JPH06313005A - Aqueous suspension of lauroyl peroxide - Google Patents

Aqueous suspension of lauroyl peroxide

Info

Publication number
JPH06313005A
JPH06313005A JP12313793A JP12313793A JPH06313005A JP H06313005 A JPH06313005 A JP H06313005A JP 12313793 A JP12313793 A JP 12313793A JP 12313793 A JP12313793 A JP 12313793A JP H06313005 A JPH06313005 A JP H06313005A
Authority
JP
Japan
Prior art keywords
lauroyl peroxide
aqueous suspension
viscosity
aqueous
weight
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.)
Granted
Application number
JP12313793A
Other languages
Japanese (ja)
Other versions
JP3412185B2 (en
Inventor
Yoshiki Higuchi
慶樹 樋口
Kazuhiro Katsumata
和宏 勝又
Shuji Suyama
修治 須山
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.)
NOF Corp
Original Assignee
Nippon Oil and Fats Co 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 Nippon Oil and Fats Co Ltd filed Critical Nippon Oil and Fats Co Ltd
Priority to JP12313793A priority Critical patent/JP3412185B2/en
Publication of JPH06313005A publication Critical patent/JPH06313005A/en
Application granted granted Critical
Publication of JP3412185B2 publication Critical patent/JP3412185B2/en
Anticipated expiration legal-status Critical
Expired - Fee Related legal-status Critical Current

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Classifications

    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F4/00Polymerisation catalysts
    • C08F4/28Oxygen or compounds releasing free oxygen
    • C08F4/32Organic compounds
    • C08F4/34Per-compounds with one peroxy-radical

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Polymerization Catalysts (AREA)

Abstract

PURPOSE:To obtain an aqueous dispersion of lauroyl peroxide retaining excellent storage stability for a long period of time. CONSTITUTION:This aqueous dispersion of lauroyl peroxide contains 30 to 60wt.% of lauroyl peroxide and, in the aqueous system excluding the lauroyl peroxide, 20 to 22wt.% of glycerol, 0.2 to 5wt.% of a surfactant of 12 to 16 HLB value and 0.02 to 5wt.% of crosslinkable acrylic water-soluble resin.

Description

【発明の詳細な説明】Detailed Description of the Invention

【0001】[0001]

【産業上の利用分野】本発明は、過酸化ラウロイルの水
性懸濁液に関する。更に詳しくは、低粘度で貯蔵安定性
に優れ、且つエチレン性不飽和単量体の重合開始剤とし
て好適な過酸化ラウイロイルの水性懸濁液に関する。
FIELD OF THE INVENTION The present invention relates to an aqueous suspension of lauroyl peroxide. More specifically, it relates to an aqueous suspension of rawiloyl peroxide, which has a low viscosity, excellent storage stability, and is suitable as a polymerization initiator for ethylenically unsaturated monomers.

【0002】[0002]

【従来の技術】所望の粒度の重合体を得るためのエチレ
ン性不飽和単量体の懸濁ないし乳化重合は、通常界面活
性剤及び/又は分散安定剤を使用し、且つ重合反応を起
こすために重合開始剤を使用することによって行われ
る。最近では、前記重合反応においては生産性向上を図
り、且つ残留及び廃棄単量体の毒性による環境汚染を防
止するため、重合設備を大型化あるいは製造設備を自動
連続化すると共に、重合反応系全体をクローズド化して
行っている。このような製造法に適した重合開始剤とし
て従来から使用されている固体ないし液体の有機過酸化
物よりも、取り扱い、安全性の観点から、より使用し易
い水で懸濁化ないし乳化した有機過酸化物の方が好まれ
る傾向にある。
The suspension or emulsion polymerization of an ethylenically unsaturated monomer to obtain a polymer having a desired particle size usually uses a surfactant and / or a dispersion stabilizer and causes a polymerization reaction. Is carried out by using a polymerization initiator. Recently, in order to improve productivity in the polymerization reaction and prevent environmental pollution due to toxicity of residual and waste monomers, the polymerization equipment is enlarged or the production equipment is automatically continuous, and the entire polymerization reaction system is Is closed. From the viewpoint of handling and safety, it is easier to use than a solid or liquid organic peroxide conventionally used as a polymerization initiator suitable for such a production method. Peroxides tend to be preferred.

【0003】前記有機過酸化物中に特に実用的なものと
して過酸化ラウロイルがある。過酸化ラウロイルは常温
で固体の有機過酸化物であり、今までに幾つかの組成の
水性懸濁液が開発されている。以下に具体的な例を示
す。乳化剤に関しては、特公昭58−51001号公報
には、15より大のHLB値を有し且つ環状内部エーテ
ル結合を含有しないエトキシル化非イオン系乳化剤と、
9より小のHLB値を有する非エトキシル化非イオン系
乳化剤の組合せの系が、特公昭60−10029号公報
に、HLB値が12.5以下と12.5以上の非イオン
系乳化剤の組合せ、又は、HLB値が12.5以下の非
イオン系乳化剤と陰イオン系乳化剤の組合せの系が開示
されている。これらにはポリビニルアルコール、セルロ
ース誘導体などが保護コロイド剤として添加されてい
る。又、特殊な分散安定剤を添加する例としては、特開
昭55−25184号公報には疎水性アルキル基含有シ
リカ化合物を含む系が、特開昭63−92605号公報
に結晶セルロースを添加した系が、特開昭62−275
104号公報に架橋型アクリル系水溶性樹脂を添加する
系が開示されている。
Among the above-mentioned organic peroxides, lauroyl peroxide is particularly practical. Lauroyl peroxide is an organic peroxide that is solid at room temperature, and aqueous suspensions of several compositions have been developed so far. A specific example is shown below. Regarding the emulsifier, JP-B-58-51001 discloses an ethoxylated nonionic emulsifier having an HLB value of more than 15 and containing no cyclic internal ether bond,
A system of a combination of non-ethoxylated nonionic emulsifiers having an HLB value of less than 9 is disclosed in Japanese Patent Publication No. Sho 60-10029, in which a combination of nonionic emulsifiers having an HLB value of 12.5 or less and 12.5 or more, Alternatively, a system of a combination of a nonionic emulsifier and an anionic emulsifier having an HLB value of 12.5 or less is disclosed. Polyvinyl alcohol, cellulose derivatives and the like are added to these as protective colloid agents. As an example of adding a special dispersion stabilizer, JP-A-55-25184 discloses a system containing a silica compound containing a hydrophobic alkyl group, and JP-A-63-92605 discloses adding a crystalline cellulose. The system is JP-A-62-275.
Japanese Patent Publication No. 104 discloses a system in which a cross-linked acrylic water-soluble resin is added.

【0004】[0004]

【発明が解決しようとする課題】しかし、これらの過酸
化ラウロイルの水性懸濁液には次のような問題点があ
る。第一に、水性懸濁液の粘度が低い場合には、貯蔵安
定性が著しく悪く、二層に分離し易い。第二に、貯蔵安
定性の比較的よい水性懸濁液の場合には高粘度となり、
又、貯蔵時においては増粘する傾向にあるため、取り扱
いずらい。従って、前述の水性懸濁液の安定性は5カ月
以下であり、6カ月以上分離、増粘等のない長期間安定
なものはなかった。
However, these aqueous suspensions of lauroyl peroxide have the following problems. First, when the viscosity of the aqueous suspension is low, the storage stability is extremely poor and the two layers are easily separated. Secondly, in the case of an aqueous suspension with relatively good storage stability, the viscosity becomes high,
In addition, it tends to thicken during storage, making it difficult to handle. Therefore, the stability of the above-mentioned aqueous suspension was 5 months or less, and there was no stable suspension for 6 months or more without separation or thickening for a long period of time.

【0005】[0005]

【課題を解決するための手段】本発明者らは前述の欠点
を解決する方法を求めて鋭意研究した結果、特定の組成
を有する過酸化ラウロイル水性懸濁液は長期間安定であ
るとの知見を得て本発明を完成した。即ち、本発明は、
過酸化ラウロイルの水性懸濁液において、過酸化ラウロ
イルを30〜60重量%、全体から過酸化ラウロイルを
除いた水系(以後単に水系と称する)中にグリセリンを
20〜22重量%、HLB値が12〜16の界面活性剤
を0.2〜5重量%、及び、架橋型アクリル系水溶性樹
脂を0.02〜5重量%含む過酸化ラウロイルの水性懸
濁液に関する。
DISCLOSURE OF THE INVENTION As a result of intensive studies conducted by the present inventors in search of a method for solving the above-mentioned drawbacks, it was found that an aqueous lauroyl peroxide suspension having a specific composition is stable for a long period of time. Thus, the present invention was completed. That is, the present invention is
In an aqueous suspension of lauroyl peroxide, 30-60 wt% of lauroyl peroxide, 20-22 wt% of glycerin in an aqueous system in which lauroyl peroxide is removed from the whole (hereinafter simply referred to as an aqueous system), and an HLB value of 12 are obtained. No. 16 to 0.2 to 5% by weight of a surfactant and 0.02 to 5% by weight of a crosslinked acrylic water-soluble resin, to an aqueous suspension of lauroyl peroxide.

【0006】一般に、有機過酸化物と水とよりなる水性
懸濁液は短時間に分離する。従って通常、水系と有機物
との親和性を良くして均一に分散させるために界面活性
剤を、分離しないように水系の粘度を高くする目的で分
散安定剤を、又はその両方を添加する。しかし、界面活
性剤や分散安定剤を含有する水系懸濁液は一般に構造粘
性を示すため、貯蔵時においては時間の経過と共に増粘
する傾向にある。又、分散安定剤を多く使用すると高粘
度になって扱いずらい。従って、分散安定剤及び界面活
性剤の量は高粘度にならないように調整されているが、
長期保存時には分離する傾向にあった。本発明の過酸化
ラウロイルの水性懸濁液は低粘度であり、且つ、分離及
び増粘することなく6カ月以上の長期間静置していても
安定な水性懸濁液が得られる。
Generally, an aqueous suspension consisting of organic peroxide and water separates in a short time. Therefore, usually, a surfactant is added in order to improve the affinity between the water system and the organic substance and to disperse it uniformly, and a dispersion stabilizer or both are added for the purpose of increasing the viscosity of the water system so as not to separate. However, since an aqueous suspension containing a surfactant or a dispersion stabilizer generally exhibits structural viscosity, it tends to thicken with time during storage. Also, if a large amount of dispersion stabilizer is used, the viscosity becomes high and it is difficult to handle. Therefore, although the amounts of the dispersion stabilizer and the surfactant are adjusted so as not to have a high viscosity,
It tended to separate during long-term storage. The aqueous suspension of lauroyl peroxide of the present invention has a low viscosity, and a stable aqueous suspension can be obtained even if it is allowed to stand for a long period of 6 months or more without separation and thickening.

【0007】本発明の過酸化ラウロイルの水性懸濁液に
用いられる過酸化ラウロイルの含有量は30〜60重量
%であり、多過ぎると水系不足のためペースト状にな
り、又、30重量%に達しない場合は経済的に不利であ
る。用いられる過酸化ラウロイルの形状は粉体、塊状い
ずれでもよく、後で述べる方法により懸濁液を製造する
ことができる。
The content of lauroyl peroxide used in the aqueous suspension of lauroyl peroxide of the present invention is from 30 to 60% by weight, and if it is too large, it becomes a paste due to lack of an aqueous system, and is 30% by weight. If it does not reach, it is economically disadvantageous. The lauroyl peroxide used may be in the form of powder or lump, and a suspension can be produced by the method described later.

【0008】本発明に用いられる界面活性剤はHLB値
が12〜16の範囲内であることが必要であり、この範
囲外では水性懸濁液は高粘度、又は分離の傾向にある。
使用される界面活性剤を具体的に示すと、ポリオキシエ
チレンアルキルエーテル、ポリオキシエチレンアルキル
フェニルエーテル、ショ糖脂肪酸エステル、ソルビタン
脂肪酸エステル、ポリオキシエチレンソルビタン脂肪酸
エステル、ポリオキシエチレングリセリン脂肪酸エステ
ル、ポリオキシエチレングリコール脂肪酸エステル、ア
セチレングリコールのエチレングリコール付加物などの
非イオン性界面活性剤、アルキルベンゼンスルホン酸ソ
ーダ、脂肪酸アルカリ金属塩などの陰イオン性界面活性
剤などを挙げることができる。界面活性剤の含有量は水
系中に0.2〜5重量%であり、少な過ぎると高粘度又
は分離してしまい、多過ぎると経済的に不利である。
The surfactant used in the present invention is required to have an HLB value within the range of 12 to 16, and outside this range, the aqueous suspension tends to have a high viscosity or tend to separate.
Specific examples of the surfactant used include polyoxyethylene alkyl ether, polyoxyethylene alkylphenyl ether, sucrose fatty acid ester, sorbitan fatty acid ester, polyoxyethylene sorbitan fatty acid ester, polyoxyethylene glycerin fatty acid ester, and polyoxyethylene glycerin fatty acid ester. Nonionic surfactants such as oxyethylene glycol fatty acid esters and ethylene glycol adducts of acetylene glycol, sodium benzenebenzenesulfonate, anionic surfactants such as fatty acid alkali metal salts and the like can be mentioned. The content of the surfactant is 0.2 to 5% by weight in the water system. If the content is too small, the viscosity will be high or the separation will occur, and if it is too large, it will be economically disadvantageous.

【0009】本発明の懸濁液において、グリセリンを含
有していなければならず、その量は水系中に20〜22
重量%である。多過ぎても少な過ぎても長期間保存時に
分離する。
The suspension of the present invention must contain glycerin in an amount of 20-22 in the aqueous system.
% By weight. Whether it is too much or too little, it separates during long-term storage.

【0010】本発明に分散安定剤として用いられる架橋
型アクリル系水溶性樹脂としては、特開昭62−275
104号公報に記載されているものである。具体的に
は、アクリル酸重合体、メタクリル酸重合体、あるいは
これらの共重合体、及びアクリル酸、メタクリル酸各単
量体とビニルアルコールや少なくとも炭素数4個と水酸
基3個を含む多価アルコールのアルケニルエーテルとの
共重合体又はそれらの塩(好ましくはナトリウム塩、カ
リウム塩のようなアルカリ金属塩)であり、それは架橋
型である。架橋型アクリル系水溶性樹脂の含有量は水系
の0.2〜5重量%である。5重量%を越えると懸濁液
の粘度が高すぎる傾向にあり、又、0.02重量%より
少ない場合は貯蔵安定性が悪い傾向にある。そして特に
架橋性アクリル系水性樹脂、グリセリン、特定の界面活
性剤と共に過酸化ラウロイルを含む本発明の水性懸濁液
は6カ月以上長期にわたって分離しないという公知の水
性懸濁液にない特徴を有する。
The crosslinkable acrylic water-soluble resin used as the dispersion stabilizer in the present invention is described in JP-A-62-275.
This is described in Japanese Patent Publication No. 104. Specifically, acrylic acid polymers, methacrylic acid polymers, or copolymers thereof, and acrylic acid or methacrylic acid monomers and vinyl alcohol, or polyhydric alcohols containing at least 4 carbon atoms and 3 hydroxyl groups. Is a copolymer thereof with an alkenyl ether or a salt thereof (preferably an alkali metal salt such as sodium salt or potassium salt), which is a cross-linking type. The content of the cross-linked acrylic water-soluble resin is 0.2 to 5% by weight of the water system. If it exceeds 5% by weight, the viscosity of the suspension tends to be too high, and if it is less than 0.02% by weight, the storage stability tends to be poor. And, in particular, the aqueous suspension of the present invention containing lauroyl peroxide together with a crosslinkable acrylic aqueous resin, glycerin and a specific surfactant has a characteristic not known in the known aqueous suspension that it does not separate for a long period of 6 months or more.

【0011】以上の配合割合で調整された水系は降伏値
を持つ粘性液体である。水系の物性値は、特に限定され
ないが、水系の20℃における粘性率が0.1〜20ポ
イズ(g/cm・sec)、降伏値が10(dyne/
cm2 )以上の関係にあるものがより好ましい。ここ
で、粘性率はB型粘度計で回転数20r.p.m.での
測定値である。又、降伏値は下記の式(1)より算出し
て得た値である。 降伏値=0.5r.p.m.のみかけの粘性率−1.0r.p.m.のみかけ の粘性率 ・・・・・・・・ (1) (式中、みかけの粘性率は20℃においてB型粘度計で
測定した値であり、単位はポイズ(g/cm・sec)
である。)
The water system prepared by the above blending ratio is a viscous liquid having a yield value. The physical properties of the water system are not particularly limited, but the viscosity of the water system at 20 ° C is 0.1 to 20 poise (g / cm · sec), and the yield value is 10 (dyne /
Those having a relationship of not less than cm 2 ) are more preferable. Here, the viscosity is measured with a B-type viscometer at a rotation speed of 20 r.p.m. p. m. It is the measured value in. The yield value is a value calculated by the following formula (1). Yield value = 0.5r. p. m. Apparent viscosity-1.0 r. p. m. Apparent viscosity ... (1) (In the formula, the apparent viscosity is a value measured by a B-type viscometer at 20 ° C., and the unit is poise (g / cm · sec).
Is. )

【0012】本発明の過酸化ラウロイルの水性懸濁液
は、必要に応じて分散助剤、凝固点降下剤、消泡剤等を
添加することができる。例えば、水性懸濁液の保存温度
が0℃以下になる場合、凝固を防ぐ目的でメチルアルコ
ールなどの低分子量モノオールやエチレングリコールな
どの低分子量ジオールを系中に添加することができる。
又、分散安定性を高めるためにヘキサメタリン酸ナトリ
ウムなどの分散助剤、その他炭酸ソーダや水酸化ナトリ
ウムのようなアルカリ性物質なども含ませることができ
る。
A dispersion aid, a freezing point depressant, a defoaming agent and the like can be added to the aqueous suspension of lauroyl peroxide of the present invention, if necessary. For example, when the storage temperature of the aqueous suspension is 0 ° C. or lower, a low molecular weight monool such as methyl alcohol or a low molecular weight diol such as ethylene glycol can be added to the system for the purpose of preventing coagulation.
Further, in order to enhance dispersion stability, a dispersion aid such as sodium hexametaphosphate and an alkaline substance such as sodium carbonate and sodium hydroxide can be contained.

【0013】本発明の過酸化ラウロイルの水性懸濁液は
以下のようにして製造することができる。即ち、先ず容
器中に水、界面活性剤、グリセリン及び架橋型アクリル
系水溶性樹脂、必要に応じ他の添加剤を入れた中に過酸
化ラウロイルを添加して分散するという順序で行うのが
普通である。しかし、添加順序は適宜変更して行うこと
もできる。又、溶融乳化後、冷却する方法(特公昭62
−25681号公報)で製造することもできる。本発明
の過酸化ラウロイルの水性懸濁液を製造するために、使
用される装置は、周知の分散装置を用いることができ
る。例えば、機械回転式の攪拌機、コロイドミル、高速
剪断装置、超音波ホモジナイザー、三本ロールミル等が
使用できる。
The aqueous suspension of lauroyl peroxide of the present invention can be produced as follows. That is, it is common practice to first add water, a surfactant, glycerin and a crosslinkable acrylic water-soluble resin, and optionally other additives in a container, and then add lauroyl peroxide and disperse in the order. Is. However, the order of addition may be changed appropriately. Further, a method of cooling after melt emulsification (Japanese Examined Patent Publication No. 62
No. 25681). The equipment used for producing the aqueous suspension of lauroyl peroxide according to the invention can be any known dispersing equipment. For example, a mechanical rotary stirrer, colloid mill, high speed shearing device, ultrasonic homogenizer, three roll mill, etc. can be used.

【0014】本発明の過酸化ラウロイルの水性懸濁液に
より重合ないし共重合が可能なエチレン性不飽和単量体
としては、例えば塩化ビニル、ペースト塩化ビニル、ス
チレン、酢酸ビニル、アクリレート、アクリロニトリル
などがある。その際、過酸化ラウロイルの水性懸濁液の
使用量は、通常の使用範囲内で用いられる。そして重合
を行うには従来の方法によって実施することができる
が、特に乳化重合、懸濁重合などの水系における重合が
好ましい。
Examples of the ethylenically unsaturated monomer which can be polymerized or copolymerized with the aqueous suspension of lauroyl peroxide of the present invention include vinyl chloride, paste vinyl chloride, styrene, vinyl acetate, acrylate, acrylonitrile and the like. is there. At this time, the amount of the aqueous suspension of lauroyl peroxide used is within the usual range of use. The polymerization can be carried out by a conventional method, but emulsion polymerization, suspension polymerization and the like in an aqueous system are particularly preferable.

【0015】[0015]

【発明の効果】本発明の過酸化ラウロイルの水性懸濁液
は従来のものに比べて以下に示すような利点を有してい
る。即ち、本発明の過酸化ラウロイルの水性懸濁液は低
粘度であり、又、長期間、具体的には6カ月以上貯蔵し
ていても増粘及び分離することがないので、取り扱い易
く、輸送も容易に行うことができる。又、容器及び配管
内に付着又は残留した場合、容易に水で洗い流せるので
安全である。従って、エチレン性不飽和単量体の重合を
安全にしかも密閉式として環境汚染の心配もなく実施で
きる。
The aqueous suspension of lauroyl peroxide of the present invention has the following advantages over the conventional suspensions. That is, the aqueous suspension of lauroyl peroxide of the present invention has a low viscosity, and since it does not thicken or separate even when stored for a long period of time, specifically 6 months or more, it is easy to handle and transport. Can also be done easily. In addition, if it adheres to or remains in the container and piping, it is safe because it can be easily washed off with water. Therefore, the polymerization of the ethylenically unsaturated monomer can be carried out safely and in a closed system without concern for environmental pollution.

【0016】[0016]

【実施例】次に、実施例により本発明を具体的に説明す
る。尚、表中の%は重量%である。
EXAMPLES Next, the present invention will be described in detail with reference to examples. In the table,% means% by weight.

【0017】実施例 1〜6 表1に示す夫々の配合割合でまず水、分散安定剤、界面
活性剤及びグリセリンを混合して均一溶液を得、次いで
過酸化ラウロイルを攪拌しながら添加した。得られた混
合組成物をスーパーマスコロイダー(増幸産業社製、M
KZA10−15型)を用いてクリアランス200μm
において処理し、過酸化ラウロイルの水性懸濁液を得
た。次に得られた水性懸濁液について、次のような方法
で粘度、貯蔵安定性及び粘度安定性を測定した。夫々の
結果を表1に示す。又、水系の粘性率及び降伏値もあわ
せて表1に示す。尚、表1中の配合割合は、過酸化ラウ
ロイルは懸濁液全体に対する重量%、界面活性剤、グリ
セリン、分散安定剤及び水は懸濁液全体から過酸化ラウ
ロイルの添加量を除いた水系に対する重量%である。 〔粘度測定〕B型粘度計(東京計器製造所製、回転数2
0r.p.m.)を用い、20℃において測定した。単
位はポイズで表した。 〔貯蔵安定性試験〕試料を20℃に保ったガラス容器に
入れて静置貯蔵し、水層が1%以上分離するまでの月数
で示した。又、増粘してクリーム状になったものは()
内に月数を示した。 〔粘度安定性試験〕試料を20℃で貯蔵し、1カ月後の
粘度が初期粘度に対して上昇率が10%以下の場合は
○、10%以上の場合は×で示した。尚、1カ月以内に
分離したものは−で示した。 〔水系の粘性率及び降伏値〕表1に示した割合で分散安
定剤、界面活性剤、グリセリン及び水を混合して水系を
調整し、20℃における水系の粘性率をB型粘度計で回
転数20r.p.m.において測定し、又、降伏値はB
型粘度計の回転数1.0r.p.m.、0.5r.p.
m.で測定し、式(1)により算出した。
Examples 1 to 6 Water, a dispersion stabilizer, a surfactant and glycerin were mixed in the respective mixing ratios shown in Table 1 to obtain a uniform solution, and then lauroyl peroxide was added with stirring. The obtained mixed composition was supermass colloider (Masuyuki Sangyo Co., Ltd., M
200 μm clearance using KZA10-15 type)
And an aqueous suspension of lauroyl peroxide was obtained. Next, the obtained aqueous suspension was measured for viscosity, storage stability and viscosity stability by the following methods. The respective results are shown in Table 1. Table 1 also shows the viscosity and yield value of the water system. The blending ratios in Table 1 are as follows: lauroyl peroxide is wt% relative to the entire suspension, and surfactant, glycerin, dispersion stabilizer and water are based on the total amount of the aqueous suspension obtained by removing the amount of lauroyl peroxide added from the entire suspension. % By weight. [Viscosity measurement] B-type viscometer (Tokyo Keiki Seisakusho, rotation speed 2
0r. p. m. ) Was used and it measured at 20 degreeC. The unit is expressed in poise. [Storage stability test] Samples were placed in a glass container kept at 20 ° C and stored by static storage, and indicated by the number of months until the water layer was separated by 1% or more. Also, the thickened and creamy product is ()
The number of months is shown in. [Viscosity Stability Test] Samples were stored at 20 ° C., and when the increase rate of the viscosity after one month was 10% or less with respect to the initial viscosity, it was shown as ◯ and when 10% or more, it was shown as x. Those separated within one month are indicated by-. [Aqueous viscosity and yield value] A dispersion stabilizer, a surfactant, glycerin and water were mixed in the proportions shown in Table 1 to prepare an aqueous system, and the aqueous system viscosity at 20 ° C was rotated with a B-type viscometer. Number 20 r. p. m. And the yield value is B
Type viscometer rotation speed 1.0r. p. m. , 0.5r. p.
m. Was calculated by the formula (1).

【0018】比較例 1〜10 表1に示す各成分を実施例に準じて処理して水性懸濁液
を得、各測定を行った。結果を表1に示す。
Comparative Examples 1 to 10 Each component shown in Table 1 was treated according to the examples to obtain an aqueous suspension, and each measurement was performed. The results are shown in Table 1.

【0019】[0019]

【表1】 [Table 1]

【0020】表1中の記号は次の通りである。 *1 レオジック252L、レオジック830Lは日本
純薬社製の架橋型アクリル酸ソーダ水溶性樹脂の商品名
である。又、カーボポール941はグッドリッチ社製の
架橋型アクリル酸水溶性樹脂の商品名であり、カセイソ
ーダで中和してから用いた。又ゴーセノールKH−17
は日本合成化学工業社製の部分ケン化ポリ酢酸ビニルで
ある。 *2 シュガーエステルL−1570は三菱化成食品社
製のショ糖ラウリン酸エステル(HLB15)の商品名
である。ノニオンNS−210、ノニオンNS−20
6、ノニオンS−40は夫々、日本油脂社製のポリオキ
シエチレンノニルフェニルエーテル(HLB13.
3)、ポリオキシエチレンノニルフェニルエーテル(H
LB10.9)、ポリオキシエチレンモノステアレート
(HLB18.2)の商品名である。サーフィノール4
65は日信化学工業社製の2,4,7,9−テトラメチ
ル−5−デシン−4,7−ジオールのエチレンオキサイ
ド付加物(HLB13〜14)の商品名である。
The symbols in Table 1 are as follows. * 1 Rheogic 252L and Rheogic 830L are trade names of water-soluble crosslinked sodium acrylate resin manufactured by Nippon Pure Chemical Co., Ltd. Carbopol 941 is a trade name of a crosslinked acrylic acid water-soluble resin manufactured by Goodrich Co., Ltd., and was used after being neutralized with caustic soda. Gohsenol KH-17
Is a partially saponified polyvinyl acetate manufactured by Nippon Synthetic Chemical Industry Co., Ltd. * 2 Sugar ester L-1570 is a trade name of sucrose laurate ester (HLB15) manufactured by Mitsubishi Kasei Foods Co., Ltd. Nonion NS-210, Nonion NS-20
6, nonion S-40 is polyoxyethylene nonyl phenyl ether (HLB13.
3), polyoxyethylene nonyl phenyl ether (H
LB10.9) and polyoxyethylene monostearate (HLB18.2) are trade names. Surfynol 4
65 is a trade name of 2,4,7,9-tetramethyl-5-decyne-4,7-diol ethylene oxide adduct (HLB13 to 14) manufactured by Nisshin Chemical Industry Co., Ltd.

【0021】表1より、本発明の水性懸濁液は、6カ月
以上の長期間貯蔵していても、安定性が優れていること
がわかる。
From Table 1, it can be seen that the aqueous suspension of the present invention has excellent stability even when stored for a long period of 6 months or more.

Claims (1)

【特許請求の範囲】[Claims] 【請求項1】 過酸化ラウロイルの水性懸濁液におい
て、過酸化ラウロイルを30〜60重量%、過酸化ラウ
ロイルを除いた水系中にグリセリンを20〜22重量
%、HLB値が12〜16の界面活性剤を0.2〜5重
量%、及び、架橋型アクリル系水溶性樹脂を0.02〜
5重量%含む過酸化ラウロイルの水性懸濁液。
1. An aqueous suspension of lauroyl peroxide containing 30 to 60% by weight of lauroyl peroxide, 20 to 22% by weight of glycerin in an aqueous system excluding lauroyl peroxide, and an interface having an HLB value of 12 to 16. 0.2-5% by weight of activator and 0.02-crosslinking acrylic water-soluble resin
Aqueous suspension of lauroyl peroxide containing 5% by weight.
JP12313793A 1993-04-28 1993-04-28 Aqueous suspension of lauroyl peroxide Expired - Fee Related JP3412185B2 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP12313793A JP3412185B2 (en) 1993-04-28 1993-04-28 Aqueous suspension of lauroyl peroxide

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP12313793A JP3412185B2 (en) 1993-04-28 1993-04-28 Aqueous suspension of lauroyl peroxide

Publications (2)

Publication Number Publication Date
JPH06313005A true JPH06313005A (en) 1994-11-08
JP3412185B2 JP3412185B2 (en) 2003-06-03

Family

ID=14853107

Family Applications (1)

Application Number Title Priority Date Filing Date
JP12313793A Expired - Fee Related JP3412185B2 (en) 1993-04-28 1993-04-28 Aqueous suspension of lauroyl peroxide

Country Status (1)

Country Link
JP (1) JP3412185B2 (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPWO2004101670A1 (en) * 2003-05-14 2006-07-13 電気化学工業株式会社 Polychloroprene latex composition and method for producing the same
US9574162B2 (en) 2010-08-31 2017-02-21 Church & Dwight Co., Inc. Liquid detergent formulation containing peroxide and a metal-based bleach catalyst

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPWO2004101670A1 (en) * 2003-05-14 2006-07-13 電気化学工業株式会社 Polychloroprene latex composition and method for producing the same
JP4819500B2 (en) * 2003-05-14 2011-11-24 電気化学工業株式会社 Process for producing polychloroprene latex composition
US9574162B2 (en) 2010-08-31 2017-02-21 Church & Dwight Co., Inc. Liquid detergent formulation containing peroxide and a metal-based bleach catalyst

Also Published As

Publication number Publication date
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