CN114084928B - Wastewater treatment method for accurately separating organic phase and water phase in preparation of L-idose - Google Patents
Wastewater treatment method for accurately separating organic phase and water phase in preparation of L-idose Download PDFInfo
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- 239000012074 organic phase Substances 0.000 title claims abstract description 243
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 74
- 239000012071 phase Substances 0.000 title claims abstract description 52
- WQZGKKKJIJFFOK-ZNVMLXAYSA-N L-idopyranose Chemical compound OC[C@@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-ZNVMLXAYSA-N 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 238000004065 wastewater treatment Methods 0.000 title claims abstract description 12
- 239000007788 liquid Substances 0.000 claims abstract description 174
- 239000002351 wastewater Substances 0.000 claims abstract description 160
- 238000000034 method Methods 0.000 claims abstract description 32
- 230000008859 change Effects 0.000 claims abstract description 29
- 238000001514 detection method Methods 0.000 claims abstract description 29
- 238000011282 treatment Methods 0.000 claims abstract description 29
- 238000000605 extraction Methods 0.000 claims abstract description 20
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 14
- 230000007246 mechanism Effects 0.000 claims description 27
- 239000008346 aqueous phase Substances 0.000 claims description 21
- 238000005259 measurement Methods 0.000 claims description 12
- 238000000926 separation method Methods 0.000 claims description 11
- 230000008569 process Effects 0.000 claims description 4
- 230000001502 supplementing effect Effects 0.000 claims description 4
- 238000003860 storage Methods 0.000 claims description 2
- 230000009286 beneficial effect Effects 0.000 abstract description 3
- 238000004064 recycling Methods 0.000 abstract description 3
- 238000005516 engineering process Methods 0.000 abstract description 2
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 29
- 239000000243 solution Substances 0.000 description 16
- 230000005540 biological transmission Effects 0.000 description 12
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 9
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 8
- 239000012044 organic layer Substances 0.000 description 7
- 238000003756 stirring Methods 0.000 description 7
- 239000000047 product Substances 0.000 description 6
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 5
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical class [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 239000008213 purified water Substances 0.000 description 4
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 4
- YYROPELSRYBVMQ-UHFFFAOYSA-N 4-toluenesulfonyl chloride Chemical compound CC1=CC=C(S(Cl)(=O)=O)C=C1 YYROPELSRYBVMQ-UHFFFAOYSA-N 0.000 description 3
- WFDIJRYMOXRFFG-UHFFFAOYSA-N Acetic anhydride Chemical compound CC(=O)OC(C)=O WFDIJRYMOXRFFG-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000003729 cation exchange resin Substances 0.000 description 3
- -1 compound salts Chemical class 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 229910052938 sodium sulfate Inorganic materials 0.000 description 3
- 235000011152 sodium sulphate Nutrition 0.000 description 3
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 239000000706 filtrate Substances 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 230000005484 gravity Effects 0.000 description 2
- 238000009434 installation Methods 0.000 description 2
- 238000012544 monitoring process Methods 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000011780 sodium chloride Substances 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- BGGCXQKYCBBHAH-OZRXBMAMSA-N (1r)-1-[(3ar,5r,6s,6ar)-6-hydroxy-2,2-dimethyl-3a,5,6,6a-tetrahydrofuro[2,3-d][1,3]dioxol-5-yl]ethane-1,2-diol Chemical compound O1[C@H]([C@H](O)CO)[C@H](O)[C@H]2OC(C)(C)O[C@H]21 BGGCXQKYCBBHAH-OZRXBMAMSA-N 0.000 description 1
- XVMSFILGAMDHEY-UHFFFAOYSA-N 6-(4-aminophenyl)sulfonylpyridin-3-amine Chemical compound C1=CC(N)=CC=C1S(=O)(=O)C1=CC=C(N)C=N1 XVMSFILGAMDHEY-UHFFFAOYSA-N 0.000 description 1
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical class [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 239000003957 anion exchange resin Substances 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 239000012043 crude product Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000011221 initial treatment Methods 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 150000003254 radicals Chemical class 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- WXMKPNITSTVMEF-UHFFFAOYSA-M sodium benzoate Chemical compound [Na+].[O-]C(=O)C1=CC=CC=C1 WXMKPNITSTVMEF-UHFFFAOYSA-M 0.000 description 1
- 239000004299 sodium benzoate Substances 0.000 description 1
- 235000010234 sodium benzoate Nutrition 0.000 description 1
- 235000017557 sodium bicarbonate Nutrition 0.000 description 1
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 1
- 229910001415 sodium ion Inorganic materials 0.000 description 1
- SUBJHSREKVAVAR-UHFFFAOYSA-N sodium;methanol;methanolate Chemical compound [Na+].OC.[O-]C SUBJHSREKVAVAR-UHFFFAOYSA-N 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/26—Treatment of water, waste water, or sewage by extraction
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/40—Devices for separating or removing fatty or oily substances or similar floating material
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/34—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32
- C02F2103/36—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32 from the manufacture of organic compounds
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Organic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Extraction Or Liquid Replacement (AREA)
Abstract
The invention belongs to the technical field of water treatment, and relates to a wastewater treatment method for accurately separating an organic phase and a water phase in the preparation of L-idose, which comprises the following steps: the method comprises the following steps: extracting; step two: judging whether an organic phase exists or not; if an organic phase is detected; calculating whether the liquid level of the organic phase is within the range of a preset liquid level H; step three: if the organic phase liquid level is detected to be larger than the preset liquid level H, calculating to obtain a rough numerical value L of the organic phase liquid level through a microwave signal detection device, and calculating the corresponding organic phase volume; step four: adding an extracting agent into the treatment solution in the pre-clear solution collecting box for extraction until no organic phase is detected in the treatment solution; according to the invention, whether the wastewater generated by preparing the L-idose contains an organic phase or not is automatically monitored by a detection mode of combining an image recognition technology and a microwave signal change curve, the organic phase in the wastewater is fully extracted by calculating the volume of the organic phase, and the productivity can be improved by 15-35%; meanwhile, the treated wastewater is more beneficial to recycling.
Description
Technical Field
The invention belongs to the field of water treatment, and particularly relates to a wastewater treatment method for accurately separating an organic phase and a water phase in the preparation of L-idose.
Background
In the existing large-scale production process for synthesizing the L-idose and the derivatives thereof, organic phases and water phases in a solution need to be separated in multiple links; the water phase after the organic phase is separated becomes waste water to be discharged; however; in the prior art, when an organic phase and an aqueous phase in a solution are separated, a boundary line between the aqueous phase and the organic phase is observed only through an observation mirror; when the discharged phase reaches the boundary of the two phases, the discharge is stopped; the operation needs manual monitoring, however, when the manual monitoring is carried out, a large error exists, so that a large amount of organic phases exist in finally discharged wastewater; therefore, a method capable of accurately separating an organic phase and an aqueous phase in wastewater is required; can reduce the pollution of waste water discharge to the environment while repeatedly recycling effective substances.
Disclosure of Invention
The invention provides a wastewater treatment method for accurately separating an organic phase and a water phase in the preparation of L-idose, and aims to solve the problems in the prior art.
The invention is realized by adopting the following technical scheme:
the wastewater treatment method for accurately separating the organic phase and the water phase in the preparation of the L-idose comprises the following steps:
the method comprises the following steps: taking wastewater generated in the L-idose preparation process, and introducing the wastewater into a wastewater collection box; when the liquid level of the wastewater in the wastewater collection tank reaches a set value; adding an extracting agent into the wastewater in the wastewater collection box for extraction;
step two: standing and layering the wastewater treated in the first step, and detecting whether an organic phase exists in the wastewater through an image scanning mechanism; if the organic phase is not detected, introducing the wastewater into a clear liquid collecting box for storage; if an organic phase is detected; calculating whether the liquid level of the organic phase is within a preset liquid level H range, if so, directly obtaining the volume of the organic phase, automatically guiding the section of organic phase with the corresponding volume into an organic phase collecting box, automatically guiding the remaining section of aqueous phase into a pre-clear liquid collecting box to realize accurate separation, and entering the fourth step;
step three: if the organic phase liquid level is detected to be larger than the preset liquid level H, calculating to obtain a rough numerical value L of the organic phase liquid level through a microwave signal detection device, and calculating the corresponding organic phase volume; automatically guiding the section of organic phase with the corresponding volume into an organic phase collecting box, detecting by an image scanning mechanism to obtain an accurate numerical value of the liquid level of the organic phase in the residual wastewater and the corresponding volume of the organic phase, automatically guiding the section of organic phase into the organic phase collecting box, automatically guiding the remaining section of aqueous phase into a pre-clear liquid collecting box to achieve accurate separation, and entering the fourth step;
step four: adding an extracting agent into the treatment solution in the pre-clear solution collecting box for extraction until no organic phase is detected in the treatment solution; during the treatment, the organic phase was introduced into an organic phase collection box and finally the aqueous phase containing no organic phase was introduced into a clear liquid collection box.
Preferably, the method for detecting whether the organic phase exists in the wastewater through the image scanning mechanism and calculating whether the liquid level of the organic phase is within the range of the preset liquid level H in the second step comprises the following steps:
a1: taking sample wastewater with a water phase and an organic phase separated; taking a picture by taking the boundary of the water phase and the organic phase as a central line through an image scanning mechanism to obtain a sample wastewater image; converting the sample wastewater image into a standard gray image to obtain a gray value G1 of a water phase region in the standard gray image; and gray value G2 of the organic phase region in the standard gray image;
a2: taking wastewater to be detected, obtaining a local image with the height of H from the boundary of an organic phase to the extension direction of the organic phase through an image scanning mechanism, and converting the obtained image into an actual gray image; randomly taking a plurality of pixel points which are transversely arranged in parallel at the top edge of the actual gray image, taking the pixel points in the row as a first base line, and downwards obtaining the gray value Gn of each pixel point in the actual gray image with the same width as the first base line, so as to obtain the gray value Gn of each pixel point in the detection area with the width as the width of the first base line and the height as H;
due to different extracting agents; the relative positions of the organic and aqueous phases are different; when the organic phase is at the bottom of the water phase, the boundary of the organic phase is the lowest surface of the wastewater; the extending direction of the organic phase is from bottom to top; when the organic phase is on the top of the water phase, the boundary of the organic phase is the highest surface of the wastewater; the extending direction of the organic phase is from top to bottom.
A3: comparing and searching whether a boundary line exists in the detection area; the dividing line divides the gray value of the pixel point in the area into two parts with difference values; the method for searching the boundary comprises the following steps: comparing the gray value Gn of each pixel point in the detection area in the actual gray image with G1 and G2; if the Gn-G1 is less than or equal to 10, replacing the gray value Gn in the actual gray image with a gray value G1, and judging as a water-phase gray value; similarly, if the value | Gn-G2| is less than or equal to 10, replacing the gray value Gn with a gray value G2, and determining the gray value Gn as an organic phase gray value; after the gray value replacement of each pixel point in the area is finished, the gray value of the pixel point in the actual gray image is divided into two parts, namely G1 and G2, and the joint of G1 and G2 is a boundary line;
if a boundary line exists, the organic phase exists in the wastewater, and the liquid level of the organic phase is within the range of the preset liquid level H; at this time, only the distance from the boundary line to the bottom edge of the actual gray image needs to be calculated; the finally measured organic phase liquid level value in the wastewater is obtained;
if no boundary exists, judging the gray value of the image, and if the gray value of the image is the same as the gray value of the water phase area of the standard gray image; judging that no organic phase exists in the wastewater;
if the image gray value is the same as the gray value of the organic phase region of the standard gray image; the liquid level of the organic phase in the wastewater is judged to be greater than the preset liquid level H.
Preferably, the method for calculating the rough value L of the organic phase liquid level and calculating the corresponding organic phase volume by the microwave signal detection device in the third step comprises the following substeps:
b1: taking sample wastewater with layered water phase and organic phase, wherein the organic phase in the sample wastewater accounts for more than 50%; taking the central point of the wastewater as a reference point; a plurality of standard measuring surfaces extending outwards are arranged in a ring shape; taking a plurality of points on the standard measuring surface, and measuring the microwave signal change parameters of each point through a microwave signal detection device to form a standard microwave signal change curve corresponding to each standard measuring surface;
b2: gradually reducing the liquid level of the organic phase in the step B1 by taking 3-5cm as a section, and simultaneously supplementing water with the same volume as the reduced organic phase so as to ensure that the liquid level of the wastewater is the same as the initial liquid level; after each section is lowered and water is supplemented, standing to enable the water phase and the organic phase to be layered; measuring the standard microwave signal change curve of each standard measurement surface corresponding to the sample wastewater after each section is reduced according to the method in the step B1; thus obtaining a standard microwave signal change curve corresponding to organic phases with different liquid levels in the wastewater;
b3: taking the central point of the wastewater to be treated as a reference point; a plurality of actual measuring surfaces extending outwards are arranged in a ring shape; measuring microwave signal variation parameters by taking a plurality of points on the actual measurement surface to form an actual microwave signal variation curve corresponding to each actual measurement surface;
b4: taking an actual microwave signal change curve of each actual measurement surface; comparing the measured data with a standard microwave signal change curve corresponding to a standard measuring surface; obtaining an organic phase liquid level corresponding to the actual measuring surface; if the actual microwave signal variation curve of the actual measurement surface is between the standard microwave signal variation curves of two adjacent sections; the organic phase liquid level of the actual measuring surface is judged as the lower section liquid level of two adjacent liquid levels; for example; aiming at a certain measuring surface, after comparison, the actual microwave signal change curve is between the standard microwave signal change curves corresponding to the organic phase liquid level of 30cm and the organic phase liquid level of 25 cm; at the moment, the liquid level of the organic phase of the measuring surface in the wastewater is determined to be 25cm, so that the organic phase in the wastewater can be accurately and cleanly removed in the subsequent image recognition, and after all actual organic phase liquid level values corresponding to all measuring surfaces of the wastewater are obtained, the value with the largest quantity in the actual organic phase liquid level values is taken, namely the rough numerical value L of the obtained organic phase liquid level;
b5: the organic phase volume T = SL is calculated from the cross-sectional area S of the container collecting the waste water and the rough value L of the level of the organic phase obtained.
Preferably, the specific method for adding the extractant into the treatment solution in the pre-clear solution collection box in the fourth step for extraction until no organic phase is detected in the treatment solution comprises the following substeps:
c1: adding an extracting agent into the treatment liquid of the pre-clear liquid collecting box for extraction; standing; detecting whether an organic phase exists in the treatment liquid or not; if an organic phase is detected, separating the organic phase from the aqueous phase; specifically, in this link, the method for separating the organic phase from the aqueous phase is as follows: detecting whether an organic phase exists in the treatment liquid through an image scanning mechanism; if an organic phase is detected; calculating whether the liquid level of the organic phase is within a preset liquid level H range, if so, directly obtaining the volume of the organic phase and automatically guiding the section of organic phase with the corresponding volume into an organic phase collecting box to complete the separation of the organic phase from the water phase; if the organic phase liquid level is detected to be larger than the preset liquid level H, calculating to obtain a rough numerical value L of the organic phase liquid level through a microwave signal detection device, and calculating the corresponding organic phase volume; after automatically guiding the section of organic phase with the corresponding volume into the organic phase collection box, detecting by an image scanning mechanism to obtain an accurate numerical value of the liquid level of the organic phase in the residual wastewater and the corresponding volume of the organic phase, and automatically guiding the section of organic phase into the organic phase collection box to complete the separation of the organic phase from the water phase;
c2: continuously adding an extracting agent into the treated liquid after the treatment of the step C1 for extraction; at the moment, water with the same volume as the reduced organic phase is supplemented and reduced at the same time, so that the liquid level of the waste water is the same as the initial liquid level; standing; detecting whether an organic phase exists in the treatment liquid or not; if an organic phase is detected, separating the organic phase from the aqueous phase; the method of separation is the same as in step C1;
c3: step C2 is repeated until no organic phase is detected in the treatment solution.
Preferably, the image scanning mechanism is a CCD image scanning mechanism, and the wastewater collection box and the pre-clear liquid collection box have the same structure and both comprise box bodies; the upper end and the lower end of the box body are respectively provided with a transparent window; the bottom edge of the transparent window at the bottom is level with the lowest liquid level of the liquid in the tank body; the top edge of the top transparent window is level with the highest liquid level of the liquid in the tank body; the width and the height of the transparent window are both H; the outer part of the transparent window is provided with an installation shell; the installation shell is internally provided with the CCD image scanning mechanism, and the CCD image scanning mechanism comprises a first driving motor, a main driving gear, a driven driving gear, a rack and a CCD scanning head assembly; the shell of the first driving motor is fixed on the outer side of the right side wall of the mounting shell, and the output shaft of the first driving motor penetrates through the end part of the right side wall of the mounting shell to be fixed with the main transmission gear; the driven transmission gear is arranged right below the main transmission gear, the rack is in transmission connection with the main transmission gear and the driven transmission gear, and the CCD scanning head assembly is fixed on one side of the rack; the CCD scanning head assembly moves up and down between the top edge and the bottom edge of the transparent window to scan and obtain an image of liquid in the transparent window; the microwave signal detection device comprises a second driving motor, a shell of the second driving motor is fixed at the top of the box body, an output end of the second driving motor penetrates through the top of the box body and penetrates through the mounting column to extend into the mounting cavity, and two ends of an output shaft of the second driving motor are respectively connected with the inner wall of the mounting column through bearings; a first mounting plate and a second mounting plate which correspond to each other up and down are respectively fixed at the upper end part and the lower end part of an output shaft of the second driving motor, the lengths of the first mounting plate and the second mounting plate are slightly smaller than the radius of the box body, and a plurality of microwave emitters which are arranged at intervals are arranged on the bottom surface of the first mounting plate; the top surface of the second mounting plate is provided with a plurality of microwave receivers which are arranged at intervals and correspond to the microwave transmitters one by one, two side surfaces of the box body close to the top end are provided with liquid inlets, the bottom surface of the box body is connected with two liquid outlet pipelines, and the liquid outlet pipelines are both connected with flow meters and control valves; the flow rate Q is controlled by a flow meter and a control valve.
Compared with the prior art, the invention has the beneficial effects that:
according to the invention, whether the wastewater generated by preparing the L-idose contains an organic phase or not is automatically monitored by a detection mode of combining an image recognition technology and a microwave signal change curve, the organic phase in the wastewater is fully extracted by calculating the volume of the organic phase, and the productivity can be improved by 15-35%; meanwhile, the treated wastewater is more beneficial to recycling; the cost is saved, and the pollution to the environment is reduced.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.
FIG. 1 is a flow chart for precisely separating an organic phase and an aqueous phase in example 1 of the present invention;
FIG. 2 is a flow chart for precisely separating an organic phase and an aqueous phase in example 2 of the present invention;
FIG. 3 is a schematic view of the construction of the waste water collection tank of the present invention;
FIG. 4 is an enlarged schematic view of A of FIG. 3;
fig. 5 is a partial schematic view of the boundary of the converted actual gray-scale image.
Detailed Description
The following further describes embodiments of the present invention with reference to the drawings. It should be noted that the description of the embodiments is provided to help understanding of the present invention, but the present invention is not limited thereto. In addition, the technical features involved in the embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
In the present example, L-idose was prepared by the following steps;
s1: to prepare 1, 2-O-isopropylidene-3-O-acetyl-alpha-D-glucopyranose; specifically, the method comprises the following steps: adding 50kg of monoacetone glucose, 100L of dichloromethane and 50L of anhydrous pyridine into a reactor in sequence, cooling to 5 ℃ after stirring, dropwise adding 10L of acetic anhydride, heating to 25 ℃ after dropwise adding, cooling to below 10 ℃ after 7 hours of reaction, adding 100L of water into the reactor, stirring, standing, layering, and separating an organic layer; adjusting pH to 7-8 with saturated sodium bicarbonate, stirring for 0.5h, sequentially washing with water and saturated sodium chloride solution once respectively, wherein the total amount of organic layer is 58.34L, and the organic layer is dried with anhydrous sodium sulfate and then spin-dried to obtain yellowish-brown viscous liquid;
s2: taking the product obtained in the step S1 to prepare 1, 2-O-isopropylidene-3-O-acetyl-5, 6-di-O-p-toluenesulfonyl-alpha-D-glucopyranose; dissolving 30kg of the product prepared in S1 in 30L of pyridine, dropwise adding a mixed solution of 12kg of tosyl chloride and 70L of dichloromethane solution under an ice bath condition, adding 12L of water after the reaction is finished, stirring, and sequentially washing for a plurality of times by using 50L of 0.05mol/L sulfuric acid solution, 50L of 2mol/L sodium hydroxide solution and 50L of water; combining the organic phases; the total amount of the organic layer is 38.23L, the organic layer is dried by anhydrous sodium sulfate, filtered, the filtrate is evaporated to dryness to obtain a crude product, and white needle-shaped crystals are obtained after ethanol recrystallization;
s3: to prepare 1, 2-O-isopropylidene-3-O-acetyl-5, 6-di-O-benzoyl-beta-L-idose; adding the product obtained in the step S2 into 100-200LDMF dissolvent, adding 20-100kg of sodium benzoate, stirring at normal temperature for reacting for 2-4h, filtering, and concentrating to obtain 1, 2-O-isopropylidene-3-O-acetyl-5, 6-di-O-benzoyl-beta-L-idose;
s4: taking the product obtained in the step S3 to prepare 1, 2-O-isopropylidene-L-idose; adding 100-200L0.1mol/L sodium methoxide-methanol solution into a second half product collecting box, stirring at normal temperature for 30-90min, adding cation exchange resin to remove Na ions, filtering, and concentrating the filtrate under reduced pressure to obtain 1, 2-O-isopropylidene-L-idose;
s5: preparing L-idose, dissolving the product obtained in the step S4 in 0.5mol/L sulfuric acid aqueous solution, and stirring and refluxing at 110 ℃ for 5 h; stopping the reaction, standing at room temperature, and adding sodium bicarbonate powder to adjust the pH of the solution to be neutral; filtered and evaporated to dryness under reduced pressure, purified as DCM: CH (CH)3Separating with eluting agent OH 3:1, purifying, crystallizing, and vacuum drying to obtain L-idose.
In the process of preparing L-iduronide by the above method, the organic phase and the aqueous phase need to be separated in both step S1 and step S2; and step S1 will produce 100L of wastewater to be treated; step S2 is to generate 300L of wastewater to be treated; 50L of pyridine is remained in the wastewater generated in the step S1 besides the organic phase; a small amount of acetic acid and a small amount of sodium chloride; the waste water produced in step S2 contains a small amount of tosyl chloride salt and a small amount of sodium sulfate in addition to the organic phase.
The method is adopted to respectively treat the wastewater collected in the step S1 and the step S2;
example 1
Treating the wastewater generated in the step S1;
preparation before experiment:
taking a container for storing sample wastewater; the length, width and height are respectively as follows: 37cm by 30cm by 60 cm; adding purified water and the organic phase generated in the step S1 into the container in sequence, wherein the liquid level of the purified water is 20 cm; obtaining sample wastewater with a water phase and an organic phase separated from each other, wherein the liquid level of the organic phase is 30cm; at the moment, the organic phase in the sample wastewater accounts for 60 percent;
(1) obtaining and storing a standard gray level image; the specific method comprises the following steps: shooting by a CCD image scanning mechanism by taking the boundary of the water phase and the organic phase as a central line to obtain a sample wastewater image; converting the sample wastewater image into a standard gray image and storing the standard gray image; obtaining a gray value 224 of a water phase region in the standard gray image; the gray value of the organic phase region was 138;
(2) obtaining and storing standard microwave signal change curves corresponding to organic phases containing different liquid levels in the wastewater; the specific method comprises the following steps: b1: taking the central point of the sample wastewater as a reference point; 7 standard measuring surfaces which extend outwards and are spaced by 2cm are arranged in a ring shape; taking 10 measuring points on the standard measuring surface, and measuring the microwave signal change parameters of each point through a microwave signal detection device to form a standard microwave signal change curve corresponding to each standard measuring surface; b2: gradually reducing the liquid level of the organic phase in the step B1 by taking 3cm as a section, and simultaneously supplementing water with the same volume as the reduced organic phase so as to ensure that the liquid level of the wastewater is the same as the initial liquid level; after each section is lowered and water is supplemented, standing to enable the water phase and the organic phase to be layered; measuring the standard microwave signal change curve of each standard measurement surface corresponding to the sample wastewater after each section is reduced according to the method in the step B1; thus obtaining a standard microwave signal change curve corresponding to organic phases with different liquid levels in the wastewater;
as shown in fig. 1, the present embodiment provides a wastewater collection tank 100 and a pre-clear liquid collection tank 102, and the wastewater treatment method for accurately separating organic phase and aqueous phase in the preparation of L-idose comprises the following steps:
the method comprises the following steps: continuously introducing the wastewater generated in step S1 into a wastewater collection tank 100; the specification of the waste water collecting box is the same as that of a container for storing sample waste water; the length, width and height are respectively as follows: 37cm by 30cm by 60 cm; when the liquid level of the wastewater in the wastewater collection tank reaches 50cm, closing the liquid inlet valve, and adding dichloromethane into the wastewater collection tank for extraction;
step two: standing for layering, wherein the specific gravity of dichloromethane is greater than that of water, so that an organic phase is at the bottom of a water phase, a local image with the height of 10cm from the bottom of wastewater is obtained through a CCD image scanning mechanism, and the obtained image is converted into an actual gray image; taking any 50 pixels transversely arranged in parallel at the top edge of the actual gray image, taking the pixels in the row as a first base line, and downwards obtaining the gray value of each pixel in the actual gray image with the same width as the first base line, so as to obtain the actual gray value of each pixel in the detection area; when the gray value of each pixel point is obtained, the gray value of each pixel point and the gray value G1=224 of the water phase region in the standard gray image are obtained; comparing the gray value G2=138 of the organic phase region in the standard gray image; obtaining an actual gray image after the comparison; after the search is carried out, no boundary line exists in the area; and the gray value of the actual image is 138, the liquid level of the organic phase in the wastewater is higher than 10 cm;
step three: calculating to obtain a rough value L of the liquid level of the organic phase through a microwave signal detection device, and calculating the corresponding volume of the organic phase; taking the central point of the wastewater to be treated as a reference point; 7 actual measuring surfaces which extend outwards and are arranged in a ring shape and have an interval of 2 cm; taking 10 measuring points on the standard measuring surface to form an actual microwave signal change curve corresponding to each actual measuring surface; comparing with a standard microwave signal change curve; obtaining the liquid levels of 12, 9 and 12 corresponding to 7 actual measuring surfaces; judging the rough value L =9 of the liquid level of the organic phase of the wastewater to be treated; after automatically guiding the organic phase of the section with the corresponding volume into the organic phase collecting box, detecting the accurate numerical value of the liquid level of the organic phase in the residual wastewater and the corresponding volume of the organic phase through a CCD image scanning mechanism, and specifically: obtaining an actual gray image after conversion, and forming a boundary in the area after searching; the image size was 8cm by 10 cm; 302 pixels 378 pixels; the corresponding possible level L to a single pixel is 0.26 mm; the number of pixel points from the boundary to the lowest edge of the picture is N = 47; the distance of the boundary line from the lowest edge of the picture is S = LN =1.23 cm; the obtained organic phase liquid level is 1.23cm, the organic phase of the section is automatically led into an organic phase collection box 101, and the residual water phase of the section is automatically led into a pre-clear liquid collection box 102 to achieve accurate separation;
step four: wastewater continues to enter the wastewater collection tank 100; when the liquid level of the treatment liquid in the pre-clear liquid collecting box 102 reaches 50 cm; closing the liquid inlet of the pre-clear liquid collecting box; the specification of the pre-clear liquid collecting box is the same as that of the waste water collecting box; adding dichloromethane for extraction and layering; after standing, obtaining a local image with the height of 10cm from the bottom of the wastewater through a CCD image scanning mechanism, and converting the obtained image into an actual gray image; taking any 50 pixels transversely arranged in parallel at the top edge of the actual gray image, taking the pixels in the row as a first base line, and downwards obtaining the gray value of each pixel in the actual gray image with the same width as the first base line, so as to obtain the actual gray value of each pixel in the detection area; when the gray value of each pixel point is obtained, the gray value of each pixel point and the gray value G1=224 of the water phase region in the standard gray image are obtained; and gray value G2=138 of the organic phase region in the standard gray-scale image; obtaining an actual gray image after the comparison; after searching, a boundary is formed in the area; calculating the distance S between the boundary line and the bottom edge of the image; the image size was still 8cm by 10 cm; obtaining the number N =20 of pixel points from the boundary to the lowest edge of the picture; the distance between the boundary line and the lowest edge of the picture is S = LN =5.2 mm; then the volume of the organic phase is calculated and the organic phase with the corresponding volume is automatically led into the organic phase collecting box 101;
step five: continuously adding an extracting agent into the pre-clear liquid collecting box 102 for extraction; at the moment, water with the same volume as the reduced organic phase is supplemented and reduced at the same time, so that the liquid level of the waste water is the same as the initial liquid level; standing; obtaining a local image with the height of 10cm from the bottom of the wastewater through a CCD image scanning mechanism, and converting the obtained image into an actual gray image; taking any 50 pixels transversely arranged in parallel at the top edge of the actual gray image, taking the pixels in the row as a first base line, and downwards obtaining the gray value of each pixel in the actual gray image with the same width as the first base line, so as to obtain the actual gray value of each pixel in the detection area; when the gray value of each pixel point is obtained, the gray value of each pixel point and the gray value G1=224 of the water phase region in the standard gray image are obtained; and gray value G2=138 of the organic phase region in the standard gray-scale image; obtaining an actual gray image after the comparison; after the search is carried out, no boundary line exists in the area; the image gray scale value is 214; judging that no organic phase exists in the wastewater; leading the wastewater into a clear liquid collecting box 103;
step six: the steps one to five are repeated until the wastewater produced in the step S1 is processed.
Example 2
Firstly, treating the wastewater generated in the step S2;
preparation before experiment:
taking a container for storing sample wastewater; the length, width and height are respectively as follows: 37cm by 30cm by 60 cm; adding purified water and the organic phase generated in the step S2 into the container in sequence, wherein the liquid level of the purified water is 20 cm; obtaining sample wastewater with a water phase and an organic phase separated from each other, wherein the liquid level of the organic phase is 30cm; at the moment, the organic phase in the sample wastewater accounts for 60 percent;
(1) obtaining and storing a standard gray level image; the specific method comprises the following steps: shooting by a CCD image scanning mechanism by taking the boundary of the water phase and the organic phase as a central line to obtain a sample wastewater image; converting the sample wastewater image into a standard gray image and storing the standard gray image; obtaining a gray value of a water phase region in the standard gray image as 214; the gray value of the organic phase region is 162;
(2) obtaining and storing standard microwave signal change curves corresponding to organic phases containing different liquid levels in the wastewater; the specific method comprises the following steps: b1: taking the central point of the sample wastewater as a reference point; 7 standard measuring surfaces which extend outwards and are spaced by 2cm are arranged in a ring shape; taking 10 measuring points on the standard measuring surface, and measuring the microwave signal change parameters of each point through a microwave signal detection device to form a standard microwave signal change curve corresponding to each standard measuring surface; b2: gradually reducing the liquid level of the organic phase in the step B1 by taking 5cm as a section, and simultaneously supplementing water with the same volume as the reduced organic phase so as to ensure that the liquid level of the wastewater is the same as the initial liquid level; after each section is lowered and water is supplemented, standing to enable the water phase and the organic phase to be layered; measuring the standard microwave signal change curve of each standard measurement surface corresponding to the sample wastewater after each section is reduced according to the method in the step B1; thus obtaining a standard microwave signal change curve corresponding to organic phases with different liquid levels in the wastewater;
the embodiment is provided with a second wastewater collection box 200 and two pre-clear liquid collection boxes, including a first pre-clear liquid collection box 201 and a second pre-clear liquid collection box 202; the second wastewater collection box and the first pre-clear liquid collection box are arranged to remove most of organic components in the water phase; can guarantee that the organic component in the second in advance clear liquid collecting box gets rid of totally in the time of completion is collected to waste water collecting box and first in advance clear liquid collecting box, and the incessant water treatment that carries on of continuous on-line is fit for using under the great condition of waste water volume.
As shown in fig. 2, the wastewater treatment method for precisely separating an organic phase and an aqueous phase in the preparation of L-idose comprises the following steps:
the method comprises the following steps: continuously introducing the wastewater generated at step S2 into the second wastewater collection tank 200; the specification of the second wastewater collection box is the same as that of a container for storing sample wastewater;
the length, width and height are respectively as follows: 37cm by 30cm by 60 cm; when the liquid level of the wastewater in the second wastewater collection box 200 reaches 50cm, closing the liquid inlet valve, and adding dichloromethane into the wastewater collection box for extraction;
step two: standing for layering, wherein the specific gravity of dichloromethane is greater than that of water, so that an organic phase is at the bottom of a water phase, a local image with the height of 10cm from the bottom of wastewater is obtained through a CCD image scanning mechanism, and the obtained image is converted into an actual gray image; taking any 50 pixels transversely arranged in parallel at the top edge of the actual gray image, taking the pixels in the row as a first base line, and downwards obtaining the gray value of each pixel in the actual gray image with the same width as the first base line, so as to obtain the actual gray value of each pixel in the detection area; when the gray value of each pixel point is obtained, the gray value of each pixel point and the gray value G1=214 of the water phase region in the standard gray image are obtained; comparing the gray value G2=162 of the organic phase region in the standard gray image; obtaining an actual gray image after the comparison; after searching, a boundary is formed in the area; the image size was 8cm by 10 cm; 302 pixels 378 pixels; the corresponding possible level L to a single pixel is 0.26 mm; the number of pixel points from the boundary to the lowest edge of the picture is N = 125; the distance of the boundary line from the lowest edge of the picture is S = LN =3.25 cm; the obtained organic phase liquid level is 3.25cm, the organic phase at the section is automatically guided into the second organic phase collection box 203, and the residual water phase at the section is automatically guided into the first pre-clear liquid collection box 201 to achieve accurate separation;
step three: wastewater continues to enter the second wastewater collection tank 200; when the liquid level of the primary treatment liquid in the first pre-clear liquid collecting box 201 reaches 50 cm; closing the first pre-clear liquid collecting box to feed liquid; the specification of the first pre-clear liquid collecting box is the same as that of the waste water collecting box; adding dichloromethane for extraction and layering; after standing, obtaining a local image with the height of 10cm from the bottom of the wastewater through a CCD image scanning mechanism, and converting the obtained image into an actual gray image; taking any 50 pixels transversely arranged in parallel at the top edge of the actual gray image, taking the pixels in the row as a first base line, and downwards obtaining the gray value of each pixel in the actual gray image with the same width as the first base line, so as to obtain the actual gray value of each pixel in the detection area; when the gray value of each pixel point is obtained, the gray value of each pixel point and the gray value G1=214 of the water phase region in the standard gray image are obtained; and gray value G2=162 of the organic phase region in the standard gray-scale image; obtaining an actual gray image after the comparison; after searching, a boundary is formed in the area; calculating the distance S between the boundary line and the bottom edge of the image; the image size was still 8cm by 10 cm; obtaining the number N =39 of pixel points from the boundary to the lowest edge of the picture; the distance between the boundary line and the lowest edge of the picture is S = LN =1.131 cm; then the volume of the organic phase is calculated, the section of organic phase with the corresponding volume is automatically led into a second organic phase collecting box 203, and the rest section of water phase is automatically led into a second pre-clear liquid collecting box 202;
step four: the first pre-clear liquid collecting box 201 continues to feed liquid; the liquid level of the secondary treatment liquid in the second pre-clear liquid collecting box 202 reaches 50 cm; the feed liquid is closed, and the dichloromethane is continuously added into the secondary treatment liquid in the second pre-clear liquid collecting tank 202 for extraction; standing; after standing, obtaining a local image with the height of 10cm from the bottom of the wastewater through a CCD image scanning mechanism, and converting the obtained image into an actual gray image; taking any 50 pixels transversely arranged in parallel at the top edge of the actual gray image, taking the pixels in the row as a first base line, and downwards obtaining the gray value of each pixel in the actual gray image with the same width as the first base line, so as to obtain the actual gray value of each pixel in the detection area; when the gray value of each pixel point is obtained, the gray value of each pixel point and the gray value G1=214 of the water phase region in the standard gray image are obtained; and gray value G2=162 of the organic phase region in the standard gray-scale image; obtaining an actual gray image after the comparison; after searching, a boundary is formed in the area; the width and height of the image are 8cm x 10cm, and the number of pixel points from a boundary line to the lowest edge of the image is N = 15; the distance S = LN =0.39cm of the boundary line from the bottom edge of the image; obtaining the volume of the organic phase and automatically guiding the section of organic phase with the corresponding volume into the second organic phase collection box 203;
step five: continuously adding an extracting agent into the second pre-clear liquid collecting box 202 for extraction; at the moment, water with the same volume as the reduced organic phase is supplemented and reduced at the same time, so that the liquid level of the waste water is the same as the initial liquid level; standing; obtaining a local image with the height of 10cm from the bottom of the wastewater through a CCD image scanning mechanism, and converting the obtained image into an actual gray image; taking any 50 pixels transversely arranged in parallel at the top edge of the actual gray image, taking the pixels in the row as a first base line, and downwards obtaining the gray value of each pixel in the actual gray image with the same width as the first base line, so as to obtain the actual gray value of each pixel in the detection area; when the gray value of each pixel point is obtained, the gray value of each pixel point and the gray value G1=214 of the water phase region in the standard gray image are obtained; and gray value G2=162 of the organic phase region in the standard gray-scale image; obtaining an actual gray image after the comparison; after the search is carried out, no boundary line exists in the area; the image grey value is not 214; judging that no organic phase exists in the wastewater; leading the wastewater into a clear liquid collecting box 204;
step six: repeating the steps one to one until the wastewater generated in the step S2 is processed.
Results of the experiment
The total amount of the organic layer obtained after the precision extraction in example 1 and the organic layer obtained after the precision extraction in example 2 is shown in table 1:
| kind of waste water | Raw wastewater volume/L | Accurately separating to obtain total amount of organic phase/L | The separation rate of organic phase in wastewater% |
| Step S1 produces |
100 | 17.65 | 17.65 |
| Step S2 produces |
300 | 18.78 | 6.26 |
As can be seen from table 1, in the process of preparing L-iduronide, the wastewater generated in step S1 and the wastewater generated in step S2 were treated and discharged, and the organic phase yield was increased by 30% and 16% compared to direct discharge; and when the amount of wastewater is great, can increase multistage processing case according to actual conditions, improve waste water treatment efficiency.
Meanwhile, after the wastewater generated in the step S1 and the wastewater generated in the step S2 are subjected to accurate separation of an organic phase and a water phase, clear liquids are collected, and the collected clear liquids contain a small amount of acetic acid, a small amount of sodium chloride, sodium sulfate and compound salts; acetic acid, sodium sulfate and compound salts can be removed through the adsorption column assembly; the adsorption column component can comprise an anion-cation exchange resin tank, wherein the cation exchange resin is macroporous weak acid type cation resin, and the anion exchange resin is strong base type anion resin with bicarbonate radical as free radical; or other adsorbing materials including activated carbon and the like, and pyridine in the clear liquid, wherein the pyridine can be recovered by distillation.
In embodiment 1, the structures of the wastewater collection tank 100, the pre-clear liquid collection tank 102, the second wastewater collection tank 200, the first pre-clear liquid collection tank 201, and the second pre-clear liquid collection tank 202 in embodiment 2 are the same, and as shown in fig. 3 to 5, each comprises a tank body; the lower end of the box body is provided with a transparent window 200; the bottom edge of the transparent window is level with the lowest liquid level of the liquid in the tank body; the width and the height of the transparent window are both 10 cm; a mounting shell 201 is arranged outside the transparent window, and a CCD image scanning mechanism is arranged in the mounting shell and comprises a first driving motor 202, a main driving gear 203, a driven driving gear 204, a rack 205 and a CCD scanning head assembly 206; the shell of the first driving motor is fixed on the outer side of the right side wall of the mounting shell, and the output shaft of the first driving motor penetrates through the end part of the right side wall of the mounting shell to be fixed with the main transmission gear; the driven transmission gear is arranged right below the main transmission gear, the rack is in transmission connection with the main transmission gear and the driven transmission gear, and the CCD scanning head assembly is fixed on one side of the rack; the CCD scanning head assembly moves up and down between the top edge and the bottom edge of the transparent window to scan and obtain an image of liquid in the transparent window; the width of the CCD scanning head assembly is slightly smaller than that of the transparent window, so that the two side edges of the obtained image do not comprise the side wall image of the box body, and the data processing amount of the image is reduced; the first driving motor is a servo driving motor, and the CCD scanning head assembly can be accurately controlled to move up and down between the top edge and the bottom edge of the transparent window by setting output parameters of an output shaft of the servo driving motor to obtain an image to be shot. The microwave signal detection device comprises a second driving motor 303, a shell of the second driving motor is fixed at the top of the box body, an output end of the second driving motor penetrates through the top of the box body and penetrates through the mounting column to extend into the mounting cavity, and two ends of an output shaft of the second driving motor are respectively connected with the inner wall of the mounting column through bearings 304; a first mounting plate 305 and a second mounting plate 306 which correspond to each other up and down are respectively fixed at the upper end part and the lower end part of an output shaft of the second driving motor, the length of the first mounting plate and the length of the second mounting plate are slightly smaller than the radius of the box body, and a plurality of microwave emitters which are arranged at intervals are arranged on the bottom surface of the first mounting plate; and the top surface of the second mounting plate is provided with a plurality of microwave receivers which are arranged at intervals and correspond to the microwave transmitters one by one. Two side surfaces of the box body close to the top end are provided with liquid inlets 307, the bottom surface is connected with two liquid outlet pipelines 308, and the liquid outlet pipelines are connected with a flow meter 309 and a control valve 310; the flow rate Q is controlled by a flow meter and a control valve. The second driving motor drives an output shaft of the second driving motor to rotate; the first mounting plate and the second mounting plate rotate synchronously with the first mounting plate and the second mounting plate, and a plurality of microwave transmitters and microwave receivers which are arranged at intervals on the first mounting plate and the second mounting plate respectively correspond to each measuring surface; the microwave signal change parameters of each measuring surface can be measured by rotating for one circle; the operation is convenient.
The embodiments of the present invention have been described in detail with reference to the accompanying drawings, but the present invention is not limited to the described embodiments. It will be apparent to those skilled in the art that various changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, and the scope of protection is still within the scope of the invention.
Claims (3)
1. The wastewater treatment method for accurately separating the organic phase and the water phase in the preparation of the L-idose is characterized by comprising the following steps of: the method comprises the following steps:
the method comprises the following steps: taking wastewater generated in the L-idose preparation process, and introducing the wastewater into a wastewater collection box; when the liquid level of the wastewater in the wastewater collection tank reaches a set value; adding an extracting agent into the wastewater in the wastewater collection box for extraction;
step two: standing and layering the wastewater treated in the first step, and detecting whether an organic phase exists in the wastewater through an image scanning mechanism; if the organic phase is not detected, introducing the wastewater into a clear liquid collecting box for storage; if an organic phase is detected; calculating whether the liquid level of the organic phase is within a preset liquid level H range, if so, directly obtaining the volume of the organic phase, automatically guiding the section of organic phase with the corresponding volume into an organic phase collecting box, automatically guiding the remaining section of aqueous phase into a pre-clear liquid collecting box to realize accurate separation, and entering the fourth step;
step three: if the organic phase liquid level is detected to be larger than the preset liquid level H, calculating to obtain a rough numerical value L of the organic phase liquid level through a microwave signal detection device, and calculating the corresponding organic phase volume; automatically guiding the section of organic phase with the corresponding volume into an organic phase collecting box, detecting by an image scanning mechanism to obtain an accurate numerical value of the liquid level of the organic phase in the residual wastewater and the corresponding volume of the organic phase, automatically guiding the section of organic phase into the organic phase collecting box, automatically guiding the remaining section of aqueous phase into a pre-clear liquid collecting box to achieve accurate separation, and entering the fourth step;
step four: adding an extracting agent into the treatment solution in the pre-clear solution collecting box for extraction until no organic phase is detected in the treatment solution; in the treatment process, the organic phase is introduced into an organic phase collecting box, and finally the water phase without the organic phase is introduced into a clear liquid collecting box;
in the second step, a method for detecting whether an organic phase exists in the wastewater or not and calculating whether the liquid level of the organic phase is within the range of the preset liquid level H or not through an image scanning mechanism comprises the following steps:
a1: taking sample wastewater with a water phase and an organic phase separated; taking a picture by taking the boundary of the water phase and the organic phase as a central line through an image scanning mechanism to obtain a sample wastewater image; converting the sample wastewater image into a standard gray image to obtain a gray value G1 of a water phase region in the standard gray image; and gray value G2 of the organic phase region in the standard gray image;
a2: taking wastewater to be detected, obtaining a local image with the height of H from the boundary of an organic phase to the extension direction of the organic phase through an image scanning mechanism, and converting the obtained image into an actual gray image; randomly taking a plurality of pixel points which are transversely arranged in parallel at the top edge of the actual gray image, taking the pixel points in the row as a first base line, and downwards obtaining the gray value Gn of each pixel point in the actual gray image with the same width as the first base line, so as to obtain the gray value Gn of each pixel point in the detection area with the width as the width of the first base line and the height as H;
a3: comparing and searching whether a boundary line exists in the detection area; the dividing line divides the gray value of the pixel point in the area into two parts with difference values; if a boundary line exists, the organic phase exists in the wastewater, and the liquid level of the organic phase is within the range of the preset liquid level H; at this time, only the distance from the boundary line to the bottom edge of the actual gray image needs to be calculated; the finally measured organic phase liquid level value in the wastewater is obtained; if no boundary exists, judging the gray value of the image, and if the gray value of the image is the same as the gray value of the water phase area of the standard gray image; judging that no organic phase exists in the wastewater; if the image gray value is the same as the gray value of the organic phase region of the standard gray image; judging that the liquid level of the organic phase in the wastewater is greater than a preset liquid level H;
in the third step, the rough value L of the liquid level of the organic phase is calculated by the microwave signal detection device, and the method for calculating the corresponding volume of the organic phase comprises the following substeps:
b1: taking sample wastewater with layered water phase and organic phase, wherein the organic phase in the sample wastewater accounts for more than 50%; taking the central point of the wastewater as a reference point; a plurality of standard measuring surfaces extending outwards are arranged in a ring shape; taking a plurality of points on the standard measuring surface, and measuring the microwave signal change parameters of each point through a microwave signal detection device to form a standard microwave signal change curve corresponding to each standard measuring surface;
b2: gradually reducing the liquid level of the organic phase in the step B1 by taking 3-5cm as a section, and simultaneously supplementing water with the same volume as the reduced organic phase so as to ensure that the liquid level of the wastewater is the same as the initial liquid level; after each section is lowered and water is supplemented, standing to enable the water phase and the organic phase to be layered; measuring the standard microwave signal change curve of each standard measurement surface corresponding to the sample wastewater after each section is reduced according to the method in the step B1; thus obtaining a standard microwave signal change curve corresponding to organic phases with different liquid levels in the wastewater;
b3: taking the central point of the wastewater to be treated as a reference point; a plurality of actual measuring surfaces extending outwards are arranged in a ring shape; measuring microwave signal variation parameters by taking a plurality of points on the actual measurement surface to form an actual microwave signal variation curve corresponding to each actual measurement surface;
b4: taking an actual microwave signal change curve of each actual measurement surface; comparing the measured data with a standard microwave signal change curve corresponding to a standard measuring surface; obtaining an organic phase liquid level corresponding to the actual measuring surface; if the actual microwave signal variation curve of the actual measurement surface is between the standard microwave signal variation curves of two adjacent sections; the organic phase liquid level of the actual measuring surface is judged as the lower section liquid level of two adjacent liquid levels; obtaining the maximum value in the actual organic phase liquid level values after obtaining all the actual organic phase liquid level values corresponding to all the measuring surfaces of the wastewater, namely obtaining a rough value L of the obtained organic phase liquid level;
b5: the organic phase volume T = SL is calculated from the cross-sectional area S of the container collecting the waste water and the rough value L of the level of the organic phase obtained.
2. The wastewater treatment method for precisely separating an organic phase and an aqueous phase in the preparation of L-idose according to claim 1, characterized in that: the method for comparing and searching whether a boundary exists in the detection area comprises the following steps: comparing the gray value Gn of each pixel point in the detection area in the actual gray image with G1 and G2; if the Gn-G1 is less than or equal to 10, replacing the gray value Gn in the actual gray image with a gray value G1, and judging as a water-phase gray value; similarly, if the value | Gn-G2| is less than or equal to 10, replacing the gray value Gn with a gray value G2, and determining the gray value Gn as an organic phase gray value; therefore, after the gray value replacement of each pixel point in the region is completed, the gray value of the pixel point in the actual gray image is divided into two parts, namely G1 and G2, and the junction of G1 and G2 is the boundary.
3. The wastewater treatment method for precisely separating an organic phase and an aqueous phase in the preparation of L-idose according to claim 1, characterized in that: in the fourth step, a specific method for adding an extracting agent into the treatment solution in the pre-clear solution collecting box for extraction until no organic phase is detected in the treatment solution comprises the following substeps:
c1: adding an extracting agent into the treatment liquid of the pre-clear liquid collecting box for extraction; standing; detecting whether an organic phase exists in the treatment liquid or not; if an organic phase is detected, separating the organic phase from the aqueous phase;
c2: continuously adding an extracting agent into the treated liquid after the treatment of the step C1 for extraction; at the moment, water with the same volume as the reduced organic phase is supplemented and reduced at the same time, so that the liquid level of the waste water is the same as the initial liquid level; standing; detecting whether an organic phase exists in the treatment liquid or not; if an organic phase is detected, separating the organic phase from the aqueous phase;
c3: step C2 is repeated until no organic phase is detected in the treatment solution.
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