JP2004043328A - New barium soap - Google Patents

New barium soap Download PDF

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Publication number
JP2004043328A
JP2004043328A JP2002200230A JP2002200230A JP2004043328A JP 2004043328 A JP2004043328 A JP 2004043328A JP 2002200230 A JP2002200230 A JP 2002200230A JP 2002200230 A JP2002200230 A JP 2002200230A JP 2004043328 A JP2004043328 A JP 2004043328A
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Japan
Prior art keywords
fatty acid
barium
granular
mixture
reaction
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JP2002200230A
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Japanese (ja)
Inventor
Toyoo Harada
原田 豊雄
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KAWAMURA KASEI KOGYO KK
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KAWAMURA KASEI KOGYO KK
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Priority to JP2002200230A priority Critical patent/JP2004043328A/en
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Abstract

<P>PROBLEM TO BE SOLVED: To provide barium soap which is a readily handleable granular shape and easily dispersible in a synthetic resin, etc. <P>SOLUTION: A fatty acid barium is a granular fatty acid barium which is not a hollow shape without substantially containing a binder. The number of foreign material-like materials is ≤5 in an area of 20 cm square in a sheet obtained by kneading a mixture of 100 g of polyvinyl chloride prepared by suspension polymerization and having degree of polymerization of about 1,100 with 100 g of 2-ethylhexyl phthalate (DOP) and 0.2 g of stearic acid using a kneading roll having 8 inches diameter at 160°C surface temperature and 0.3 mm roll spacing for 3 min, then adding the granular fatty acid barium salt and further carrying out kneading for 1 min. <P>COPYRIGHT: (C)2004,JPO

Description

【0001】
【発明の属する技術分野】本発明は新規なバリウム石ケン及びその製造方法に関する。
【0002】
【従来の技術】バリウム石ケンはプラスチック産業界に広く用いられており、特に安定剤、潤滑剤および離型剤としてポリ塩化ビニル、ポリエチレン、ポリプロピレン、ポリスチレン、ABS樹脂等のような熱可塑性樹脂の加工に用いられている。
【0003】
バリウム石ケンは脂肪酸のアルカリ塩などの水溶液にバリウム塩の水溶液を加えるいわゆる複分解反応によって得られる。また、溶融法といわれる方法によっても得られる。この方法は酸化バリウムまたは水酸化バリウムを溶融状、コロイド状、フレーク状または粉状の脂肪酸のいずれかと、必要に応じて触媒または湿潤剤を用い、混合することによつて、炭素原子8〜30個を有する脂肪酸の、電解質を含まないバリウム塩が得られている。これらの方法によって得られたバリウム石ケンは微細で軽く、かさ高い粉末であり、微細なダストを非常に形成しやすく、製造時と取り扱い時に粉じん爆発の原因となる可能性がある。粉状の金属石ケンの他の欠点は、十分な流動性を有しないことである。このため輸送や貯蔵に問題があり、また自動化された配合装置内で使用することも困難である。
【0004】
ダストのない金属石ケンを製造するため多くの検討がなされている。特開昭52−89612号公報や特開昭57−98236号公報には添加物を添加し顆粒状の金属石ケンを得る方法が記載されている。しかし、添加物は合成樹脂の特性に悪い影響を与えることが多く、添加物が含有される顆粒状の金属石ケンは好ましいものではない。特開昭54−154709号公報には添加物が含有されない中空状の構造を有する金属石ケンが記載されているが粒子表面の密度が高いため分散性は良好なものではなく、製造方法もやや煩雑である。特開昭55−136244号公報にも添加物が含有されない粒子状の金属石ケンの製法が記載されているが、外部からの加熱なしに反応を進行させるため反応の進行が十分でなく、また、分散性も満足できるものではない。また、特開平9−100253号公報や特開平10−147550号公報にも顆粒状の金属石ケンの製法が記載されており、これらの公報にはバリウム石ケンも製造できることが記載されているが、実施例にはバリウム石ケンの記載はなく、実施例の製造方法に従っても実用に供することができるバリウム石ケンを得ることはできない。またこれらに公報に記載された製造方法は非常に特殊なものである。
【0005】
【発明が解決しようとする課題】本発明の課題は、結合剤などを含まずダストの発生がなくかつ合成樹脂中への分散性にすぐれたバリウム石ケン及びその簡便な製造方法を提供することにある。
【0006】
【課題を解決するための手段】本発明者は、鋭意検討を重ねた結果、本発明に至った。すなわち本発明は、次の発明に関する。
【0007】
(1) 実質的に結合剤を含有しない中空状でない顆粒状脂肪酸バリウムであり、直径8インチ、表面温度160℃、ロール間隔0.3mm、前ロール回転数20rpm、後ロール回転数20rpmの混練ロールに重合度約1100の懸濁重合によって得られたポリ塩化ビニル100g、2−エチルヘキシルフタレート(DOP)100g、ステアリン酸0.2gの混合物を3分間混練した後、該顆粒状脂肪酸バリウムを添加後さらに1分間混練して得られたシートの異物状物が20cm角の面積中に5個以下である脂肪酸バリウム。
(2) 篩による分級において100メッシュオン分の割合が50重量%以上である(1)記載の顆粒状脂肪酸バリウム。
(3) 篩による分級において100メッシュオン分の割合が80重量%以上である(1)記載の顆粒状脂肪酸バリウム。
(4) 脂肪酸がステアリン酸を主成分とする脂肪酸である(1)〜(3)いずれかに記載の顆粒状脂肪酸バリウム。
(5) 脂肪酸と水酸化バリウムの混合物を密閉容器内に載置し、混合物が略水平に移動することにより混合する混合手段を用いて混合させながら反応させることを特徴とする顆粒状脂肪酸バリウムの製造方法。
(6) 脂肪酸と水酸化バリウムを粉体あるいは顆粒状など固体状の状態で密閉容器内に載置して反応を開始する(5)記載の顆粒状脂肪酸バリウムの製造方法。
(7) 脂肪酸と水酸化バリウムを粉体あるいは顆粒状など固体状の状態で密閉容器内に載置して反応を実質的に粉体あるいは顆粒状で反応する(5)〜(6)記載の顆粒状脂肪酸バリウムの製造方法。
(8) 反応時に外部から加熱する(5)〜(7)記載の顆粒状脂肪酸バリウムの製造方法。
(9) 脂肪酸と水酸化バリウムの混合物にさらに水を存在させる(5)〜(8)いずれかに記載の顆粒状脂肪酸バリウムの製造方法。
【0008】
【発明の実施の形態】
本発明の顆粒状脂肪酸バリウムの脂肪酸成分としては、炭素数6〜22の脂肪酸、たとえばカプロン酸、カプリル酸、ラウリン酸(融点:44.2℃)、ミリスチン酸、パルミチン酸、ステアリン酸(融点:69.6℃)、アラキジン酸、ベヘニン酸、イソステアリン酸、オレイン酸、リノール酸、リノレン酸、リシノール酸、12−ヒドロキシステアリン酸、あるいはこれらの混合物等をあげることができる。これらの脂肪酸は、勿論牛脂脂肪酸、パーム油脂肪酸のように混合脂肪酸であってもよい。特に、ステアリン酸及びラウリン酸が好適なものである。
【0009】
本発明の顆粒状脂肪酸バリウムは実質的に結合剤を含有するものではない。結合材を全く含まないことが望ましいが、1.0重量%以下、好ましくは0.5重量%以下、さらに好ましく0.2重量%以下、特に好ましくは、0.1重量%以下を含有することを妨げるものではない。結合材を多く含有すると、合成樹脂の安定剤に用いたとき、生成する合成樹脂製品の機械特性などの物性に悪い影響を及ぼす場合がある。
【0010】
本発明の脂肪酸バリウムは顆粒状であることが必要である。顆粒状にすることにより、粉体状のものに比較し、粉塵爆発の危険性がなくなり、空気中に飛散しにくく環境問題を生じることもなくなる。また、カサ比重が大きくなり運搬や保管が容易となり、押出機等の加工機器においても移送することが容易になる。本発明の顆粒状脂肪酸バリウムはカサ比重(振動などによる圧縮なし)が0.6〜0.9になる。好ましい範囲は0.65〜0.85である。
【0011】
本発明の脂肪酸バリウムは、実質的に結合剤を含有しない中空状でない顆粒状脂肪酸バリウムであり、直径8インチ、表面温度160℃、ロール間隔0.3mm、前ロール回転数20rpm、後ロール回転数20rpmの混練ロールに重合度約1100の懸濁重合によって得られたポリ塩化ビニル100g、2−エチルヘキシルフタレート(DOP)100g、ステアリン酸0.2gの混合物を3分間混練した後、該顆粒状脂肪酸バリウムを添加後さらに1分間混練して得られたシートの異物状物が20cm角の面積中に5個以下であることが必要である。顆粒状の脂肪酸バリウムはカサ比重が大きく、合成樹脂の安定剤等に用いた場合、通常合成樹脂中への分散性が悪化し、合成樹脂製品の表面にぶつやフィッシュアイと呼ばれる異物が現れる。しかし、本発明の脂肪酸バリウムは安定剤として合成樹脂の成形加工に用いた場合、どのような合成樹脂であってもまた、通常の加工条件においては異物状物が生じることがない。
【0012】
本発明の脂肪酸バリウムは粒状であれば特に限定はないが、100メッシュオン分の割合が50重量%以上、さらには80重量%以上、であることが好ましい。
【0013】
本発明の顆粒状脂肪酸バリウムの形状として粒子内部まで顆粒状脂肪酸バリウムが存在していることが望ましい。特に、中空状でないことが必要である。中空状とは1つの顆粒において、脂肪酸バリウムが表面に局在する状態をいい、この場合、合成樹脂中への分散が容易でないことが多い。
【0014】
本発明の顆粒状脂肪酸バリウム中の遊離脂肪酸の量は1%以下、好ましくは0.5%以下である。
【0015】
本発明の顆粒状脂肪酸バリウムにおいて用いる原料バリウム化合物としては、水酸化バリウムを挙げることができる。水酸化物の粉末は、95重量%以上の純度を有することが望ましい。
【0016】
本発明の顆粒状脂肪酸バリウムにおいて用いる原料高級脂肪酸としては、炭素数6〜22の脂肪酸、たとえばカプロン酸、カプリル酸、ラウリン酸(融点:44.2℃)、ミリスチン酸、パルミチン酸、ステアリン酸、アラキジン酸、ベヘニン酸、イソステアリン酸、オレイン酸、リノール酸、リノレン酸、リシノール酸、12−ヒドロキシステアリン酸、あるいはこれらの混合物等をあげることができる。これらの脂肪酸は、勿論牛脂脂肪酸、パーム油脂肪酸のように混合脂肪酸であってもよい。特に、ステアリン酸及びラウリン酸が好適なものである。ステアリン酸を用いる場合、ステアリン酸の純品を用いることは通常なく、ステアリン酸を主成分とする脂肪酸を用いることが普通である。ステアリン酸を主成分とする脂肪酸とはステアリン酸含量が最も多い脂肪酸をいう。ステアリン酸含量が60〜70重量%のものを用いることができ、40重量%程度のものも使用することができる。反応機に投入する際、これらの脂肪酸を溶融状態あるいは液体状態でなく、粉体状あるいは顆粒状などの固体状態で投入することが重要である。溶融状態あるいは液体状態で投入すると本発明の顆粒状脂肪酸バリウムを得ることは非常に困難である。
【0017】
本発明の脂肪酸バリウムは水酸化バリウムと脂肪酸を反応させることによって得られる。反応温度は反応が進行すれば特に制限はないが90℃〜150℃、好ましくは95℃〜130℃、さらに好ましくは100℃〜110℃である。反応は密閉容器の中で行うことが望ましい。反応中の反応物は溶融しておらず、粉状あるいは粒状の状態で反応しており、溶融状態にない。反応時の反応系の圧力は0.2気圧〜5気圧(ゲージ)さらには0.3気圧〜3気圧(ゲージ)、特には0.4気圧〜1.5気圧(ゲージ)が好ましい。反応温度を100℃〜120℃とし、反応圧力を0.3気圧〜2気圧とするのが好ましい。反応系には脂肪酸とバリウム化合物合計量100重量部に対して、水を0.1〜10重量部、好ましくは1.0〜5重量部、共存させることが望ましい。水を存在させることにより本発明の脂肪酸バリウムを容易に得ることができるようになる。
【0018】
本発明の脂肪酸バリウムを製造するには反応容器における反応物の混合方法が重要なポイントになる。通常の攪拌翼、すなわち、垂直方向に取り付けた回転軸を有する攪拌翼では本発明の顆粒状脂肪酸バリウムを製造することは不可能である。回転軸が略水平に取り付けられており、反応物が水平方向に移動することにより、反応物の混合がなされるような攪拌翼を有する反応器が必要である。このような反応機の1例を図1に示す。回転数は100回転/分以下、好ましくは10〜50回転/分、さらに好ましくは15〜30回転/分の回転速度で回転し、反応物の移動はゆっくりなされることが好ましい。回転翼(攪拌翼)の形状はスキ型が好ましい。回転翼先端の線速度は0.5m/sec〜3.0m/sec、さらには1.0m/sec〜2.0m/secが望ましい。
【0019】
【実施例】
次に本発明の方法を実施例に基づき具体的に説明する。
【0020】
(分散度試験法)
直径8インチ、表面温度160℃、ロール間隔0.3mm、前ロール回転数20rpm、後ロール回転数20rpmの混練ロールに、平均重合度約1100の懸濁重合によって得られたポリ塩化ビニル100g、2−エチルヘキシルフタレート(DOP)100g、ステアリン酸0.2gの混合物を3分間混練し、さらに脂肪酸バリウムを添加し1分間混練して取り出す。得られたロールシート20cm角の面積における異物状物を目視で数える。
【0021】
(実施例1)
図1と同種形状の20リットルの反応槽に混合脂肪酸6kg(鹸化値208、2mol相当)、Ba(OH)・HO 2.16kg(純度換算1mol相当)を投入、水300gを仕込んだ。25回転/分で攪拌翼の回転軸を回転させ、105℃、0.5気圧になるように加熱し20分間反応を進行させた。やや硬い顆粒状のバリウム石ケンを得た。100メッシュオンの顆粒は60重量%、異物状物の数は0個であった。また、遊離酸の量は0.5%以下であった。
このバリウム石ケンを安定剤として用い軟質塩化ビニルフィルムおよびABS樹脂板を製造したが分散性は非常に良好で異物がまったくない製品が得られた。
【0022】
【発明の効果】
本発明のバリウム石ケンは取り扱いやすい顆粒状でかつ合成樹脂などの中に容易に分散する。
【0023】
【図面の簡単な説明】
【図1】本発明のバリウム石ケンの製造に用いる反応機の1例である。
【0024】
【符号の説明】
1モーターおよび変速機
2回転軸
3スキ型攪拌翼
[0001]
The present invention relates to a novel barium soap and a method for producing the same.
[0002]
BACKGROUND OF THE INVENTION Barium soap is widely used in the plastics industry, especially as a stabilizer, lubricant and release agent for thermoplastic resins such as polyvinyl chloride, polyethylene, polypropylene, polystyrene and ABS resin. Used for processing.
[0003]
Barium soap is obtained by a so-called metathesis reaction in which an aqueous solution of a barium salt is added to an aqueous solution of an alkali salt of a fatty acid or the like. It can also be obtained by a method called a melting method. This method comprises mixing barium oxide or barium hydroxide with any of molten, colloidal, flake or powdered fatty acids, optionally using a catalyst or a wetting agent, to obtain a carbon atom of 8 to 30 carbon atoms. An electrolyte-free barium salt of a fatty acid having a single salt has been obtained. The barium soap obtained by these methods is a fine, light, and bulky powder, very easily forms fine dust, and may cause a dust explosion during production and handling. Another disadvantage of powdered metal soaps is that they do not have sufficient flowability. This has problems with transport and storage, and is difficult to use in automated compounding equipment.
[0004]
Many studies have been made to produce dust-free metal soaps. JP-A-52-89612 and JP-A-57-98236 describe a method of obtaining a granular metal soap by adding an additive. However, additives often adversely affect the properties of the synthetic resin, and granular soap containing the additives is not preferred. Japanese Patent Application Laid-Open No. 54-154709 describes a metal soap having a hollow structure containing no additive, but the dispersibility is not good due to the high density of the particle surface, and the production method is somewhat poor. It is complicated. JP-A-55-136244 also discloses a method for producing particulate metallic soap containing no additives, but the reaction proceeds without heating from the outside, and the progress of the reaction is not sufficient. Also, dispersibility is not satisfactory. JP-A-9-100253 and JP-A-10-147550 also describe a method for producing granular metal soap, and these publications also describe that barium soap can be produced. However, there is no description of barium soap in the examples, and barium soap that can be practically used cannot be obtained according to the production method of the examples. Further, the production methods described in these publications are very special.
[0005]
SUMMARY OF THE INVENTION It is an object of the present invention to provide a barium soap which does not contain a binder or the like, does not generate dust and has excellent dispersibility in a synthetic resin, and a simple method for producing the same. It is in.
[0006]
Means for Solving the Problems The present inventors have made intensive studies and as a result have arrived at the present invention. That is, the present invention relates to the following inventions.
[0007]
(1) A kneading roll having a diameter of 8 inches, a surface temperature of 160 ° C., a roll interval of 0.3 mm, a front roll rotation speed of 20 rpm, and a rear roll rotation speed of 20 rpm, which is barium-containing granular fatty acid barium substantially containing no binder. After kneading a mixture of 100 g of polyvinyl chloride, 100 g of 2-ethylhexyl phthalate (DOP) and 0.2 g of stearic acid obtained by suspension polymerization having a polymerization degree of about 1100 for 3 minutes, the granular fatty acid barium is added, and the mixture is further kneaded. Fatty acid barium in which the number of foreign substances on the sheet obtained by kneading for 1 minute is 5 or less in an area of 20 cm square.
(2) The granular fatty acid barium according to (1), wherein the ratio of 100 mesh-on in the classification by the sieve is 50% by weight or more.
(3) The barium fatty acid barium according to (1), wherein the ratio of 100 mesh-on in the classification by the sieve is 80% by weight or more.
(4) The granular fatty acid barium according to any one of (1) to (3), wherein the fatty acid is a fatty acid containing stearic acid as a main component.
(5) A granular fatty acid barium hydroxide characterized in that a mixture of a fatty acid and barium hydroxide is placed in a closed container, and the mixture is reacted while mixing using a mixing means that moves the mixture substantially horizontally. Production method.
(6) The method for producing a granular fatty acid barium according to (5), wherein the fatty acid and barium hydroxide are placed in a closed container in a solid state such as powder or granules to initiate a reaction.
(7) The method according to (5) to (6), wherein the fatty acid and barium hydroxide are placed in a closed container in a solid state such as powder or granules, and the reaction is substantially carried out in powder or granules. A method for producing a granular fatty acid barium.
(8) The method for producing a granular fatty acid barium according to (5) to (7), wherein the barium fatty acid is externally heated during the reaction.
(9) The method for producing granular fatty acid barium according to any one of (5) to (8), wherein water is further present in the mixture of the fatty acid and barium hydroxide.
[0008]
BEST MODE FOR CARRYING OUT THE INVENTION
The fatty acid component of the granular fatty acid barium of the present invention includes fatty acids having 6 to 22 carbon atoms, such as caproic acid, caprylic acid, lauric acid (melting point: 44.2 ° C.), myristic acid, palmitic acid, and stearic acid (melting point: 69.6 ° C.), arachidic acid, behenic acid, isostearic acid, oleic acid, linoleic acid, linolenic acid, ricinoleic acid, 12-hydroxystearic acid, and mixtures thereof. These fatty acids may of course be mixed fatty acids such as tallow fatty acids and palm oil fatty acids. In particular, stearic acid and lauric acid are preferred.
[0009]
The granular fatty acid barium of the present invention does not substantially contain a binder. It is desirable that no binder is contained at all, but 1.0% by weight or less, preferably 0.5% by weight or less, more preferably 0.2% by weight or less, particularly preferably 0.1% by weight or less It does not hinder. When the binder is contained in a large amount, when it is used as a stabilizer for a synthetic resin, it may have a bad influence on physical properties such as mechanical properties of a synthetic resin product to be produced.
[0010]
The fatty acid barium of the present invention needs to be in a granular form. By making it into a granular form, there is no danger of dust explosion as compared with a powdery form, and it does not easily scatter in the air and does not cause environmental problems. Further, the bulk specific gravity increases, which facilitates transportation and storage, and facilitates transfer to processing equipment such as an extruder. The granular fatty acid barium of the present invention has a bulk specific gravity (no compression by vibration or the like) of 0.6 to 0.9. The preferred range is 0.65 to 0.85.
[0011]
The barium fatty acid of the present invention is a solid barium fatty acid which does not substantially contain a binder and has a diameter of 8 inches, a surface temperature of 160 ° C., a roll interval of 0.3 mm, a front roll rotation speed of 20 rpm, and a rear roll rotation speed. A mixture of 100 g of polyvinyl chloride, 100 g of 2-ethylhexyl phthalate (DOP), and 0.2 g of stearic acid obtained by suspension polymerization having a polymerization degree of about 1100 was kneaded on a kneading roll at 20 rpm for 3 minutes, and then the granular fatty acid barium fatty acid was kneaded. , The number of foreign substances on the sheet obtained by kneading for 1 minute after addition is 5 or less in a 20 cm square area. Granular fatty acid barium has a large bulk specific gravity, and when used as a stabilizer for a synthetic resin or the like, usually dispersibility in the synthetic resin is deteriorated, and foreign matters called bumps and fish eyes appear on the surface of the synthetic resin product. However, when the fatty acid barium of the present invention is used as a stabilizer in molding a synthetic resin, no matter what kind of synthetic resin is used, no foreign matter is generated under ordinary processing conditions.
[0012]
The fatty acid barium of the present invention is not particularly limited as long as it is granular, but the proportion of 100 mesh-on is preferably 50% by weight or more, more preferably 80% by weight or more.
[0013]
As the shape of the granular fatty acid barium of the present invention, it is desirable that the granular fatty acid barium is present up to the inside of the particle. In particular, it is necessary that it is not hollow. Hollow refers to a state in which the fatty acid barium is localized on the surface of one granule, and in this case, dispersion in a synthetic resin is often not easy.
[0014]
The amount of free fatty acids in the granular fatty acid barium of the present invention is 1% or less, preferably 0.5% or less.
[0015]
Examples of the raw material barium compound used in the granular fatty acid barium of the present invention include barium hydroxide. It is desirable that the hydroxide powder has a purity of 95% by weight or more.
[0016]
The raw material higher fatty acid used in the granular fatty acid barium of the present invention includes fatty acids having 6 to 22 carbon atoms, such as caproic acid, caprylic acid, lauric acid (melting point: 44.2 ° C.), myristic acid, palmitic acid, stearic acid, Examples include arachidic acid, behenic acid, isostearic acid, oleic acid, linoleic acid, linolenic acid, ricinoleic acid, 12-hydroxystearic acid, and mixtures thereof. These fatty acids may of course be mixed fatty acids such as tallow fatty acids and palm oil fatty acids. In particular, stearic acid and lauric acid are preferred. In the case of using stearic acid, a pure product of stearic acid is not usually used, and a fatty acid containing stearic acid as a main component is usually used. The fatty acid containing stearic acid as a main component refers to a fatty acid having the highest stearic acid content. Those having a stearic acid content of 60 to 70% by weight can be used, and those having a stearic acid content of about 40% by weight can also be used. When charged into a reactor, it is important that these fatty acids are charged not in a molten state or a liquid state but in a solid state such as a powder or a granule. It is very difficult to obtain the granular fatty acid barium of the present invention when charged in a molten state or a liquid state.
[0017]
The fatty acid barium of the present invention is obtained by reacting barium hydroxide with a fatty acid. The reaction temperature is not particularly limited as long as the reaction proceeds, but it is preferably from 90C to 150C, preferably from 95C to 130C, and more preferably from 100C to 110C. The reaction is desirably performed in a closed container. The reactants during the reaction are not melted, are reacted in a powdery or granular state, and are not in a molten state. The pressure of the reaction system during the reaction is preferably 0.2 to 5 atm (gauge), more preferably 0.3 to 3 atm (gauge), and particularly preferably 0.4 to 1.5 atm (gauge). It is preferable that the reaction temperature is 100 ° C to 120 ° C and the reaction pressure is 0.3 to 2 atm. In the reaction system, 0.1 to 10 parts by weight, preferably 1.0 to 5 parts by weight of water is desirably coexistent with respect to 100 parts by weight of the total amount of the fatty acid and the barium compound. The presence of water enables the fatty acid barium of the present invention to be easily obtained.
[0018]
An important point in producing the fatty acid barium of the present invention is a method of mixing reactants in a reaction vessel. It is not possible to produce the granular fatty acid barium of the present invention with a conventional stirring blade, that is, a stirring blade having a rotating shaft mounted vertically. There is a need for a reactor having a rotating shaft mounted substantially horizontally and having a stirring blade so that the reactants move in the horizontal direction to mix the reactants. One example of such a reactor is shown in FIG. The number of revolutions is 100 rpm or less, preferably 10 to 50 rpm, and more preferably 15 to 30 rpm, and the reactants are preferably moved slowly. The shape of the rotating blade (stirring blade) is preferably a ski shape. The linear velocity at the tip of the rotary blade is preferably 0.5 m / sec to 3.0 m / sec, more preferably 1.0 m / sec to 2.0 m / sec.
[0019]
【Example】
Next, the method of the present invention will be specifically described based on examples.
[0020]
(Dispersion test method)
A kneading roll having a diameter of 8 inches, a surface temperature of 160 ° C., a roll interval of 0.3 mm, a front roll rotation speed of 20 rpm, and a rear roll rotation speed of 20 rpm was charged with 100 g of polyvinyl chloride obtained by suspension polymerization having an average degree of polymerization of about 1100. -A mixture of 100 g of ethylhexyl phthalate (DOP) and 0.2 g of stearic acid is kneaded for 3 minutes, and further, barium fatty acid is added and kneaded for 1 minute to take out. The number of foreign matters in the obtained roll sheet having an area of 20 cm square is visually counted.
[0021]
(Example 1)
6 kg of a mixed fatty acid (corresponding to a saponification value of 208 and 2 mol) and 2.16 kg of Ba (OH) 2 .H 2 O (corresponding to a purity of 1 mol) were charged into a 20 liter reaction tank having the same shape as in FIG. 1 and 300 g of water were charged. . The rotation axis of the stirring blade was rotated at 25 revolutions / minute, heated to 105 ° C. and 0.5 atm, and the reaction was allowed to proceed for 20 minutes. A slightly hard granular barium soap was obtained. The granules of 100 mesh on were 60% by weight, and the number of foreign matters was 0. The amount of free acid was 0.5% or less.
Using this barium soap as a stabilizer, a soft vinyl chloride film and an ABS resin plate were produced, but a product having very good dispersibility and having no foreign matter was obtained.
[0022]
【The invention's effect】
The barium soap of the present invention is in a granular form that is easy to handle and easily dispersed in a synthetic resin or the like.
[0023]
[Brief description of the drawings]
FIG. 1 is an example of a reactor used for producing barium soap of the present invention.
[0024]
[Explanation of symbols]
1 motor and transmission 2 rotating shaft 3 ski type stirring blade

Claims (9)

実質的に結合剤を含有しない中空状でない顆粒状脂肪酸バリウムであり、直径8インチ、表面温度160℃、ロール間隔0.3mm、前ロール回転数20rpm、後ロール回転数20rpmの混練ロールに重合度約1100の懸濁重合によって得られたポリ塩化ビニル100g、2−エチルヘキシルフタレート(DOP)100g、ステアリン酸0.2gの混合物を3分間混練した後、該顆粒状脂肪酸バリウムを添加後さらに1分間混練して得られたシートの異物状物が20cm角の面積中に5個以下である脂肪酸バリウム。Barium-free solid fatty acid barium containing substantially no binder and having a diameter of 8 inches, a surface temperature of 160 ° C., a roll interval of 0.3 mm, a front roll rotation speed of 20 rpm, and a rear roll rotation speed of 20 rpm. A mixture of 100 g of polyvinyl chloride, 100 g of 2-ethylhexyl phthalate (DOP) and 0.2 g of stearic acid obtained by suspension polymerization of about 1100 was kneaded for 3 minutes, and then kneaded for 1 minute after adding the granular fatty acid barium. Fatty acid barium having 5 or less foreign matters in a sheet obtained by subjecting to an area of 20 cm square. 篩による分級において100メッシュオン分の割合が50重量%以上である請求項1記載の顆粒状脂肪酸バリウム。The granular fatty acid barium according to claim 1, wherein the ratio of 100 mesh-on in the classification by the sieve is 50% by weight or more. 篩による分級において100メッシュオン分の割合が80重量%以上である請求項1記載の顆粒状脂肪酸バリウム。The granular fatty acid barium according to claim 1, wherein a ratio of 100 mesh-on in the classification by the sieve is 80% by weight or more. 脂肪酸がステアリン酸を主成分とする脂肪酸である請求項1〜3いずれかに記載の顆粒状脂肪酸バリウム。The granular fatty acid barium according to any one of claims 1 to 3, wherein the fatty acid is a fatty acid containing stearic acid as a main component. 脂肪酸と水酸化バリウムの混合物を密閉容器内に載置し、混合物が略水平に移動することにより混合する混合手段を用いて混合させながら反応させることを特徴とする顆粒状脂肪酸バリウムの製造方法。A method for producing a granular fatty acid barium, wherein a mixture of a fatty acid and barium hydroxide is placed in a closed container, and the mixture is reacted while mixing using a mixing means that moves the mixture substantially horizontally. 脂肪酸と水酸化バリウムを粉体あるいは顆粒状など固体状の状態で密閉容器内に載置して反応を開始する請求項5記載の顆粒状脂肪酸バリウムの製造方法。The method for producing a granular fatty acid barium according to claim 5, wherein the fatty acid and barium hydroxide are placed in a closed container in a powdered state or a solid state such as a granular state to initiate a reaction. 脂肪酸と水酸化バリウムを粉体あるいは顆粒状など固体状の状態で密閉容器内に載置して反応を実質的に粉体あるいは顆粒状で反応する請求項5〜6記載の顆粒状脂肪酸バリウムの製造方法。7. The method of claim 5, wherein the fatty acid and barium hydroxide are placed in a closed container in a solid state such as powder or granules, and the reaction is substantially carried out in powder or granules. Production method. 反応時に外部から加熱する請求項5〜7記載の顆粒状脂肪酸バリウムの製造方法。The method for producing a granular fatty acid barium according to claim 5, wherein the reaction is heated from the outside during the reaction. 脂肪酸と水酸化バリウムの混合物にさらに水を存在させる請求項5〜8いずれかに記載の顆粒状脂肪酸バリウムの製造方法。The method for producing a granular fatty acid barium according to any one of claims 5 to 8, wherein water is further present in the mixture of the fatty acid and barium hydroxide.
JP2002200230A 2002-07-09 2002-07-09 New barium soap Pending JP2004043328A (en)

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