JP2005126501A - Granular aromatic hydrocarbon resin excellent in caking resistance and method for attaching anti-caking agent - Google Patents

Granular aromatic hydrocarbon resin excellent in caking resistance and method for attaching anti-caking agent Download PDF

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JP2005126501A
JP2005126501A JP2003361528A JP2003361528A JP2005126501A JP 2005126501 A JP2005126501 A JP 2005126501A JP 2003361528 A JP2003361528 A JP 2003361528A JP 2003361528 A JP2003361528 A JP 2003361528A JP 2005126501 A JP2005126501 A JP 2005126501A
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aromatic hydrocarbon
hydrocarbon resin
granular
caking
granular aromatic
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Masato Ohira
正人 大平
Masashi Hayashi
正士 林
Kazuyoshi Ishii
一由 石井
Mikio Oka
幹夫 岡
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Air Water Inc
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Air Water Chemical Inc
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<P>PROBLEM TO BE SOLVED: To provide a granular aromatic hydrocarbon resin excellent in caking resistance caused by fusion, and to provide a method for attaching an anti-caking agent. <P>SOLUTION: After an aromatic hydrocarbon resin is granulated, a finely divided powder of an inorganic compound such as magnesium silicate, talc or clay is uniformly attached on the surface thereof to prevent granules with caking properties from coming into direct contact with each other to prevent caking. Alternatively, after an aromatic hydrocarbon resin is granulated, it is uniformly mixed with a finely divided powder of an inorganic compound such as magnesium silicate, talc or clay to attach the finely divided powder of an inorganic compound on the surface of the granular aromatic hydrocarbon resin. <P>COPYRIGHT: (C)2005,JPO&NCIPI

Description

本発明は、貯蔵、輸送時の固結防止性に優れ、ゴムとの相溶性、混練作業性の良好な粒状芳香族炭化水素樹脂および固結防止剤付着方法に関するものである。   The present invention relates to a granular aromatic hydrocarbon resin excellent in anti-caking property during storage and transportation, good compatibility with rubber and good kneading workability, and an anti-caking agent adhesion method.

粒状芳香族炭化水素樹脂は、自動車のタイヤ用ゴムの添加剤として使用されており、ゴムとの相溶性やロール混練作業性の良好なものが求められている。   The granular aromatic hydrocarbon resin is used as an additive for rubber for automobile tires, and is required to have good compatibility with rubber and roll kneading workability.

粒状芳香族炭化水素樹脂は、石油系のピッチを反応釜に仕込み、270〜330℃に加熱昇温したのち、反応釜の底部から空気を吹き込みながら、5〜15時間程度保持して酸化重合させて軟化点が所定の温度に到達すると、反応を終了する。生成した芳香族炭化水素樹脂は、ノズルから冷却されたベルト上に滴下して造粒し、袋詰めして一時貯蔵されたのち出荷される。   The granular aromatic hydrocarbon resin is charged with petroleum-based pitch in a reaction kettle, heated to 270-330 ° C, heated and then oxidatively polymerized by holding it for 5-15 hours while blowing air from the bottom of the kettle. When the softening point reaches a predetermined temperature, the reaction is terminated. The produced aromatic hydrocarbon resin is dropped on a belt cooled from a nozzle, granulated, packed in a bag, temporarily stored, and then shipped.

通常、粒状芳香族炭化水素樹脂は、ゴムとの相溶性、混練温度100〜110℃におけるロール混練作業性の観点から、軟化点100〜110℃の低軟化点のものが要求されている。芳香族炭化水素樹脂の軟化点は、反応終点を制御することにより、軟化点100〜130℃のものを製造することが可能である。しかし、低軟化点(100〜110℃)のものは、袋詰めして室温で保管した場合、夏場では製造後、2〜3日で融着して固結してしまい、実用に耐えられないといった問題があった。   Usually, the granular aromatic hydrocarbon resin is required to have a softening point of 100 to 110 ° C. from the viewpoint of compatibility with rubber and workability of roll kneading at a kneading temperature of 100 to 110 ° C. The softening point of the aromatic hydrocarbon resin can be controlled to 100 to 130 ° C. by controlling the reaction end point. However, those with a low softening point (100-110 ° C), which are packed in bags and stored at room temperature, will melt and consolidate in 2-3 days after production in the summer, making them unusable for practical use There was a problem.

また、粒状芳香族炭化水素樹脂は、軟化点120℃のものでも、夏場に南方などに船便で出荷する場合、船内の温度が40℃以上に達するため、輸送中に固結してしまうといった問題があった。   In addition, even if the granular aromatic hydrocarbon resin has a softening point of 120 ° C, when shipped by ship to the south, etc. in the summer, the temperature inside the ship reaches 40 ° C or more, so it becomes hardened during transportation. was there.

粒状物質の固結防止方法、例えば、吸湿性を有する粒状肥料の固結防止法としては、珪藻土、タルク、カオリン、珪酸粉末などの無機質微粉末を肥料に付着させ、固結性物質の直接接触を防止する方法、鉱物油、水溶性高分子等で固結性物質の表面をコーティングして防水性皮膜を形成せしめ、水分の出入りを少なくし、これに伴う塩類の析出を防ぎ粒子間のブリッジの生成を防止する方法などが知られている。
特開平6-24885号公報 As a method for preventing solidification of particulate matter, for example, as a method for preventing solidification of hygroscopic granular fertilizer, inorganic fine powders such as diatomaceous earth, talc, kaolin, and silicic acid powder are adhered to the fertilizer and direct contact of the solidified material A method for preventing water, coating the surface of solidifying substances with mineral oil, water-soluble polymers, etc. to form a waterproof film, reducing the ingress and egress of moisture, preventing the precipitation of salts accompanying this, and bridging between particles There are known methods for preventing the generation of.
Japanese Unexamined Patent Publication No. 6-24885

しかし、粒状芳香族炭化水素樹脂の固結は、軟化溶融による固結であるため、粒状肥料と異なり吸湿性を有しておらず、吸湿による塩類の析出を防ぎ粒子間のブリッジの生成を防止する粒状肥料の固結防止方法をそのまま採用することはできない。   However, since solidification of granular aromatic hydrocarbon resin is due to softening and melting, it does not have hygroscopicity unlike granular fertilizer, preventing salt precipitation due to moisture absorption and preventing the formation of bridges between particles. The method of preventing solidification of granular fertilizer to be used cannot be adopted as it is.

本発明の目的は、固結防止性に優れ、ゴムとの相溶性、混練作業性の良好な粒状芳香族炭化水素樹脂および固結防止剤付着方法を提供することにある。   An object of the present invention is to provide a granular aromatic hydrocarbon resin having excellent anti-caking property, good compatibility with rubber, and good kneading workability, and a method for attaching an anti-caking agent.

本発明の請求項1の粒状芳香族炭化水素樹脂は、芳香族炭化水素樹脂を造粒後、珪酸塩、タルク、クレイなどの微粉末の無機系化合物を表面に均一に付着させたことを特徴とする。   The granular aromatic hydrocarbon resin according to claim 1 of the present invention is characterized in that after the aromatic hydrocarbon resin is granulated, fine powder inorganic compounds such as silicate, talc and clay are uniformly attached to the surface. And

また、本発明の請求項2の粒状芳香族炭化水素樹脂は、珪酸塩、タルク、クレイなどの微粉末の無機系化合物を、粒状芳香族炭化水素樹脂に対し0.01〜3重量%、好ましくは0.1〜1重量%表面に付着させてなる。   Further, the granular aromatic hydrocarbon resin according to claim 2 of the present invention is a fine powder inorganic compound such as silicate, talc, clay, etc., in an amount of 0.01 to 3% by weight, preferably 0.1% to the granular aromatic hydrocarbon resin. ~ 1% by weight attached to the surface.

本発明の請求項3の粒状芳香族炭化水素樹脂への固結防止剤付着方法は、造粒した芳香族炭化水素樹脂と珪酸塩、タルク、クレイなどの微粉末の無機系化合物を、ミキサーに仕込み、混合して粒状芳香族炭化水素樹脂表面に微粉末の無機系化合物を付着させたのち、篩を通して余剰の微粉末の無機系化合物を除去する。   The method of attaching an anti-caking agent to the granular aromatic hydrocarbon resin according to claim 3 of the present invention uses a granulated aromatic hydrocarbon resin and a finely divided inorganic compound such as silicate, talc and clay in a mixer. After charging and mixing to adhere the fine powdered inorganic compound to the surface of the granular aromatic hydrocarbon resin, the excess fine powdered inorganic compound is removed through a sieve.

本発明の請求項1の粒状芳香族炭化水素樹脂は、芳香族炭化水素樹脂を造粒後、珪酸塩、タルク、クレイなどの微粉末の無機系化合物を表面に均一に付着させたことによって、固結性の粒状芳香族炭化水素樹脂同士の直接接触が表面に均一に付着した無機系化合物の微粉末によって防止され、固結することなく長期間の保管が可能となる。また、固結防止が図れることで、軟化点100〜110℃の低軟化点の樹脂が製造可能となり、ゴムとの相溶性、混練作業性が向上する。なお、珪酸塩、タルク、クレイなどの無機系化合物は、タイヤ用を含めてゴムの充填材としてよく使用されているため、粒状芳香族炭化水素樹脂に付着させて使用しても問題がない。   The granular aromatic hydrocarbon resin according to claim 1 of the present invention, after granulating the aromatic hydrocarbon resin, by uniformly attaching fine inorganic compounds such as silicate, talc and clay to the surface, Direct contact between the solidified granular aromatic hydrocarbon resins is prevented by the fine powder of the inorganic compound uniformly adhered to the surface, and long-term storage is possible without solidification. Further, by preventing the caking, it becomes possible to produce a resin having a low softening point of 100 to 110 ° C., and compatibility with rubber and kneading workability are improved. Inorganic compounds such as silicate, talc, and clay are often used as rubber fillers, including those for tires, so there is no problem even if they are used by attaching them to granular aromatic hydrocarbon resins.

また、本発明の請求項2の粒状芳香族炭化水素樹脂は、珪酸塩、タルク、クレイなどの微粉末の無機系化合物を、粒状芳香族炭化水素樹脂に対し0.01〜3重量%、好ましくは0.1〜1重量%表面に付着させたことによって、固結性の粒状芳香族炭化水素樹脂同士の直接接触が表面に均一に付着した無機系化合物の微粉末によって防止され、軟化点100〜110℃の粒状芳香族炭化水素樹脂であっても、固結することなく長期間の保管が可能となる。また、固結防止が図れることで、軟化点100〜110℃の低軟化点の樹脂が製造可能となり、ゴムとの相溶性、混練作業性が向上する。   Further, the granular aromatic hydrocarbon resin according to claim 2 of the present invention is a fine powder inorganic compound such as silicate, talc, clay, etc., in an amount of 0.01 to 3% by weight, preferably 0.1% to the granular aromatic hydrocarbon resin. By attaching to the surface by ~ 1% by weight, direct contact between the caking particulate aromatic hydrocarbon resins is prevented by the fine powder of the inorganic compound uniformly attached to the surface, and the softening point is 100 to 110 ° C. Even a granular aromatic hydrocarbon resin can be stored for a long time without solidifying. Further, by preventing the caking, it becomes possible to produce a resin having a low softening point of 100 to 110 ° C., and compatibility with rubber and kneading workability are improved.

本発明の請求項3の粒状芳香族炭化水素樹脂への固結防止剤付着方法は、造粒した芳香族炭化水素樹脂と珪酸塩、タルク、クレイなどの微粉末の無機系化合物を、ミキサーに仕込み、混合して粒状芳香族炭化水素樹脂表面に微粉末の無機系化合物を付着させたのち、篩を通して余剰の微粉末の無機系化合物を除去することによって、余分な無機系化合物が除去され、ゴムとの相溶性、混練作業性が良好となる。   The method of attaching an anti-caking agent to the granular aromatic hydrocarbon resin according to claim 3 of the present invention uses a granulated aromatic hydrocarbon resin and a finely divided inorganic compound such as silicate, talc and clay in a mixer. After charging and mixing to adhere the fine inorganic compound to the surface of the granular aromatic hydrocarbon resin, the excess fine inorganic compound is removed by removing the excess fine inorganic compound through a sieve. Good compatibility with rubber and kneading workability.

芳香族炭化水素樹脂の原料として用いる石油ピッチの代表的性状は、密度1.0〜1.3(試験法:JIS K-2249)、引火点150℃以上(試験法:JIS K-2265)のものが使用できる。本発明の対象とする粒状芳香族炭化水素樹脂の製造は、酸化重合法、具体的には以下の方法で行う。石油系のピッチをステンレス鋼製の反応釜に仕込み、釜底から空気を吹き込みながら加熱昇温し、270〜330℃に5〜15時間程度保持して酸化重合反応させ、軟化点100〜130℃に調整した後、例えば、反応液をノズルから冷却されたベルト上に滴下して造粒したものである。   The typical properties of petroleum pitch used as a raw material for aromatic hydrocarbon resins are those with a density of 1.0 to 1.3 (test method: JIS K-2249) and a flash point of 150 ° C or higher (test method: JIS K-2265). . Production of the granular aromatic hydrocarbon resin which is the subject of the present invention is carried out by an oxidative polymerization method, specifically by the following method. A petroleum-based pitch is charged into a stainless steel reaction kettle, heated to a temperature while blowing air from the bottom of the kettle, and kept at 270-330 ° C for about 5-15 hours to undergo an oxidative polymerization reaction, with a softening point of 100-130 ° C Then, for example, the reaction liquid is dropped on a belt cooled from a nozzle and granulated.

芳香族炭化水素樹脂の軟化点の調整は、酸化重合時にサンプルを採取し、JIS K-2207に規定の軟化点測定器を用いて軟化点を測定し、所定の軟化点となった時点で酸化重合反応を停止する。   To adjust the softening point of the aromatic hydrocarbon resin, take a sample during oxidative polymerization, measure the softening point using the softening point measuring instrument specified in JIS K-2207, and oxidize when the softening point is reached. Stop the polymerization reaction.

造粒した芳香族炭化水素樹脂は、固結防止剤を均一に付着させたのち、所定重量、例えば、10kgづつポリエチレン製の袋に充填し、パレット上に段積みして出荷するまで保管する。   After the granulated aromatic hydrocarbon resin is uniformly attached with an anti-caking agent, it is filled into polyethylene bags of a predetermined weight, for example, 10 kg, and stored until being stacked on a pallet and shipped.

本発明で用いる粒状芳香族炭化水素樹脂の固結防止剤としては、粒状芳香族炭化水素樹脂に付着させても問題とならない自動車のタイヤ用を含めてゴムの充填材として使用されているもので、珪酸マグネシウム、珪酸カルシウムなどの珪酸塩、タルク、クレーなどの無機質化合物の微粉末を用いる。   The anti-caking agent for the granular aromatic hydrocarbon resin used in the present invention is used as a rubber filler, including for automobile tires that do not pose a problem even if attached to the granular aromatic hydrocarbon resin. Fine powders of inorganic compounds such as silicates such as magnesium silicate and calcium silicate, talc and clay are used.

粒状芳香族炭化水素樹脂表面へ固結防止剤を均一に付着させるには、ナウターミキサー、モルタルミキサー、タービュライザー等のミキサーに造粒した芳香族炭化水素樹脂と固結防止剤を仕込み、撹拌混合して造粒した樹脂表面に固結防止剤を付着させたのち、篩を用いて余剰の固結防止剤を除去する。篩のメッシュサイズは、造粒品が落下せずに固結防止剤が落下するサイズであればよい。具体的には10〜30メッシュ程度が好ましい。   In order to uniformly attach the anti-caking agent to the surface of the granular aromatic hydrocarbon resin, an aromatic hydrocarbon resin and an anti-caking agent that are granulated are mixed in a mixer such as a Nauter mixer, a mortar mixer, or a turbulizer. After the anti-caking agent is adhered to the surface of the granulated resin by stirring and mixing, the excess anti-caking agent is removed using a sieve. The mesh size of the sieve may be a size that allows the anti-caking agent to fall without dropping the granulated product. Specifically, about 10 to 30 mesh is preferable.

粒状芳香族炭化水素樹脂への固結防止剤の付着量は、粒状芳香族炭化水素樹脂に対して0.01〜3重量%、好ましくは0.1〜1重量%である。固結防止剤の付着量が0.01重量%未満では、固結防止効果がなく、3重量%を超えると付着ロスが多くなる。   The adhesion amount of the anti-caking agent to the granular aromatic hydrocarbon resin is 0.01 to 3% by weight, preferably 0.1 to 1% by weight, based on the granular aromatic hydrocarbon resin. When the adhesion amount of the anti-caking agent is less than 0.01% by weight, there is no anti-caking effect, and when it exceeds 3% by weight, the adhesion loss increases.

実施例1
原料として石油系のピッチ(富士興産(株)製、商品名フッコールアロマックス#1)10Tonをステンレス鋼製の反応釜に仕込み、釜底から空気を50m3/hrで吹き込みながら、300℃まで加熱昇温し、300℃で9時間保持して酸化重合反応を行い、試験法JIS K-2207に規定の軟化点測定器を用いて軟化点を測定し、軟化点が110℃となった時点で反応液を中間品タンクに移送し、冷却したベルト上に反応液をノズルから滴下させて造粒を行い、粒状芳香族炭化水素樹脂を製造した。得られた粒状芳香族炭化水素樹脂は、密度1.149、軟化点110℃、全酸価2.8mgKOH/g、固定炭素28.3%であった。 Example 1
Petroleum-based pitch (Fujikosan Co., Ltd., product name Fukkor Aromax # 1) 10Ton as a raw material was charged into a stainless steel reaction kettle, and air was blown from the kettle bottom at 50 m 3 / hr up to 300 ° C When the temperature is raised by heating and held at 300 ° C for 9 hours to conduct an oxidation polymerization reaction, the softening point is measured using a softening point measuring instrument specified in test method JIS K-2207, and the softening point is 110 ° C Then, the reaction liquid was transferred to an intermediate product tank and granulated by dropping the reaction liquid from a nozzle onto a cooled belt to produce a granular aromatic hydrocarbon resin. The obtained granular aromatic hydrocarbon resin had a density of 1.149, a softening point of 110 ° C., a total acid value of 2.8 mgKOH / g, and fixed carbon of 28.3%.

得られた粒径3〜6mmの粒状芳香族炭化水素樹脂50kgと固結防止剤として珪酸マグネシウム(富田製薬(株)製、トミタ−AD600CY)500g(芳香族炭化水素樹脂に対して1重量%)を、内径750mm、高さ350mm、内容積97リットルのモルタルミキサーにそれぞれ仕込み、約1分間撹拌して粒状芳香族炭化水素樹脂の表面に珪酸マグネシウムを付着させた。珪酸マグネシウムを付着させた粒状芳香族炭化水素樹脂は、モルタルミキサーから取出し、20メッシュの篩を用いて余分な珪酸マグネシウムを除去した後、ホッパーに投入した。上記操作を繰り返し、それぞれ300kgの粒状芳香族炭化水素樹脂を処理して珪酸マグネシウム付着粒状芳香族炭化水素樹脂を製造した。   50 kg of the obtained granular aromatic hydrocarbon resin having a particle size of 3 to 6 mm and magnesium silicate (Tomita Pharmaceutical Co., Ltd., Tomita-AD600CY) as an anti-caking agent (1% by weight with respect to the aromatic hydrocarbon resin) Were put in a mortar mixer having an inner diameter of 750 mm, a height of 350 mm, and an internal volume of 97 liters, and stirred for about 1 minute to adhere magnesium silicate to the surface of the granular aromatic hydrocarbon resin. The granular aromatic hydrocarbon resin to which magnesium silicate was adhered was taken out of the mortar mixer, and after removing excess magnesium silicate using a 20-mesh sieve, it was put into a hopper. The above operation was repeated, and each 300 kg of the granular aromatic hydrocarbon resin was processed to produce a magnesium silicate-attached granular aromatic hydrocarbon resin.

同様に得られた粒径3〜6mmの粒状芳香族炭化水素樹脂50kgと固結防止剤として珪酸マグネシウム(富田製薬(株)製、トミタ−AD600CY)250g(芳香族炭化水素樹脂に対して0.5重量%)、タルク(山陽クレー工業(株)製、タルクH)500g(芳香族炭化水素樹脂に対して1.0重量%)、またはクレー(山陽クレー工業(株)製、O,Aクレー)2.0kg(芳香族炭化水素樹脂に対して4.0重量%)をそれぞれモルタルミキサーに仕込み、約1分間撹拌して粒状芳香族炭化水素樹脂の表面に珪酸マグネシウム、タルクまたはクレーを付着させ、余分な珪酸マグネシウム、タルクまたはクレーを除去した後、ホッパーに投入することを繰り返し、各300kgの粒状芳香族炭化水素樹脂を処理して珪酸マグネシウム、タルクまたはクレー付着粒状芳香族炭化水素樹脂を製造した。   Similarly, 50 kg of granular aromatic hydrocarbon resin having a particle size of 3 to 6 mm obtained and 250 g of magnesium silicate (Tomita Pharmaceutical Co., Ltd., Tomita-AD600CY) as an anti-caking agent (0.5 wt.% With respect to the aromatic hydrocarbon resin) %), Talc (Sanyo Clay Industry Co., Ltd., Talc H) 500 g (1.0% by weight relative to the aromatic hydrocarbon resin), or clay (Sanyo Clay Industry Co., Ltd., O, A clay) 2.0 kg ( (4.0% by weight with respect to the aromatic hydrocarbon resin) in a mortar mixer and stirred for about 1 minute to adhere magnesium silicate, talc or clay to the surface of the granular aromatic hydrocarbon resin, and excess magnesium silicate and talc. Alternatively, after removing the clay, it was repeatedly put into a hopper, and each 300 kg of the granular aromatic hydrocarbon resin was processed to produce a magnesium silicate, talc or clay-attached granular aromatic hydrocarbon resin.

さらに、各固結防止剤付着粒状芳香族炭化水素樹脂は、各ホッパーから10kgづつポリエチレン製の袋に小分け充填してそれぞれ合計30袋を袋詰めし、図1に示すように、パレット1上に袋詰めした固結防止剤付着粒状芳香族炭化水素樹脂袋2を6列で5段積みし、パレット1を保温庫に入れ、内温50℃となるように設定し、さらに、固結防止剤付着粒状芳香族炭化水素樹脂袋2の上にパレット3を積み、パレット3の上に水を入れたドラム缶4を乗せて700kgの荷重を懸けた。この状態で放置し、3日、7日、14日、30日後に最下段の固結防止剤付着粒状芳香族炭化水素樹脂袋2を取出し、固結状態を目視で観察した。その結果を表1に示す。また、固結防止剤付着粒状芳香族炭化水素樹脂は、固結防止剤付着量を測定した。   Furthermore, each anti-caking agent-attached granular aromatic hydrocarbon resin is divided into 10 kg polyethylene bags from each hopper, and each is packed into a total of 30 bags, as shown in FIG. Packed anti-caking agent-attached granular aromatic hydrocarbon resin bags 2 are stacked in 6 rows and 5 tiers, pallet 1 is placed in a heat storage, set to an internal temperature of 50 ° C, and anti-caking agent A pallet 3 was stacked on the adhered granular aromatic hydrocarbon resin bag 2, and a drum 4 with water was put on the pallet 3 and a load of 700 kg was applied. The product was left in this state, and after 3, 7, 14, and 30 days, the bottom anti-caking agent-attached granular aromatic hydrocarbon resin bag 2 was taken out, and the caking state was visually observed. The results are shown in Table 1. Moreover, the anti-caking agent adhesion granular aromatic hydrocarbon resin measured the anti-caking agent adhesion amount.

比較のため、前記により製造した粒状芳香族炭化水素樹脂300kgは、固結防止剤を付着させることなく、そのまま10kgづつポリエチレン製の袋に小分け充填して合計30袋を袋詰めし、固結防止剤付着粒状芳香族炭化水素樹脂袋2と同条件で荷重試験を行い、固結状態を目視で観察した。その結果を表1に示す。   For comparison, 300 kg of the granular aromatic hydrocarbon resin produced as described above was packed in 10 kg as it is into polyethylene bags without attaching an anti-caking agent, and a total of 30 bags were packed to prevent caking. A load test was performed under the same conditions as the agent-attached granular aromatic hydrocarbon resin bag 2, and the consolidated state was visually observed. The results are shown in Table 1.

なお、粒状芳香族炭化水素樹脂の密度は、試験法JIS K-2249により測定した。また、全酸価は、試験法JIS K-2501により測定した。固定炭素は、試験法JIS M-8812により測定した。固結防止剤の付着量の測定は、珪酸マグネシウム、タルクまたはクレー付着造粒品の各サンプル25gをそれぞれ100mlの水の入ったビーカーに入れ、超音波洗浄器で20分間超音波洗浄して付着した固結防止剤を落とし、この各洗浄水を濾紙で濾過し、乾燥後重量を測定して固結防止剤の付着量を求めた。また、表1中の目視観察による固結状態欄の◎印は、全く固結は認められず、○印は、少し融着気味であるが、袋から出すとほぐれる、×印は、融着して袋全体が固結した状態を示す。   The density of the granular aromatic hydrocarbon resin was measured by the test method JIS K-2249. The total acid value was measured by the test method JIS K-2501. Fixed carbon was measured by the test method JIS M-8812. The amount of anti-caking agent deposited was measured by placing 25 g of each sample of magnesium silicate, talc or clay-attached granulated product in a beaker containing 100 ml of water and ultrasonically washing with an ultrasonic cleaner for 20 minutes. The anti-caking agent was dropped, each washing water was filtered with a filter paper, and after drying, the weight was measured to determine the adhesion amount of the anti-caking agent. In addition, in the consolidated state column by visual observation in Table 1, ◎ marks indicate no consolidation at all, ○ marks are slightly fused, but loosen when removed from the bag, X marks indicate fusion. And the state which the whole bag consolidated was shown.

Figure 2005126501
Figure 2005126501

表1に示すように、固結防止剤として珪酸マグネシウムを付着させた粒状芳香族炭化水素樹脂は、30日経過後も全く固結は認められず、タルク、クレーを付着させた粒状芳香族炭化水素樹脂は、14日経過後も全く固結は認められず、30日経過後に少し融着気味であるが、袋から出すとほぐれる状態であった。これに対し、固結防止剤を付着させなかった粒状芳香族炭化水素樹脂は、3日経過後に袋全体が固結して一枚岩のような状態であった。   As shown in Table 1, the granular aromatic hydrocarbon resin to which magnesium silicate was attached as an anti-caking agent showed no caking after 30 days, and granular aromatic hydrocarbon to which talc and clay were attached. The resin was not solidified at all even after 14 days, and was slightly fused after 30 days, but it was in a state of loosening when removed from the bag. On the other hand, the granular aromatic hydrocarbon resin to which no anti-caking agent was attached was in a monolithic state with the entire bag consolidated after 3 days.

本発明は、例えば、粒状芳香族炭化水素樹脂以外の比較的低軟化点(100〜110℃)の炭化水素樹脂の固結防止に効果があるものと推測される。   The present invention is presumed to be effective in preventing caking of hydrocarbon resins having a relatively low softening point (100 to 110 ° C.) other than the granular aromatic hydrocarbon resin, for example.

図1は、実施例における固結状態測定のための荷重試験の説明図である。FIG. 1 is an explanatory diagram of a load test for measuring a consolidated state in an example.

符号の説明Explanation of symbols

1、3 パレット
2 固結防止剤付着粒状芳香族炭化水素樹脂袋
4 ドラム缶 1, 3 pallets
2 Granulated aromatic hydrocarbon resin bag with anti-caking agent
4 drums

Claims (3)

芳香族炭化水素樹脂を造粒後、珪酸塩、タルク、クレイなどの微粉末の無機系化合物を表面に付着させたことを特徴とする粒状芳香族炭化水素樹脂。   A granular aromatic hydrocarbon resin, characterized in that fine particles of an inorganic compound such as silicate, talc, and clay are adhered to the surface after granulating the aromatic hydrocarbon resin. 珪酸塩、タルク、クレイなどの微粉末の無機系化合物を、粒状芳香族炭化水素樹脂に対し0.01〜3重量%、好ましくは0.1〜1重量%付着させてなる請求項1記載の粒状芳香族炭化水素樹脂。   The granular aromatic carbonization according to claim 1, wherein a fine powder inorganic compound such as silicate, talc, clay, etc. is adhered to the granular aromatic hydrocarbon resin in an amount of 0.01 to 3% by weight, preferably 0.1 to 1% by weight. Hydrogen resin. 造粒した芳香族炭化水素樹脂と珪酸塩、タルク、クレイなどの微粉末の無機系化合物を、ミキサーに仕込み、混合して粒状芳香族炭化水素樹脂表面に微粉末の無機系化合物を付着させたのち、篩を通して余剰の微粉末の無機系化合物を除去することを特徴とする粒状芳香族炭化水素樹脂への固結防止剤付着方法。   The granulated aromatic hydrocarbon resin and fine powder inorganic compound such as silicate, talc, and clay were charged into a mixer and mixed to adhere the fine inorganic compound to the surface of the granular aromatic hydrocarbon resin. Then, a method of attaching an anti-caking agent to the granular aromatic hydrocarbon resin, wherein the inorganic compound in excess fine powder is removed through a sieve.
JP2003361528A 2003-10-22 2003-10-22 Granular aromatic hydrocarbon resin excellent in caking resistance and method for attaching anti-caking agent Pending JP2005126501A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2008538125A (en) * 2005-03-31 2008-10-09 シェブロン ユー．エス．エー． インコーポレイテッド Granular solid wax particles

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2008538125A (en) * 2005-03-31 2008-10-09 シェブロン ユー．エス．エー． インコーポレイテッド Granular solid wax particles
JP2012162746A (en) * 2005-03-31 2012-08-30 Chevron Usa Inc Granular solid wax particle
JP2012162745A (en) * 2005-03-31 2012-08-30 Chevron Usa Inc Granular solid wax particle

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