CN115650873A - L-carnitine recovery process in wastewater generated in L-carnitine production process - Google Patents

L-carnitine recovery process in wastewater generated in L-carnitine production process Download PDF

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Publication number
CN115650873A
CN115650873A CN202211238275.XA CN202211238275A CN115650873A CN 115650873 A CN115650873 A CN 115650873A CN 202211238275 A CN202211238275 A CN 202211238275A CN 115650873 A CN115650873 A CN 115650873A
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China
Prior art keywords
carnitine
resin
waste liquid
recycling
cylinder mould
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CN202211238275.XA
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Chinese (zh)
Inventor
张芳
毕永锐
黎锋
蔡耿林
李日魏
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Guangzhou Rand Environmental Protection Resources Technology Co ltd
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Guangzhou Rand Environmental Protection Resources Technology Co ltd
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Priority to CN202211238275.XA priority Critical patent/CN115650873A/en
Publication of CN115650873A publication Critical patent/CN115650873A/en
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Abstract

The invention discloses a left-handed carnitine recycling process in waste water in a left-handed carnitine production process, which relates to the field of left-handed carnitine waste water recycling processes, and aims to solve the problems of left-handed carnitine resource waste and environmental pollution caused by the discharge of the existing left-handed carnitine-containing waste water, the following scheme is provided, the process comprises a process flow, the process flow adopts a mode of firstly resin adsorption and then separation recycling, and the process comprises the following steps: s1, adjusting the pH value of L-carnitine production wastewater to 6-7; s2, after the resin is washed for multiple times, the resin is filled into a chromatographic column by a wet method and is transferred into the chromatographic column, and hydrochloric acid and a sodium hydroxide solution are sequentially used for activation; and S3, washing the activated resin for multiple times until the activated resin is neutral. The invention has novel structure, and the process equipment and the recovery process method solve the problems of L-carnitine resource waste and environmental pollution caused by the discharge of the existing L-carnitine-containing wastewater.

Description

L-carnitine recovery process in wastewater generated in L-carnitine production process
Technical Field
The invention relates to the field of L-carnitine wastewater recovery processes, in particular to a L-carnitine recovery process in wastewater generated in an L-carnitine production process.
Background
L-carnitine was first extracted and separated from muscle, and later research found that L-carnitine is an essential substance for human body. L-carnitine is the only carrier for transferring fatty acid to cell mitochondria and can promote the beta-oxidation of fatty acid;
the waste water produced in the production process of the L-carnitine has higher external treatment cost and contains more recyclable materials, and the L-carnitine in the L-carnitine waste water is recovered, so that the COD (chemical oxygen demand) of the waste water can be reduced, the waste water treatment is facilitated, and the economic value is higher.
Disclosure of Invention
The invention provides a process for recovering L-carnitine in wastewater generated in the production process of L-carnitine, which solves the problems of L-carnitine resource waste and environmental pollution caused by the discharge of the existing wastewater containing L-carnitine.
In order to achieve the purpose, the invention adopts the following technical scheme:
the process for recycling the L-carnitine in the wastewater generated in the L-carnitine production process comprises the following steps of:
s1, adjusting the pH value of L-carnitine production wastewater to 6-7;
s2, after the resin is washed for multiple times, filling the resin into a chromatographic column by a wet method, and activating the resin by hydrochloric acid and a sodium hydroxide solution in sequence;
s3, cleaning the activated resin for multiple times until the activated resin is neutral;
s4, adsorbing the L-carnitine production wastewater by using resin;
and S5, resolving the resin after the L-carnitine is adsorbed, and separating the L-carnitine from the resin for recycling.
As a preferred technical scheme of the invention, the resin is macroporous cation exchange resin, the mass fraction of the hydrochloric acid solution used for activating the resin is 2-4%, and the mass fraction of the sodium hydroxide solution is 2-4%.
As a preferred technical scheme of the invention, the volume ratio of hydrochloric acid and sodium hydroxide solution used for resin activation to resin volume is 2.
As a preferred technical scheme of the invention, the effluent liquid after the resolution of the L-carnitine can be added into the L-carnitine production process for recycling.
As a preferred technical scheme of the invention, the invention also comprises process equipment, wherein the process equipment comprises a cylinder mould mechanism and a spraying mechanism;
the net cage mechanism comprises: the two ends of the inner sleeve are fixedly connected with baffle plates, a tubular metal screen plate is fixedly connected between the baffle plates, resin particles are filled among the metal screen plate, the inner sleeve and the baffle plates, a diversion shell is sleeved outside the cylinder mould mechanism, the two ends of the diversion shell are both fixedly provided with a bracket, and the baffle plates at the two ends of the cylinder mould mechanism are rotatably connected with the diversion shell and the bracket through short shafts;
the spraying mechanism comprises: be located the blower inlet bottom department between two sets of supports and be provided with the waste liquid case, just be provided with the second water pump in the waste liquid case, the outlet connection of second water pump has the hose, just the end-to-end connection of hose has the shower, the outer wall of shower is provided with the multiunit shower nozzle, just the both ends of shower are passed through the fixed plate and are connected with the blower inlet, and the shower is gone into to the waste liquid through the second water pump, sprays to the resin in the cylinder mould mechanism through the shower nozzle.
As a preferable technical scheme, the top end of the diversion shell is provided with a notch in a V shape, and the bottom end of the cylinder mould mechanism penetrates through the diversion shell.
As a preferred technical scheme of the present invention, the cover plate is made of the same material as the metal mesh plate, fixing lugs are arranged at two ends of the cover plate, the fixing lugs are fastened with the baffle plates through screws, supporting rods are fixedly connected between the baffle plates, and the supporting rods are distributed in an annular array with respect to the mesh cage mechanism.
According to a preferable technical scheme of the invention, three corners in the waste liquid tank are all arranged in a round angle mode, a first water pump is arranged at the right-angle corner of the waste liquid tank, and the first water pump drives waste liquid in the waste liquid tank to keep a circulating flowing state.
As a preferable technical scheme, two ends of the spray pipe are rotatably inserted into the fixing plate, and one end of the spray pipe is in threaded connection with the nut clamping fixing plate to fix the spray angle of the spray pipe and the spray head.
As a preferable technical scheme of the invention, the top end of the bracket is provided with a motor, and an output shaft of the motor is coaxially connected with the mesh cage mechanism.
The invention has the beneficial effects that:
1. the invention provides a process for recovering L-carnitine in L-carnitine wastewater, which adopts a chromatographic separation technology to activate resin and then adsorb L-carnitine production wastewater for multiple times, so that L-carnitine is adsorbed into the resin, effluent liquid is collected after the L-carnitine is resolved, and the effluent liquid can be added into the L-carnitine production process for recycling after further treatment;
2. this process equipment passes through the second water pump with the waste liquid through the hose pump in the shower, sprays through the cylinder mould mechanism that the shower nozzle descends, and the waste water flows back to the waste liquid incasement after the resin in the cylinder mould mechanism is absorbed the L-carnitine composition, and continuous circulation realizes the abundant recovery to L-carnitine in the waste liquid, and constantly rotates through motor drive cylinder mould mechanism for the resin granule is evenly sprayed the waste liquid, helps improving the efficiency that the resin granule absorbed L-carnitine.
In conclusion, the process equipment and the recovery process method solve the problems of resource waste and environmental pollution of the L-carnitine caused by the discharge of the existing L-carnitine-containing wastewater.
Drawings
FIG. 1 is a schematic view of the present invention.
Fig. 2 is a schematic structural diagram of another view angle of fig. 1 according to the present invention.
Fig. 3 is a structural sectional view of the present invention.
Fig. 4 is a schematic structural view of the netpen mechanism of the present invention.
Fig. 5 is a schematic structural view of the spray mechanism of the present invention.
Fig. 6 is a partially enlarged view showing an assembly structure of the nozzle tube and the fixing plate according to the present invention.
Reference numbers in the figures: 1. a guide shell; 2. a cylinder mould mechanism; 201. an inner sleeve; 202. a baffle plate; 203. a support bar; 204. a metal mesh plate; 205. a cover plate; 206. fixing the lug; 207. a screw; 208. a motor; 3. a support; 4. a waste liquid tank; 401. round corners; 402. a first water pump; 5. a second water pump; 501. a shower pipe; 502. a spray head; 503. a fixing plate; 504. a hose; 505. and a nut.
Detailed Description
The technical scheme of the invention is clearly and completely described in the following with reference to the accompanying drawings. In the description of the present invention, it should be noted that the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", etc., indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, and are only for convenience of description and simplicity of description, but do not indicate or imply that the device or element being referred to must have a particular orientation, be constructed and operated in a particular orientation, and thus, should not be construed as limiting the present invention. Moreover, the terms "first," "second," and "third" are used for descriptive purposes only and are not to be construed as indicating or implying a relative importance.
In the description of the present invention, it should be noted that, unless otherwise explicitly specified or limited, the terms "mounted," "connected," and "connected" are to be construed broadly, e.g., as meaning either a fixed connection, a removable connection, or an integral connection; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.
Referring to fig. 1-6, a process for recovering l-carnitine in wastewater from l-carnitine production process comprises a process flow, wherein the process flow is a mode of firstly resin adsorption and then separation recovery, the l-carnitine is recycled, and the process comprises the following steps:
s1, adjusting the pH value of L-carnitine production wastewater to 6-7;
s2, after the resin is washed for multiple times, the resin is filled into a chromatographic column by a wet method and is transferred into the chromatographic column, and hydrochloric acid and a sodium hydroxide solution are sequentially used for activation;
s3, cleaning the activated resin for multiple times until the activated resin is neutral;
s4, adsorbing the L-carnitine production wastewater by using resin;
and S5, resolving the resin after the L-carnitine is adsorbed, and separating the L-carnitine from the resin for recycling.
The resin is macroporous cation exchange resin, the mass fraction of hydrochloric acid solution used for activating the resin is 2-4%, the mass fraction of sodium hydroxide solution is 2-4%, the volume ratio of hydrochloric acid used for activating the resin to sodium hydroxide solution to the resin is 2-1, the flow rate is controlled in the process of resin adsorption, the volume of a water sample flowing through a chromatographic column per hour is 2-4 times of the volume of the resin, the solution used for resin analysis is sodium hydroxide or ammonia water, and the effluent liquid after L-carnitine analysis can be added into the L-carnitine production process for recycling.
A process unit for recovering L-carnitine in the wastewater generated in the L-carnitine production process comprises a net cage mechanism 2 and a spraying mechanism;
referring to fig. 3 and 4, the netpen mechanism 2: the two ends of the inner sleeve 201 are fixedly connected with baffle plates 202, a tubular metal screen plate 204 is fixedly connected among the baffle plates 202, resin particles are filled among the metal screen plate 204, the inner sleeve 201 and the baffle plates 202, the diversion shell 1 is sleeved outside the cylinder mould mechanism 2, the two ends of the diversion shell 1 are both fixedly provided with a support 3, and the baffle plates 202 at the two ends of the cylinder mould mechanism 2 are rotatably connected with the diversion shell 1 and the support 3 through short shafts; the top of support 3 is provided with motor 208, and motor 208 output shaft and cylinder mould mechanism 2 coaxial coupling, loads the resin through cylinder mould mechanism 2 for adsorb recovery waste liquid levogyration carnitine composition in spraying, constantly rotatory through motor 208 drive cylinder mould mechanism 2, make the resin granule evenly spray the waste liquid, help improving the efficiency that the resin granule absorbed levogyration carnitine.
Referring to fig. 2, 5 and 6, the spray mechanism: a waste liquid tank 4 is arranged at the bottom end of the diversion shell 1 between the two groups of supports 3, a second water pump 5 is arranged in the waste liquid tank 4, a water outlet of the second water pump 5 is connected with a hose 504, the tail end of the hose 504 is connected with a spray pipe 501, the outer wall of the spray pipe 501 is provided with a plurality of groups of spray heads 502, two ends of the spray pipe 501 are connected with the diversion shell 1 through fixing plates 503, waste liquid is pumped into the spray pipe 501 through the second water pump 5, and resin in the cylinder mould mechanism 2 is sprayed through the spray heads 502.
Referring to fig. 1, the top of blower inlet housing 1 is the notch that has seted up in the V-arrangement, and blower inlet housing 1 is run through to the bottom of cylinder mould mechanism 2, and the waste liquid that appears when the design of wide-mouthed can prevent to spray splashes to the outside.
The cover plate 205 and the metal mesh plate 204 are made of the same material, the two ends of the cover plate 205 are provided with fixing lugs 206, the fixing lugs 206 and the baffle plates 202 are fastened through screws 207, the support rods 203 are fixedly connected between the baffle plates 202, and the support rods 203 are distributed in an annular array relative to the netpen mechanism 2.
Referring to the setting that three corner in the waste liquid case 4 of picture all is fillet 401, and waste liquid case 4 is located right angle corner and is provided with first water pump 402, and waste liquid keeps the circulation flow state in the first water pump 402 drive waste liquid case 4, and first water pump 402 draws the waste liquid from the bottom and spouts along 4 lateral walls of waste liquid case for the waste liquid flows along the lateral wall circulation of waste liquid case 4, thereby avoids second water pump 5 can only take out local waste liquid in the waste liquid case 4.
Two ends of the spray pipe 501 are rotatably inserted into the fixing plate 503, and one end of the spray pipe 501 is in threaded connection with a nut 505 for clamping the fixing plate 503, so as to fix the spray angle of the spray pipe 501 and the spray head 502.
The working principle of the process equipment for recovering the L-carnitine from the L-carnitine wastewater is as follows:
the method comprises the following steps of pouring waste liquid for producing the L-carnitine into a waste liquid tank 4, sucking the waste liquid from the bottom by a first water pump 402 and spraying the waste liquid along the side wall of the waste liquid tank 4, enabling the waste liquid to circularly flow along the side wall of the waste liquid tank 4, so that the situation that the second water pump 5 can only pump partial waste liquid in the waste liquid tank 4 is avoided, pumping the waste liquid into a spray pipe 501 through a hose 504 by the second water pump 5, spraying the waste liquid through a mesh cage mechanism 2 which is downwards placed by a spray head 502, enabling the waste water to flow back into the waste liquid tank 4 after the L-carnitine components are absorbed by resin in the mesh cage mechanism 2, and continuously circulating to realize the full recovery of the L-carnitine in the waste liquid;
the spraying angle of the spray head 502 can be adjusted, and the nut 505 can be screwed after the spray head 502 and the spray pipe 501 are deflected by unscrewing the nut 505;
resin feeding and discharging of the cylinder mould mechanism 2: during the resin feeding, the cover plate 205 in the net cage mechanism 2 is rotated to the top through the motor 208, the screw 207 is disassembled, the cover plate 205 is disassembled, resin particles can be filled in the net cage mechanism 2, after the waste liquid is circularly filtered, the waste liquid box 4 is removed, the resin recovery box is moved to the net cage mechanism 2 to be placed, the cover plate 205 is disassembled in the same mode during the resin feeding, the cover plate 205 is rotated to the orientation to be placed through the motor 208, and the resin particles in the net cage mechanism 2 are poured in the recovery box.
Example (b):
a process for recovering L-carnitine in L-carnitine wastewater adopts a method of resin adsorption and then separation recovery, and comprises the following steps:
s1, taking 200ml of L-carnitine production wastewater discharged by a certain manufacturer, adjusting the pH value to 6-7, and measuring the concentration of the L-carnitine in the wastewater to be 5mg/g;
s2, measuring 100ml of WZ-613 resin, placing the resin in a 250ml beaker, washing the resin for multiple times, and transferring the resin to a chromatographic column by adopting wet column packing. Measuring 200ml 2% HCl solution, and adding dropwise into the chromatographic column within 40min while controlling the dropping speed. Adding 200ml of 2% NaOH solution dropwise into the chromatographic column, controlling the dropwise adding speed, and completing dropwise adding within 40 min;
s3, washing the resin with distilled water until the pH of an effluent liquid is 6-7;
and S4, dropwise adding 200ml of L-carnitine production wastewater into the chromatographic column at a dropping speed of 1 second/drop, collecting an effluent, and measuring the concentration of the L-carnitine in the effluent to be 3.7mg/g.
The above is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, without departing from the principle of the present invention, several improvements and modifications may be made, which should also be regarded as the protection scope of the present invention, and other parts of the present invention which are not described in detail belong to the prior art, and therefore are not described herein again, and finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.

Claims (10)

1. The process for recycling the L-carnitine in the wastewater generated in the L-carnitine production process is characterized by comprising the following steps of:
s1, adjusting the pH value of L-carnitine production wastewater to 6-7;
s2, after the resin is washed for multiple times, the resin is filled into a chromatographic column by a wet method and is transferred into the chromatographic column, and hydrochloric acid and a sodium hydroxide solution are sequentially used for activation;
s3, cleaning the activated resin for multiple times until the activated resin is neutral;
s4, adsorbing the L-carnitine production wastewater by using resin;
and S5, resolving the resin after the L-carnitine is adsorbed, and separating and recycling the L-carnitine from the resin.
2. The process of claim 1, wherein the resin used is macroporous cation exchange resin, the mass fraction of the hydrochloric acid solution used for resin activation is 2-4%, and the mass fraction of the sodium hydroxide solution is 2-4%.
3. The process of claim 1, wherein the volume ratio of hydrochloric acid to sodium hydroxide solution used for resin activation to resin is 2.
4. The process for recycling the L-carnitine in the wastewater generated in the L-carnitine production process of claim 1, wherein the eluate after the L-carnitine is resolved can be added into the L-carnitine production process for recycling.
5. The L-carnitine recycling process in the waste water of the L-carnitine production process according to claim 1, further comprising process equipment, wherein the process equipment comprises a cylinder mould mechanism (2) and a spraying mechanism;
the cylinder mould mechanism (2): the two ends of the inner sleeve (201) are fixedly connected with baffle plates (202), a tubular metal screen plate (204) is fixedly connected between the baffle plates (202), resin particles are filled among the metal screen plate (204), the inner sleeve (201) and the baffle plates (202), a diversion shell (1) is sleeved outside the cylinder mould mechanism (2), supports (3) are fixedly arranged at the two ends of the diversion shell (1), and the baffle plates (202) at the two ends of the cylinder mould mechanism (2) are rotatably connected with the diversion shell (1) and the supports (3) through short shafts;
the spraying mechanism comprises: be located dome (1) bottom department between two sets of supports (3) and be provided with waste liquid case (4), just be provided with second water pump (5) in waste liquid case (4), the outlet connection of second water pump (5) has hose (504), just the end-to-end connection of hose (504) has shower (501), the outer wall of shower (501) is provided with multiunit shower nozzle (502), just the both ends of shower (501) are passed through fixed plate (503) and are connected with dome (1), and shower (501) are gone into to the waste liquid pump through second water pump (5), sprays to the resin in cylinder mould mechanism (2) through shower nozzle (502).
6. The process for recovering L-carnitine in the waste water from the L-carnitine production process according to claim 5, wherein the top end of the diversion shell (1) is notched in a V shape, and the bottom end of the cylinder mould mechanism (2) penetrates through the diversion shell (1).
7. The L-carnitine recycling process according to claim 5, wherein said cover plate (205) is made of the same material as the metal mesh plate (204), fixing lugs (206) are disposed at both ends of said cover plate (205), said fixing lugs (206) are fastened to the baffle plates (202) by screws (207), support rods (203) are fixedly connected between said baffle plates (202), and said support rods (203) are distributed in a circular array with respect to the cylinder mould mechanism (2).
8. The L-carnitine recycling process according to claim 5, wherein said three corners of said waste liquid tank (4) are rounded (401), said waste liquid tank (4) is provided with a first water pump (402) at the right corner, said first water pump (402) drives the waste liquid in the waste liquid tank (4) to keep circulating flow.
9. The L-carnitine recycling process according to claim 5, wherein two ends of said spraying pipe (501) are rotatably inserted into a fixing plate (503), and a nut (505) is screwed into one end of said spraying pipe (501) to clamp said fixing plate (503), so as to fix the spraying angle of said spraying pipe (501) and said spraying head (502).
10. The L-carnitine recycling process according to claim 5, wherein a motor (208) is disposed at the top end of the bracket (3), and the output shaft of the motor (208) is coaxially connected to the cylinder mould mechanism (2).
CN202211238275.XA 2022-10-11 2022-10-11 L-carnitine recovery process in wastewater generated in L-carnitine production process Pending CN115650873A (en)

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Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN211570173U (en) * 2019-08-23 2020-09-25 天津晟瑞通市政工程有限公司 Resin adds fill steady flow spray set
CN213202436U (en) * 2020-09-09 2021-05-14 盈祥过滤设备(上海)有限公司 Novel resin filtering and purifying device
CN113979589A (en) * 2021-11-30 2022-01-28 范小松 Heavy metal wastewater treatment device based on resin adsorption and use method thereof
CN114105357A (en) * 2021-11-18 2022-03-01 广州兰德环保资源科技有限公司 Method for recovering L-carnitine from pharmaceutical wastewater
CN215940825U (en) * 2021-09-18 2022-03-04 吴巧巧 Terpene resin particle washing equipment
CN216512968U (en) * 2021-12-27 2022-05-13 广州兰德环保资源科技有限公司 Resin cleaning device for recycling pharmaceutical wastewater
CN216711748U (en) * 2021-12-27 2022-06-10 广州兰德环保资源科技有限公司 Resin adsorption device for extracting L-carnitine from pharmaceutical wastewater
CN114853209A (en) * 2022-04-27 2022-08-05 安徽永昌新材料有限公司 High-safety resin wastewater treatment device and treatment method thereof
CN217350837U (en) * 2022-07-01 2022-09-02 四川泰一美特科技有限公司 Cyanide-removing resin ion exchanger for cyanide ion-containing wastewater treatment

Patent Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN211570173U (en) * 2019-08-23 2020-09-25 天津晟瑞通市政工程有限公司 Resin adds fill steady flow spray set
CN213202436U (en) * 2020-09-09 2021-05-14 盈祥过滤设备(上海)有限公司 Novel resin filtering and purifying device
CN215940825U (en) * 2021-09-18 2022-03-04 吴巧巧 Terpene resin particle washing equipment
CN114105357A (en) * 2021-11-18 2022-03-01 广州兰德环保资源科技有限公司 Method for recovering L-carnitine from pharmaceutical wastewater
CN113979589A (en) * 2021-11-30 2022-01-28 范小松 Heavy metal wastewater treatment device based on resin adsorption and use method thereof
CN216512968U (en) * 2021-12-27 2022-05-13 广州兰德环保资源科技有限公司 Resin cleaning device for recycling pharmaceutical wastewater
CN216711748U (en) * 2021-12-27 2022-06-10 广州兰德环保资源科技有限公司 Resin adsorption device for extracting L-carnitine from pharmaceutical wastewater
CN114853209A (en) * 2022-04-27 2022-08-05 安徽永昌新材料有限公司 High-safety resin wastewater treatment device and treatment method thereof
CN217350837U (en) * 2022-07-01 2022-09-02 四川泰一美特科技有限公司 Cyanide-removing resin ion exchanger for cyanide ion-containing wastewater treatment

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