JP2010090382A - Wax for candle, method of manufacturing the same, and candle using the wax - Google Patents
Wax for candle, method of manufacturing the same, and candle using the wax Download PDFInfo
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本発明は、廃食用油より製造された硬化油を原料としたワックス、特にローソク用ワックスとその製造方法及び該ローソク用ワックスを使用したローソクとその製造方法に関するものである。原料供給に不安のある石油製品の一つであるパラフィンワックスの代替として、大部分が廃棄されていた廃食用油をローソク原料として有効に再利用した、環境にやさしいワックス、特にローソク用ワックスとその製造方法及び該ローソク用ワックスを使用したローソクとその製造方法に関するものである。The present invention relates to a wax made from a hardened oil produced from waste edible oil as a raw material, in particular, a candle wax and a production method thereof, and a candle using the candle wax and a production method thereof. As an alternative to paraffin wax, which is one of the petroleum products that are worried about the supply of raw materials, environmentally friendly waxes, in particular candle waxes, and their waxes, which have been effectively reused as waste candles, are mostly discarded. The present invention relates to a production method, a candle using the candle wax, and a production method thereof.
従来より、家庭、外食産業、ホテル等で食品の加工に使用された使用済みの食用油の大部分が廃棄処分されていたが、最近再利用に関して、種々の方法が提案され、一部実用化されている。例えば食品関連事業者から排出される廃食用油は油脂再生配合業者等に集められて物理・化学処理後、成分調整されて、飼料、肥料、油脂関係会社や化学会社で肥料に添加されたり、飼料や工業油脂に加工されている。Traditionally, most of the used cooking oil used for food processing in the home, restaurant industry, hotels, etc. has been disposed of, but recently various methods have been proposed for reuse and some have been put into practical use. Has been. For example, waste edible oil discharged from food-related businesses is collected by fat and oil recycling companies, etc., physical and chemical treatment, component adjustment, feed, fertilizer, oil and fat affiliated companies and chemical companies added to fertilizer, Processed into feed and industrial fats and oils.
また、セッケンへの加工が比較的容易であるため昔から一部の家庭では、廃食用油からセッケンをつくって再利用しているが、セッケンを作る際にアルカリ性の強い苛性ソーダを使用するため、家庭での使用に危険を伴うことや、セッケンの使用により河川の富栄養化が促されるとの指摘もある。最近の石油製品の高騰から廃食用油を原料としたバイオディーゼル燃料が注目され、官民あげて技術開発が活発化しているものの、化学反応過程で生じる１０％程度のグリセリン等の有効利用が進んでおらず、しかも軽油代替燃料とするには製造コストが高いため、未だ実用化の目途が立っていない。Also, because it is relatively easy to process into soap, some households have been making soap from waste cooking oil and reusing it, but since caustic soda with strong alkalinity is used when making soap, Some point out that it is dangerous to use at home, and that the use of soap promotes eutrophication of rivers. Biodiesel fuel made from waste edible oil has attracted attention due to the recent rise in petroleum products, and while technological development has been actively promoted by both the public and private sectors, effective use of about 10% glycerin, etc. generated in the chemical reaction process has progressed. In addition, since the production cost is high for a light oil alternative fuel, there is still no prospect of practical use.
さらに、廃食用油の一部はボイラーなどの熱源として使用されているが、精製の必要性や回収コストなどの点から利用できる場所が限定されている。最近、イベント等で家庭から集められた廃食用油を小型容器に入れ、ゲル化剤を添加してゲル化したローソクがエコローソクの名称で使用されているが、ゲルローソクは燃焼の際の油煙が多い、燃焼芯を消耗させる、炎が小さい、燃焼芯に大量に煤がたまって炎が消える等の問題があるため、自分で作って楽しむローソクとして細々と再利用されているにすぎない。Furthermore, some of the waste edible oil is used as a heat source for boilers and the like, but the places where it can be used are limited in view of the necessity for purification and recovery costs. Recently, waste candle oil collected from households at events, etc., is put in a small container and gelled by adding a gelling agent, and the name of Eco Candle is used. There are many problems, such as a lot of burning, exhausting the burning wick, small flames, and a large amount of soot on the burning wick, and the flame disappears, so it is only reused as a candle that you can make and enjoy yourself.
このように、大量に発生する廃食用油はその一部が再利用されているに過ぎず、残りの大部分は固化剤で固めたり、吸油剤に吸わせてゴミとして焼却処理されたり、活性汚泥で生分解処理されたり、処理されずにそのまま河川に垂れ流されているのが現状である。
本発明者らは大量に廃棄されている廃食用油を、パラフィンワックス代替のローソク原料として再利用すると、石油枯渇による原料問題、廃棄による環境汚染問題等が一挙に解決されることに着目し、廃食用油を原料としたローソク用ワックス及びローソクについて更に検討した。In this way, only a part of the waste edible oil generated in large quantities is reused, and most of the rest is hardened with a solidifying agent, incinerated as garbage by absorbing it with an oil absorbing agent, or activated. At present, it is biodegraded with sludge or spilled into the river without being treated.
The present inventors pay attention to the fact that waste edible oil, which has been disposed of in large quantities, is reused as a candle raw material instead of paraffin wax, so that the problems of raw materials due to oil depletion, environmental pollution problems due to disposal, etc. are solved at once. We further investigated candle wax and candles made from waste cooking oil.
まず、従来の石油を原料とするパラフィンワックスに代わり、廃食用油の主成分である植物油を原料とした植物性ワックスを使用したローソクについて検討した。かかる植物性ワックスを使用したローソクに関し、３件の文献が提案されている（特許文献１、特許文献２、特許文献３参照）。First, instead of the conventional paraffin wax made from petroleum, a candle using vegetable wax made from vegetable oil, which is the main component of waste cooking oil, was examined. Regarding the candle using such vegetable wax, three documents have been proposed (see Patent Document 1, Patent Document 2, and Patent Document 3).
例えば、特許文献１には、植物油を原料とする高級脂肪酸を母材の主体成分とする植物性ローソク組成物であって、高級脂肪酸が５〜１５℃の融点差を有し、かつ融点５０℃以上の飽和高級脂肪酸の２種以上の混合物からなる植物性ローソク組成物が記載されている。また従来技術として、植物由来の原料を使用してなる植物性ローソクとしては、硬化油を原料として製造されたものが公知であるが、硬化油を原料とする植物性ローソクは、補助容器の必要な５ｃｍ３未満の小さなローソクばかりであった。その理由は、硬化油の主成分は単一の脂肪酸エステルからなり、ローソクの母材であるパラフィンなどに比べて融点の分布幅がシャープであるため、ローソクの製造に際してクラックが発生しやすいと記載されている。For example, Patent Document 1 discloses a vegetable candle composition having a higher fatty acid derived from vegetable oil as a main component, the higher fatty acid having a melting point difference of 5 to 15 ° C, and a melting point of 50 ° C. A vegetable candle composition comprising a mixture of two or more of the above saturated higher fatty acids is described. In addition, as a conventional technique, a plant candle using a plant-derived raw material is known to be manufactured using a hardened oil as a raw material. However, a plant candle using a hardened oil as a raw material requires an auxiliary container. Only small candles of less than 5 cm3. The reason is that the main component of the hardened oil is a single fatty acid ester, and the distribution range of the melting point is sharper than that of paraffin, which is the base material of the candle, so that cracks are likely to occur during candle production. Has been.
特許文献２には、植物性ローソクの成型性を改善する効果を持つグリセリン脂肪酸エステル及び／又はポリグリセリン脂肪酸エステルを用いて製造した植物性ローソクが記載されている。また、従来技術としてパラフィンワックスは、石油から得られるため、環境面においても石油枯渇問題、環境破壊問題等、数多くの問題を抱えているのが現状である。そこで、最近、ローソク用の油脂として、天然ろうやパラフィンワックスの代わりに、植物油から得られる硬化油を使用する方法が注目されてきた。しかし上記植物硬化油のみではローソクに成型する際、油脂の固化状態が悪く、粗大結晶の発生により表面が粗くなり、更にひび割れが生じるなど、パラフィンワックス等に比べて一般的なローソクの形に成型することは難しいという問題を抱えていると記載されている。Patent Document 2 describes a plant candle produced using a glycerin fatty acid ester and / or a polyglycerin fatty acid ester having an effect of improving the moldability of the plant candle. In addition, since paraffin wax is obtained from petroleum as a conventional technique, it currently has a number of problems in terms of environment, such as oil depletion and environmental destruction. Therefore, recently, a method of using hardened oil obtained from vegetable oil instead of natural wax or paraffin wax as a fat and oil for candles has attracted attention. However, when molding into a candle with only the above-mentioned plant-hardened oil, the solidified state of the fats and oils is poor, the surface becomes rough due to the generation of coarse crystals, and further cracks occur, so it is molded into a general candle shape compared to paraffin wax etc. It is stated that it has a problem that it is difficult to do.
特許文献３には、ローソク組成物が、ゲル化剤であるベンジリデンソルビトール類と植物油とを含み、ベンジリデンソルビトール類が植物油１００重量部に対し０．５〜５重量部であるとし、これらを混合してガラスなどの容器に入れて形成するゲルローソクが記載されている。
しかしながら、各特許文献にローソク原料として記載された植物性ワックスの多くが、食用となる植物性油脂を原料としているため、石油を原料とするパラフィンワックスのような枯渇のおそれはないが、昨今の世界的な食料不足の折から、食料以外の用途であるローソク原料に使用するには好ましくない。また植物性油脂として廃食用油を使用することについては各文献には、全く記載されていない。However, since many of the vegetable waxes described as candle raw materials in each patent document are made from edible vegetable oils and fats, there is no fear of depletion like paraffin waxes made from petroleum. Due to the global food shortage, it is not preferable for use as a raw material for candles that are used for purposes other than food. Moreover, it is not described at all about using waste edible oil as vegetable oil.
特許文献１及び特許文献２に従来技術として記載されている植物油から得られる硬化油を使用した植物性ローソクは、文献中にも、ローソクの製造に際に、クラックが発生しやすいという問題がある。また不飽和分の分解揮発臭がする。炎が小さくなる。燃焼芯に煤が付着する。燃焼芯への吸い上げが悪い。等の問題がある。そのため、硬化油を原料とする植物性ローソクは、上記影響を比較的受けにくい小型（小径）のローソクに限定され、大型（直径２０ｍｍ以上）のローソクは上市されていないと、硬化油を原料とした大型ローソクはいまだ実用化されていないことが記載されている。The plant candle using the hardened oil obtained from the vegetable oil described as the prior art in Patent Document 1 and Patent Document 2 has a problem that cracks are easily generated in the literature even in the production of the candle. . There is also a decomposition volatile odor of unsaturated components. The flame becomes smaller. Soot adheres to the combustion core. The suction to the combustion core is bad. There are problems such as. Therefore, vegetable candles that use hardened oil as a raw material are limited to small (small diameter) candles that are relatively unaffected by the above-mentioned effects. If large (20 mm or more diameter) candles are not marketed, It is described that the large-sized candle that has not been put into practical use yet.
、
特許文献３に記載されているゲル化ローソクは、容器の中でゲル化させた容器ローソクの形でしか使用できない。また燃焼芯への吸い上げが悪く、炎が小さく、しかも燃焼芯に煤がたまったりして燃焼芯を消耗させる等の問題がある。また、ローソクの燃焼終了時には、容器は不燃物として分別廃棄する必要がある。特許文献３に記載されているゲル化ローソクは自立できず、自立して形状が保持できる本発明のローソクとは異なるローソクである。,
The gelled candle described in Patent Document 3 can only be used in the form of a container candle gelled in a container. Further, there is a problem that the suction to the combustion wick is poor, the flame is small, and the combustion wick accumulates on the combustion wick and wears the combustion wick. Also, at the end of burning the candle, the container must be disposed of as non-combustible material. The gelled candle described in Patent Document 3 is a candle that is different from the candle of the present invention that cannot be self-supporting and can hold its shape.
食用となる植物性油脂を原料とした従来の植物性ワックスに代わるローソク原料として、廃食用油から硬化油が製造できれば、廃食用油を原料としたローソク用ワックス及び該ワックスを使用したローソクが製造できるため、更に検討した結果、油脂である廃食用油の多くが融点の低い不飽和脂肪酸を多く含むため常温で液体となり、ローソク原料としては好ましくない。そこで廃食用油に水素添加を行い、融点の高い飽和脂肪酸の割合を増加させると、常温で固形化した油脂が製造でき、該油脂はローソク原料として使用できる。また、水素添加の程度で一部の不飽和脂肪酸を残すと液体と固体の中間の柔らかい硬化油とすることもできるし、完全に飽和脂肪酸とすると硬い硬化油とすることもできる。水素添加の程度を示す指標となるヨウ素価の小さい硬い硬化油は、ローソク製造時にクラックを生じやすい。一方ヨウ素価の大きい硬化油は柔らかくて融点が低くなり夏場の保管中に溶融したり、不快な油脂臭が残ったり、燃焼時に油煙が発生しやすくなるといった不都合を生じる。If hardened oil can be produced from waste edible oil as a candle raw material instead of the conventional vegetable wax made from edible vegetable oil, the wax using the edible oil and the candle using the wax will be produced. Therefore, as a result of further investigation, since many of the waste edible oils that are fats and oils contain a lot of unsaturated fatty acids having a low melting point, they become liquid at room temperature, which is not preferable as a candle raw material. Therefore, by hydrogenating waste cooking oil and increasing the ratio of saturated fatty acids having a high melting point, fats and oils solidified at room temperature can be produced, and the fats and oils can be used as candle raw materials. Moreover, if some unsaturated fatty acids are left in the degree of hydrogenation, a soft hardened oil between liquid and solid can be obtained, and if fully saturated fatty acids are obtained, a hard hardened oil can be obtained. A hard hydrogenated oil having a small iodine value, which serves as an index indicating the degree of hydrogenation, is liable to crack during candle production. On the other hand, hardened oils with a high iodine value are soft and have a low melting point, which causes problems such as melting during storage in the summer, unpleasant oily odor, and oily smoke being easily generated during combustion.
本発明者らは、硬化油のヨウ素価と融点を特定の範囲に調整すれば、クラックの発生がなく、不快な油脂臭や燃焼時に油煙の発生しないローソク、特に従来製造が困難であった直径２０ｍｍ以上の大型のローソクが製造できるとの確信の下に、さらに鋭意検討した結果、本発明に到達したものである。By adjusting the iodine value and melting point of the hardened oil to a specific range, the inventors of the present invention have no cracks, an unpleasant oily odor, and a candle that does not generate oil smoke during combustion, particularly a diameter that has been difficult to manufacture in the past. As a result of further diligent studies with the belief that a large candle of 20 mm or more can be produced, the present invention has been achieved.
したがって、本発明の第一の目的は、廃食用油を原料とする特定のヨウ素価を有する硬化油からなるワックスを提供することである。
本発明の第二の目的は、ローソク製造時にクラックを生じにくく、油煙が少なく、燃焼性に優れたローソク原料として、廃食用油を原料とする特定のヨウ素価を有する硬化油からなるローソク用ワックスを提供することである。Accordingly, a first object of the present invention is to provide a wax comprising a hardened oil having a specific iodine value, which is made from waste edible oil.
A second object of the present invention is a wax for candles comprising a hardened oil having a specific iodine value as a raw material of waste edible oil, as a candle raw material that is less prone to cracking during candle production, has less oil smoke, and is excellent in combustibility. Is to provide.
本発明の第三の目的は、廃食用油を原料とした、特定のヨウ素価を有する硬化油からなるローソク用ワックスの製造方法を提供することである。
本発明の第四の目的は、廃食用油を原料とした、特定のヨウ素価を有する硬化油を使用したローソクを提供することである。The third object of the present invention is to provide a method for producing a candle wax made of a hardened oil having a specific iodine value, using waste edible oil as a raw material.
The fourth object of the present invention is to provide a candle using a hardened oil having a specific iodine value and using waste edible oil as a raw material.
すなわち、第１の発明は、廃食用油を水素添加して得られた、融点が４０〜７０℃、ヨウ素価が５５以下の硬化油からなるワックスである。
第２の発明は、融点が４５〜６５℃、ヨウ素価が５〜４５の硬化油からなる第１の発明記載のローソク用ワックスである。
第３の発明は、廃食用油を原料とし、金属触媒の存在下で、水素添加して製造された硬化油を脱臭・ろ過して第２の発明記載の硬化油を製造するローソク用ワックスの製造方法である。That is, the first invention is a wax made of hydrogenated waste edible oil and having a melting point of 40 to 70 ° C. and an iodine value of 55 or less.
The second invention is a candle wax according to the first invention, which comprises a hardened oil having a melting point of 45 to 65 ° C. and an iodine value of 5 to 45.
According to a third aspect of the present invention, there is provided a candle wax for producing a hardened oil according to the second invention by deodorizing and filtering a hardened oil produced by adding hydrogen in the presence of a metal catalyst in the presence of a metal catalyst. It is a manufacturing method.
第４の発明は、第２の発明記載のローソク用ワックスから製造されたローソクである。4th invention is the candle manufactured from the wax for candles of 2nd invention description.
本発明は、大量に廃棄されている廃食用油をワックス、特にローソク用ワックスとして再利用することにより、石油枯渇による原料枯渇問題、廃棄による環境汚染問題等を解決することができる。また、植物性油脂をローソク原料とする植物性ローソクのように食用となる植物性油脂を原料とするのではなく、廃棄される廃植物油を原料とするため、世界的な食料不足問題にも対応した環境にやさしいローソク用ワックス及び該ワックスを原料としたローソクが提供できる。
また、硬化油のヨウ素価を特定の範囲に設定することで、クラックが生じにくく、油煙の少ない、燃焼性に優れた、従来のパラフィンワックスと同等のローソク用ワックス及びローソクが提供できる。According to the present invention, waste edible oil that has been disposed of in large quantities is reused as wax, particularly candle wax, so that the problem of exhaustion of raw materials due to exhaustion of oil, the problem of environmental pollution due to disposal, and the like can be solved. In addition, the plant does not use edible vegetable oils and fats as raw materials like plant candles that use vegetable oils and candles as raw materials. An environment-friendly candle wax and a candle using the wax as a raw material can be provided.
In addition, by setting the iodine value of the hardened oil within a specific range, it is possible to provide a wax for candles and candles that are less likely to cause cracking, have less oil smoke, and have excellent flammability, equivalent to conventional paraffin wax.
次に本発明のローソク用ワックスの製造システムの一例について図１にて説明する。図１はシステムのフロー図であり、本システムは、反応槽１、水素ボンベ２、窒素ボンベ３、脱臭手段及びろ過手段１０で構成されている。反応槽１は耐圧構造であり、胴体部に防爆型のバンドヒーター４が取り付けられている。反応槽１には防爆型の撹拌機５が取り付けられている。また、反応槽１の上部には、水素ガスボンベ２と配管で接続された水素ガス導入口６、窒素ガスボンベ３と配管で接続された窒素ガス導入口７、触媒や廃食用油の投入口８が設けられている。反応槽１の下部には、硬化油の排出口９が設けられている。１０は硬化油から触媒を取り除くためのろ過手段である。１１はボトムバルブ、１２はローソク原料配合槽である。Next, an example of the candle wax production system of the present invention will be described with reference to FIG. FIG. 1 is a flow chart of the system, and this system includes a reaction tank 1, a hydrogen cylinder 2, a nitrogen cylinder 3, a deodorizing means and a filtering means 10. The reaction tank 1 has a pressure-resistant structure, and an explosion-proof band heater 4 is attached to the body part. An explosion-proof stirrer 5 is attached to the reaction tank 1. In addition, a hydrogen gas inlet 6 connected to the hydrogen gas cylinder 2 by piping, a nitrogen gas inlet 7 connected to the nitrogen gas cylinder 3 by piping, and a catalyst and waste cooking oil inlet 8 are provided at the top of the reaction tank 1. Is provided. At the lower part of the reaction tank 1, a hardened oil discharge port 9 is provided. 10 is a filtration means for removing the catalyst from the hardened oil. 11 is a bottom valve, 12 is a candle raw material mixing tank.
システムは、まずバンドヒーター４で加熱された反応槽１の投入口８から一定量の廃食用油と触媒を投入した後、窒素ガスボンベ３から反応槽内に窒素ガスを導入して反応槽内の空気を完全に窒素置換する。その後、水素ガスボンベ２から水素ガスを導入口６から槽内に導入するとともに、撹拌機５を回転させて、廃食用油と水素を反応させる。予め設定された単位時間当たりの水素ガスの消費量とヨウ素価との関係から、設定されたヨウ素価に対応する水素ガスが消費されると水素ガスの供給を中止して、硬化油反応を終了する。反応終了後、ボトムバルブ１１を開放して、製造された硬化油を排出する。製造された硬化油には、金属触媒が含まれていたり、廃食用油に含まれる不純物の分解臭がするため、ろ過手段１０で金属触媒を除去し、また、脱臭手段（図示せず）でローソク原料として使用するのに支障にならない程度に臭気成分を除去する。脱臭手段及びろ過手段で処理された硬化油は、一旦ローソク原料配合槽１２に貯蔵し、公知の方法でローソクを製造することができる。In the system, first, after a certain amount of waste cooking oil and catalyst are introduced from the inlet 8 of the reaction tank 1 heated by the band heater 4, nitrogen gas is introduced from the nitrogen gas cylinder 3 into the reaction tank. The air is completely replaced with nitrogen. Thereafter, hydrogen gas is introduced from the hydrogen gas cylinder 2 into the tank through the inlet port 6 and the agitator 5 is rotated to react waste cooking oil and hydrogen. Based on the relationship between the hydrogen gas consumption per unit time set in advance and the iodine value, when hydrogen gas corresponding to the set iodine value is consumed, the supply of hydrogen gas is stopped and the hardened oil reaction is terminated. To do. After completion of the reaction, the bottom valve 11 is opened and the produced hardened oil is discharged. Since the produced hardened oil contains a metal catalyst or has a decomposition odor of impurities contained in the waste edible oil, the metal catalyst is removed by the filtering means 10, and the deodorizing means (not shown) is used. Remove odor components to the extent that they do not hinder use as a candle raw material. The hardened oil treated by the deodorizing means and the filtering means can be temporarily stored in the candle raw material mixing tank 12, and a candle can be produced by a known method.
食品加工には、通常牛脂、豚脂、魚油、鶏油などの動物性油脂からなる動物油、大豆油、ナタネ油、ゴマ油、綿実油、パーム油、サフラワー油、コーン油、米ぬか油、やし油、オリーブ油などの植物性油脂からなる植物油が使用されているが、ローソク原料となる廃食用油は、食品を加工した後の使用済みで、かつ上記動植物由来の油あれば特に制限はない。
原料の廃食用油には、揚げ物の場合は、加工工程で小麦粉、原料かす、水分等が混入するため、予めろ布や遠心分離等の公知のろ過手段でろ過して、廃食用油に含まれる水分、小麦粉などのゴミやかす等を取り除いておく必要がある。For food processing, animal oil consisting of animal fats such as beef tallow, pork tallow, fish oil, chicken oil, soybean oil, rapeseed oil, sesame oil, cottonseed oil, palm oil, safflower oil, corn oil, rice bran oil, palm oil Vegetable oils made of vegetable oils such as olive oil are used, but waste edible oils used as candle raw materials are not particularly limited as long as they are used after processing foods and are derived from the animals and plants.
In the case of fried food, the raw waste cooking oil contains wheat flour, raw material grounds, moisture, etc. in the processing process, so it is filtered in advance with a known filtering means such as filter cloth or centrifugal separation and included in the waste cooking oil It is necessary to remove the moisture, flour and other debris.
硬化油の臭気は、硬化油中に含まれる不純物の分解成分である。この分解成分は、硬化油をローソク原料として使用するのに支障にならない程度まで除去する必要がある。硬化油に含まれる分解成分を除去して脱臭する脱臭手段は、公知の脱臭手段が採用できる。例えば溶融状態の硬化油を活性炭や活性白土などを用いて吸着脱臭したり、反応槽１内の溶融状態の硬化油を真空（減圧）下で脱臭することができる。真空下での脱臭時に溶融状態の硬化油を撹拌したり、水蒸気や窒素ガスなどを吹き込むと、脱臭効果が向上して好ましい。The odor of the hardened oil is a decomposition component of impurities contained in the hardened oil. It is necessary to remove this decomposition component to such an extent that it does not hinder the use of the hardened oil as a candle raw material. Known deodorizing means can be adopted as the deodorizing means for removing the decomposing component contained in the hardened oil and deodorizing. For example, the molten hardened oil can be adsorbed and deodorized using activated carbon or activated clay, or the molten hardened oil in the reaction tank 1 can be deodorized under vacuum (reduced pressure). It is preferable to stir the molten oil at the time of deodorization under vacuum or to blow water vapor or nitrogen gas to improve the deodorizing effect.
硬化油の合成に使用した金属触媒は公知の手段で除去することができる。除去手段ではローソクの燃焼に阻害が生じない程度に金属触媒を除去すればよい。例えば、遠心分離で溶融した硬化油から金属触媒を除去してもよいし、ろ紙やろ布を用いた加圧ろ過、減圧ろ過、自然ろ過でも良いが、通常加圧ろ過や減圧ろ過が好ましく適用される。The metal catalyst used for the synthesis of the hardened oil can be removed by a known means. The removal means may remove the metal catalyst to such an extent that the burning of the candle is not hindered. For example, the metal catalyst may be removed from the hardened oil melted by centrifugal separation, or pressure filtration using filter paper or filter cloth, vacuum filtration, or natural filtration may be used, but usually pressure filtration or vacuum filtration is preferably applied. The
廃食用油の水素添加で用いられる金属触媒は特に限定されるものではなく、ニッケル、白金、パラジウム、ロジウム、ルテニウム、イリジウム、銅、銅−クロム、銅−ニッケル等が使用でき、ニッケル、白金、銅−クロム、銅−ニッケルが好ましく、なかでもニッケル、白金が好ましい。特にコスト面からニッケルが好ましい。The metal catalyst used in hydrogenation of waste cooking oil is not particularly limited, and nickel, platinum, palladium, rhodium, ruthenium, iridium, copper, copper-chromium, copper-nickel, etc. can be used, nickel, platinum, Copper-chromium and copper-nickel are preferable, and nickel and platinum are particularly preferable. Nickel is particularly preferable from the viewpoint of cost.
さらに上記のニッケル触媒は、湿式還元ニッケル触媒、乾式還元ニッケル触媒等を使用することができる。触媒の添加量は反応温度、水素分圧、反応時間、などに左右されるが、添加量は特に限定されるものではない。金属触媒は製造コストに占める割合が高いため、コストを考慮すると原料となる廃食用油１００重量部に対して０．００５〜２．０重量部程度が好ましい。通常０．０１〜０．５重量部が適当である。上記範囲未満であれば水添反応が進みにくく、上記範囲を超えるとコストアップとなり、パラフィンワックスの価格に対抗できない。Further, as the above nickel catalyst, a wet reduced nickel catalyst, a dry reduced nickel catalyst, or the like can be used. The addition amount of the catalyst depends on the reaction temperature, hydrogen partial pressure, reaction time, etc., but the addition amount is not particularly limited. Since the proportion of the metal catalyst in the production cost is high, considering the cost, about 0.005 to 2.0 parts by weight is preferable with respect to 100 parts by weight of the edible cooking oil as a raw material. Usually 0.01 to 0.5 parts by weight is appropriate. If it is less than the above range, the hydrogenation reaction is difficult to proceed, and if it exceeds the above range, the cost increases and the price of paraffin wax cannot be countered.
水素添加の反応条件は、通常の反応条件と同様な条件でよく、廃食用油と金属触媒を反応槽に入れた後に、撹拌下で、反応させる。水素添加反応は反応温度、水素分圧、反応時間、金属触媒量などに左右されるが、パラフィンワックスに対し、競争力のあるコストで製造できる条件に設定すればよい。廃食用油１００重量部に対して０．００５〜２．０重量部の金属触媒を使用する場合は、通常、反応温度は１３０〜２５０℃、水素分圧は１．０×１０−１ＭＰａ（常圧）（７６０ｍｍＨｇ）〜２．０ＭＰａ（２０気圧）（１５，２００ｍｍＨｇ）の範囲に設定される。反応時間は上記条件で硬化油が製造できる時間に適宜設定される。上記範囲未満であれば水添反応が進みにくく、上記範囲を超えるとエネルギーコストが大きくなり、製品のコストアップが避けられない。The reaction conditions for the hydrogenation may be the same as the normal reaction conditions, and the waste edible oil and the metal catalyst are put into the reaction tank and then reacted under stirring. The hydrogenation reaction depends on the reaction temperature, the hydrogen partial pressure, the reaction time, the amount of metal catalyst, and the like, but it may be set to conditions that can be produced at a competitive cost for paraffin wax. When using 0.005 to 2.0 parts by weight of metal catalyst with respect to 100 parts by weight of waste cooking oil, the reaction temperature is usually 130 to 250 ° C. and the hydrogen partial pressure is 1.0 × 10 −1 MPa ( Normal pressure) (760 mmHg) to 2.0 MPa (20 atm) (15,200 mmHg). The reaction time is appropriately set to a time during which the hardened oil can be produced under the above conditions. If it is less than the above range, the hydrogenation reaction is difficult to proceed, and if it exceeds the above range, the energy cost increases and the cost of the product cannot be avoided.
廃食用油を水素添加した硬化油は、融点は４０〜７０℃、ヨウ素価は５５以下である。ローソクに適した硬化油の融点は、通常４５〜６５℃、ヨウ素価は５〜４５である。成形時にクラックが発生しやすい大型ローソクの場合はヨウ素価が１５〜３０の硬化油を使用するのが好ましい。ヨウ素価が上記の範囲未満では硬くて融点が高くなりローソク製造時にクラックを生じやすく、上記範囲を超えると柔らかくて融点が低くなり夏場の保管中に溶融したり、不快な油脂臭が残ったり燃焼時に油煙が発生しやすいという問題がある。Hardened oil obtained by hydrogenating waste cooking oil has a melting point of 40 to 70 ° C. and an iodine value of 55 or less. The melting point of the hardened oil suitable for the candle is usually 45 to 65 ° C., and the iodine value is 5 to 45. In the case of a large candle that easily cracks during molding, it is preferable to use a hardened oil having an iodine value of 15 to 30. If the iodine value is less than the above range, it is hard and has a high melting point, and cracks are likely to occur during candle production, and if it exceeds the above range, it is soft and has a low melting point that melts during storage in the summer, or an unpleasant oily odor remains or burns There is a problem that oil smoke tends to be generated sometimes.
本発明の廃食用油を水素添加した硬化油をローソク原料とする場合は、特にヨウ素価が５未満の硬化油は硬すぎて、該硬化油のみでローソクを製造すると成形時にクラックが発生するため、ローソク用ワックスとして不適当であるが、成形改善剤として他のワックスを混合すると成形性が向上してローソクが製造可能となる。また、融点が４５〜６５℃、ヨウ素価が５〜４５のローソク用ワックスは、該ローソク用ワックスのみでローソクを製造することができるが、成形改善剤として他のワックスを混合すると成形性を更に向上させることができる。成形改善剤としてのワックスとしては、例えば硬化ひまし油などの硬化油、パラフィンワックスやマイクロクリスタリンワックスなどの石油ワックス、ポリエチレンワックスなどの合成炭化水素系ワックス、ステアリン酸やパルミチン酸などの高級脂肪酸、ミツロウや木ロウなどの天然ワックスなどがある。When the hydrogenated hydrogenated edible oil of the present invention is used as the raw material for the candle, especially the hardened oil having an iodine value of less than 5 is too hard, and cracks are generated during molding if the candle is produced only with the hardened oil. Although it is not suitable as a wax for candles, when other waxes are mixed as a molding improver, moldability is improved and a candle can be produced. In addition, a candle wax having a melting point of 45 to 65 ° C. and an iodine value of 5 to 45 can produce a candle only with the candle wax. However, when other waxes are mixed as a molding improver, the moldability is further improved. Can be improved. Examples of waxes as molding improvers include hardened oils such as hardened castor oil, petroleum waxes such as paraffin wax and microcrystalline wax, synthetic hydrocarbon waxes such as polyethylene wax, higher fatty acids such as stearic acid and palmitic acid, beeswax, There are natural waxes such as wood wax.
さらに本発明のローソク用ワックスに顔料、染料、香料、酸化防止剤、紫外線吸収剤などを添加すると、ローソクの品質を安定化させたり、機能性を高めることができる。Furthermore, the addition of pigments, dyes, fragrances, antioxidants, ultraviolet absorbers and the like to the wax for candles of the present invention can stabilize the quality of the candle and enhance its functionality.
実施例１〜実施例４及び比較例１〜比較例２
家庭から回収された、ゴミやかすを取り除いた使用済みてんぷら油６０ｇをニッケル触媒（ＳＯ−８５０：堺化学製）０．６ｇとともに１００ｍＬ容量のステンレス製小型圧力容器に入れ、窒素ガスで３回パージし、２００℃に加熱した後、容器に水素ガスを供給し、容器内のガス圧を０．９Ｍｐａに維持しつつマグネット式撹拌装置で撹拌しながら２時間３０分水素添加反応を行って得られた硬化油を比較例１とした。
また、同じ条件で３時間反応させて得られた硬化油を実施例１とし、４時間反応させて得られた硬化油を実施例２とし、６時間反応させて得られた硬化油を実施例３とし、７時間反応させて得られた硬化油を実施例４とし、８時間反応させて得られた硬化油を比較例２とした。Examples 1 to 4 and Comparative Examples 1 to 2
60g of used tempura oil collected from households with removed dust and debris is put together with 0.6g of nickel catalyst (SO-850: Sakai Chemical) into a small 100mL stainless steel pressure vessel and purged three times with nitrogen gas Then, after heating to 200 ° C., hydrogen gas is supplied to the container, and the hydrogenation reaction is performed for 2 hours 30 minutes while stirring with a magnetic stirring device while maintaining the gas pressure in the container at 0.9 MPa. The hardened oil was designated as Comparative Example 1.
Moreover, the hardened oil obtained by making it react on the same conditions for 3 hours is made into Example 1, the hardened oil obtained by making it react for 4 hours is made into Example 2, and the hardened oil obtained by making it react for 6 hours is made into Example. The cured oil obtained by reacting for 3 hours and 7 hours was designated as Example 4, and the cured oil obtained by reacting for 8 hours was designated as Comparative Example 2.
各実施例及び比較例で製造された硬化油のヨウ素価、融点とそれら原料としてを用いたローソクの成形性、燃焼性及びローソクとしての評価を［表−１］に示す。
比較例１は融点が４２℃と低いため、気温の高い夏場に溶融するおそれがあり、しかも、比較例１の硬化油で製造したローソクは柔らかくて、べとつき、油脂臭も残っており、燃焼の際には油煙が発生するためローソク用の硬化油（ワックス）としては不適である。
比較例２の硬化油で製造したローソクは、油脂臭なく燃焼の際の油煙が発生しないものの、硬化油は硬く成形時に激しいクラックを発生するためローソク用ワックスとしては不適である。Since Comparative Example 1 has a low melting point of 42 ° C., there is a risk of melting in summer when the temperature is high. Moreover, the candle produced from the hardened oil of Comparative Example 1 is soft, sticky, and fat and oily odors remain, and the combustion of In some cases, oily smoke is generated, which is not suitable as a hardened oil (wax) for candles.
The candle produced with the hardened oil of Comparative Example 2 is not suitable as a wax for candles, although it does not generate oily odor and does not generate smoke during combustion, but the hardened oil is hard and generates severe cracks during molding.
実施例１の硬化油で製造したローソクは、燃焼時にやや油煙が発生するものの、ワックスはやや柔らかく良好な成形性を示すため容器入りローソク用のワックスとして好ましく使用できる。
実施例２及び実施例３の硬化油で製造したローソクは、成形性が良好で燃焼時の油煙もないため、通常の大型ローソクにも使用できる。
実施例４の硬化油で製造したローソクは、水冷下で成形した場合は、少々クラックを生じるものの、通常の空冷下の成形においてはクラックを生じず、また燃焼の際の油煙なく、ローソク用のワックスとして使用できる。Although the candle manufactured with the hardened oil of Example 1 generates a little oil smoke at the time of combustion, since the wax is slightly soft and exhibits good moldability, it can be preferably used as a wax for a candle in a container.
The candles produced with the hardened oils of Example 2 and Example 3 have good moldability and no smoke during combustion, and can be used for ordinary large candles.
The candle produced with the hardened oil of Example 4 is slightly cracked when molded under water cooling, but does not crack in ordinary air-cooled molding, and does not cause oil smoke during combustion. Can be used as a wax.
実施例５〜実施例６
予めろ紙にてゴミやかすを取り除いた、ホテル厨房の使用済み揚げ油３ｋｇをニッケル触媒（プリキャット９９２０：ユニケマ インターナショナル社製）１３ｇとともにて６Ｌ容量のステンレス製圧力反応容器に入れ、窒素ガスで３回パージし、１９０℃に加熱した後、水素ガスを注入し、容器内の水素ガス圧を０．７Ｍｐａに維持しつつ、毎分７００回転の撹拌機で２時間３０分撹拌した。その後、排出弁を開放し、製造された硬化油をろ紙でろ過して、触媒を分離することにより溶融状態の硬化油を得た。得られた硬化油のヨウ素価は２２、融点は５８℃であった。Example 5 to Example 6
Place 3 kg of used fried oil from the hotel kitchen, pre-filtered with filter paper, together with 13 g of nickel catalyst (Precat 9920: made by Unikema International) into a 6-liter stainless steel pressure reactor and 3 times with nitrogen gas After purging and heating to 190 ° C., hydrogen gas was injected, and the mixture was stirred for 2 hours and 30 minutes with a stirrer at 700 rpm while maintaining the hydrogen gas pressure in the container at 0.7 MPa. Thereafter, the discharge valve was opened, and the produced hardened oil was filtered with a filter paper to separate the catalyst, thereby obtaining a hardened oil in a molten state. The obtained hydrogenated oil had an iodine value of 22 and a melting point of 58 ° C.
次に、溶融状態の硬化油をローソク原料配合槽に移し、硬化油１００重量部に対して２０重量部のステアリン酸と溶融混合した約８０℃のローソク配合原料を、芯を配置したローソク金型に注入し燃焼剤を冷却固化して、図−２に示すような直径５０ｍｍ、高さ１５０ｍｍの円筒形状のローソク１５を製造した。１６は燃焼芯である。このローソクを実施例５とする。Next, the melted hardened oil is transferred to a candle raw material blending tank, and the candle blended raw material of about 80 ° C. melted and mixed with 20 parts by weight of stearic acid with respect to 100 parts by weight of the hardened oil is a candle mold in which a core is arranged. Then, the combustion agent was cooled and solidified to produce a
実施例５のローソクは、硬化油のややくすんだ色合いが市販の白色ステアリン酸を配合することで落ち着いた色合いとなり、完全に飽和脂肪酸とした硬化油は硬くて、冷却固化させる際に亀裂を生じやすいがステアリン酸を配合することで成型性を高めることができる。
次に、芯に点火し燃焼性を観察したところ、油煙や煤の発生もなく、良好な燃焼状態を保った。また、ローソクの上面外周部が堰となって燃焼中のロウが垂れることもなく、燃焼に伴う悪臭も認められなかった。In the candle of Example 5, the slightly dull color of the hardened oil becomes a calm color by blending commercially available white stearic acid, and the hardened oil completely saturated fatty acid is hard and causes cracks when cooled and solidified. Although easy, moldability can be improved by adding stearic acid.
Next, when the core was ignited and the flammability was observed, there was no generation of oily smoke or soot, and a good combustion state was maintained. Further, the upper peripheral portion of the candle became a weir and the burning wax did not sag, and no bad odor associated with combustion was observed.
実施例５で用いたローソク原料配合槽内の溶融状態の硬化油に、等量の１３５°Ｆパラフィンワックスを溶融混合し、公知の造粒手段で造粒した。該造粒体を金型に入れて圧縮成形したローソク１７の中心に芯１８を装着して図−３に示す直径３６ｍｍ、高さ２０ｍｍのローソクを製造した。このローソクを実施例６とする。An equal amount of 135 ° F. paraffin wax was melted and mixed with the molten hardened oil in the candle raw material blending tank used in Example 5 and granulated by a known granulating means. A core 18 was attached to the center of a
一般に硬化油だけで造粒されたローソク原料は圧縮成形に不向きであることが多いが、実施例６のローソクは、圧縮成形に向くパラフィンワックスを等量配合することで、圧縮成形が可能であった。成形されたローソク１７の中心に設けられた孔に芯１８を装通し、その芯の下端をスチール製の座金で固定した。次に実施例６のローソクを、内径３８ｍｍ深さ２４ｍｍのポリカーボネート製カップ内に入れて、芯に点火し４時間燃焼性を観察したところ、油煙や煤の発生や臭いもなく良好な燃焼状態であった。In general, candle raw materials granulated with only hardened oil are often unsuitable for compression molding, but the candle of Example 6 can be compression molded by blending an equal amount of paraffin wax suitable for compression molding. It was. A core 18 was inserted into a hole provided in the center of the molded
本発明のローソクは、廃食用油より製造された硬化油をそのままローソクの原料とするもので、廃食用油の有効な活用のみならず、昨今の石油高騰によりローソクの主たる原料であるパラフィンワックスの供給不安を払拭する代替ワックスとしての硬化油を用いた環境にやさしいローソクである。The candle of the present invention uses the hardened oil produced from waste edible oil as the raw material of the candle as it is, and not only the effective use of the waste edible oil but also the paraffin wax which is the main raw material of the candle due to the recent rise in oil. This is an environmentally friendly candle using hardened oil as an alternative wax to eliminate supply concerns.
１・・反応槽
２・・水素ボンベ
３・・窒素ボンベ
４・・バンドヒーター
５・・撹拌機
６・・水素ガス導入口
７・・窒素ガス導入口
８・・廃食用油投入口
９・・硬化油排出口
１０・・ろ過手段
１１・・ボトムバルブ
１５、１７・・ローソク
１６、１８・・燃焼芯1 .... Reaction tank 2 .... Hydrogen cylinder 3 .... Nitrogen cylinder 4 .... Band heater 5 .... Stirrer 6 .... Hydrogen gas inlet 7 .... Nitrogen gas inlet 8 .... Waste cooking oil inlet 9 .... Hardened oil outlet 10 .. Filtration means 11..
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| WO2011146841A1 (en) * | 2010-05-21 | 2011-11-24 | Hrd Corp. | Process for upgrading law value renewable oils |
| JP2011252136A (en) * | 2010-06-01 | 2011-12-15 | Pegasus Candle Kk | Wax for candle, method for manufacturing the same, and candle using the wax |
| WO2018036993A1 (en) * | 2016-08-24 | 2018-03-01 | Dieter Tischendorf | Fuels and ignition aids made of modified, renewable raw materials |
| KR20220078225A (en) * | 2020-12-03 | 2022-06-10 | 지용한 | Cream-type candle paste and its manufacturing method |
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| US8735616B2 (en) | 2010-05-21 | 2014-05-27 | H R D Corporation | Process for upgrading low value renewable oils |
| JP2011252136A (en) * | 2010-06-01 | 2011-12-15 | Pegasus Candle Kk | Wax for candle, method for manufacturing the same, and candle using the wax |
| WO2018036993A1 (en) * | 2016-08-24 | 2018-03-01 | Dieter Tischendorf | Fuels and ignition aids made of modified, renewable raw materials |
| KR20220078225A (en) * | 2020-12-03 | 2022-06-10 | 지용한 | Cream-type candle paste and its manufacturing method |
| KR102549904B1 (en) | 2020-12-03 | 2023-06-30 | 지용한 | Cream-type candle paste and its manufacturing method |
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