル％以下
が好ましい。 The saponified ethylene-vinyl acetate copolymer used in the present invention contains, in addition to ethylene and vinyl acetate components, copolymerizable monomers such as acrylic acid, methacrylic acid, acrylic ester, methacrylic ester, A terpolymer with a third component such as maleic anhydride or acrylamide may also be used, and the amount thereof is preferably 10 mol % or less.
本発明で用いられるアルコールとしては炭素数
が１〜５のものであり、メチルアルコール、エチ
ルアルコール、ｎ−プロピルアルコール、iso−
プロピルアルコール、ｎ−ブチルアルコール、
iso−ブチルアルコール、ｔ−ブチルアルコール、
アミルアルコールなどの１種又は２種以上の混合
アルコールがあげられるが、工業的には、価格及
び除去性の点からメチルアルコールが好ましい。 The alcohol used in the present invention has 1 to 5 carbon atoms, such as methyl alcohol, ethyl alcohol, n-propyl alcohol, iso-
Propyl alcohol, n-butyl alcohol,
iso-butyl alcohol, t-butyl alcohol,
Examples include one or more mixed alcohols such as amyl alcohol, but methyl alcohol is preferred industrially from the viewpoint of cost and removability.
水とアルコールの比率は水／アルコール＝５／
５〜２／８（容積比）が好ましく、溶解温度はア
ルコールの沸点近くまで上げられるが、好ましく
は60〜90℃の範囲である。水−アルコール混合溶
媒に対するエチレン−酢酸ビニル系共重合体けん
化物の量は、温度60〜90℃に於ける溶解度まで加
えることが出来る。加温溶解後、アルコールを除
去する過程に於いて、該けん化物の溶解度が減少
し、該けん化物が極微粒子状に析出し、強制高速
撹拌によつて乳化分散する。 The ratio of water and alcohol is water/alcohol = 5/
A ratio of 5 to 2/8 (volume ratio) is preferred, and the dissolution temperature is raised to near the boiling point of the alcohol, preferably in the range of 60 to 90°C. The amount of saponified ethylene-vinyl acetate copolymer added to the water-alcohol mixed solvent can be adjusted up to the solubility at a temperature of 60 to 90°C. After heating and dissolving, in the process of removing alcohol, the solubility of the saponified product decreases, and the saponified product precipitates into ultrafine particles, which are emulsified and dispersed by forced high-speed stirring.
本発明で用いられる界面活性剤としては、通常
のアニオン系、ノニオン系があげられる。アニオ
ン系としては、ビニルスルフオン酸ソーダ、ドデ
シルベンゼンスルフオン酸ソーダ、ラウリルスル
フオン酸ソーダ、などであり、ノニオン系として
は、ポリオキシエチレンラウリルエーテル、ポリ
オキシエチレンノニルフエノールエーテル、ポリ
オキシエチレンソルビタンモノオレートなどであ
る。界面活性剤の使用量としては、乳化分散可能
であり、且つ形成被膜の特性を損なわない量とし
て、樹脂100部に対して0.1〜４部の範囲が好まし
い。 Examples of the surfactant used in the present invention include ordinary anionic and nonionic surfactants. Examples of anionic compounds include sodium vinyl sulfonate, sodium dodecylbenzenesulfonate, sodium lauryl sulfonate, etc.; examples of nonionic compounds include polyoxyethylene lauryl ether, polyoxyethylene nonylphenol ether, and polyoxyethylene sorbitan. These include monooleate. The amount of the surfactant to be used is preferably in the range of 0.1 to 4 parts per 100 parts of the resin, which allows emulsification and dispersion and does not impair the properties of the formed film.
本発明では、さらに通常の造膜助剤のほかに、
エチレングリコール、グリセリン、ジグリセリ
ン、ペンタエリスリトールなどのポリオールなど
を少量添加しうる。 In the present invention, in addition to the usual film forming aid,
Small amounts of polyols such as ethylene glycol, glycerin, diglycerin, and pentaerythritol may be added.
本発明で用いられる強制高速撹拌装置として
は、高速ミキサー、ホモジナイザー、などがあげ
られる。 Examples of the forced high-speed stirring device used in the present invention include a high-speed mixer, a homogenizer, and the like.
次に本発明の実施態様を示す。 Next, embodiments of the present invention will be shown.
(1) エチレン含有量20〜50モル％、けん化度80モ
ル％以上のエチレン−酢酸ビニル系共重合体け
ん化物を炭素１〜５のアルコール群から選ばれ
た１種又は２種以上の混合物と水及び界面活性
剤の存在下、加温溶解する。次に強制高速撹拌
下に、減圧によつて、アルコール成分を除去し
ながら均一な乳化分散液をうる。(1) A saponified ethylene-vinyl acetate copolymer having an ethylene content of 20 to 50 mol% and a saponification degree of 80 mol% or more is mixed with one type or a mixture of two or more selected from the group of alcohols having 1 to 5 carbon atoms. Dissolve by heating in the presence of water and surfactant. Next, under forced high-speed stirring and under reduced pressure, a uniform emulsified dispersion is obtained while removing the alcohol component.
(2) エチレン含有量20〜50モル％、けん化度80モ
ル％以上のエチレン−酢酸ビニル系共重合体け
ん化物を(1)と同様にして加温溶解する。次に冷
却によつて、該けん化物を微粒子分散ゲル状に
析出させる。この微粒子分散ゲル状物を界面活
性剤を含む水中に強制高速撹拌下に添加し、同
時に減圧によつてアルコール成分を除去して均
一な乳化分散液とする。(1)に於けるよりも、よ
り均一微細な乳化分散液が得られる。(2) A saponified ethylene-vinyl acetate copolymer having an ethylene content of 20 to 50 mol% and a saponification degree of 80 mol% or more is heated and dissolved in the same manner as in (1). Next, by cooling, the saponified product is precipitated into a fine particle-dispersed gel. This fine particle-dispersed gel is added to water containing a surfactant under forced high-speed stirring, and at the same time the alcohol component is removed under reduced pressure to form a uniform emulsified dispersion. A more uniform and fine emulsified dispersion can be obtained than in (1).
(3) エチレン含有量20〜50モル％、けん化度80モ
ル％以上のエチレン−酢酸ビニル系共重合体け
ん化物とエチレン含有量85〜95モル％、けん化
度80モル％以上のエチレン−酢酸ビニル系共重
合体けん化物との混合物を炭素数が１〜５のア
ルコール群から選ばれた１種又は２種以上の混
合物と水及び界面活性剤の存在下、強制高速撹
拌し加温溶解分散させる。次に減圧によつて、
アルコール成分を除去し、乳化分散液とする。
エチレン含有量85〜90モル％、けん化度80モル
％以上のエチレン−酢酸ビニル系共重合体けん
化物(B)は、加温時に於いても単に分散状態にあ
るが、脱アルコール過程に於いて、エチレン含
有量20〜50モル％、けん化度80モル％以上のエ
チレン−酢酸ビニル系共重合体けん化物(A)が微
粒子状に乳化するにともない全体が均一な乳化
分散液として得られる。(3) A saponified ethylene-vinyl acetate copolymer with an ethylene content of 20 to 50 mol% and a saponification degree of 80 mol% or more and an ethylene-vinyl acetate copolymer with an ethylene content of 85 to 95 mol% and a saponification degree of 80 mol% or more. A mixture of a saponified copolymer and a mixture of one or more selected from the group of alcohols having 1 to 5 carbon atoms is subjected to forced high-speed stirring in the presence of water and a surfactant to dissolve and disperse by heating. . Then, by reducing the pressure,
The alcohol component is removed to form an emulsified dispersion.
The saponified ethylene-vinyl acetate copolymer (B) with an ethylene content of 85 to 90 mol% and a saponification degree of 80 mol% or more remains in a dispersed state even during heating, but in the dealcoholization process. As the saponified ethylene-vinyl acetate copolymer (A) having an ethylene content of 20 to 50 mol% and a saponification degree of 80 mol% or more is emulsified into fine particles, an entirely uniform emulsified dispersion is obtained.
(B)成分の量としては30重量％以下が好ましく、
(B)成分の添加によつて、造膜性と密着性が向上す
るものである。 The amount of component (B) is preferably 30% by weight or less,
Addition of component (B) improves film-forming properties and adhesion.
次に本発明を実施例によつて具体的に説明す
る。実施例中「部」は「重量部」を示す。 Next, the present invention will be specifically explained using examples. In the examples, "parts" indicate "parts by weight."
実施例 １
エチレン含有量30モル％、けん化度99モル％の
エチレン−酢酸ビニル共重合体けん化物20部をメ
タノール170部、水90部、界面活性剤（ラウリル
硫酸ソーダ）0.2部に加え、撹拌し温度60〜65℃
にて溶解する。次に高速ミキサーにて、強制高速
撹拌しながら、真空ポンプにて減圧下、メタノー
ルを系外に除去した。メタノールが系外に除去さ
れるにつれて乳化分散し、均一な乳化液が得られ
た。得られた乳化分散液の固形分量は約20重量％
であり、平均粒子径は1.0μであつた。Example 1 20 parts of a saponified ethylene-vinyl acetate copolymer with an ethylene content of 30 mol% and a saponification degree of 99 mol% were added to 170 parts of methanol, 90 parts of water, and 0.2 parts of a surfactant (sodium lauryl sulfate), and the mixture was stirred. Temperature 60-65℃
Dissolve at . Next, methanol was removed from the system under reduced pressure using a vacuum pump while forced high-speed stirring was performed using a high-speed mixer. As methanol was removed from the system, it was emulsified and dispersed, and a uniform emulsion was obtained. The solid content of the obtained emulsified dispersion was approximately 20% by weight.
The average particle diameter was 1.0μ.
実施例 ２
実施例１と同様にして溶解液を得た後、これを
室温まで冷却し、微粒子状ゲル物を得た。次に水
90部に界面活性剤（ラウリル硫酸ソーダ）0.2部
を添加し、高速ミキサーにて撹拌しながら、上記
微粒子状ゲル物を添加すると均一な乳化液が得ら
れた。実施例１と同様にして、メタノール臭がな
くなるまで、メタノールを除去した。得られた乳
化分散液の固形分量は約10重量％であり、平均粒
子径は0.5μであつた。この乳化液をガラス板に塗
布し、室温にて乾燥したところ透明な被膜が形成
された。Example 2 A solution was obtained in the same manner as in Example 1, and then cooled to room temperature to obtain a particulate gel. then water
To 90 parts, 0.2 part of a surfactant (sodium lauryl sulfate) was added, and while stirring with a high-speed mixer, the above-mentioned particulate gel was added, and a uniform emulsion was obtained. Methanol was removed in the same manner as in Example 1 until the methanol odor disappeared. The solid content of the obtained emulsified dispersion was about 10% by weight, and the average particle size was 0.5μ. When this emulsion was applied to a glass plate and dried at room temperature, a transparent film was formed.
実施例 ３
エチレン含有量30モル％、けん化度99モル％の
エチレン−酢酸ビニル共重合体けん化物16部とエ
チレン含有量約86モル％、けん化度約90モル％の
エチレン−酢酸ビニル系共重合体けん化物４部を
メタノール170部、水90部、界面活性剤0.2部に加
え、撹拌し温度60〜65℃にて溶解分散した。次に
高速ミキサーにて、強制高速撹拌しながら、真空
ポンプにて減圧下、メタノールを系外に除去し、
乳化分散液を得た。得られた乳化分散液の固形分
量は約20重量％であり、平均粒子径は2μであつ
た。Example 3 16 parts of saponified ethylene-vinyl acetate copolymer with an ethylene content of 30 mol% and a saponification degree of 99 mol% and an ethylene-vinyl acetate copolymer with an ethylene content of about 86 mol% and a saponification degree of about 90 mol% 4 parts of the combined saponified product were added to 170 parts of methanol, 90 parts of water, and 0.2 parts of surfactant, and the mixture was stirred and dissolved and dispersed at a temperature of 60 to 65°C. Next, methanol is removed from the system under reduced pressure using a vacuum pump while forced high-speed stirring is performed using a high-speed mixer.
An emulsified dispersion was obtained. The solid content of the obtained emulsified dispersion was about 20% by weight, and the average particle size was 2μ.
対照例
実施例１において真空ポンプによるメタノール
除去を行わずに強制高速撹拌のみを行つて乳化分
散液を得、しかる後減圧下にアルコールを除去し
た。得られた乳化分散液の固形分量は約20重量％
で実施例１と同程度であつたが、粒度分布は0.05
〜5μとかなりばらつきがあり、均一性の点で劣
つていた。Comparative Example In Example 1, only forced high-speed stirring was performed without removing methanol using a vacuum pump to obtain an emulsified dispersion, and then the alcohol was removed under reduced pressure. The solid content of the obtained emulsified dispersion was approximately 20% by weight.
The particle size distribution was about the same as in Example 1, but the particle size distribution was 0.05.
There was considerable variation of ~5μ, and the uniformity was poor.
Claims (1)
ル％以上のエチレン−酢酸ビニル系共重合体けん
化物を炭素数１〜５のアルコール群から選ばれた
１種又は２種以上の混合物と水及び界面活性剤存
在下に加温溶解し、強制高速撹拌下に於いて、該
アルコールを除去しながら乳化分散することを特
徴とするエチレン−酢酸ビニル系共重合体けん化
物乳化分散液の製造法。 ２ エチレン−酢酸ビニル系共重合体けん化物
が、エチレン含有量20〜50モル％、けん化度80モ
ル％以上のエチレン−酢酸ビニル共重合体けん化
物とエチレン含有量85〜90モル％、けん化度80モ
ル％以上のエチレン−酢酸ビニル共重合体けん化
物とを100／０〜70／30（重量比）の割合で併用す
る特許請求の範囲第１項記載のエチレン−酢酸ビ
ニル系共重合体けん化物乳化分散液の製造法。 ３ 界面活性剤量が、エチレン−酢酸ビニル系共
重合体けん化物100重量部に対して0.1〜４重量部
である特許請求の範囲第１項記載のエチレン−酢
酸ビニル系共重合体けん化物乳化分散液の製造
法。[Scope of Claims] 1. A saponified ethylene-vinyl acetate copolymer having an ethylene content of 20 to 50 mol% and a saponification degree of 80 mol% or more, and one or two selected from the group of alcohols having 1 to 5 carbon atoms. A saponified ethylene-vinyl acetate copolymer characterized in that it is dissolved under heating in the presence of water and a surfactant with a mixture of at least one species, and is emulsified and dispersed while removing the alcohol under forced high-speed stirring. Method for producing emulsified dispersion. 2 A saponified ethylene-vinyl acetate copolymer with an ethylene content of 20 to 50 mol% and a saponification degree of 80 mol% or more and a saponified ethylene-vinyl acetate copolymer with an ethylene content of 85 to 90 mol% and a saponification degree of 80 mol% or more The ethylene-vinyl acetate copolymer sapon according to claim 1, which is used in combination with 80 mol% or more of saponified ethylene-vinyl acetate copolymer in a ratio of 100/0 to 70/30 (weight ratio). A method for producing a chemical emulsion dispersion. 3. The emulsion of a saponified ethylene-vinyl acetate copolymer according to claim 1, wherein the amount of surfactant is 0.1 to 4 parts by weight per 100 parts by weight of the saponified ethylene-vinyl acetate copolymer. Dispersion manufacturing method.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP869278A JPS54101844A (en) | 1978-01-27 | 1978-01-27 | Preparation of emulsion of ethylene-vinyl acetate copolymer saponificate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP869278A JPS54101844A (en) | 1978-01-27 | 1978-01-27 | Preparation of emulsion of ethylene-vinyl acetate copolymer saponificate |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS54101844A JPS54101844A (en) | 1979-08-10 |
| JPS6363568B2 true JPS6363568B2 (en) | 1988-12-07 |
Family
ID=11699963
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP869278A Granted JPS54101844A (en) | 1978-01-27 | 1978-01-27 | Preparation of emulsion of ethylene-vinyl acetate copolymer saponificate |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS54101844A (en) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CA2080494C (en) * | 1991-02-15 | 1999-11-02 | Junnosuke Yamauchi | Aqueous dispersion and substrate coated with the same |
| JPH0682646U (en) * | 1993-04-30 | 1994-11-25 | トキワ工業株式会社 | Screen sheet for projector |
| WO2005111118A1 (en) * | 2004-05-14 | 2005-11-24 | Sumitomo Seika Chemicals Co., Ltd. | Method for producing aqueous ethylene/vinyl alcohol based copolymer dispersion |
| US8912264B2 (en) | 2004-11-25 | 2014-12-16 | Sumitomo Seika Chemicals Co., Ltd. | Aqueous ethylene/vinyl alcohol copolymer dispersion |
| CN110760197A (en) * | 2019-11-29 | 2020-02-07 | 湖南工业大学 | Soft wood chip/EVA composite material |
-
1978
- 1978-01-27 JP JP869278A patent/JPS54101844A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS54101844A (en) | 1979-08-10 |
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