JP2010065187A - Method and apparatus for producing asphalt - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a method and apparatus for simply and efficiently producing purified asphalt from asphalt ores such as Buton Rock Asphalt at a comparatively low temperature without using high concentration sulfuric acid or the like. <P>SOLUTION: The method for producing asphalt is to produce purified asphalt from asphalt ores and comprises (I) a process for obtaining an agitation mixture comprising a raw solid material comprising asphalt ores, an organic solvent and a water-based solvent, (II) a process for separating the agitation mixture into an asphalt-containing organic solvent layer and a water-based solvent layer and a solid component layer, and separately collecting the organic solvent layer and (III) a process for recovering the asphalt in the organic solvent layer, wherein the organic solvent used in the process (I) has ≤80°C temperature. <P>COPYRIGHT: (C)2010,JPO&INPIT

Description

  The present invention relates to an asphalt manufacturing method and a manufacturing apparatus for manufacturing purified asphalt from asphalt ore.

  Asphalt ore is an asphalt-containing mineral containing natural asphalt, and in the production of purified asphalt from asphalt ore, it is required to efficiently recover high-purity asphalt with a low solid content.

  As methods for recovering asphalt from oil shale and tar sand, extraction with an organic solvent, extraction with hot water, extraction by high-temperature steam injection, and the like are known, but in these methods, for example, Buton asphalt rock (Natural asphalt produced on Buton Island, Indonesia) and Trinidad asphalt rock, etc., there was a problem that sufficient extraction could not be performed when using asphalt ore containing porous asphalt in the porous holes .

  As a method for purifying asphalt from Buton asphalt rock, Patent Document 1 proposes that calcium carbonate, which is a substrate of Buton asphalt rock, is dissolved in sulfuric acid and extracted up to asphalt present in the pores. Has been. According to this method, it is predicted that the asphalt content inside the pores of Buton asphalt rock, which has been difficult to recover, is exposed and can be recovered with high yield. However, in this method, it is necessary to use a large amount of high-concentration sulfuric acid, neutralization is required for the treatment of the residue, equipment having high resistance to any of high-concentration sulfuric acid, oil and high-temperature conditions. There are problems such as being necessary.

  In addition, as a method for extracting asphalt from asphalt-containing minerals without using sulfuric acid, etc., an asphalt-containing mineral and a volatile organic solvent such as kerosene can be extracted at high temperatures using an extraction device with a specific configuration that prevents ignition and explosion. Patent Document 2 proposes stirring contact. According to Patent Document 2, it is taught that slurrying can be easily carried out when charged into a high-temperature volatile organic solvent such as 110 ° C. to 120 ° C., for example. Further, it is described that the obtained slurry is subjected to solid-liquid separation with a hermetic rotary screen to remove a solid residue which is an impurity that is not extracted.

  However, since this method uses a high-temperature volatile organic solvent, it is necessary to pay close attention to measures to prevent ignition and explosion, and there is a problem that energy consumption due to heating is large. In addition, since the solid residue is separated from the slurry containing the organic solvent by a rotary screen, the organic solvent residue in the solid residue is large and the flammability may be high.

For this reason, the advent of a technique for producing asphalt from asphalt ore such as Buton asphalt rock under relatively low temperature conditions without using high-concentration sulfuric acid or the like has been demanded.
Japanese Patent Laid-Open No. 9-169799 JP 2000-210502 A

An object of the present invention is to provide a method and an apparatus for easily and efficiently producing purified asphalt from asphalt ore such as Buton asphalt rock at a relatively low temperature without using high-concentration sulfuric acid or the like. .

The method for producing asphalt of the present invention is a method for producing purified asphalt from asphalt ore,
(I) a step of obtaining a stirring mixture comprising a solid raw material comprising an asphalt ore, an organic solvent, and an aqueous solvent;
(II) The step of separating the stirred mixture into an organic solvent layer containing an asphalt component, an aqueous solvent layer and a solid component layer, and separating the organic solvent layer; and (III) collecting the asphalt in the organic solvent layer. And the temperature of the organic solvent used in the step (I) is 80 ° C. or lower.

In such an asphalt production method of the present invention, the step (I) of obtaining the stirring mixture is a step of stirring and mixing a solid raw material made of asphalt ore and an organic solvent, and further adding an aqueous solvent and stirring and mixing. Preferably there is
In the asphalt production method of the present invention, the organic solvent is preferably a hydrocarbon solvent containing 80% by mass or more of hydrocarbons having 8 to 25 carbon atoms, and the organic solvent has a boiling point of 140 ° C. or higher and 400 ° C. or higher. It is also preferable that the hydrocarbon solvent contains 80% by mass or more of hydrocarbons having a temperature of 0 ° C. or lower.

In the asphalt production method of the present invention, in step (I), the temperature of the organic solvent to be mixed is preferably a temperature equal to or lower than the flash point of the organic solvent.
In the asphalt production method of the present invention, the aqueous solvent is preferably water.

  In the asphalt production method of the present invention, in the step (II), the organic solvent layer, the aqueous solvent layer, and the solid content layer are preferably separated by any one or more of stationary, filtration, and centrifugation. .

In the asphalt production method of the present invention, it is preferable that at least a part of the aqueous solvent obtained from the aqueous solvent layer separated in step (II) is introduced into step (I).
In the asphalt production method of the present invention, it is preferable to recover the organic solvent contained in the solid content layer by heating the solid content layer separated in step (II) to 80 to 260 ° C.

In the asphalt production method of the present invention, the organic solvent is separated by evaporation from the solid content layer separated in step (II), and at least a part of the obtained organic solvent is removed from step (I) and / or step (III). It is preferable to introduce into.

In the asphalt production method of the present invention, the recovery of asphalt in step (III),
It is preferable to carry out by separating the organic solvent by distillation, and it is more preferable to introduce at least a part of the organic solvent separated in the step (III) into the step (I).

In the asphalt production method of the present invention, the asphalt ore preferably contains 30% by mass or more of calcium carbonate.
The asphalt production apparatus of the present invention is an apparatus for producing asphalt from asphalt ore,
(A) Means for obtaining a stirred mixture comprising a solid raw material comprising asphalt ore, an organic solvent, and an aqueous solvent;
(B) A means for separating the stirred mixture into an organic solvent layer containing an asphalt component, an aqueous solvent layer and a solid component layer, and separating the organic solvent layer; and (C) collecting asphalt in the organic solvent layer. It has the means to do.

  In such an asphalt production apparatus of the present invention, means for recovering the organic solvent in the solid content layer obtained from the means (B), means (A) and / or at least part of the recovered organic solvent. It is preferable to further have a means for introducing into (C).

  ADVANTAGE OF THE INVENTION According to this invention, while being able to manufacture highly purified refined asphalt with few solid content contents from asphalt ore simply and efficiently, the manufacturing method and apparatus of asphalt excellent also in safety can be provided.

Hereinafter, the present invention will be specifically described.
The method for producing asphalt according to the present invention includes (I) a step of obtaining a stirring mixture consisting of a solid raw material consisting of asphalt ore, an organic solvent, and an aqueous solvent, and (II) an organic solvent layer containing the asphalt component, It has the process of isolate | separating into an aqueous | water-based solvent layer and a solid content layer, and fractionating an organic solvent layer, and (III) The process of collect | recovering asphalts in an organic solvent layer.

Process (I)
Step (I) in the asphalt production method of the present invention is a step of obtaining a stirred mixture comprising a solid raw material composed of asphalt ore, an organic solvent, and an aqueous solvent.

The solid raw material used for the step (I) is obtained from asphalt ore. Asphalt ores, minerals containing asphalt can be used without limitation, and are not particularly limited. However, asphalt ores in which asphalt is contained in the pores of the porous substrate have been conventionally effective asphalt refining. The asphalt ore which has been difficult can also be used suitably. For example, even asphalt ore containing about 30% by mass or more and further about 40 to 70% by mass of calcium carbonate can be suitably used. The preferable asphalt content of the asphalt ore used in the present invention is 10% by weight or more, preferably about 15 to 30% by mass.

  Specific examples of such asphalt ore include Buton asphalt rock and Trinidad asphalt rock, and Buton asphalt rock (hereinafter also referred to as aston) is preferably used.

The solid raw material used for step (I) may be the asphalt ore as it is mined,
It may have been subjected to a pretreatment such as pulverization. Examples of the pretreatment include crushing and washing, and these may be performed in combination.

  In the present invention, it is preferable to use asphalt ore that has been pulverized (cut) as the solid raw material. The asphalt ore grinding process may be a process of grinding the asphalt ore as it is, or may be a process of grinding in the presence of an organic solvent or an aqueous solvent. Although the grade of a grinding | pulverization process is not specifically limited, For example, it is desirable to grind | pulverize to the grade from which an average particle diameter is set to 100 mm or less, Preferably it is 20-70 mm, More preferably, it is 30-60 mm. When the asphalt ore that has been pulverized is used as a solid raw material, a stirred mixture can be obtained efficiently, and in particular when asphalt ore containing a porous substrate such as asphalt ore containing calcium carbonate is used as a raw material. The surface area is increased by pulverization, and even asphalt components existing in the pores of the porous substrate are easily extracted, which is preferable.

As the organic solvent used in the step (I), an organic solvent capable of dissolving an asphalt component is used without particular limitation, but a hydrocarbon solvent is preferable from the viewpoint of operability and safety. As the hydrocarbon solvent, a solvent containing a hydrocarbon having 8 to 25 carbon atoms is preferable, and a hydrocarbon having 8 to 25 carbon atoms is 70% by mass or more, preferably 80% by mass or more, more preferably 90% by mass. The hydrocarbon solvent contained above is desirable. Further, as the hydrocarbon solvent, a hydrocarbon solvent containing 70% by mass or more, preferably 80% by mass or more, more preferably 90% by mass or more of a hydrocarbon having a boiling point of 140 ° C. or more and 400 ° C. or less is desirable.

  As the organic solvent suitably used in the present invention, specifically, an aromatic solvent such as toluene and xylene, and a petroleum solvent such as kerosene and light oil are preferably used, and in particular, a petroleum system such as kerosene and light oil. A solvent is preferably used.

In step (I), the organic solvent component separated in step (II) or (III) described later may be used as part or all of the organic solvent. The organic solvent component separated in the step (II) or (III) may be one obtained by recovering the organic solvent component initially added in the step (I), or a component contained in the asphalt ore. There may be.

As the aqueous solvent used in the step (I), a solvent containing water as a main component, that is, water or an aqueous solution can be used without particular limitation, but water is preferable. In step (I), the aqueous solvent component separated in step (II) described later may be used as part or all of the aqueous solvent.

In step (I), an organic solvent and an aqueous solvent may be added simultaneously to the solid raw material made of asphalt ore as described above to obtain a stirred mixture, or sequentially added to obtain a stirred mixture. May be. The dissolution / stirring mixing may be performed in one stage or in multiple stages. Further, there may be only one dissolution / stirring mixing device, or two or more dissolution devices and stirring / mixing devices may be arranged in series or in parallel.

  When the organic solvent and the aqueous solvent are sequentially added to the solid raw material, it is preferable to stir and mix the solid raw material and the organic solvent, and further add the aqueous solvent and stir and mix. In this case, the solid raw material and the organic solvent are stirred and mixed, and the asphalt content in the solid raw material is sufficiently eluted in the organic solvent to obtain a slurry-like stirring mixture, and then an aqueous solvent is added and stirred and mixed. A stirring mixture is preferred. In addition, for example, when a solid raw material is prepared by a pretreatment in which asphalt ore is pulverized in the presence of water, an organic solvent is added to the mixture of the solid raw material and the aqueous solvent and the mixture is stirred to obtain a stirred mixture. it can.

  The temperature of the organic solvent to be added when preparing the stirred mixture is 80 ° C. or lower, preferably about room temperature to 60 ° C. Moreover, it is also preferable that the temperature of the organic solvent to add is the temperature below the flash point of the organic solvent to be used. Conventionally, it has been common knowledge to use a high-temperature organic solvent to dissolve asphalt in an organic solvent, but in the method of the present invention, even if such an organic solvent is added under such a low-temperature condition, a solid raw material is used. The asphalt content therein is sufficiently dissolved in the organic solvent. In particular, when a solid raw material obtained by pulverizing asphalt ore is sufficiently mixed with stirring, it is preferable that the asphalt content can be recovered in a high yield. In the present invention, since the temperature of the organic solvent when dissolving the asphalt component is low, the risk of ignition or explosion is highly suppressed, the volatilization of the organic solvent is suppressed, and the amount of heat energy used is an economical method. The asphalt content in the solid raw material can be sufficiently dissolved with high safety.

The temperature of the aqueous solvent to be added when preparing the stirred mixture is not particularly limited and may be higher or lower than the temperature of the organic solvent at the time of addition, but is preferably 80 ° C. or lower, More preferably, it is equivalent to the temperature of the solvent.

In the present invention, it is desirable that the stirring mixture obtained in the step (I) is in a substantially homogeneous slurry form. The amount of the organic solvent and the aqueous solvent used in the step (I) is not particularly limited. For example, the organic solvent is 30 to 200 parts by mass, preferably 50 to 150 parts per 100 parts by mass of the solid raw material. It is preferable that the amount of the aqueous solvent is about 30 to 200 parts by mass, preferably about 50 to 150 parts by mass, since the dissolution of the asphalt is smooth and the separation operation in (II) is easy.

The step (I) is preferably performed in the means (A) for obtaining a stirring mixture composed of a solid raw material composed of asphalt ore, an organic solvent, and an aqueous solvent. The means (A) is not particularly limited as long as it is a means capable of stirring and mixing the solid raw material, the organic solvent, and the aqueous solvent. A stirring and mixing device is preferably used. There may be only one dissolving / stirring device, or two or more melting devices and stirring / mixing devices may be connected in series or in parallel.

In the asphalt manufacturing apparatus according to the present invention, it is also preferable to have pretreatment means such as means for pulverizing asphalt ore upstream of the means (A).
Process (II)
In the step (II) of the asphalt production method of the present invention, the stirring mixture obtained in the step (I) is separated into an organic solvent layer containing an asphalt component, an aqueous solvent layer and a solid component layer, and an organic solvent This is a step of separating the layers.

In step (II), the organic solvent layer containing the asphalt component, the aqueous solvent layer, and the solid component layer may be separated by any method. For example, the method of standing, filtration, and centrifugation Can be performed alone or in combination of two or more of these methods. Preferably, the organic solvent layer containing the asphalt component in step (II) is separated from the aqueous solvent layer and the solid component layer. It is desirable to carry out by a method including stationary or centrifugation. Specifically, the stirring mixture obtained in the step (I) is allowed to stand as it is or centrifuged, and separated into three layers, an organic solvent layer containing an asphalt component, an aqueous solvent layer, and a solid component layer, Examples include a method in which the stirred mixture obtained in step (I) is filtered to remove a solid content layer, and then an organic solvent layer containing an asphalt content and an aqueous solvent layer are allowed to stand or separated by centrifugation.

  In standing or centrifuging, an organic solvent layer containing asphalt is usually formed above the aqueous solvent layer. When the asphalt ore contains components such as kerosene and light oil, usually at least a part of these components is also included in the organic solvent layer.

  In the step (II) of the present invention, since the stirring mixture contains an aqueous solvent, the organic solvent containing asphalt and the solid can be clearly separated through the aqueous solvent layer. It is possible to highly suppress the mixing of solid content into the layer.

In this invention, the isolate | separated organic solvent layer is fractionated and it uses for process (III). Components other than the organic solvent layer, that is, the aqueous solvent layer and the solid content layer may be separated separately, or in the form of a slurry in which the aqueous solvent content and the solid content are mixed. Alternatively, the two may be separated by a method such as placement, filtration, and centrifugation, and each may be recovered.

Such step (II) is performed by means (B) for separating the stirred mixture into an organic solvent layer containing an asphalt component, an aqueous solvent layer and a solid component layer, and separating the organic solvent layer. Is preferred. The means (B) may be integrated with the means (A) or may be provided separately. When the means (A) and the means (B) are integrated, for example, the means (
A) After stirring and mixing each component in the stirring and mixing tank which is A), the stirring mixture is produced, and then stirring is stopped and the mixture is left to stand. The stirring mixture is mixed with the organic solvent layer, the aqueous solvent layer and the solid in the mixture layer. It means the case where the organic solvent layer is separated from the extraction port provided in the mixing tank after separating into layers.

  However, when producing asphalt continuously, the means (B) and the means (A) are preferably provided separately. Of the means (B), the part where the stirred mixture is separated into the organic solvent layer containing the asphalt component, the aqueous solvent layer and the solid content layer is any one of a stationary means, a filtration means and a centrifugal separation means. Or a combination of two or more of these. Among these, a stationary means is particularly preferable. Examples of the site for separating the organic solvent layer containing the asphalt component include an extraction port provided in the stationary means or the centrifugal separation means.

As described above, in the step (II), the separated solid content layer and aqueous solvent layer may be recovered, respectively. The separated / recovered aqueous solvent layer can be used as an aqueous solvent to be introduced into the step (I) after separation of impurities by filtration or the like, if necessary. In addition, when a large amount of organic solvent is mixed in the aqueous solvent layer, the organic solvent in the aqueous solvent layer can be separated by a method such as standing and filtration, and can be purified and used as necessary. . For example, as described as an optional step in FIG. 2, an organic solvent separated and recovered from the aqueous solvent layer is introduced into a distillation apparatus for recovering asphalt in step (III) to dissolve the asphalt component. The organic solvent can be recovered together with the organic solvent and used as the organic solvent to be added in the step (I).

  Since the separated / recovered solid content layer is separated from the organic solvent layer through the aqueous solvent layer, the content of the organic solvent is remarkably reduced as compared with the case where no aqueous solvent is used. For this reason, in this invention, it is also possible to discard the collect | recovered solid content layer as it is, without post-processing.

  It is also preferable to separate and recover the organic solvent contained from the solid content layer. Recovery of the organic solvent from the solid content layer can be performed by evaporation. Specifically, the solid content layer is heated to collect the oil and water contained in the solid content layer, and then recovered and separated as appropriate. Can be done.

  In the present invention, the organic solvent contained in the solid content layer is preferably heated to 80 to 260 ° C., more preferably 80 to 120 ° C., whereby the organic solvent in the solid content layer can be distilled. When the asphalt ore is asbuton, the solid content layer usually contains calcium carbonate derived from asbuton, oil containing water and asphalt, and residual organic and aqueous solvents. When the organic solvent is recovered by heat treatment of such a solid content layer, the organic solvent may be distilled by heating to a temperature equal to or higher than the boiling point of the organic solvent, but heating at a temperature lower than the boiling point of the organic solvent. However, a significant amount of organic solvent can be recovered. Furthermore, in the present invention, when asbuton ore is used as a raw material, for example, even when the solid content layer is heated at a temperature below the boiling point of the organic solvent, such as 80 to 140 ° C., the organic solvent in the solid content layer Of these, the amount of 50% by mass or more is often distilled, and the organic solvent can be efficiently recovered with less heat energy. This is because in the solid content layer when using asbuton ore, moisture adheres to the surface of calcium carbonate, and it is easy to take a state in which oil adheres to it. This is thought to be due to distillation accompanied by heating to a degree of volatilization.

  In the present invention, the recovery of the organic solvent or the aqueous solvent from the aqueous solvent layer or the solid content layer may be carried out at normal pressure or under reduced pressure. When the organic solvent or the aqueous solvent is recovered by heat treatment under reduced pressure, the temperature condition of the heat treatment may be lower than the temperature range described above.

When the organic solvent contained in the solid content layer is recovered, part or all of the organic solvent is recovered from step (I).
Introduce directly into step (I) as the organic solvent used in step 1, or introduce it into the asphalt recovery device in step (III) and recover the asphalt together with the dissolved organic solvent before introducing it into step (I) Can be used.

  As described above, the solid content layer in which the organic solvent or the like is recovered may be discarded as it is, or may be subjected to treatment such as firing and washing as necessary to obtain a neutralizing agent, a cement raw material, etc. It can also be used for

Process (III)
Step (III) in the asphalt production method of the present invention is a step of recovering asphalt in the organic solvent layer.

The organic solvent layer contains the organic solvent used in the step (I) and an oil component including an asphalt component eluted from the solid raw material into the organic solvent. In the method of the present invention, the organic solvent layer may be filtered before the asphalt step in step (III), but in step (II) the organic solvent layer and the solid content layer are passed through the aqueous solvent layer. Since it is separated, the solid content in the organic solvent layer is extremely small, and asphalt can be recovered by distilling and separating the components of the organic solvent layer as they are. Specifically, a method of distilling the organic solvent layer collected in step (II), distilling and separating the organic solvent, and collecting asphalt as a non-distilled portion (residual oil) can be mentioned. Here, the distillation may be carried out under normal pressure or under reduced pressure. A part or all of the separated organic solvent can be introduced into step (I) and used. Distillation conditions such as the distillation temperature can be selected by appropriately selecting conditions that can separate the asphalt.

When the asphalt ore contains a light oil component other than the asphalt component such as a light oil fraction, it can be recovered by distilling with the organic solvent used in the step (I). The collected light oil derived from asphalt ore may be separated as appropriate to obtain a light oil product.
Part or all of the organic solvent used in step (I) may be introduced into step (I).

Such step (III) is preferably performed by means (C) for recovering asphalt in the organic solvent layer. The means (C) is not particularly limited as long as it can recover asphalt from the organic solvent layer, but is preferably a distillation apparatus. The distillation apparatus may be an atmospheric distillation apparatus or a vacuum distillation apparatus. The distillation apparatus may have a means for extracting asphalt which is a non-distilled portion and a means for extracting an organic solvent or the like which is a distillate. You may have a structure. Moreover, it is also preferable to have a means for introducing the extracted organic solvent into the step (I).

  Such an asphalt manufacturing method and apparatus of the present invention are not particularly limited, and may be, for example, an embodiment shown in the flowchart shown in FIG. 1 or FIG. In these flowcharts, the lines represented by broken lines are arbitrarily provided.

  The solid raw material made of asphalt ore is introduced into the dissolving / stirring mixing apparatus, which is means (A) for obtaining a stirred mixture, through line (1), and is usually introduced into means (A) through line (2). The mixture is stirred and mixed with the organic solvent in the means (A), and then further stirred and mixed with an aqueous solvent such as water introduced into the means (A) through the line (3) to form a stirred mixture. Here, the organic solvent and the aqueous solvent may be introduced sequentially or simultaneously.

The stirred mixture obtained from the means (A) is introduced into the separation apparatus as the means (B) through the line (4). In the separation device (B), the organic solvent layer, the aqueous solvent layer, and the solid content layer are separated into three layers by one or more methods of standing, filtration, and centrifugation. This organic solvent layer contains asphalt in the solid raw material, and is a means (C) for separating the asphalt from the separator (B) through the line (5) and collecting the asphalt through the line (6). Introduced into the distillation apparatus. The distillation apparatus (C) may be an atmospheric distillation apparatus or a vacuum distillation apparatus, but is operated under a condition capable of separating an asphalt component and a light component containing an organic solvent, and the asphalt through a line (8). A product is obtained and the organic solvent is recovered through line (7). The organic solvent recovered through the line (7) may be partly or wholly recycled into the dissolution / stirring mixing device (A) through the line (9) as necessary, and may be purified as appropriate. It may be an organic solvent product.

  The aqueous solvent layer and the solid content layer, which are the residue obtained by separating the organic solvent layer from the separation device (B), may be separated from the separation device (B) or extracted together, for example, the line (10 ) In a slurry form. The slurry containing the aqueous solvent layer and the solid content layer is introduced into the separation device through the line (11). This separation device preferably includes any one of stationary, filtration, and centrifugal separation, where the slurry is separated into a solid component and a liquid component mainly containing an aqueous solvent. The aqueous solvent which is the separated liquid component is extracted from the line (13), and if necessary, after separation of the components, the organic solvent may be separated out. You may recycle in a melt | dissolution and stirring mixing apparatus (A) through (14). The solid content obtained by the separation device is extracted through a line (12), and may be discarded as it is or after being appropriately subjected to a treatment such as firing, or may be used as a neutralizing agent or a raw material for cement.

EXAMPLES Hereinafter, although this invention is demonstrated further more concretely based on an Example, this invention is not limited to these Examples.
[Example 1]
Asbuton ore was cut to obtain pulverized asbuton having an average particle size of 30 mm. The asphalt content in the asbuton ore confirmed by analysis was 20% by mass. This was used as a solid raw material.

  In a 500 ml beaker, 100 g of 45 ° C. kerosene is added to 100 g of solid raw material, and a stirrer having four blades is rotated at 100 rpm and stirred for 16 minutes to dissolve, and the oil content of asbuton is extracted into kerosene. did. The kerosene used here had a flash point of 45 ° C., contained 95 mass% of a component having a boiling point of 140 to 250 ° C., and contained 95 mass% of a hydrocarbon having 8 to 15 carbon atoms.

  While continuing stirring, 100 g of water at 45 ° C. was added thereto, and stirring was continued for about 1 hour, and then the stirring bar was removed. When this was allowed to stand for 6 minutes, it was separated into a kerosene layer (upper layer), an aqueous layer (intermediate layer) and a solid content layer (lower layer).

  When the kerosene layer was collected, no solid content was contained. Subsequently, the fractionated kerosene layer was distilled under reduced pressure, the distillate was separated to produce asphalt, and the kerosene fraction as the distillate was recovered. The recovery rate of the obtained asphalt was 75% of the asphalt content in the solid raw material determined by analysis.

[Example 2]
In a 500 ml beaker, 100 g of the same solid material used in Example 1 was added kerosene (similar to that used in Example) or light oil (LGO, flash point 68 ° C., boiling point 165 to 165) as an organic solvent. (360 ° C.) 100 g was added, and a stirrer having 4 blades was rotated at 100 rpm, and dissolved by stirring until sufficient dissolution was visually observed (16 to 90 minutes). Extracted into organic solvent. While stirring was continued, 100 g of water having the same temperature as that of the organic solvent (kerosene or light oil) added thereto was added, and stirring was continued for about 1 hour, and then the stirring bar was removed. When this was allowed to stand for 6 minutes, it was separated into an organic solvent layer (upper layer), an aqueous layer (intermediate layer) and a solid content layer (lower layer). The organic solvent layer was separated, and asphalt was recovered in the same manner as in Example 1, and the asphalt recovery rate was determined. The results are shown in the graph of FIG.

[Comparative Example 1]
100 g of kerosene at 90 ° C. is added to a solid raw material having an average particle diameter of 30 mm obtained by pulverizing 100 g of asbuton, and a stirrer having four blades is rotated at 100 rpm and stirred for 16 minutes. Were extracted into kerosene. After completion of stirring, the mixture was allowed to stand at room temperature for 6 minutes to separate into a kerosene layer (upper layer) and a solid content layer (lower layer).

When the kerosene layer and the solid content layer were divided, it was confirmed that a solid content was present in the kerosene layer and a kerosene content was present in the solid content layer.
[Example 3]
In Example 1, after standing, the solid content layer separated into a kerosene layer (upper layer), an aqueous layer (intermediate layer) and a solid content layer (lower layer) was collected.

  The obtained solid content layer was evaporated by heating to 115 ° C. at normal pressure, the distillate was recovered, and the recovered amount was determined by the amount of liquid condensed. The results are shown in the table of FIG. Thus, it was confirmed that 70% of the kerosene remaining in the solid content layer could be recovered even at the evaporation at 115 ° C. and a temperature much lower than the solvent boiling point.

  According to the present invention, purified asphalt can be produced by a simpler method than asphalt ores such as asbuton.

FIG. 1 is a schematic flow diagram showing one embodiment of the asphalt production method and apparatus of the present invention. FIG. 2 is a schematic flow diagram showing one embodiment of the asphalt production method and apparatus of the present invention, including the case of recycling the organic solvent recovered from the aqueous solvent layer and / or the solid content layer. FIG. 3 is a table showing the results of Example 2. FIG. 4 is a table showing the results of Example 3.

Explanation of symbols

(1) to (14): line (A): means (A) (dissolution / stirring mixing device)
(B): Means (B) (Separator)
(C): Means (C) (Distillation apparatus)

Claims (15)

A method for producing purified asphalt from asphalt ore,
(I) a step of obtaining a stirring mixture comprising a solid raw material comprising an asphalt ore, an organic solvent, and an aqueous solvent;
(II) The step of separating the stirred mixture into an organic solvent layer containing an asphalt component, an aqueous solvent layer and a solid component layer, and separating the organic solvent layer; and (III) collecting the asphalt in the organic solvent layer. And a temperature of the organic solvent used in the step (I) is 80 ° C. or less. The step (I) of obtaining the stirring mixture is a step of stirring and mixing a solid raw material made of asphalt ore and an organic solvent, and further adding an aqueous solvent and stirring and mixing. Asphalt manufacturing method.   The method for producing asphalt according to claim 1 or 2, wherein the organic solvent is a hydrocarbon solvent containing 80% by mass or more of a hydrocarbon having 8 to 25 carbon atoms.   The method for producing asphalt according to any one of claims 1 to 3, wherein the organic solvent is a hydrocarbon solvent containing 80 mass% or more of hydrocarbon having a boiling point of 140 ° C or higher and 400 ° C or lower. The method for producing asphalt according to any one of claims 1 to 4, wherein in the step (I), the temperature of the organic solvent to be mixed is a temperature equal to or lower than the flash point of the organic solvent.   The method for producing asphalt according to any one of claims 1 to 5, wherein the aqueous solvent is water.   In the step (II), the organic solvent layer, the aqueous solvent layer and the solid content layer are separated by any one or more of stationary, filtration and centrifugation. A method for producing asphalt according to claim 1. At least a part of the aqueous solvent obtained from the aqueous solvent layer separated in step (II) is subjected to step (I).
The asphalt production method according to claim 1, wherein the asphalt production method is introduced into the asphalt.   The organic solvent contained in a solid content layer is collect | recovered by heating the solid content layer isolate | separated at process (II) to 80-260 degreeC, It is characterized by the above-mentioned. Asphalt manufacturing method. An organic solvent is separated from the solid content layer separated in step (II) by evaporation, and at least a part of the obtained organic solvent is introduced into step (I) and / or step (III) Item 10. A method for producing asphalt according to any one of Items 1 to 9. The method for producing asphalt according to any one of claims 1 to 10, wherein the recovery of asphalt in the step (III) is performed by separating an organic solvent by distillation.   The method for producing asphalt according to claim 11, wherein at least a part of the organic solvent separated in step (III) is introduced into step (I).   The asphalt ore according to any one of claims 1 to 12, wherein the asphalt ore contains 30% by mass or more of calcium carbonate. An apparatus for producing asphalt from asphalt ore,
(A) Means for obtaining a stirred mixture comprising a solid raw material comprising asphalt ore, an organic solvent, and an aqueous solvent;
(B) A means for separating the stirred mixture into an organic solvent layer containing an asphalt component, an aqueous solvent layer and a solid component layer, and separating the organic solvent layer; and (C) collecting asphalt in the organic solvent layer. An asphalt manufacturing apparatus characterized by comprising means for:   It further comprises means for recovering the organic solvent in the solid content layer obtained from the means (B), and means for introducing at least a part of the recovered organic solvent into the means (A) and / or (C). The asphalt manufacturing apparatus according to claim 14.

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