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JPH0830151B2 - Method for producing tackifying resin aqueous emulsion - Google Patents
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JPH0830151B2 - Method for producing tackifying resin aqueous emulsion - Google Patents

Method for producing tackifying resin aqueous emulsion

Info

Publication number
JPH0830151B2
JPH0830151B2 JP19797587A JP19797587A JPH0830151B2 JP H0830151 B2 JPH0830151 B2 JP H0830151B2 JP 19797587 A JP19797587 A JP 19797587A JP 19797587 A JP19797587 A JP 19797587A JP H0830151 B2 JPH0830151 B2 JP H0830151B2
Authority
JP
Japan
Prior art keywords
tackifying resin
emulsion
water
aqueous emulsion
resin
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 - Lifetime
Application number
JP19797587A
Other languages
Japanese (ja)
Other versions
JPS6440585A (en
Inventor
吉広 児玉
宏有 原
俊之 岸
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Arakawa Chemical Industries Ltd
Original Assignee
Arakawa Chemical Industries Ltd
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Arakawa Chemical Industries Ltd filed Critical Arakawa Chemical Industries Ltd
Priority to JP19797587A priority Critical patent/JPH0830151B2/en
Publication of JPS6440585A publication Critical patent/JPS6440585A/en
Publication of JPH0830151B2 publication Critical patent/JPH0830151B2/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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  • Compositions Of Macromolecular Compounds (AREA)
  • Paints Or Removers (AREA)
  • Adhesives Or Adhesive Processes (AREA)

Description

【発明の詳細な説明】 産業上の利用分野 本発明は、粘着付与樹脂の水性エマルジョンを製造す
る方法に関する。
FIELD OF THE INVENTION The present invention relates to a method of making an aqueous emulsion of a tackifying resin.

従来の技術 従来、粘接着業界に於て溶剤型の粘接着剤が汎用され
てきたが、近年では労働安全衛生や省資源等の見地から
水性エマルジョン型へ移行してきている。これに伴い、
粘接着剤の構成成分たる粘着付与樹脂についても水性エ
マルジョン化が要望されている。
2. Description of the Related Art Conventionally, solvent-based adhesives have been widely used in the adhesive industry, but in recent years, they have been shifting to aqueous emulsion types from the viewpoint of occupational safety and health and resource saving. With this,
A tackifying resin which is a constituent of the tacky-adhesive is also required to be an aqueous emulsion.

従来、粘着付与樹脂エマルジョンの製造方法は次の2
方法に大別される。一方はいわゆる高圧乳化法であり、
他方は転相乳化法である。前者は、粘着付与樹脂を有機
溶剤に溶解して通常60〜70重量%程度の溶液とし、これ
に適当な分散剤と水を添加して固形分濃度40重量%程度
の状態となし、次いで高せん断力乳化機(例えば高圧乳
化機)を使用し強制乳化を行い水中油型エマルジョンと
なす方法である。後者は、加熱溶融した粘着付与樹脂に
適当な分散剤と必要に応じ可塑剤、アルカリ等を添加混
合した後、水を添加して一旦油中水型エマルジョンとな
し、これに更に水を添加して転相せしめることにより水
中油型エマルジョンをうる方法である。
Conventionally, the method for producing a tackifying resin emulsion is the following 2
The methods are roughly classified. One is the so-called high pressure emulsification method,
The other is the phase inversion emulsification method. In the former, the tackifying resin is usually dissolved in an organic solvent to form a solution of about 60 to 70% by weight, and a suitable dispersant and water are added to the solution to form a solid concentration of about 40% by weight, and then a high concentration. This is a method of forming an oil-in-water emulsion by forcibly emulsifying using a shearing force emulsifying machine (for example, a high-pressure emulsifying machine). In the latter, after adding and mixing an appropriate dispersant and a plasticizer, an alkali, etc., to the heat-melted tackifying resin, water is added to once form a water-in-oil emulsion, to which water is further added. It is a method of obtaining an oil-in-water emulsion by inversion.

しかしながら、前者方法では、溶剤を使用するため粘
着付与樹脂エマルジョンの製造時に尚、労働安全衛生上
の問題を有すること、また溶剤を減圧蒸留により除去す
る工程が必須となるため必ずしも省エネルギー的方法で
あるとはいい難く、更には溶剤を完全には除去しえない
ため粘接着剤として使用した場合に臭気の問題が生じる
などの欠点を有する。他方、後者方法では、粘着付与樹
脂エマルジョンの製造時に溶剤を使用しないという利点
があるため前者より優れた方法であるとされている。し
かしながら、従来使用の分散剤では、多くの粘着付与樹
脂について、水性エマルジョン製造時に粘着付与樹脂の
分散が悪いため凝固物が多量に副生し収率や過時の作
業性が低下したり、生成エマルジョンの放置安定性、あ
るいは各種アクリルエマルジョンやゴムラテックスとの
混合安定性が前者方法を採用した場合より劣るという欠
点があった。そのため、通常は適用樹脂が制限され汎用
粘着付与樹脂を広く水性エマルジョン化することはでき
ず、殊に高軟化点樹脂の場合にこの傾向が強いものであ
った。高軟化点樹脂のエマルジョン化に際しては可塑剤
成分を添加する方法もあるが、実質的に粘着付与樹脂の
軟化点が低下するため得られる粘接着剤の耐熱性、接着
力、凝集力を著しく低下させるという不利があった。
However, the former method is not always an energy-saving method because it uses a solvent and thus has a problem in terms of occupational safety and health during the production of a tackifying resin emulsion, and a step of removing the solvent by vacuum distillation is essential. However, the solvent cannot be completely removed, and it has a drawback that it causes an odor problem when used as an adhesive. On the other hand, the latter method is said to be superior to the former method because it has the advantage that no solvent is used during the production of the tackifying resin emulsion. However, with many dispersants used in the past, many tackifier resins have poor dispersion of the tackifier resin during the production of an aqueous emulsion, so that a large amount of coagulate is produced as a by-product, which lowers the yield and the workability at the time of production. The storage stability of No. 1 or the mixing stability with various acrylic emulsions and rubber latex was inferior to that obtained when the former method was adopted. Therefore, the applicable resins are usually limited, and general-purpose tackifier resins cannot be widely made into an aqueous emulsion, and this tendency is particularly strong in the case of a high softening point resin. There is also a method of adding a plasticizer component when emulsifying a high softening point resin, but since the softening point of the tackifying resin is substantially lowered, the heat resistance, adhesive strength, and cohesive force of the resulting adhesive are significantly improved. It had the disadvantage of lowering it.

発明が解決しようとする問題点 本発明は、従来技術で解決し得なかった問題点−前者
方法では労働安全衛生、省資源の点で充分ではないこ
と、後者方法では水性エマルジョン製造時に粘着付与樹
脂の分散が悪いため凝固物が多量に副生すること、生成
エマルジョンの安定性が劣ること等の事実−を考慮し
て、これら諸問題を悉く解決することを目的としたもの
である。
DISCLOSURE OF THE INVENTION Problems to be Solved by the Invention The present invention is a problem that cannot be solved by the prior art-the former method is not sufficient in terms of occupational safety and health and resource saving, and the latter method is a tackifying resin during the production of an aqueous emulsion. In view of the fact that a large amount of coagulate is produced as a by-product due to poor dispersion and the stability of the produced emulsion is inferior, these problems are all solved.

問題点を解決するための手段 本発明者らは、前記従来技術の問題点を解決せんとし
て、前記の転相乳化法における使用分散剤の種類につい
て鋭意研究を重ねた結果、特定の構造を有するスルホン
酸系乳化剤を使用することにより始めて前記問題点を悉
く解決しうることを見い出し本発明を完成するに至った
のである。
Means for Solving the Problems As a result of solving the problems of the above-mentioned conventional techniques, the present inventors have earnestly studied the kind of the dispersant used in the phase inversion emulsification method, and as a result, have a specific structure. The present invention has been completed by finding that the above problems can be solved completely by using a sulfonic acid emulsifier.

即ち本発明は、 溶融した粘着付与樹脂に、分散剤及び水を混合して粘
着付与樹脂が連続相で水が分散相であるエマルジョンを
形成し、次いで水を添加して該エマルジョンを相反転さ
せて粘着付与樹脂が分散相で水が連続相である水性エマ
ルジョンを得るに際し、分散剤として式 (式中、Rは炭素数4〜18の炭化水素残基、mは1又は
2、nは1〜3の整数、Mは1価のカチオンを示す。)
で表わされるスルホン酸塩を用いることを特徴とする粘
着付与樹脂水性エマルジョンの製造法に係わる。
That is, in the present invention, a molten tackifying resin is mixed with a dispersant and water to form an emulsion in which the tackifying resin is a continuous phase and water is a dispersed phase, and then water is added to cause phase inversion of the emulsion. In order to obtain an aqueous emulsion in which the tackifying resin is the dispersed phase and water is the continuous phase, (In the formula, R represents a hydrocarbon residue having 4 to 18 carbon atoms, m represents 1 or 2, n represents an integer of 1 to 3, and M represents a monovalent cation.)
And a method for producing an aqueous emulsion of a tackifying resin, which comprises using a sulfonate represented by

本発明において使用される粘着付与樹脂としては、特
に制限はされず、溶剤型粘接着剤に使用されていた各種
公知のものを挙げることができ、具体的には、ロジンエ
ステル類、石油樹脂、水添石油樹脂、テルペン樹脂、水
添テルペン樹脂等を例示しうる。ここで、ロジンエステ
ル類としては、ガムロジン、ウッドロジン及びトール油
ロジン並びにこれらを不均化、水素添加処理した安定化
ロジン等の原料ロジンと各種多価アルコールとをエステ
ル化反応させて得られるもの、更には該エステル化物を
部分的にフマル化又はマレイン化して得られるもの、前
記原料ロジンをマレイン化又はフマルし次いでエステル
化して得られるもの、重合ロジンのエステル化物等を例
示できる。これらは通常は70〜140℃の軟化点を有する
ものが適当とされる。尚、ロジンエステル類のエステル
化に用いられる多価アルコールとしては、特に制限はさ
れず、ジエチレングリコール、グリセリン、トリメチロ
ールプロパン、トリメチロールエタン、1,2,6−ヘキサ
ントリオール、1,2,4−ブタントリオール、ペンタエリ
スリトール等の各種を例示し得る。石油樹脂としては、
ナフサのクラッキング等の石油精製により得たC9留分を
カチオン重合することにより得られるC9系石油樹脂、シ
クロペンタジエンやジシクロペンタジエン等のC5留分を
熱重合して得られたC5系石油樹脂、更にはC5留分〜C9留
分を重合して得られるC5〜C9系石油樹脂等を例示でき
る。水添石油樹脂としては、上記各種石油樹脂をそれぞ
れ水素化して得られる脂環族系の水添石油樹脂等を例示
できる。テルペン樹脂としては、α−ピネン、β−ピネ
ン、ジペンテンのような単環テルペンの重合体又はこれ
らテルペン留分とスチレン類からなる共重合体等を例示
できる。水添テルペン樹脂としては上記テルペン樹脂を
それぞれ水素化して得られるもの等を例示できる。
The tackifying resin used in the present invention is not particularly limited, and various known resins used for solvent-type tacky adhesives can be mentioned, and specifically, rosin esters and petroleum resins. , Hydrogenated petroleum resin, terpene resin, hydrogenated terpene resin and the like. Here, as rosin esters, gum rosin, wood rosin and tall oil rosin and those disproportionated, those obtained by esterification reaction of various polyhydric alcohols with raw material rosin such as hydrogenated stabilized rosin, Further, examples thereof include those obtained by partially fumarizing or maleating the esterified product, those obtained by maleating or fumarizing the raw material rosin and then esterifying it, and esterified products of polymerized rosin. Usually, those having a softening point of 70 to 140 ° C. are suitable. Incidentally, the polyhydric alcohol used for esterification of rosin esters is not particularly limited, diethylene glycol, glycerin, trimethylolpropane, trimethylolethane, 1,2,6-hexanetriol, 1,2,4- Examples thereof include butanetriol and pentaerythritol. As a petroleum resin,
C9 petroleum resin obtained by cationically polymerizing C9 fraction obtained by petroleum refining such as cracking of naphtha, C5 petroleum resin obtained by thermally polymerizing C5 fraction such as cyclopentadiene and dicyclopentadiene, Further, C5-C9 petroleum resin and the like obtained by polymerizing C5 fraction-C9 fraction can be exemplified. Examples of the hydrogenated petroleum resin include alicyclic hydrogenated petroleum resins obtained by hydrogenating each of the above various petroleum resins. Examples of the terpene resin include polymers of monocyclic terpenes such as α-pinene, β-pinene and dipentene, and copolymers of these terpene fractions and styrenes. Examples of hydrogenated terpene resins include those obtained by hydrogenating the above terpene resins.

本発明では、分散剤として前記一般式〔I〕で表わさ
れるスルホン酸塩を用いることを必須とする。一般式
〔I〕中、Rで定義されるは基は炭素数4〜18の炭化水
素残基であり、好ましくは8〜16の炭化水素残基であ
る。該炭化水素残基とは、具体的には直鎖もしくは分枝
鎖のアルキル基またはアルケニル基並びにスチリル基ま
たはジスチリル基をいう。その具体例としては、直鎖ま
たは分枝鎖のブチル基、ペンチル基、ヘキシル基、ヘプ
チル基、オクチル基、ノニル基、デシル基、ウンデシル
基、ドデシル基、トリデシル基、テトラデシル基、ペン
タデシル基、ヘキサデシル基、ヘプタデシル基、オクタ
デシル基、5−デセニル基、6−ドデセニル基、7−テ
トラデセニル基、9−オクタデセニル基等が挙げられ
る。mは1又は2である。mは3以上の場合は当該分散
剤の疎水性が大となり、分散能が低下し、安定なエマル
ジョンが得られ難いので好ましくない。また、 (R)mの置換位置は、特に制限はないが、オルソ又は(及
び)パラ位が一般的である。エチレンオキシドの付加モ
ル数nは1〜3である。nが4を越える分散剤を使用し
た場合には、粘着付与樹脂エマルジョンの放置安定性
や、アクリルエマルジョンやゴムラテックスとの混合安
定性が低下する。この場合、分散剤使用量を増加すれば
ある程度は上記安定性を改良しうるものの耐水性が著し
く低下するため好ましくない。Mで定義される1価のカ
チオンとしては、リチウム、ナトリウム、カリウム、セ
シウム等のアルカリ金属イオン、アンモニア及びトリメ
チルアミン、ジメチルアミン、ジエチルアミン、トリエ
タノールアミン等の各種アミンから誘導されるアンモニ
ウム基を例示できる。
In the present invention, it is essential to use the sulfonate represented by the general formula [I] as the dispersant. In the general formula [I], the group defined by R is a hydrocarbon residue having 4 to 18 carbon atoms, preferably 8 to 16 hydrocarbon residues. The hydrocarbon residue specifically means a linear or branched alkyl group or alkenyl group, and a styryl group or a distyryl group. Specific examples thereof include linear or branched butyl group, pentyl group, hexyl group, heptyl group, octyl group, nonyl group, decyl group, undecyl group, dodecyl group, tridecyl group, tetradecyl group, pentadecyl group, hexadecyl group. Group, heptadecyl group, octadecyl group, 5-decenyl group, 6-dodecenyl group, 7-tetradecenyl group, 9-octadecenyl group and the like. m is 1 or 2. If m is 3 or more, the hydrophobicity of the dispersant becomes large, the dispersibility decreases, and it is difficult to obtain a stable emulsion, which is not preferable. Further, the substitution position of (R) m is not particularly limited, but it is generally the ortho or (and) para position. The added mole number n of ethylene oxide is 1 to 3. When a dispersant with n exceeding 4 is used, the leaving stability of the tackifying resin emulsion and the mixing stability with the acrylic emulsion or the rubber latex decrease. In this case, if the amount of the dispersant used is increased, the stability can be improved to some extent, but the water resistance is significantly reduced, which is not preferable. Examples of the monovalent cation defined by M include alkali metal ions such as lithium, sodium, potassium and cesium, and ammonium groups derived from ammonia and various amines such as trimethylamine, dimethylamine, diethylamine and triethanolamine. .

本発明方法は、転相乳化法に従って実施され、前記分
散剤は固形分換算で、前記粘着付与樹脂固形分100重量
部(以下、単に部という)に対して通常3〜10部、好ま
しくは5〜7部の割合で使用される。3部に満たない場
合は分散力が充分でなく、10部を越える場合は耐水性、
経済性の点で不利となる。
The method of the present invention is carried out according to the phase inversion emulsification method, and the dispersant is generally 3 to 10 parts, preferably 5 parts by weight, based on 100 parts by weight of the tackifying resin solid content (hereinafter simply referred to as "parts"). Used at a rate of ~ 7 parts. If it is less than 3 parts, the dispersive power is not sufficient, and if it exceeds 10 parts, it is water resistant.
It is disadvantageous in terms of economy.

上記方法は、より具体的には、以下の通り実施され
る。即ちまず粘着付与樹脂を加熱攪拌して溶融物を調製
する。その際の加熱温度は粘着付与樹脂の軟化点を考慮
して適宜決定され、一般には90〜160℃の範囲とされ
る。
More specifically, the above method is carried out as follows. That is, first, the tackifying resin is heated and stirred to prepare a melt. The heating temperature at that time is appropriately determined in consideration of the softening point of the tackifying resin, and is generally in the range of 90 to 160 ° C.

次いで上記溶融物を攪拌しながらこれに分散剤水溶液
または分散剤と水とを添加して粘着付与樹脂が連続相で
水が分散相であるエマルジョンを形成させる。この際使
用する水の量は、得られるエマルジョンが約70〜90重量
%の固形分を含有するように調製されるのがよい。
Then, the above-mentioned melt is stirred and an aqueous dispersant solution or a dispersant and water are added thereto to form an emulsion in which the tackifying resin is a continuous phase and water is a dispersed phase. The amount of water used here should be adjusted so that the resulting emulsion contains about 70 to 90% by weight of solids.

次に、通常約70〜100℃程度の熱水を上記エマルジョ
ンに激しく攪拌しながら追加する。これによりエマルジ
ョンの相反転が生起し、粘着付与樹脂が分散相で水が連
続相である水性エマルジョンが得られるのである。この
際、粘着付与樹脂の分散は極めて良好であり、凝固物の
副生は非常に少ない。
Next, hot water at a temperature of about 70 to 100 ° C. is added to the above emulsion with vigorous stirring. This causes phase inversion of the emulsion, resulting in an aqueous emulsion in which the tackifying resin is the dispersed phase and the water is the continuous phase. At this time, the dispersion of the tackifying resin is extremely good, and the by-product of the solidified product is very small.

尚、上記方法に於ては系内圧力につき特に制限はない
が、粘着付与樹脂の軟化点が100℃以上の場合には密封
系、加圧系を採用しうるのはもとよりである。
In the above method, the system pressure is not particularly limited, but it is a matter of course that a sealed system or a pressurized system can be used when the softening point of the tackifying resin is 100 ° C. or higher.

尚、必要に応じてジエタノールアミン、トリエタノー
ルアミン、水酸化ナトリウム等の塩基性物質を前記製造
の任意の段階で使用でき、これにより製品pHの調節はも
ちろんのこと製造時の樹脂分散性、得られるエマルジョ
ンの機械的安定性を一層向上させることもできる。
If necessary, a basic substance such as diethanolamine, triethanolamine, sodium hydroxide or the like can be used at any stage of the above production, whereby not only the pH of the product can be adjusted but also the resin dispersibility at the time of production can be obtained. It is also possible to further improve the mechanical stability of the emulsion.

かくして得られた水性エマルジョンは、通常50〜70重
量%、好ましくは55〜65重量%の固形分濃度であり、粘
度は数十〜数千cps程度となる。また、該エマルジョン
の粒子径は通常0.1〜0.5μ程度となる。
The thus obtained aqueous emulsion has a solid content concentration of usually 50 to 70% by weight, preferably 55 to 65% by weight, and a viscosity of about tens to thousands of cps. The particle size of the emulsion is usually about 0.1 to 0.5 µ.

本発明方法により得られる粘着付与樹脂水性エマルジ
ョンは、アクリル系エマルジョン、天然ゴムラテック
ス、合成ゴムラテックス等の各種水性分散体と組合わせ
ることにより、アクリル系、ゴム系等の水性粘接着剤を
容易に製造し得る。尚、該粘接着剤を調製する場合は、
粘着付与樹脂水性エマルジョンの使用量は得られる粘接
着剤の使用目的、用途等を勘案して適宜決定でき、通常
はアクリルエマルジョンやゴムラテックス固形分100重
量部に対して10〜150重量部の範囲で使用される。また
該粘接着剤には増粘剤、防かび剤、造膜助剤等を適宜配
合しうることはもとよりである。
The tackifying resin aqueous emulsion obtained by the method of the present invention can be easily combined with various aqueous dispersions such as acrylic emulsion, natural rubber latex and synthetic rubber latex to easily prepare an acrylic or rubber aqueous tacky adhesive. Can be manufactured. When preparing the adhesive,
The amount of the tackifying resin aqueous emulsion to be used can be appropriately determined in consideration of the purpose of use of the resulting tacky-adhesive agent, the application, etc., and is usually 10 to 150 parts by weight per 100 parts by weight of acrylic emulsion or rubber latex solid content. Used in the range. Further, it goes without saying that a thickener, a fungicide, a film-forming aid and the like can be appropriately added to the adhesive.

発明の効果 本発明により、粘着付与樹脂の水性エマルジョン化に
関する従来技術で解決し得なかった問題点を解決でき、
この結果、粘着付与樹脂の分散が極めて良好で、凝固物
の副生が非常に少ないので収率や過時の作業性に優
れ、更には生成エマルジョンの安定性、粘接着特性のい
ずれの点をも同時に満足しうる新規且つ有用な粘着付与
樹脂水性エマルジョンの製造法が提供される。更に、本
発明により、労働安全衛生、省資源も達成できる。
Effects of the Invention According to the present invention, it is possible to solve the problems that could not be solved by the prior art regarding the aqueous emulsification of tackifier resin,
As a result, the dispersion of the tackifying resin is extremely good, and the co-product of the coagulation is very small, so that the yield and the workability at the time of excellence are excellent. At the same time, a new and useful method for producing an aqueous emulsion of a tackifying resin is provided. Furthermore, occupational safety and health and resource saving can be achieved by the present invention.

実施例 以下、実施例及び比較例を挙げて本発明を詳細に説明
するが、本発明はこれら各例に限定されるものではな
い。尚、各例中、部及び%は特記しない限り全て重量基
準である。
EXAMPLES Hereinafter, the present invention will be described in detail with reference to examples and comparative examples, but the present invention is not limited to these examples. In the examples, all parts and% are by weight unless otherwise specified.

実施例1 撹拌機、冷却管、温度計及び滴下ロートを備えた反応
装置に、不均化ロジンのグリセリンエステル(酸価4、
軟化点98℃)100部を仕込み系内を約120℃まで加熱して
溶融させた。次いで、2−ヒドロキシ−3−(ノニルフ
ェノキシジオキシエチレン)プロピルスルホン酸ソーダ
(前記一般式〔I〕で表わされる化合物でありm=1、
n=2のもの、第一工業製薬(株)製、商品名「ハイテ
ノールS」、固形分50%)10部及びトリエタノールアミ
ン0.7部を攪拌しながら5分間で添加した。その後系内
を約100℃に保ちながら、滴下ロートから95℃の熱水15
部を40分間で添加することにより、クリーム状の油中水
型エマルジョンを得た。次いで、激しく攪拌しながら、
熱水54部を2分間で添加すると相反転が起こり、水中油
型エマルジョンとなった。該エマルジョンを25℃迄冷却
し、250メッシュ金網で過して粘着付与樹脂水性エマ
ルジョンを得た。エマルジョンの収率は、下記式により
求めた。
Example 1 A reactor equipped with a stirrer, a condenser, a thermometer and a dropping funnel was charged with a glycerol ester of disproportionated rosin (acid value 4,
100 parts of a softening point of 98 ° C) was charged and the inside of the system was heated to about 120 ° C to melt. Next, sodium 2-hydroxy-3- (nonylphenoxydioxyethylene) propyl sulfonate (a compound represented by the above general formula [I], m = 1,
n = 2, manufactured by Dai-ichi Kogyo Seiyaku Co., Ltd., trade name “HITENOL S”, solid content 50%) 10 parts and triethanolamine 0.7 part were added with stirring for 5 minutes. Then, while maintaining the system temperature at approximately 100 ° C, use hot water at 95 ° C from the dropping funnel.
Parts were added over 40 minutes to give a creamy water-in-oil emulsion. Then, with vigorous stirring,
When 54 parts of hot water was added over 2 minutes, phase inversion occurred and an oil-in-water emulsion was obtained. The emulsion was cooled to 25 ° C. and passed through a 250 mesh wire gauze to obtain a tackifying resin aqueous emulsion. The yield of the emulsion was calculated by the following formula.

尚、金網上の凝固物は乾燥及び秤量を行ない、この量
を仕込樹脂量で除することにより、凝固物量を百分率で
示した。得られたエマルジョンの性状は第3表に示す。
The coagulated product on the wire net was dried and weighed, and this amount was divided by the amount of the charged resin to show the coagulated product in percentage. The properties of the obtained emulsion are shown in Table 3.

実施例2 撹拌機、温度計及び滴下ポンプを備えたオートクレー
ブに、部分フマル化不均化ロジンのペンタエリスリトー
ルエステル(フマル化率3.5%、酸価15、軟化点125℃)
100部を仕込み系内を約135℃まで加熱して溶融させた。
次いで実施例1で用いた分散剤10部及びトリエタノール
アミン0.7部を添加し、密封後10分間撹拌しながら約130
℃に保った。更に、95℃の熱水15部を40分間を要して滴
下ポンプにより圧入することにより、クリーム状の油中
水型エマルジョンを得た。更に熱水54部を2分間で圧入
すると相反転が起こり、水中油型エマルジョンとなっ
た。該エマルジョンを25℃迄冷却し、250メッシュ金網
で過して粘着付与樹脂水性エマルジョンを得た。得ら
れたエマルジョンの凝固物量及び性状は第3表に示す。
Example 2 A pentaerythritol ester of partially fumarized disproportionated rosin was added to an autoclave equipped with a stirrer, a thermometer and a dropping pump (fumaration rate 3.5%, acid value 15, softening point 125 ° C.).
100 parts were charged and the inside of the system was heated to about 135 ° C. to be melted.
Then, 10 parts of the dispersant used in Example 1 and 0.7 part of triethanolamine were added, and after sealing, about 130 parts with stirring for 10 minutes.
It was kept at ℃. Furthermore, 15 parts of hot water at 95 ° C. was pressed for 40 minutes with a dropping pump to obtain a creamy water-in-oil emulsion. Further, when 54 parts of hot water was pressed in for 2 minutes, phase inversion occurred and an oil-in-water emulsion was formed. The emulsion was cooled to 25 ° C. and passed through a 250 mesh wire gauze to obtain a tackifying resin aqueous emulsion. The amount and properties of the obtained emulsion are shown in Table 3.

実施例3〜7 実施例1又は実施例2の方法において、第1表に示す
ように使用粘着付与樹脂又は分散剤の種類を代えた他は
同様にして各種の粘着付与樹脂水性エマルジョンを得
た。得られた各種エマルジョンの凝固物量及び性状は第
3表に示す。
Examples 3 to 7 Various tackifier resin aqueous emulsions were obtained in the same manner as in the method of Example 1 or Example 2 except that the type of tackifier resin or dispersant used was changed as shown in Table 1. . Table 3 shows the amount and properties of the various emulsions obtained.

比較例1〜7 実施例1又は実施例2の方法において、第2表に示す
ように粘着付与樹脂もしくは分散剤の種類又はアルカリ
種もしくはその使用の有無を代えた他は同様にして各種
の粘着付与樹脂水性エマルジョンを得た。得られた各種
エマルジョンの凝固物量及び性状は第3表に示す。
Comparative Examples 1 to 7 In the method of Example 1 or Example 2, as shown in Table 2, various kinds of tackiness were similarly obtained except that the kind of tackifying resin or dispersant or the alkali species or the presence or absence thereof was changed. An applied resin aqueous emulsion was obtained. Table 3 shows the amount and properties of the various emulsions obtained.

但し、比較例4では粘着付与樹脂の分散が極めて悪く
エマルジョンは得られなかった。
However, in Comparative Example 4, the dispersion of the tackifying resin was extremely poor and an emulsion could not be obtained.

第3表中、放置安定性は、エマルジョンを室温に放置
し、離水現象が生じ始めるまでの日数により調べた。ま
た、混合安定性は、アクリルエマルジョン(pH=4、不
揮発分濃度40%、ブチルアクリレート/アクリル酸=97
/3(重量比)からなる共重合体エマルジョン)及び天然
ゴムラテックス(pH=10、不揮発分濃度62%)に、配合
比率を前者ではアクリル/粘着付与樹脂=90/10(固形
分比)で、後者では天然ゴム/粘着付与樹脂=50/50
(固形分比)で混合した場合に凝固物を生じたものを
×、生じないものを○として調べた。
In Table 3, the storage stability was examined by the number of days until the water separation phenomenon began to occur after the emulsion was stored at room temperature. In addition, the mixing stability is as follows: acrylic emulsion (pH = 4, nonvolatile concentration 40%, butyl acrylate / acrylic acid = 97
/ 3 (weight ratio) copolymer emulsion) and natural rubber latex (pH = 10, nonvolatile concentration 62%), the former compounding ratio is acrylic / tackifying resin = 90/10 (solid content ratio) , The latter is natural rubber / tackifying resin = 50/50
When mixed at a (solid content ratio), a product that produced a solidified product was examined as X, and a product that did not produce solidified product was evaluated as O.

Claims (2)

【特許請求の範囲】[Claims] 【請求項1】溶融した粘着付与樹脂に、分散剤及び水を
混合して粘着付与樹脂が連続相で水が分散相であるエマ
ルジョンを形成し、次いで水を添加して該エマルジョン
を相反転させて粘着付与樹脂が分散相で水が連続相であ
る水性エマルジョンを得るに際し、分散剤として一般式 (式中、Rは炭素数4〜18の炭化水素残基、mは1又は
2、nは1〜3の整数、Mは1価のカチオンを示す。)
で表わされるスルホン酸塩を用いることを特徴とする粘
着付与樹脂水性エマルジョンの製造法。
1. A molten tackifying resin is mixed with a dispersant and water to form an emulsion in which the tackifying resin is a continuous phase and water is a dispersed phase, and then water is added to invert the emulsion. In order to obtain an aqueous emulsion in which the tackifying resin is the disperse phase and water is the continuous phase, a general formula is used as a dispersant. (In the formula, R represents a hydrocarbon residue having 4 to 18 carbon atoms, m represents 1 or 2, n represents an integer of 1 to 3, and M represents a monovalent cation.)
A method for producing an aqueous emulsion of a tackifying resin, which comprises using a sulfonate represented by:
【請求項2】粘着付与樹脂が、ロジンエステル類、石油
樹脂、水添石油樹脂、テルペン樹脂及び水添テルペン樹
脂から選ばれる少くとも1種である特許請求の範囲第1
項記載の水性エマルジョンの製造法。
2. The tackifying resin is at least one selected from rosin esters, petroleum resins, hydrogenated petroleum resins, terpene resins and hydrogenated terpene resins.
A method for producing an aqueous emulsion according to the item 1.
JP19797587A 1987-08-06 1987-08-06 Method for producing tackifying resin aqueous emulsion Expired - Lifetime JPH0830151B2 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP19797587A JPH0830151B2 (en) 1987-08-06 1987-08-06 Method for producing tackifying resin aqueous emulsion

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP19797587A JPH0830151B2 (en) 1987-08-06 1987-08-06 Method for producing tackifying resin aqueous emulsion

Publications (2)

Publication Number Publication Date
JPS6440585A JPS6440585A (en) 1989-02-10
JPH0830151B2 true JPH0830151B2 (en) 1996-03-27

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ID=16383431

Family Applications (1)

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Country Status (1)

Country Link
JP (1) JPH0830151B2 (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107722299A (en) * 2017-11-03 2018-02-23 黎月清 Terpene resin dispersion agent and preparation method thereof

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0655824B2 (en) * 1987-09-01 1994-07-27 三菱石油株式会社 Method for producing resin emulsion
JP5135662B2 (en) * 2004-07-27 2013-02-06 東洋紡株式会社 Aqueous resin composition and method for producing the same
JP4595439B2 (en) * 2004-08-18 2010-12-08 東亞合成株式会社 Adhesive composition

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107722299A (en) * 2017-11-03 2018-02-23 黎月清 Terpene resin dispersion agent and preparation method thereof

Also Published As

Publication number Publication date
JPS6440585A (en) 1989-02-10

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