JP5875140B2 - Method for refining jatropha oil - Google Patents
Method for refining jatropha oil Download PDFInfo
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- JP5875140B2 JP5875140B2 JP2011132524A JP2011132524A JP5875140B2 JP 5875140 B2 JP5875140 B2 JP 5875140B2 JP 2011132524 A JP2011132524 A JP 2011132524A JP 2011132524 A JP2011132524 A JP 2011132524A JP 5875140 B2 JP5875140 B2 JP 5875140B2
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- 241000221089 Jatropha Species 0.000 title claims description 88
- 238000000034 method Methods 0.000 title claims description 47
- 238000007670 refining Methods 0.000 title claims description 20
- 239000011574 phosphorus Substances 0.000 claims description 108
- 229910052698 phosphorus Inorganic materials 0.000 claims description 108
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 105
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 57
- 239000002893 slag Substances 0.000 claims description 31
- 238000003756 stirring Methods 0.000 claims description 14
- 238000010438 heat treatment Methods 0.000 claims description 11
- 238000000746 purification Methods 0.000 claims description 8
- 239000003921 oil Substances 0.000 description 215
- 239000010779 crude oil Substances 0.000 description 97
- 238000012790 confirmation Methods 0.000 description 27
- 238000001556 precipitation Methods 0.000 description 15
- 238000000926 separation method Methods 0.000 description 6
- 238000004062 sedimentation Methods 0.000 description 5
- 150000003017 phosphorus Chemical class 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000010903 husk Substances 0.000 description 2
- 239000006228 supernatant Substances 0.000 description 2
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 244000184734 Pyrus japonica Species 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000000295 fuel oil Substances 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
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Description
本発明は、ジャトロファ油の精製方法に関する。 The present invention relates to a method for refining jatropha oil.
ジャトロファの種子を圧搾して得たジャトロファ油には、粉砕された種子殻等の搾油粕が混入している場合がある。この搾油粕をジャトロファ油から除去する方法としては、例えば、ジャトロファ油を放置して搾油粕を沈殿させた後、上澄みをフィルタを用いてろ過することが知られている（例えば特許文献１を参照）。 In some cases, jatropha oil obtained by squeezing jatropha seeds may contain squeezed cocoons such as crushed seed shells. As a method for removing the oil slag from the jatropha oil, for example, it is known that the jatropha oil is allowed to stand and the oil slag is precipitated, and then the supernatant is filtered using a filter (see, for example, Patent Document 1). ).
しかしながら、前述した方法を用いて、ジャトロファ油から搾油粕を除去する場合、ジャトロファ油の粘性が水や軽油等に比べて高いため、搾油粕が沈殿するまでに要する時間や、ジャトロファ油がフィルタを通過するのに要する時間が膨大となる虞がある。また、ジャトロファ油をろ過する作業は、フィルタの目詰まり等を防止するため、数回に分けて行う必要がある。さらに、ジャトロファ油を燃料油として用いるためには、ジャトロファ油中に含まれるリンも除去する必要がある。よって、前述した方法を用いて、ジャトロファ油から搾油粕を除去した後、さらにリンを除去してジャトロファ油を精製するためには、膨大な時間及び手間がかかるという問題があった。 However, when oil slag is removed from Jatropha oil using the method described above, the viscosity of Jatropha oil is higher than that of water, light oil, etc. There is a risk that the time required to pass will be enormous. Moreover, it is necessary to perform the operation | work which filters jatropha oil in several steps, in order to prevent clogging etc. of a filter. Furthermore, in order to use jatropha oil as a fuel oil, it is necessary to remove phosphorus contained in the jatropha oil. Therefore, there has been a problem that enormous time and effort are required to remove japonica from jatropha oil using the above-described method and then further remove phosphorus to refine jatropha oil.
本発明はかかる課題に鑑みてなされたものであり、その目的とするところは、ジャトロファ油に含まれる搾油粕をジャトロファ油から除去する時間を短縮でき且つ搾油粕とともにリンも除去できるジャトロファ油の精製方法を提供することにある。 This invention is made | formed in view of this subject, The place made into the objective is refinement | purification of the Jatropha oil which can shorten the time which removes the oil squeeze contained in Jatropha oil from Jatropha oil, and can also remove phosphorus with a squeeze oil sachet It is to provide a method.
前記課題を解決するための発明は、ジャトロファの種子を圧搾してジャトロファ油を得る第１工程と、前記ジャトロファ油を加熱する第２工程と、加熱された前記ジャトロファ油を水とともに攪拌する第３工程と、攪拌された前記ジャトロファ油及び前記水を放置し、油層と水層とに分離する第４工程と、前記水層に含まれる、前記種子の圧搾によって生じた搾油粕と、リンとを、前記水とともに除去する第５工程と、前記搾油粕と、前記リンと、前記水とが除去された前記ジャトロファ油を加熱する第６工程と、加熱された前記ジャトロファ油を水とともに攪拌する第７工程と、攪拌された前記ジャトロファ油を及び前記水を放置し、油層と水層とに分離する第８工程と、前記水層に含まれるリンを、前記水とともに除去する第９工程と、を備えたことを特徴とするジャトロファ油の精製方法である。
The invention for solving the problems includes a first step of squeezing jatropha seeds to obtain jatropha oil, a second step of heating the jatropha oil, and a third step of stirring the heated jatropha oil with water. A step, a fourth step of leaving the agitated jatropha oil and the water and separating them into an oil layer and an aqueous layer, an oil culm produced by pressing the seeds contained in the aqueous layer, and phosphorus The sixth step of removing together with the water, the sixth step of heating the jatropha oil from which the oil slag, the phosphorus, and the water have been removed, and the step of stirring the heated jatropha oil together with water and seventh step, stirred and left to Oyobi the water the Jatropha oil, a eighth step of separating into a oil layer and an aqueous layer, the phosphorus contained in the aqueous layer, a ninth step of removing with the water, A method of purifying Jatropha oil, characterized in that it includes.
本発明の他の特徴については、添付図面及び本明細書の記載により明らかとなる。 Other features of the present invention will become apparent from the accompanying drawings and the description of this specification.
本発明によれば、ジャトロファ油に含まれる搾油粕をジャトロファ油から除去する時間を短縮でき且つ搾油粕とともにリンも除去できるジャトロファ油の精製方法を提供することができる。 ADVANTAGE OF THE INVENTION According to this invention, the refinement | purification method of the Jatropha oil which can shorten the time which removes the squeezed sachet contained in a Jatropha oil from a Jatropha oil and can also remove phosphorus with a squeezed sachet can be provided.
===ジャトロファ油の精製方法について===
図１及び図２を参照しつつ、本実施形態にかかるジャトロファ油の精製方法について説明する。尚、図１は、本実施形態にかかるジャトロファ油の精製方法を説明するためのフローチャートである。また、図２は、本実施形態にかかるジャトロファ油の精製方法を説明するための模式図である。
=== About the refining method of Jatropha oil ===
A method for refining jatropha oil according to the present embodiment will be described with reference to FIGS. 1 and 2. FIG. 1 is a flowchart for explaining a method for refining jatropha oil according to this embodiment. FIG. 2 is a schematic diagram for explaining a method for refining jatropha oil according to the present embodiment.
図１に示すように、この精製方法では、ジャトロファの種子を圧搾してジャトロファ油を得る第１工程（Ｓ１）と、第１工程で得られたジャトロファ油（粗油）を加熱する第２工程（Ｓ２）と、第２工程で加熱された粗油を水とともに攪拌する第３工程（Ｓ３）と、第３工程で攪拌された粗油及び水を放置し、油層と水層とに分離する第４工程（Ｓ４）と、第４工程で分離された水層を除去する第５工程（Ｓ５）と、リン除去工程（Ｓ６〜Ｓ９）とを行う。 As shown in FIG. 1, in this refinement | purification method, the 1st process (S1) which squeezes the seed of Jatropha and obtains Jatropha oil, and the 2nd process of heating the Jatropha oil (crude oil) obtained at the 1st process (S2), the third step (S3) in which the crude oil heated in the second step is stirred together with water, and the crude oil and water stirred in the third step are allowed to stand and are separated into an oil layer and an aqueous layer A fourth step (S4), a fifth step (S5) for removing the aqueous layer separated in the fourth step, and a phosphorus removal step (S6 to S9) are performed.
先ず、図２を参照しつつ、第１工程乃至第５工程について説明する。第１工程では、搾油機１によって、不図示の種子タンクから送られたジャトロファの種子に圧力をかけて、ジャトロファ油を搾り取る。これによって、ジャトロファ油（粗油）と、ジャトロファ油が搾り取られた後の種子殻等からなる搾油残渣とが得られる。本実施形態では、粗油に混入している微細な種子殻等を搾油粕と称する。 First, the first to fifth steps will be described with reference to FIG. In the first step, the oil press 1 applies pressure to jatropha seeds sent from a seed tank (not shown) to squeeze out jatropha oil. Thereby, jatropha oil (crude oil) and an oil residue consisting of seed husks and the like after the jatropha oil has been squeezed out are obtained. In this embodiment, the fine seed husk etc. which are mixed in the crude oil are referred to as an oil culm.
第２工程では、例えばヒータ等を備える加熱装置２によって、粗油を例えば６０度以上９０度以下の範囲内の所定温度となるように、より望ましくは７０度の温度となるように加熱する。第３工程では、加熱された粗油と、粗油に対し例えば略２０重量％となる水とを、攪拌装置３によって攪拌する。第４工程では、攪拌された粗油及び水を、分離装置４に投入して一定時間放置し、油層（上層）と水層（下層）とに分離する。この際、比重等から粗油に含まれていた搾油粕は沈殿し、水層に含まれることになる。また、粗油に含まれていたリンは、水溶性であることから、水層に含まれることになる。つまり、油層は、搾油粕及びリンが除去されたジャトロファ油（第１精製油）からなる。第５工程では、分離装置４によって、油層のみを取り出し、水層を除去する。例えば、分離装置４は、底部に開閉弁を有し、この開閉弁を開放することで、下層である水層を抜き取ることができる。これによって、粗油に含まれていた搾油粕及びリンを除去して、第１精製油を得ることができる。 In the second step, the crude oil is heated to a predetermined temperature within a range of 60 degrees to 90 degrees, for example, and more desirably 70 degrees, by the heating device 2 including, for example, a heater. In the third step, the heated crude oil and water that is, for example, approximately 20% by weight with respect to the crude oil are stirred by the stirring device 3. In the fourth step, the stirred crude oil and water are put into the separation device 4 and left for a certain period of time to separate into an oil layer (upper layer) and an aqueous layer (lower layer). At this time, the oil slag contained in the crude oil due to the specific gravity and the like is precipitated and included in the aqueous layer. Moreover, since phosphorus contained in the crude oil is water-soluble, it is contained in the aqueous layer. That is, the oil layer is made of jatropha oil (first refined oil) from which the oil slag and phosphorus are removed. In the fifth step, only the oil layer is taken out by the separation device 4 and the aqueous layer is removed. For example, the separation device 4 has an opening / closing valve at the bottom, and by opening the opening / closing valve, the water layer as the lower layer can be extracted. As a result, the first refined oil can be obtained by removing the oil slag and phosphorus contained in the crude oil.
尚、第３工程において、粗油の温度を例えば６０度以上９０度以下の範囲内の所定温度となるように、より望ましくは７０度となるように加熱することとした。また、第４工程において、粗油と、粗油に対し例えば略２０重量％となる水とを攪拌することとした。これによって、効率よく粗油に含まれている搾油粕及びリンを水層に移行させて粗油から除去できる。しかし、第３工程において加熱される粗油の温度及び、第４工程において粗油と混合される水の重量の割合は、前述した範囲に限られるものではなく、粗油から搾油粕及びリンを除去できる範囲であればよい。 In the third step, the crude oil is heated so that the temperature of the crude oil becomes a predetermined temperature within a range of 60 degrees to 90 degrees, for example, and more desirably 70 degrees. In the fourth step, the crude oil and water that is, for example, approximately 20% by weight with respect to the crude oil are stirred. As a result, the squeezed slag and phosphorus contained in the crude oil can be efficiently transferred to the aqueous layer and removed from the crude oil. However, the ratio of the weight of the crude oil heated in the third step and the weight ratio of the water mixed with the crude oil in the fourth step is not limited to the above-described range. Any range that can be removed is acceptable.
次に、図１を参照しつつ、リン除去工程について説明する。リン除去工程は、第１乃至第５工程によって得られた第１精製油に更にリンが含まれる場合に、このリンを除去するための工程である。本実施形態にかかるジャトロファ油の精製方法では、第１乃至第５工程において、粗油から搾油粕とともにリンが除去された第１精製油に対して、リン除去工程を行う。このため、リン除去工程において、リンの除去を効率よく行うことができる。 Next, the phosphorus removal step will be described with reference to FIG. The phosphorus removal step is a step for removing phosphorus when the first refined oil obtained in the first to fifth steps further contains phosphorus. In the method for refining jatropha oil according to the present embodiment, in the first to fifth steps, the phosphorus removal step is performed on the first refined oil from which the phosphorus has been removed together with the squeezed oil from the crude oil. For this reason, phosphorus can be efficiently removed in the phosphorus removal step.
本実施形態にかかるリン除去工程では、第１精製油を加熱する第６工程（Ｓ６）と、第６工程で加熱された第１精製油を水とともに攪拌する第７工程（Ｓ７）と、第７工程で攪拌された第１精製油及び水を放置し、油層と水層とに分離する第８工程（Ｓ８）と、第７工程で分離された水層を除去する第９工程（Ｓ９）とを行う。 In the phosphorus removal step according to the present embodiment, a sixth step (S6) for heating the first refined oil, a seventh step (S7) for stirring the first refined oil heated in the sixth step with water, The 8th process (S8) which leaves the 1st refined oil and water stirred at 7 processes, and separates into an oil layer and a water layer, and the 9th process (S9) which removes the water layer separated at the 7th process And do.
第６工程では、第２工程における粗油と同様に、第１精製油を例えば６０度以上９０度以下の範囲内の所定温度となるように、より望ましくは７０度の温度となるように加熱する。第７工程では、加熱された第１精製油と、第１精製油に対し例えば略５重量％となる水とを、攪拌装置３と同様の攪拌装置によって攪拌する。第８工程では、攪拌された第１精製油及び水を、分離装置４と同様の分離装置に投入して一定時間放置し、油層（上層）と水層（下層）とに分離する。この際、第１精製油に含まれていたリンは、水溶性であることから、水層に含まれることになる。つまり、油層は、第１精製油から更にリンが除去された第２精製油からなる。第９工程では、第５工程と同様に、油層のみを取り出し、水層を除去する。これによって、第２精製油を得ることができる。 In the sixth step, as in the case of the crude oil in the second step, the first refined oil is heated to a predetermined temperature within a range of, for example, 60 degrees to 90 degrees, and more desirably 70 degrees. To do. In the seventh step, the heated first refined oil and water that is, for example, approximately 5% by weight with respect to the first refined oil are agitated by the agitator similar to the agitator 3. In the eighth step, the stirred first refined oil and water are put into a separation device similar to the separation device 4 and left for a certain period of time to separate into an oil layer (upper layer) and an aqueous layer (lower layer). At this time, the phosphorus contained in the first refined oil is water-soluble, so it is contained in the aqueous layer. That is, the oil layer is made of the second refined oil from which the phosphorus has been further removed from the first refined oil. In the ninth step, as in the fifth step, only the oil layer is taken out and the aqueous layer is removed. Thereby, the second refined oil can be obtained.
尚、第２精製油にリンが含まれている場合、第１精製油と同様に、第２精製油に対して第６工程乃至第９工程を行うことで、第２精製油からさらにリンが除去された第３精製油を得ることができる。同様に、第３精製油に対して第６工程乃至第９工程を行うことで、第３精製油からさらにリンが除去された第４精製油を得ることができる。このように、第６工程乃至第９工程は、ジャトロファ油中のリンが除去されて、所定の濃度よりも低くなるまで繰り返し行われる。尚、前述したように第１乃至第５工程や、第６乃至第９工程において、搾油粕やリンが除去された第１乃至第４精製油等のジャトロファ油を精製油と総称する。 In addition, when phosphorus is contained in the second refined oil, phosphorus is further added from the second refined oil by performing the sixth to ninth steps on the second refined oil in the same manner as the first refined oil. A removed third refined oil can be obtained. Similarly, by performing the sixth to ninth steps on the third refined oil, a fourth refined oil from which phosphorus has been further removed from the third refined oil can be obtained. As described above, the sixth to ninth steps are repeatedly performed until the phosphorus in the Jatropha oil is removed and becomes lower than the predetermined concentration. As described above, jatropha oils such as the first to fourth refined oils from which the squeezed oil and phosphorus are removed in the first to fifth steps and the sixth to ninth steps are collectively referred to as refined oils.
本実施形態にかかるジャトロファ油の精製方法では、粗油から搾油粕及びリンを除去する第２工程乃至第５工程と、精製油からリンを除去する第６工程乃至第９工程とが、ほぼ同様の工程からなる。このため、ジャトロファ油に含まれる搾油粕及びリンを効率よく除去できる。さらに、第１乃至第５工程によって得られた第１精製油に搾油粕が含まれていた場合であっても、第６乃至第９工程において、この搾油粕をリンとともに除去できる。 In the method for refining jatropha oil according to the present embodiment, the second step to the fifth step for removing expelled rice cake and phosphorus from the crude oil and the sixth step to the ninth step for removing phosphorus from the refined oil are substantially the same. It consists of the process. For this reason, the oil slag and phosphorus contained in Jatropha oil can be removed efficiently. Furthermore, even if the first refined oil obtained by the first to fifth steps contains an oil squeeze, it can be removed together with phosphorus in the sixth to ninth steps.
尚、第６工程において、精製油の温度を例えば６０度以上９０度以下の範囲内の所定温度となるように、より望ましくは７０度となるように加熱することとした。また、第７工程において、精製油と、精製油に対し例えば略５重量％となる水とを攪拌することとした。これによって、効率よく粗油に含まれているリンを水層に移行させて粗油から除去できる。しかし、第６工程において加熱される精製油の温度及び、第７工程において精製油と混合される水の重量の割合は、前述した範囲に限られるものではなく、精製油からリンを除去できる範囲であればよい。 In the sixth step, the refined oil is heated so that the temperature of the refined oil becomes a predetermined temperature within a range of 60 degrees to 90 degrees, for example, and more desirably 70 degrees. In the seventh step, the refined oil and water that is, for example, about 5% by weight with respect to the refined oil are stirred. Thus, phosphorus contained in the crude oil can be efficiently transferred to the aqueous layer and removed from the crude oil. However, the temperature of the refined oil heated in the sixth step and the ratio of the weight of the water mixed with the refined oil in the seventh step are not limited to the above-mentioned ranges, but a range in which phosphorus can be removed from the refined oil. If it is.
===沈殿確認試験について===
本実施形態にかかるジャトロファ油の精製方法では、第２工程において加熱され、第３工程において水と攪拌された粗油に含まれる搾油粕を、第４工程において沈殿させて水層側に分離することで、第５工程において水及びリンともに粗油中から除去する。このため、粗油から搾油粕を除去するのに要する時間は、搾油粕が沈殿するのに要する時間に主に影響される。そこで、搾油粕の沈殿時間と、粗油の温度との関係等を確認するため、搾油粕の沈殿確認試験を行った。尚、この沈殿確認試験は、粗油に対して１６重量％（wet）の割合で搾油粕を含む粗油を用いて行った。
=== About the precipitation confirmation test ===
In the method for purifying jatropha oil according to the present embodiment, the oil slag contained in the crude oil heated in the second step and stirred with water in the third step is precipitated in the fourth step and separated to the water layer side. Thus, both water and phosphorus are removed from the crude oil in the fifth step. For this reason, the time required to remove the oil slag from the crude oil is mainly influenced by the time required for the oil slag to settle. Then, in order to confirm the relationship between the settling time of the oil slag and the temperature of the crude oil, a sedimentation confirmation test of the oil slag was conducted. In addition, this precipitation confirmation test was performed using the crude oil containing the squeezed sachet at a ratio of 16% by weight (wet) to the crude oil.
具体的には、沈殿確認試験では、先ず、粗油を６０度に加熱し、加熱した粗油と、粗油に対して５重量％となる水とを攪拌した。次に、この６０度に加熱され、水と攪拌混合された粗油（６０度混合粗油）２００ｍｌをメスシリンダに注入した。このとき、搾油粕は、メスシリンダ内において、６０度混合粗油中に分散している。尚、メスシリンダに注入された２００ｍｌの６０度混合粗油は、メスシリンダの底からの高さ（以下、単に高さと称する）が１８０ｍｍとなる。 Specifically, in the precipitation confirmation test, first, the crude oil was heated to 60 degrees, and the heated crude oil and water that was 5% by weight with respect to the crude oil were stirred. Next, 200 ml of crude oil (60 degree mixed crude oil) heated to 60 degrees and stirred and mixed with water was poured into a measuring cylinder. At this time, the oil slag is dispersed in the 60-degree mixed crude oil in the measuring cylinder. The 200 ml of 60 ° mixed crude oil injected into the measuring cylinder has a height from the bottom of the measuring cylinder (hereinafter, simply referred to as height) of 180 mm.
次に、メスシリンダに注入された６０度混合粗油を放置して、搾油粕の沈殿時間を測定した。尚、搾油粕は、粗油に対して１６重量％の割合で含まれている。このため、搾油粕がメスシリンダ内を沈降し、搾油粕の高さが略３２.４ｍｍとなったとき、搾油粕が沈殿したとみなすことができる。つまり、６０度混合粗油を放置してから、搾油粕の高さが略３２.４ｍｍとなるまでの時間を沈殿時間とした。 Next, the 60 degree mixed crude oil injected into the graduated cylinder was allowed to stand and the settling time of the oil slag was measured. In addition, the squeezed lees are contained in a proportion of 16% by weight with respect to the crude oil. For this reason, it can be considered that the oil squeeze has settled when the oil slag has settled in the graduated cylinder and the height of the oil squeeze has become approximately 32.4 mm. That is, the time from leaving the 60-degree mixed crude oil until the height of the squeezed culm was approximately 32.4 mm was defined as the settling time.
また、この沈殿確認試験では、粗油を７０度に加熱し、加熱した粗油と、粗油に対して５重量％となる水とを攪拌混合し、７０度混合粗油を作成した。そして、７０度混合粗油についても、６０度混合粗油と同様に沈殿時間を測定した。さらに、比較用として、３０度に加熱したのみの粗油についても、６０度混合粗油と同様に沈殿時間を測定した。 In this precipitation confirmation test, the crude oil was heated to 70 degrees, and the heated crude oil and water that was 5% by weight with respect to the crude oil were stirred and mixed to prepare a 70-degree mixed crude oil. And about 70 degree | times mixed crude oil, precipitation time was measured similarly to 60 degree | times mixed crude oil. Further, as a comparative example, the precipitation time was measured for the crude oil only heated to 30 degrees as in the case of the 60 degree mixed crude oil.
===沈殿確認試験の結果について===
図３乃至図５を参照しつつ、沈殿確認試験の結果について説明する。図３は、６０度混合粗油についての沈殿確認試験の結果である。図４は、７０度混合粗油についての沈殿確認試験の結果である。図５は、３０度に加熱した粗油について比較用の沈殿確認試験の結果である。尚、図３乃至図５は夫々、メスシリンダ内における搾油粕の沈降の様子と、時間との関係を示している。図３に示すメスシリンダ内における６０度混合粗油では、濃度の濃い部分が搾油粕の存在箇所となっている。これは、図４に示される７０度混合粗油及び図５に示される３０度に加熱した粗油についても同様である。
=== About the result of precipitation confirmation test ===
The results of the precipitation confirmation test will be described with reference to FIGS. FIG. 3 shows the results of a sedimentation confirmation test for 60-degree mixed crude oil. FIG. 4 shows the results of a precipitation confirmation test for a 70-degree mixed crude oil. FIG. 5 shows the results of a comparative precipitation confirmation test for crude oil heated to 30 degrees. FIGS. 3 to 5 show the relationship between the state of the settling of the oil slag in the graduated cylinder and the time, respectively. In the 60-degree mixed crude oil in the measuring cylinder shown in FIG. The same applies to the 70 ° mixed crude oil shown in FIG. 4 and the crude oil heated to 30 ° shown in FIG.
図３に示すように、６０度混合粗油では、搾油粕の沈殿時間は略６時間であった。図４に示すように、７０度混合粗油では、搾油粕の沈殿時間は１時間３０分〜２時間であった。図５に示すように、３０度に加熱したのみの粗油では、搾油粕の沈殿時間は略９日間であった。よって、粗油を、３０度よりも高い温度（例えば６０度以上）に加熱した後に、水と攪拌することで、搾油粕の沈殿時間を大幅に短縮できることが確認された。さらに、加熱する粗油の温度を７０度とすることで、より沈殿時間を短縮できることが確認された。 As shown in FIG. 3, in 60 degree | times mixed crude oil, the settling time of the oil slag was about 6 hours. As shown in FIG. 4, in the 70-degree mixed crude oil, the settling time of the oil slag was 1 hour 30 minutes to 2 hours. As shown in FIG. 5, in the crude oil heated only to 30 degrees, the settling time of the oil slag was about 9 days. Therefore, after heating crude oil to temperature higher than 30 degree | times (for example, 60 degree | times or more), it was confirmed that the sedimentation time of an oil slag can be shortened significantly by stirring with water. Furthermore, it was confirmed that the precipitation time can be further shortened by setting the temperature of the crude oil to be heated to 70 degrees.
以上の沈殿確認試験の結果より、例えば、ジャトロファ油を放置して搾油粕を自然沈殿させた後に上澄みをフィルタでろ過することで、ジャトロファ油から搾油粕を除去する場合等に比べて、本実施形態にかかるジャトロファ油の精製方法は、搾油粕の沈殿時間を短縮できる点及びフィルタを介さない点で、搾油粕を除去する時間を大幅に短縮できる。また、本実施形態にかかるジャトロファ油の精製方法では、第２工程において粗油を７０度に加熱することで、第４工程において搾油粕をより迅速に沈殿させて水層側に分離できるため、ジャトロファ油から搾油粕を除去する時間をより短縮できる。 From the results of the above sedimentation confirmation test, for example, compared to the case of removing the oil cake from the Jatropha oil by allowing the Jatropha oil to stand and allowing the oil residue to settle naturally, then filtering the supernatant with a filter. The method for refining jatropha oil according to the embodiment can significantly reduce the time for removing the oil cake in terms of reducing the sedimentation time of the oil cake and not using a filter. Further, in the method for refining jatropha oil according to this embodiment, the crude oil is heated to 70 degrees in the second step, so that the oil slag can be more quickly precipitated in the fourth step and separated to the water layer side. The time for removing the squeezed lees from the Jatropha oil can be further shortened.
===リン除去確認試験について===
本実施形態にかかるジャトロファ油の精製方法において、リンの除去作用を確認するため、リン除去確認試験を行った。このリン除去確認試験では、粗油から第１乃至第４精製油を得て、粗油及び第１乃至第４精製油に含まれるリンの濃度を夫々測定した。
=== About phosphorus removal confirmation test ===
In the method for purifying jatropha oil according to the present embodiment, a phosphorus removal confirmation test was performed in order to confirm the phosphorus removal action. In this phosphorus removal confirmation test, first to fourth refined oils were obtained from the crude oil, and the concentrations of phosphorus contained in the crude oil and the first to fourth refined oils were measured.
具体的には、リン除去確認試験では、先ず、粗油５ｇをサンプリングして、粗油に含まれるリンの濃度を分光光度計によって測定した。次に、粗油１２０ｇをビーカに注入し、粗油の温度が６０度となるように、ヒータによって加熱した。尚、粗油を効率よく加熱するため、粗油の加熱は、マグネチックスターラによって４００ｒｐｍの回転速度で攪拌しながら行った。 Specifically, in the phosphorus removal confirmation test, first, 5 g of crude oil was sampled, and the concentration of phosphorus contained in the crude oil was measured with a spectrophotometer. Next, 120 g of crude oil was poured into a beaker and heated with a heater so that the temperature of the crude oil was 60 degrees. In order to efficiently heat the crude oil, the crude oil was heated while being stirred with a magnetic stirrer at a rotational speed of 400 rpm.
次に、ビーカに粗油に対して２０重量％となる水を加え、同様に粗油及び水を４００ｒｐｍの回転速度で３０分間攪拌した。その後、攪拌によって混合された粗油及び水を、分液漏斗に移して３０分間放置することで、油層と水層とに分離した。尚、粗油及び水についての攪拌と放置は、粗油及び水の温度を６０度に維持したまま行った。次に、分液漏斗のコックを開き、水層を除去することで、第１精製油を得た。この第１精製油５ｇをサンプリングし、前述した粗油と同様に、第１精製油に含まれるリンの濃度を測定した。 Next, 20% by weight of water with respect to the crude oil was added to the beaker, and the crude oil and water were similarly stirred at a rotational speed of 400 rpm for 30 minutes. Thereafter, the crude oil and water mixed by stirring were transferred to a separatory funnel and allowed to stand for 30 minutes to separate into an oil layer and an aqueous layer. The stirring and leaving of the crude oil and water was performed while maintaining the temperature of the crude oil and water at 60 degrees. Next, the cock of the separatory funnel was opened, and the first refined oil was obtained by removing the aqueous layer. 5 g of this first refined oil was sampled, and the concentration of phosphorus contained in the first refined oil was measured in the same manner as the crude oil described above.
次に、得られた第１精製油をビーカに注入し、前述した粗油と同様に、第１精製油の温度が６０度となるように加熱した。次に、ビーカに第１精製油に対して５重量％となる水を加え、第１精製油及び水を前述した粗油と同様に３０分間攪拌した。その後、攪拌によって混合された第１精製油及び水を、前述した粗油と同様に分液漏斗に移して３０分間放置することで、油層と水層とに分離した。次に、分液漏斗のコックを開き、水層を除去して、第２精製油を得た。この第２精製油５ｇをサンプリングし、前述した粗油と同様に、第２精製油に含まれるリンの濃度を測定した。 Next, the obtained 1st refined oil was inject | poured into the beaker, and it heated so that the temperature of a 1st refined oil might be 60 degree | times similarly to the crude oil mentioned above. Next, 5% by weight of water with respect to the first refined oil was added to the beaker, and the first refined oil and water were stirred for 30 minutes in the same manner as the crude oil described above. Then, the 1st refined oil and water mixed by stirring were separated into the oil layer and the water layer by moving to a separatory funnel like the above-mentioned crude oil, and leaving it for 30 minutes. Next, the cock of the separatory funnel was opened and the aqueous layer was removed to obtain a second refined oil. 5 g of this second refined oil was sampled, and the concentration of phosphorus contained in the second refined oil was measured in the same manner as the crude oil described above.
以下、第１精製油から第２精製油を得た手順と同様の手順で、第３精製油、第４精製油を得て、夫々に含まれるリンの濃度を測定した。 Thereafter, the third refined oil and the fourth refined oil were obtained in the same procedure as the procedure for obtaining the second refined oil from the first refined oil, and the concentration of phosphorus contained in each was measured.
また、このリン除去確認試験では、前述した第１精製油乃至第４精製油を得る過程において、ヒータによって加熱する温度を７０度として、同様に第１精製油乃至第４精製油を得て、夫々に含まれるリンの濃度を測定した。さらに、このリン除去確認試験では、比較用として、ヒータによって加熱する温度を７０度として得られた第４精製油について、室温で４日間放置した後に再度リンの濃度を測定した。 Further, in this phosphorus removal confirmation test, in the process of obtaining the first to fourth refined oils described above, the temperature heated by the heater is set to 70 degrees, and similarly the first to fourth refined oils are obtained. The concentration of phosphorus contained in each was measured. Further, in this phosphorus removal confirmation test, for comparison, the fourth refined oil obtained at a temperature heated by a heater of 70 degrees was allowed to stand at room temperature for 4 days, and then the phosphorus concentration was measured again.
===リン除去確認試験の結果について===
図６を参照しつつ、リン除去確認試験の結果について説明する。図６では、粗油に含まれるリン濃度（ｐｐｍ）を斜線の棒グラフで示した。また図６では、６０度に加熱して水と攪拌した、粗油及び第１乃至第３精製油から夫々得られた第１乃至第４精製油（以下、第１乃至第４精製油Ａと称する）に含まれるリンの濃度を夫々黒塗りの棒グラフで示した。また、図６では、７０度に加熱して水と攪拌した、粗油及び第１乃至第３精製油から夫々得られた第１乃至第４精製油（以下、第１乃至第４精製油Ｂと称する）及び４日間放置した後の第４精製油Ｂに含まれるリンの濃度を夫々白塗りの棒グラフで示した。
=== About the results of the phosphorus removal confirmation test ===
The result of the phosphorus removal confirmation test will be described with reference to FIG. In FIG. 6, the phosphorus concentration (ppm) contained in the crude oil is shown by a hatched bar graph. In FIG. 6, the first to fourth refined oils (hereinafter referred to as the first to fourth refined oils A and 4) obtained from the crude oil and the first to third refined oils heated to 60 ° C. and stirred with water, respectively. The concentration of phosphorus contained in each of the black bars is indicated by a black bar graph. Moreover, in FIG. 6, the 1st thru | or 4th refined oil (henceforth 1st thru | or 4th refined oil B) each obtained from the crude oil and the 1st thru | or 3rd refined oil which were heated at 70 degree | times and stirred with water. And the concentration of phosphorus contained in the fourth refined oil B after standing for 4 days is indicated by a white bar graph.
図６に斜線で示す棒グラフから、粗油に含まれるリンの濃度は１２６０．０９ｐｐｍであった。 From the bar graph indicated by diagonal lines in FIG. 6, the concentration of phosphorus contained in the crude oil was 1260.09 ppm.
図６に黒塗りで示す棒グラフから、第１精製油Ａに含まれるリン濃度は２６３．５８ｐｐｍであった。つまり、第１精製油Ａでは、粗油からのリンの除去率（以下、リン除去率と称する）が７９．１％であった。第２精製油Ａに含まれるリンの濃度は７１．６９ｐｐｍであり、リン除去率は９４．３％であった。第３精製油Ａに含まれるリンの濃度は４９．１４ｐｐｍであり、リン除去率は９６．１％であった。第４精製油Ａに含まれるリンの濃度は３０．２５ｐｐｍであり、リン除去率は９７.６％であった。 From the bar graph shown in black in FIG. 6, the concentration of phosphorus contained in the first refined oil A was 263.58 ppm. That is, in the first refined oil A, the removal rate of phosphorus from the crude oil (hereinafter referred to as phosphorus removal rate) was 79.1%. The concentration of phosphorus contained in the second refined oil A was 71.69 ppm, and the phosphorus removal rate was 94.3%. The concentration of phosphorus contained in the third refined oil A was 49.14 ppm, and the phosphorus removal rate was 96.1%. The concentration of phosphorus contained in the fourth refined oil A was 30.25 ppm, and the phosphorus removal rate was 97.6%.
図６に白塗りで示す棒グラフから、第１精製油Ｂに含まれるリン濃度は２１１．９７ｐｐｍであり、リン除去率は８３．２％であった。第２精製油Ｂに含まれるリンの濃度は４１．２ｐｐｍであり、リン除去率は９６．７％であった。第３精製油Ｂに含まれるリンの濃度は２１．７５ｐｐｍであり、リン除去率は９８．３％であった。第４精製油Ｂに含まれるリンの濃度は１２．７ｐｐｍであり、リン除去率は９９．０％であった。４日間放置した後の第４精製油Ｂに含まれるリンの濃度は３．５７ｐｐｍであり、リン除去率は９９．７％であった。 From the bar graph shown in white in FIG. 6, the concentration of phosphorus contained in the first refined oil B was 211.97 ppm, and the phosphorus removal rate was 83.2%. The concentration of phosphorus contained in the second refined oil B was 41.2 ppm, and the phosphorus removal rate was 96.7%. The concentration of phosphorus contained in the third refined oil B was 21.75 ppm, and the phosphorus removal rate was 98.3%. The concentration of phosphorus contained in the fourth refined oil B was 12.7 ppm, and the phosphorus removal rate was 99.0%. The concentration of phosphorus contained in the fourth refined oil B after standing for 4 days was 3.57 ppm, and the phosphorus removal rate was 99.7%.
以上のリン除去確認試験の結果より、第１精製油Ａ及び第１精製油Ｂのリン除去率から、本実施形態にかかるジャトロファ油の精製方法では、第１工程から第５工程を行うことで、粗油に含まれるリンの略８割を搾油粕とともに除去できることが確認された。 From the results of the phosphorus removal confirmation test described above, from the phosphorus removal rates of the first refined oil A and the first refined oil B, in the method for refining jatropha oil according to the present embodiment, the first to fifth steps are performed. It was confirmed that approximately 80% of the phosphorus contained in the crude oil can be removed together with the squeezed oil.
また、第２乃至第４精製油Ａ及び第２乃至第４精製油Ｂのリン除去率から、本実施形態にかかるジャトロファ油の精製方法では、第１工程から第５工程を行った後に、第６工程から第９工程を行うことで、粗油に含まれるリンを９割以上除去できることが確認された。さらに、第６工程から第９工程を繰り返し行うことで、粗油に含まれるリンのほぼ１０割を除去できることが確認された。 Further, from the phosphorus removal rates of the second to fourth refined oil A and the second to fourth refined oil B, in the method for refining jatropha oil according to the present embodiment, after performing the first to fifth steps, It was confirmed that 90% or more of phosphorus contained in the crude oil can be removed by performing the sixth to ninth steps. Furthermore, it was confirmed that by repeating the sixth to ninth steps, almost 100% of the phosphorus contained in the crude oil can be removed.
また、第１精製油Ａのリン除去率と第１精製油Ｂのリン除去率とを比較した結果、第１精製油Ｂの方がリン除去率が高いことが確認された。同様に、第２乃至第４精製油Ｂ夫々についても、第２乃至第４精製油Ａ夫々よりもリン除去率が高いことが確認された。これより、第２工程において粗油を加熱する温度及び第６工程において精製油を加熱する温度を７０度とすることで、リンをより効率よく除去できることがわかった。 Moreover, as a result of comparing the phosphorus removal rate of the first refined oil A and the phosphorus removal rate of the first refined oil B, it was confirmed that the first refined oil B had a higher phosphorus removal rate. Similarly, it was confirmed that each of the second to fourth refined oils B has a higher phosphorus removal rate than each of the second to fourth refined oils A. From this, it was found that phosphorus can be more efficiently removed by setting the temperature for heating the crude oil in the second step and the temperature for heating the refined oil in the sixth step to 70 degrees.
また、室温で４日間放置した第４精製油Ｂのリン除去率から、搾油粕及びリンを除去したジャトロファ油をさらに放置することで、リンの除去率を高められることが確認された。 Moreover, it was confirmed from the phosphorus removal rate of the 4th refined oil B left to stand at room temperature for 4 days that the phosphorus removal rate can be increased by further leaving the oil trough and jatropha oil from which phosphorus has been removed.
===搾油粕及びリンの除去作用について===
以上より、本実施形態にかかるジャトロファ油の精製方法では、第１乃至第５工程を行うことで、ジャトロファ油に含まれる搾油粕を迅速に除去できるとともに、ジャトロファ油に含まれるリンも除去できる。
=== Removal of oil slag and phosphorus ===
As described above, in the method for refining jatropha oil according to the present embodiment, by performing the first to fifth steps, it is possible to quickly remove the oil squeeze contained in the jatropha oil and also remove phosphorus contained in the jatropha oil.
また、本実施形態にかかるジャトロファ油の精製方法では、第１乃至第５工程において、搾油粕とともにリンを除去した第１精製油に対して、リン除去工程を行うため、ジャトロファ油に含まれるリンを効率よく除去できる。 Further, in the method for refining jatropha oil according to the present embodiment, in the first to fifth steps, the phosphorus removal step is performed on the first refined oil from which phosphorus has been removed together with the squeezed slag. Can be efficiently removed.
また、本実施形態にかかるジャトロファ油の精製方法では、粗油から搾油粕及びリンを除去する第２乃至第５工程と、リン除去工程である第６乃至第９工程とがほぼ同じ工程からなるため、搾油粕及びリンを効率よく除去できる。さらに、第１乃至第５工程によって得られた第１精製油に搾油粕が含まれていた場合であっても、第６乃至第９工程において、この搾油粕をリンとともに除去できる。これによって、ジャトロファ油からより確実に搾油粕を除去できる。 Further, in the method for refining jatropha oil according to the present embodiment, the second to fifth steps for removing the squeezed slag and phosphorus from the crude oil and the sixth to ninth steps that are the phosphorus removal step are substantially the same steps. Therefore, oil slag and phosphorus can be removed efficiently. Furthermore, even if the first refined oil obtained by the first to fifth steps contains an oil squeeze, it can be removed together with phosphorus in the sixth to ninth steps. As a result, it is possible to more reliably remove the squeezed residue from the Jatropha oil.
また、本実施形態にかかるジャトロファ油の精製方法では、第３工程において、粗油の温度を例えば６０度以上９０度以下の範囲内の所定温度となるように、より望ましくは７０度となるように加熱することによって、沈殿確認試験からも確認されたように、搾油粕の沈殿時間を短縮することができる。このため、ジャトロファ油から搾油粕を除去する時間を大幅に短縮できる。また、リン除去確認試験からも確認されたように、リンの除去率を高めることができる。 Further, in the method for refining jatropha oil according to the present embodiment, in the third step, the temperature of the crude oil is set to a predetermined temperature within a range of, for example, 60 degrees to 90 degrees, and more desirably 70 degrees. As is confirmed from the precipitation confirmation test, it is possible to shorten the settling time of the oil culm. For this reason, it is possible to greatly reduce the time for removing the oil slag from the Jatropha oil. Moreover, the phosphorus removal rate can be increased as confirmed from the phosphorus removal confirmation test.
また、本実施形態にかかるジャトロファ油の精製方法では、第４工程において、粗油と、この粗油に対し略２０重量％となる水とを攪拌することとし、第７工程において、精製油と、この精製油に対し略５重量％となる水とを攪拌することとした。これによって、粗油に含まれている搾油粕及びリンを効率よく水層に移行させて除去すること、精製油に含まれているリンを効率よく除去することができる。 Further, in the method for refining jatropha oil according to the present embodiment, in the fourth step, the crude oil and water that is approximately 20% by weight with respect to the crude oil are stirred, and in the seventh step, the refined oil and Then, it was decided to stir the water which was about 5% by weight with respect to this refined oil. As a result, it is possible to efficiently move the oil slag and phosphorus contained in the crude oil to the water layer and remove them, and to remove phosphorus contained in the refined oil efficiently.
また、本実施形態にかかるジャトロファ油の精製方法では、第６工程において、精製油の温度を例えば６０度以上９０度以下の範囲内の所定温度となるように、より望ましくは７０度となるように加熱することで、リン除去確認試験からも確認されたように、リンをより効率よく除去することができる。 Further, in the method for refining jatropha oil according to the present embodiment, in the sixth step, the temperature of the refined oil is set to a predetermined temperature within a range of, for example, 60 degrees to 90 degrees, and more desirably 70 degrees. As can be confirmed from the phosphorus removal confirmation test, phosphorus can be removed more efficiently.
===その他の実施形態について===
前述した実施形態は、本発明の理解を容易にするためのものであり、本発明を限定して解釈するためのものではない。本発明は、その趣旨を逸脱することなく変更、改良されると共に、本発明にはその等価物も含まれる。
=== About other embodiments ===
The above-described embodiments are intended to facilitate understanding of the present invention, and are not intended to limit the present invention. The present invention is changed and improved without departing from the gist thereof, and the present invention includes equivalents thereof.
例えば、粗油と攪拌する水の割合及び精製油と攪拌する水の割合は、ジャトロファ油に含まれる搾油粕の量やリンの量に応じて、ジャトロファ油から搾油粕及びリンを効率よく除去できる範囲で夫々選定されればよい。 For example, the ratio of the water to be agitated with the crude oil and the ratio of the water to be agitated with the refined oil can efficiently remove the oil cake and phosphorus from the jatropha oil according to the amount of the oil cake contained in the jatropha oil and the amount of phosphorus. What is necessary is just to select each in the range.
１…搾油機，２…加熱装置，３…攪拌装置，４…分離装置 DESCRIPTION OF SYMBOLS 1 ... Oil press, 2 ... Heating device, 3 ... Stirring device, 4 ... Separation device
Claims (5)
前記ジャトロファ油を加熱する第２工程と、
加熱された前記ジャトロファ油を水とともに攪拌する第３工程と、
攪拌された前記ジャトロファ油及び前記水を放置し、油層と水層とに分離する第４工程と、
前記水層に含まれる、前記種子の圧搾によって生じた搾油粕と、リンとを、前記水とともに除去する第５工程と、
前記搾油粕と、前記リンと、前記水とが除去された前記ジャトロファ油を加熱する第６工程と、
加熱された前記ジャトロファ油を水とともに攪拌する第７工程と、
攪拌された前記ジャトロファ油を及び前記水を放置し、油層と水層とに分離する第８工程と、
前記水層に含まれるリンを、前記水とともに除去する第９工程と、
を備えたことを特徴とするジャトロファ油の精製方法。 A first step of squeezing jatropha seeds to obtain jatropha oil;
A second step of heating the jatropha oil;
A third step of stirring the heated Jatropha oil with water;
A fourth step of leaving the agitated Jatropha oil and water and separating them into an oil layer and an aqueous layer;
A fifth step of removing, together with the water, oil slag produced by pressing the seeds and phosphorus contained in the water layer;
A sixth step of heating the jatropha oil from which the oil slag, the phosphorus, and the water have been removed;
A seventh step of stirring the heated Jatropha oil with water;
An eighth step of leaving the agitated Jatropha oil and the water and separating them into an oil layer and an aqueous layer;
A ninth step of removing phosphorus contained in the aqueous layer together with the water;
A method for refining jatropha oil, comprising:
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