CN115717084A - External circulation type extraction device and extraction method for extracting montan wax - Google Patents
External circulation type extraction device and extraction method for extracting montan wax Download PDFInfo
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- CN115717084A CN115717084A CN202110975213.6A CN202110975213A CN115717084A CN 115717084 A CN115717084 A CN 115717084A CN 202110975213 A CN202110975213 A CN 202110975213A CN 115717084 A CN115717084 A CN 115717084A
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- 238000000605 extraction Methods 0.000 title claims abstract description 183
- 239000012170 montan wax Substances 0.000 title claims abstract description 33
- 239000003077 lignite Substances 0.000 claims abstract description 110
- 239000002994 raw material Substances 0.000 claims abstract description 41
- 239000011259 mixed solution Substances 0.000 claims abstract description 34
- 239000003245 coal Substances 0.000 claims abstract description 33
- 238000000034 method Methods 0.000 claims abstract description 33
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 32
- 239000011362 coarse particle Substances 0.000 claims abstract description 23
- 239000010419 fine particle Substances 0.000 claims abstract description 22
- 238000011049 filling Methods 0.000 claims abstract description 6
- 239000007788 liquid Substances 0.000 claims description 88
- 238000007599 discharging Methods 0.000 claims description 25
- 239000002245 particle Substances 0.000 claims description 20
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 15
- 230000008569 process Effects 0.000 claims description 15
- DKPFZGUDAPQIHT-UHFFFAOYSA-N Butyl acetate Natural products CCCCOC(C)=O DKPFZGUDAPQIHT-UHFFFAOYSA-N 0.000 claims description 7
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 claims description 7
- 239000000243 solution Substances 0.000 claims description 7
- 239000002904 solvent Substances 0.000 claims description 6
- XBDQKXXYIPTUBI-UHFFFAOYSA-M Propionate Chemical compound CCC([O-])=O XBDQKXXYIPTUBI-UHFFFAOYSA-M 0.000 claims description 5
- KXKVLQRXCPHEJC-UHFFFAOYSA-N acetic acid trimethyl ester Natural products COC(C)=O KXKVLQRXCPHEJC-UHFFFAOYSA-N 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 238000011001 backwashing Methods 0.000 claims description 4
- 238000011010 flushing procedure Methods 0.000 claims description 4
- 239000000463 material Substances 0.000 claims description 4
- 238000012423 maintenance Methods 0.000 claims description 2
- 239000001993 wax Substances 0.000 abstract description 19
- 239000011347 resin Substances 0.000 abstract description 12
- 229920005989 resin Polymers 0.000 abstract description 12
- 238000012216 screening Methods 0.000 abstract description 7
- 230000018044 dehydration Effects 0.000 abstract description 4
- 238000006297 dehydration reaction Methods 0.000 abstract description 4
- 238000002360 preparation method Methods 0.000 abstract description 2
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
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- 150000002646 long chain fatty acid esters Chemical class 0.000 description 1
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- 238000004519 manufacturing process Methods 0.000 description 1
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Abstract
The invention relates to the field of lignite wax preparation, in particular to an external circulation type extraction device and an extraction method for extracting lignite wax. The method comprises the following steps: (I) Filling an extraction column with a first extracting agent, and continuously performing self-circulation on the first extracting agent in the extraction column through an external circulation pipeline; (II) introducing the raw materials of the lignite and a second extractant into a cyclone distributor, and contacting and extracting in the presence of a cyclone field to form a mixed solution; wherein the upper part of the mixed solution contains lignite fine particles, and the lower part of the mixed solution contains lignite coarse particles; (III) the mixed liquor is divided into A strands and B strands, wherein the B strand of mixed liquor is circulated from the upper part to the lower part of the extraction column through an external circulation pipeline to continuously participate in extraction; and removing coal from the A-strand mixed liquor through a filter screen to obtain a finished product extract, and recovering the fine discharge liquor and coarse-particle residual coal at the bottom of the extraction column. The pretreatment such as dehydration, granularity screening and the like is not needed, and the yield of the montan wax and the resin is high.
Description
Technical Field
The invention relates to the field of lignite wax preparation, in particular to an external circulation type extraction device and an extraction method for extracting lignite wax.
Background
Montan wax is a natural wax extracted from low-metamorphic lignite or peat, the main components of which comprise long-chain fatty acid, fatty acid ester and alkane, and the montan wax is widely applied to the industries of daily chemicals, precision casting, rubber, plastics and the like by virtue of the characteristics of good physical and chemical properties, low harm to human bodies, good biodegradability, no pollution to the environment and the like.
The wax content, moisture content, particle size and mechanical strength of the particles of the lignite itself are major factors affecting the quality of the montan wax product. The wax content and the mechanical strength of the particles are inherent characteristics of the lignite, and the extraction rate of the lignite wax can be improved only by regulating and controlling the moisture and the particle size in the prior art, so that the quality of the lignite wax product is improved. On one hand, because of incompatibility of water and an extracting agent, moisture can prevent the extracting agent from wetting lignite particles so as not to enter the particles, and the extraction rate is low, the lignite is generally required to be dried firstly in the existing extraction process so as to reduce the moisture content in the lignite and improve the extraction effect; on the other hand, the particle size of the lignite is controlled by screening, fine particles are screened out, or the fine particles are formed, so that the difficulty of subsequent solid-liquid separation can be reduced, and the influence on the quality of the lignite wax product caused by excessive fine coal powder remained in the extraction liquid is avoided. The above-described methods, however, all undoubtedly increase process equipment investment and energy consumption.
In view of the above, it is highly desirable to develop a new extraction technology for extracting montan wax to solve the above problems.
Disclosure of Invention
The invention aims to solve the problems of long process flow, high energy consumption and large equipment investment caused by the pretreatment of drying, dehydrating, screening or molding raw material lignite in the lignite wax extraction process in the prior art, and provides an external circulation type extraction device and an extraction method for extracting lignite wax.
In order to achieve the above object, a first aspect of the present invention provides an external circulation type extraction apparatus for extracting montan wax, comprising: the device comprises an extraction column 1, a feeding screw 2, a discharging screw 3, a cyclone distributor 9, a filter screen 12, a fine liquid discharge pipeline 7 and an external circulation pipeline 6; wherein, the first and the second end of the pipe are connected with each other,
the feeding screw 2 penetrates through the side wall of the extraction column 1 and extends into the cyclone distributor 9, and is used for feeding raw lignite to the cyclone distributor 9 to be contacted with an extracting agent;
the cyclone distributor 9 is used for generating a cyclone field and enabling the raw material lignite to contact with an extractant for extraction in the presence of the cyclone field;
the external circulation pipeline 6 is externally communicated with the upper part and the lower part of the extraction column 1 and is used for dividing mixed liquor formed in the extraction process into a strand A and a strand B and circulating the strand B from the upper part to the lower part of the extraction column 1 to continue to participate in extraction;
the filter screen 12 is annular, the outer ring of the filter screen is connected with the inner wall of the upper part of the extraction column 1, the inner ring of the filter screen is connected with the closed top surface of the cyclone distributor 9, and the filter screen is used for carrying out coal removal treatment on the A-strand mixed solution to obtain a finished product extract and fine particle residual coal mixed solution;
the thin liquid discharging pipeline 7 is communicated with the extraction column 1 and the discharging spiral 3 and is used for feeding the thin liquid into the discharging spiral 3;
the discharge screw 3 is respectively connected with the bottom of the extraction column 1 and the fine liquid discharge pipeline 7, and is used for mixing coarse particle residual coal and fine liquid obtained after extraction, draining a solvent and discharging.
The invention provides a method for extracting montan wax by using the external circulation type extraction device for extracting montan wax, which is described in the first aspect, and comprises the following steps:
(I) Filling an extraction column with a first extracting agent, and continuously performing self-circulation on the first extracting agent in the extraction column through an external circulation pipeline;
(II) introducing the raw materials of lignite and a second extractant into a cyclone distributor, and contacting and extracting in the presence of a cyclone field to form a mixed solution; wherein the upper part of the mixed solution contains lignite fine particles, and the lower part of the mixed solution contains lignite coarse particles;
(III) the mixed liquor is divided into A strands and B strands, wherein the B strand of mixed liquor is circulated from the upper part to the lower part of the extraction column through an external circulation pipeline to continuously participate in extraction; and (3) removing coal from the A-strand mixed solution through a filter screen to obtain a finished product extract, and recovering the fine-discharging solution and coarse-particle residual coal at the bottom of the extraction column.
Through the technical scheme, the invention has the following beneficial effects:
(1) Pretreatment such as dehydration and granularity screening is not needed to be carried out on the raw material lignite, so that direct extraction of lignite wax is realized, the solid-liquid mass transfer effect of lignite and an extracting agent is enhanced through external circulation, and the extraction rate is improved;
(2) The cyclone distributor in the device can increase the contact time of lignite particles and an extracting agent, and concentrates fine particles in the cyclone, so that pulverization caused by collision among coarse particles is reduced;
(3) The quality requirement on the raw material lignite is low, the process is simple, and the yield of the lignite wax and the resin is high.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the principles of the invention and not to limit the invention. In the drawings:
FIG. 1 is a schematic view of an external circulation type extraction apparatus for extracting montan wax according to the present invention;
fig. 2 is a top view of the interior of an extraction column of the external circulation type extraction apparatus for extracting montan wax according to the present invention.
Description of the reference numerals
1-extraction column 2-feeding screw 3-discharging screw
4-extractant inlet 5-finished product extract outlet 6-external circulation pipeline
7-fine liquid discharge pipeline 8-flushing liquid inlet 9-cyclone distributor
10-discharge opening 11-circulating pump 12-filter screen
Detailed Description
The endpoints of the ranges and any values disclosed herein are not limited to the precise range or value, and these ranges or values should be understood to encompass values close to these ranges or values. For ranges of values, between the endpoints of each of the ranges and the individual points, and between the individual points may be combined with each other to give one or more new ranges of values, and these ranges of values should be considered as specifically disclosed herein.
The following describes in detail specific embodiments of the present invention. It should be understood that the detailed description and specific examples, while indicating the preferred embodiment of the invention, are given by way of illustration and explanation only, not limitation.
The first aspect of the present invention provides an external circulation type extraction apparatus for extracting montan wax, as shown in fig. 1, comprising: the device comprises an extraction column 1, a feeding screw 2, a discharging screw 3, a cyclone distributor 9, a filter screen 12, a fine liquid discharge pipeline 7 and an external circulation pipeline 6; wherein the content of the first and second substances,
the feeding screw 2 penetrates through the side wall of the extraction column 1 and extends into the cyclone distributor 9, and is used for feeding raw lignite to the cyclone distributor 9 to be contacted with an extracting agent;
the cyclone distributor 9 is used for generating a cyclone field and enabling the raw material lignite to be contacted with an extracting agent for extraction in the presence of the cyclone field;
the external circulation pipeline 6 is externally communicated with the upper part and the lower part of the extraction column 1 and is used for dividing mixed liquor formed in the extraction process into a strand A and a strand B and circulating the strand B from the upper part to the lower part of the extraction column 1 to continue to participate in extraction;
the filter screen 12 is annular, the outer ring of the filter screen is connected with the inner wall of the upper part of the extraction column 1, the inner ring of the filter screen is connected with the closed top surface of the cyclone distributor 9, and the filter screen is used for carrying out coal removal treatment on the A-strand mixed solution to obtain a finished product extraction liquid and a fine particle residue coal mixed drainage liquid;
the fine liquid discharge pipeline 7 is communicated with the extraction column 1 and the discharge screw 3 and is used for conveying the fine liquid into the discharge screw 3;
the discharge screw 3 is respectively connected with the bottom of the extraction column 1 and the fine liquid discharge pipeline 7, and is used for mixing coarse particle residual coal and fine liquid obtained after extraction, draining a solvent and discharging.
In some embodiments of the present invention, the extraction column 1 may be a conventional cylindrical container for extraction, and it is sufficient to contact and extract raw material lignite with an extractant, and it is preferable to use a cylindrical container with a circular cross section.
In the invention, the upper part of the extraction column 1 is provided with an extractant inlet 4 and a finished product extraction liquid outlet 5; the position of the extractant inlet 4 is lower than that of the filter screen 12 and is communicated with the inside of the cyclone distributor 9; the position of the finished product extract outlet 5 is higher than the filter screen 12. Before the apparatus of the present invention is operated, it is necessary to fill the extraction column 1 with extractant through extractant inlet 4. In the initial operation stage of the device, because the raw lignite and new extractant need to be continuously fed into the extraction column 1 filled with the extractant, part of the pre-injected extractant is driven to be discharged from the finished extraction liquid outlet 5, and after the device is stably operated, all the material flow discharged from the outlet is finished extraction liquid.
In the present invention, as shown in fig. 2, the extractant inlet 4 may be communicated with the upper feed inlet of the cyclone distributor 9 through a feed line, for realizing the entrance of the extractant from the upper part of the cyclone distributor 9. The feed line is also located below the filter screen 12.
In the present invention, a washing liquid inlet 8 is provided at the top of the extraction column 1 for periodically back-washing the filter screen 12. The fine coal powder blocked by the net can be removed by using the extractant for back washing and is discharged by the fine liquid discharge pipeline 7, so that the pressure rise in the extraction column caused by the net blocking is effectively reduced, the stable operation of the extraction process in the column is ensured, and the smooth discharge of the finished extraction liquid is ensured.
In the invention, the bottom of the extraction column 1 is also provided with a discharge outlet 10 for discharging all materials during parking and maintenance. During normal daily operation of the extraction plant, the discharge opening 10 is closed.
In some embodiments of the present invention, the cyclone distributor 9 has a trumpet-shaped inner cavity, the top of the inner cavity is closed, the bottom of the inner cavity is open, the cross section of the inner cavity is circular, and the radius of the cross section is gradually reduced from top to bottom. The extractant fed from the extractant inlet 4 enters tangentially from the upper part of the cyclone distributor 9 at a certain speed and moves downwards spirally in the cavity of the cyclone distributor 9 to form a cyclone field. Raw material lignite conveyed to the cavity of the cyclone distributor 9 by the feeding screw 2 is contacted with an extractant and starts to be extracted, under the action of a cyclone field, coarse particle components in the raw material lignite slowly move downwards along the axial direction of the cyclone distributor 9, simultaneously move outwards along the radial direction, gradually move downwards along the wall of the cyclone distributor and are discharged from the outlet at the bottom of the cyclone distributor 9, then are continuously settled in the extraction column 1 under the action of gravity, and continuously carry out mass transfer with a mixed solution (containing the extractant) formed in the extraction process during settlement, and finally settle to the bottom of the extraction column 1; meanwhile, fine particle components in the raw material lignite move along the radial direction towards the central axis direction of the cyclone 9, are continuously enriched, slowly move downwards under the action of an extractant liquid flow and are discharged from a bottom outlet of the cyclone distributor 9, and then the light components move upwards under the action of disturbance generated by an external circulation liquid and continue to carry out mass transfer with mixed liquid formed in the extraction process, and finally reach the upper part of the extraction column 1. In the invention, the cyclone distributor 9 can effectively prolong the settling time of the lignite particles, increase the contact time of the lignite particles and the extracting agent, enrich the fine particles in the cyclone and reduce pulverization caused by collision among coarse particles.
In the present invention, in order to obtain a swirl field with better swirl effect, it is preferable that the velocity of the extractant fed from the extractant inlet 4 entering tangentially from the upper part of the swirl distributor 9 is not lower than 0.8m/s.
In some embodiments of the invention, the liquid inlet of the external circulation line 6 is at a lower level than the liquid inlet of the fine liquid discharge line 7; the liquid outlet end of the external circulation pipeline 6 extends into the lower part of the extraction column 1, and the liquid outlet faces upwards; preferably, the external circulation pipeline 6 is provided with a circulation pump 11 for adjusting the flow rate of the B strands of extraction liquid.
In the invention, a part of the mixed liquor (namely the mixed liquor B) formed in the extraction process enters the lower part of the extraction column 1 through the external circulation pipeline 6 and forms an upward moving liquid flow, and the mixed liquor (containing an extracting agent) in the extraction column 1 can be disturbed under the driving of the liquid flow, so that the sedimentation speed of the lignite in the extraction column 1 can be further slowed down, the effective residence time of the lignite in the extraction column 1 is prolonged, and the extraction can be more fully performed. Meanwhile, the upward liquid flow moves opposite to the downward moving lignite particles, and liquid-solid countercurrent mass transfer is facilitated. The circulating pump 11 is used for adjusting the flow of the B-strand mixed liquid of the external circulation, the degree of the disturbance effect and the residence time of the lignite in the extraction column 1 can be further controlled, so that the solid-liquid mass transfer effect is enhanced, the extraction rate is improved and the direct extraction of the lignite wax is realized under the condition that the raw material lignite is not subjected to dehydration pretreatment.
In some embodiments of the present invention, the filter screen 12 is used for separating the finished extract from the fine particle residual coal, i.e., coal removal. Preferably, the mesh number of the filter screen 12 is 150-300, so as to obtain a better fine coal powder separation effect and ensure smooth discharge of the finished product extract.
In some embodiments of the present invention, the liquid inlet of the fine liquid discharge pipeline 7 is lower than the position of the filter screen 12, preferably lower than and close to the position of the filter screen 12, so as to facilitate the discharge of fine particle residual coal as soon as possible and prevent the excessive aggregation from causing the blockage of the screen.
In some embodiments of the present invention, the feeding screw 2 and the discharging screw 3 may be a spiral feeding device conventionally used in the art, and may include a feeding screw and a sleeve pipe sleeved outside thereof, which is not particularly limited by the present invention.
In the present invention, the feeding screw 2 may extend into the cyclone distributor 9 along the horizontal direction, or may extend into the cyclone distributor 9 obliquely downward at a certain angle with the horizontal direction, and in order to obtain a better feeding effect, the latter method is preferably adopted.
In the invention, the discharge screw 3 comprises a horizontal section and a vertical section which are communicated, the horizontal section extends into the bottom of the extraction column 1, and the vertical section is connected with the fine liquid discharge pipeline 7. Coarse particle residual coal obtained after extraction is firstly output from the extraction column 1 through the horizontal section of the discharge screw 3, then enters the vertical section to be mixed with the fine discharge liquid, and is finally discharged after the solvent is jointly drained under the action of gravity. The residence time of the lignite in the extraction column 1 can be controlled by adjusting the rotating speed of the discharging spiral 3.
In a second aspect, the present invention provides an extraction method for extracting montan wax, comprising:
(I) Filling an extraction column with a first extracting agent, and continuously performing self-circulation on the first extracting agent in the extraction column through an external circulation pipeline;
(II) introducing the raw materials of lignite and a second extractant into a cyclone distributor, and contacting and extracting in the presence of a cyclone field to form a mixed solution; wherein the upper part of the mixed solution contains lignite fine particles, and the lower part of the mixed solution contains lignite coarse particles;
(III) the mixed liquor is divided into A strands and B strands, wherein the B strand of mixed liquor is circulated from the upper part to the lower part of the extraction column through an external circulation pipeline to continuously participate in extraction; and (3) removing coal from the A-strand mixed solution through a filter screen to obtain a finished product extract, and recovering the fine-discharging solution and coarse-particle residual coal at the bottom of the extraction column.
In some embodiments of the invention, the swirl field may be formed by a liquid extractant entering the swirl distributor at a velocity, preferably a velocity of the liquid extractant entering the swirl distributor tangentially of not less than 0.8m/s.
In the present invention, the raw material lignite is only required to satisfy the raw material component requirements for extracting montan wax, which are conventional in the art, and the moisture content and the particle size of the raw material lignite are not particularly limited in the present invention. From the viewpoint of facilitating extraction, the particle size of the raw material lignite is preferably less than 20mm, and more preferably less than 13mm.
In some embodiments of the invention, the first extractant and the second extractant are the same, preferably methyl acetate, ethyl acetate, or butyl acetate. By combining the method, the invention can obtain good extraction effect by using a single ester compound extracting agent, and can not generate the problem of complicated subsequent distillation and separation procedures caused by a plurality of extracting agents.
In the invention, the components of the mixed solution comprise an extracting agent, lignite wax and resin dissolved in the extracting agent, lignite particles in the extracting process and residual coal obtained after partial extraction.
In some embodiments of the present invention, in order to obtain better cyclone separation effect and extraction efficiency, it is preferable that in step (II), the mass ratio of the raw lignite to the second extractant is 1: (1-1.8); in step (II) and step (III), the extraction conditions include: the extraction temperature is 70-100 ℃, and the total extraction time is 1-3h.
In some embodiments of the present invention, in order to obtain better extraction effect and efficiency, the ratio of the circulation amount of the B-strand mixed liquor to the volume of the extraction column is preferably 1-3h -1 。
The extraction method provided by the invention has low quality requirement on the raw material lignite, can save pretreatment processes such as drying, dewatering, screening or forming and the like on the raw material lignite, realizes direct extraction, and has the advantages of simple process, low energy consumption and high product yield.
The following description will be made with reference to fig. 1 for the application of the extraction method provided by the present invention to the external circulation type extraction apparatus for extracting montan wax according to the present invention.
A. Starting and initial operation stage:
(1) Filling a first extractant into the extraction column 1 through a feed inlet at the upper part of a cyclone distributor 9 through an extract inlet 4, enabling the liquid level to reach the top of the cyclone distributor 9, and then starting a circulating pump 11 to enable the first extractant to continuously perform self-circulation in the extraction column 1 through an external circulating pipeline 6;
(2) Feeding raw lignite into a cyclone distributor 9 through a feeding screw 2, and meanwhile tangentially inputting a second extractant from the upper part of the cyclone distributor 9 at a certain speed through an extract inlet 4 to form a cyclone field; in the cyclone distributor 9, the raw lignite is contacted with an extractant and extraction is started. Under the action of the swirling flow field, lignite coarse particles moving outwards along the radial direction and lignite fine particles gradually enriched in the central axis area of the swirling flow distributor 9 slowly move downwards and are discharged from the bottom outlet of the swirling flow distributor 9, and then solid-liquid mass transfer is continuously carried out on the lignite coarse particles and the lignite fine particles and the extracting agent (mixed liquid in the stable operation stage) in the extraction column 1 respectively to form mixed liquid. The upper part of the mixed solution contains lignite fine particles, and the lower part of the mixed solution contains lignite coarse particles;
(3) The mixed liquid is divided into a strand A and a strand B, wherein the strand B of mixed liquid circulates from the upper part to the lower part of the extraction column 1 through the external circulation pipeline 6, and forms an upward moving liquid flow in the mixed liquid, so that the mixed liquid in the extraction column 1 can be disturbed, and the solid-liquid mass transfer is enhanced. The mixed liquor of the A strand is subjected to coal removal treatment through a filter screen 12, and a finished product extract obtained at the upper part of the filter screen is discharged from a finished product extract outlet 5 (when the device is just started, part of the first extractant injected in advance is also discharged from the outlet, the content of montan wax in the discharged extractant is gradually increased, and a discharge material flow of the outlet is gradually converted into the finished product extract).
B. A transition stage:
after the process A is operated for 1-2h, the discharging screw 3 is started, coarse particle residual coal at the bottom of the extraction column 1 is output by the horizontal section of the discharging screw 3, and fine particle residual coal intercepted at the lower part of the filter screen 12 is sent to the vertical section of the discharging screw 3 by the fine liquid discharging pipeline 6 in a form of fine liquid discharging. And mixing the coarse and fine particle residual coal in the vertical section of the discharge screw 3, draining the solvent under the action of gravity, and finally discharging the mixture out of the device for recycling. And adjusting the rotating speeds of the discharge screw 3 and the feeding screw 2 and the flow of the circulating pump 11 to gradually match the rotating speeds, adjusting and operating for a period of time, gradually achieving dynamic balance of the feeding of the raw material lignite and the second extracting agent, the output of the residual lignite and the discharge of the finished product extracting solution, and enabling the device to enter a stable operation stage.
C. And (3) a stable operation stage:
keeping the feeding mass ratio of the raw material lignite to the second extracting agent as 1: (1-1.8), and the temperature of the fed second extracting agent is 70-100 ℃; adjusting the rotating speed of the discharge screw 3 (which is consistent with that of the feed screw 2), and adjusting the volume ratio of the circulation volume of the B strand of mixed solution to the extraction column to be 1-3h -1 The residence time (extraction time) of the lignite in the extraction column 1 is controlled to be 1-3h, and the inlet and outlet amount of the lignite in the extraction column 1 is kept balanced. And regularly backwashing the filter screen 12 by using an extractant through the flushing liquid inlet 8 to relieve the blockage of the screen in time so as to ensure continuous and stable operation of the device. And obtaining a finished product extract product with stable components at an extract outlet 5.
The present invention will be described in detail below by way of examples. In the following examples and comparative examples,
the raw material lignite is taken from Baoqing county of Heilongjiang, is simulated lignite with different water contents and particle sizes, is dried and screened respectively to obtain different raw material lignite, and is marked as R1-R3, and the components and particle size distribution of the raw material lignite are shown in Table 1.
TABLE 1
Note: r1 is not treated, R2 is obtained by drying R1, and R3 is obtained by sieving R1.
Example 1
The external circulation type extraction apparatus for extracting montan wax according to the present invention, as shown in fig. 1, was used to perform montan wax extraction.
A. Start-up and initial run phases:
(1) Filling butyl acetate with the temperature of 80 ℃ into the extraction column 1 through a feed inlet at the upper part of a cyclone distributor 9 through an extraction liquid inlet 4, enabling the liquid level to reach the top of the cyclone distributor 9, and then starting a circulating pump 11 to enable the first extracting agent to continuously perform self-circulation in the extraction column 1 through an external circulating pipeline 6;
(2) Feeding raw material lignite R1 into a cyclone distributor 9 through a feeding screw 2, and meanwhile tangentially inputting butyl acetate from the upper part of the cyclone distributor 9 through an extract liquid inlet 4 at the speed of 0.8m/s to form a cyclone field; in the cyclone distributor 9, the raw material lignite R1 was contacted with butyl acetate and extraction was started. Under the action of the rotational flow field, the lignite coarse particles and the lignite fine particles slowly move downwards and are discharged from the bottom outlet of the rotational flow distributor 9, and then solid-liquid mass transfer is continuously performed in the extraction column 1 respectively to form a mixed solution. The upper part of the mixed solution contains lignite fine particles, and the lower part of the mixed solution contains lignite coarse particles;
(3) And the mixed solution is divided into a strand A and a strand B, wherein the strand B of mixed solution circulates from the upper part to the lower part of the extraction column 1 through an external circulation pipeline 6, and forms an upward moving liquid flow in the mixed solution, so that disturbance is formed on the mixed solution, and solid-liquid mass transfer is enhanced. And the A mixed solution is subjected to coal removal treatment through a filter screen 12 (300 meshes), and a finished product extract obtained at the upper part of the filter screen is discharged from a finished product extract outlet 5.
B. A transition stage:
above-mentioned A process operation 2h back, start ejection of compact spiral 3, the residual coal of coarse grain in extraction column 1 bottom is exported by ejection of compact spiral 3's horizontal segment, is intercepted simultaneously and is sent into the vertical section of ejection of compact spiral 3 by row thin liquid pipeline 6 in the form of row thin liquid at the residual coal of fine grain of filter screen 12 lower part. And mixing the coarse and fine particle residual coal in the vertical section of the discharge screw 3, draining the solvent under the action of gravity, and finally discharging the mixture out of the device for recycling. And adjusting the rotating speeds of the discharge screw 3 and the feeding screw 2 and the flow of the circulating pump 11 to gradually match the rotating speeds, adjusting and operating for a period of time, gradually achieving dynamic balance of the feeding of the raw material lignite and the second extracting agent, the output of the residual lignite and the discharge of the finished product extracting solution, and enabling the device to enter a stable operation stage.
C. And (3) a stable operation stage:
keeping the feeding mass ratio of raw materials of lignite and butyl acetate as 1:1, feeding butyl acetate at the temperature of 80 ℃; adjusting the rotating speed of the discharging screw 3 (which is consistent with the rotating speed of the feeding screw 2), and adjusting the volume ratio of the circulation amount of the B-strand mixed solution to the volume of the extraction column to be 2h -1 So as to control the residence time (extraction time) of the lignite in the extraction column 1 to be 3h and keep the lignite inlet and outlet amount of the extraction column 1 balanced. The filter screen 12 is backwashed with an extractant through the flushing liquid inlet 8 periodically, so that the screen blockage is relieved in time, and the continuous and stable operation of the device is guaranteed. And obtaining a finished extraction liquid product with stable components, namely S1, at an extraction liquid outlet 5.
Example 2
The process according to example 1 is distinguished by: the raw material of lignite R2 is used, the extracting agent is methyl acetate, and a filter screen is 150 meshes; in the stable operation stage of the device, the feeding mass ratio of the raw material lignite R2 to the methyl acetate is kept to be 1:1.8, the temperature of the fed methyl acetate is 80 ℃, and the volume ratio of the circulation volume of the B strand of mixed liquor to the extraction column is 2h -1 The residence time (extraction time) of the lignite in the extraction column 1 is 1h. The other procedures and conditions were the same as in example 1. And after the device operates stably, obtaining a finished product extract product with stable components at an extract outlet 5, and recording the finished product extract product as S2.
Example 3
The process according to example 1 is distinguished by: the raw material of lignite R3 is used, the extracting agent is ethyl acetate, and a filter screen is 200 meshes; in the stable operation stage of the device, the feeding mass ratio of the raw material lignite R3 to the ethyl acetate is kept to be 1:1.2, the temperature of the fed ethyl acetate is 80 ℃, and the volume ratio of the circulation quantity of the mixed solution of the B strand to the volume of the extraction column is 2h -1 The residence time (extraction time) of the lignite in the extraction column 1 is 2h. The other procedures and conditions were the same as in example 1. After the device operates stably, a finished extraction liquid product with stable components is obtained at an extraction liquid outlet 5 and is marked as S3.
Comparative example 1
The process according to example 1 is distinguished by: the device is not provided with a cyclone distributor 9, an extracting agent directly enters the extraction column 1 from an extracting agent inlet 4, and a filter screen 12 is circular and is connected with the inner wall of the upper part of the extraction column (1). The other procedures and conditions were the same as in example 1. After the device operates stably, a finished extraction liquid product with stable components is obtained at an extraction liquid outlet 5 and is marked as D1.
Comparative example 2
The process according to example 1 is distinguished by: the device is not provided with an external circulation pipeline 6, namely the extractant and the mixed liquid formed in the extraction process are not subjected to external circulation. The other procedures and conditions were the same as in example 1. And after the device operates stably, obtaining a finished product extract product with stable components at an extract outlet 5, and recording the finished product extract product as D2.
Comparative example 3
Extraction of montan wax was carried out according to the method disclosed on page 3, practice of the specification of CN101434868A to obtain a montan wax-rich organic solvent, denoted as D3.
Test example
The finished extract products S1 to S3 and D1 to D3 obtained in examples 1 to 3 and comparative examples 1 to 3 were subjected to a montan wax and resin recovery process, and the yields of montan wax and resin were calculated, and the results are shown in Table 2.
The process of the lignite wax and resin recovery treatment comprises the following steps:
step 1: respectively introducing S1-S3 and D1-D3 into a sleeve crystallizer, cooling to 5-10 ℃, washing out the montan wax from the extraction liquid, then carrying out solid-liquid separation on the extraction liquid from which the montan wax is separated out by a centrifugal machine to obtain a solid-phase montan wax product, and collecting the obtained liquid phase in a falling film evaporator;
step 2: and in the falling-film evaporator, evaporating the liquid phase under the condition of-10 to-50 kPa to obtain a resin product.
Montan wax yield = (montan wax production/dry basis lignite) = 100%;
resin yield = (resin yield/dry lignite) × 100%.
TABLE 2
| Extracting liquid | Montan wax yield/% | Resin yield/% |
| S1 | 4.8％ | 2.2％ |
| S2 | 4.9％ | 2.2％ |
| S3 | 4.6％ | 2.0％ |
| D1 | 4.2％ | 1.7％ |
| D2 | 4.3％ | 1.8％ |
| D3 | 4.3％ | 1.6％ |
As can be seen from Table 2, S1-S3 gave higher yields of montan wax and resin, while D1-D3 gave significantly lower yields of these two products than S1-S3. Compared with S1 and S2, the moisture content of the raw material lignite used by the former is remarkably high, compared with S1 and S3, the raw material lignite used by the former is not subjected to particle size screening, but the device and the method disclosed by the invention are used, the three raw material lignite are high in product yield and basically equivalent in yield level, which shows that the device and the method disclosed by the invention can be used for directly extracting lignite wax without being limited by the moisture content and the particle size of the raw material lignite, the pretreatment processes such as dehydration, particle size screening or forming and the like on the raw material lignite are omitted, the requirements on the quality of the raw material lignite are wide, the process is simple, the extraction rate is high, and the higher yield of the lignite wax and resin is brought.
The comparative example did not employ the apparatus and method of the present invention, and the above-described effects of the present invention could not be obtained.
The preferred embodiments of the present invention have been described above in detail, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, many simple modifications can be made to the technical solution of the invention, including combinations of various technical features in any other suitable way, and these simple modifications and combinations should also be regarded as the disclosure of the invention, and all fall within the scope of the invention.
Claims (10)
1. An external circulation type extraction device for extracting montan wax, characterized by comprising: the device comprises an extraction column (1), a feeding screw (2), a discharging screw (3), a cyclone distributor (9), a filter screen (12), a fine liquid discharge pipeline (7) and an external circulation pipeline (6); wherein, the first and the second end of the pipe are connected with each other,
the feeding screw (2) penetrates through the side wall of the extraction column (1) and extends into the cyclone (9) for feeding raw lignite to the cyclone distributor (9) to be contacted with an extractant;
the cyclone distributor (9) is used for generating a cyclone field and enabling the raw material lignite to be contacted with an extracting agent for extraction in the presence of the cyclone field;
the external circulation pipeline (6) is externally communicated with the upper part and the lower part of the extraction column (1) and is used for dividing mixed liquid formed in the extraction process into a strand A and a strand B and circulating the strand B from the upper part to the lower part of the extraction column (1) to continue to participate in extraction;
the filter screen (12) is annular, the outer ring of the filter screen is connected with the inner wall of the upper part of the extraction column (1), the inner ring of the filter screen is connected with the closed top surface of the cyclone distributor (9), and the filter screen is used for carrying out coal removal treatment on the A-strand mixed solution to obtain a finished product extract and a fine discharge solution mixed with fine particle residual coal;
the fine liquid discharge pipeline (7) is communicated with the extraction column (1) and the discharge screw (3) and is used for conveying the fine liquid into the discharge screw (3);
and the discharge screw (3) is respectively connected with the bottom of the extraction column (1) and the fine liquid discharge pipeline (7) and is used for mixing coarse particle residual coal and fine liquid obtained after extraction, draining a solvent and discharging.
2. The apparatus of claim 1, wherein the upper part of the extraction column (1) is provided with an extractant inlet (4) and a finished extract outlet (5); the position of the extractant inlet (4) is lower than that of the filter screen (12) and is communicated with the inside of the cyclone distributor (9); the position of the finished product extract outlet (5) is higher than the filter screen (12);
preferably, the top of the extraction column (1) is provided with a flushing liquid inlet (8) for periodically backwashing the filter screen (12);
preferably, the bottom of the extraction column (1) is also provided with a discharge port (10) for discharging all materials during parking maintenance;
preferably, the mesh number of the filter screen (12) is 150-300.
3. The device according to claim 1, wherein the inlet of the fine liquid draining pipe (7) is at a lower level than the filter screen (12).
4. The device according to claim 1, wherein the liquid inlet of the external circulation line (6) is at a lower level than the liquid inlet of the fine liquid draining line (7); the liquid outlet end of the external circulation pipeline (6) extends into the lower part of the extraction column (1), and the liquid outlet faces upwards;
preferably, the external circulation pipeline (6) is provided with a circulation pump (11) for adjusting the flow rate of the B strands of extraction liquid.
5. The device according to claim 1, wherein the discharge screw (3) comprises a horizontal section and a vertical section which are communicated, the horizontal section extends into the bottom of the extraction column (1), and the vertical section is connected with the fine liquid discharge pipeline (7).
6. The method for extracting montan wax by using the external circulation type extraction apparatus for extracting montan wax according to any one of claims 1 to 5, which comprises:
(I) Filling an extraction column with a first extracting agent, and continuously performing self-circulation on the first extracting agent in the extraction column through an external circulation pipeline;
(II) introducing the raw materials of lignite and a second extractant into a cyclone distributor, and contacting and extracting in the presence of a cyclone field to form a mixed solution; wherein the upper part of the mixed solution contains lignite fine particles, and the lower part of the mixed solution contains lignite coarse particles;
(III) the mixed liquor is divided into A strands and B strands, wherein the B strand of mixed liquor is circulated from the upper part to the lower part of the extraction column through an external circulation pipeline to continuously participate in extraction; and (3) removing coal from the A-strand mixed solution through a filter screen to obtain a finished product extract, and recovering the fine-discharging solution and coarse-particle residual coal at the bottom of the extraction column.
7. The method according to claim 6, wherein the raw lignite has a particle size of less than 20mm, preferably less than 13mm;
preferably, the first and second extractants are the same, preferably methyl acetate, ethyl acetate or butyl acetate.
8. The method according to claim 6 or 7, wherein in the step (II), the mass ratio of the raw material lignite to the second extractant is 1: (1-1.8).
9. The process of any one of claims 6-8, wherein in step (II) and step (III), the extraction conditions comprise: the extraction temperature is 70-100 ℃, and the total extraction time is 1-3h.
10. The method of any one of claims 1-9, wherein the ratio of the circulation amount of the B-strand mixed liquor to the volume of the extraction column is 1-3h -1 。
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| CN106147863A (en) * | 2016-06-21 | 2016-11-23 | 金正大生态工程集团股份有限公司 | A kind of method extracting lignite wax from brown coal |
| CN112694913A (en) * | 2020-03-18 | 2021-04-23 | 国家能源投资集团有限责任公司 | Extraction process of montan wax |
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| CN106147863A (en) * | 2016-06-21 | 2016-11-23 | 金正大生态工程集团股份有限公司 | A kind of method extracting lignite wax from brown coal |
| CN112694913A (en) * | 2020-03-18 | 2021-04-23 | 国家能源投资集团有限责任公司 | Extraction process of montan wax |
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