CN114198994B - Crystallization drying method capable of accurately monitoring water content in biological sugar preparation process - Google Patents
Crystallization drying method capable of accurately monitoring water content in biological sugar preparation process Download PDFInfo
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- 238000001035 drying Methods 0.000 title claims abstract description 165
- 238000002425 crystallisation Methods 0.000 title claims abstract description 52
- 230000008025 crystallization Effects 0.000 title claims abstract description 51
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 20
- 238000012544 monitoring process Methods 0.000 title claims abstract description 13
- 238000002360 preparation method Methods 0.000 title abstract description 6
- 239000013078 crystal Substances 0.000 claims abstract description 319
- 230000008859 change Effects 0.000 claims abstract description 58
- 238000000034 method Methods 0.000 claims abstract description 42
- 238000001514 detection method Methods 0.000 claims abstract description 37
- 239000002904 solvent Substances 0.000 claims abstract description 32
- 230000008569 process Effects 0.000 claims abstract description 19
- 238000007689 inspection Methods 0.000 claims abstract description 9
- 238000005070 sampling Methods 0.000 claims abstract description 9
- 238000007599 discharging Methods 0.000 claims abstract description 3
- 230000007246 mechanism Effects 0.000 claims description 27
- 239000007788 liquid Substances 0.000 claims description 24
- 239000012488 sample solution Substances 0.000 claims description 22
- 238000012935 Averaging Methods 0.000 claims description 16
- 238000005259 measurement Methods 0.000 claims description 16
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 14
- 238000001556 precipitation Methods 0.000 claims description 13
- 238000001704 evaporation Methods 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 12
- 230000008020 evaporation Effects 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 9
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 7
- 235000011152 sodium sulphate Nutrition 0.000 claims description 7
- 230000018044 dehydration Effects 0.000 claims description 6
- 238000006297 dehydration reaction Methods 0.000 claims description 6
- 230000001502 supplementing effect Effects 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 238000005516 engineering process Methods 0.000 abstract description 2
- 238000001953 recrystallisation Methods 0.000 abstract description 2
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 39
- 239000000047 product Substances 0.000 description 19
- WQZGKKKJIJFFOK-QTVWNMPRSA-N D-mannopyranose Chemical compound OC[C@H]1OC(O)[C@@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-QTVWNMPRSA-N 0.000 description 13
- 239000012295 chemical reaction liquid Substances 0.000 description 9
- 238000003860 storage Methods 0.000 description 9
- 230000005540 biological transmission Effects 0.000 description 8
- 238000006243 chemical reaction Methods 0.000 description 7
- 239000012074 organic phase Substances 0.000 description 7
- WFDIJRYMOXRFFG-UHFFFAOYSA-N Acetic anhydride Chemical compound CC(=O)OC(C)=O WFDIJRYMOXRFFG-UHFFFAOYSA-N 0.000 description 6
- 239000011229 interlayer Substances 0.000 description 6
- 239000000523 sample Substances 0.000 description 6
- 208000005156 Dehydration Diseases 0.000 description 5
- 238000003756 stirring Methods 0.000 description 5
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 4
- ZIQPQYFSSSHQBP-UHFFFAOYSA-N acetyl 2,3-dihydroxypropanoate Chemical compound CC(=O)OC(=O)C(O)CO ZIQPQYFSSSHQBP-UHFFFAOYSA-N 0.000 description 4
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 description 4
- 238000009434 installation Methods 0.000 description 4
- 230000002194 synthesizing effect Effects 0.000 description 4
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 3
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 description 3
- 239000000945 filler Substances 0.000 description 3
- 239000000706 filtrate Substances 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 239000012141 concentrate Substances 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000012530 fluid Substances 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 238000003672 processing method Methods 0.000 description 2
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- JOXIMZWYDAKGHI-UHFFFAOYSA-N toluene-4-sulfonic acid Chemical compound CC1=CC=C(S(O)(=O)=O)C=C1 JOXIMZWYDAKGHI-UHFFFAOYSA-N 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- YOWQWFMSQCOSBA-UHFFFAOYSA-N 2-methoxypropene Chemical compound COC(C)=C YOWQWFMSQCOSBA-UHFFFAOYSA-N 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 239000012468 concentrated sample Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 239000005457 ice water Substances 0.000 description 1
- 239000013067 intermediate product Substances 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
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Images
Classifications
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F26—DRYING
- F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
- F26B9/00—Machines or apparatus for drying solid materials or objects at rest or with only local agitation; Domestic airing cupboards
- F26B9/06—Machines or apparatus for drying solid materials or objects at rest or with only local agitation; Domestic airing cupboards in stationary drums or chambers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D9/0018—Evaporation of components of the mixture to be separated
- B01D9/0031—Evaporation of components of the mixture to be separated by heating
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D9/0059—General arrangements of crystallisation plant, e.g. flow sheets
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D9/0063—Control or regulation
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F26—DRYING
- F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
- F26B25/00—Details of general application not covered by group F26B21/00 or F26B23/00
- F26B25/22—Controlling the drying process in dependence on liquid content of solid materials or objects
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D2009/0086—Processes or apparatus therefor
Abstract
The invention belongs to the technical field of drying, and relates to a crystallization drying method capable of accurately monitoring water content in a biological sugar preparation process, which comprises the following steps: the method comprises the following steps: forming a primary concentrated solution; step two: judging whether the moisture contained in the primary concentrated solution is in a preset range or not; step three: judging whether the volume of the crystal precipitated by recrystallization is full; if all crystals are separated out, discharging the solvent, and entering the step four; step four: drying the crystals in the crystallization box, and performing online sampling inspection on the dried crystals; according to the invention, through a detection mode of combining an image recognition technology and a microwave signal change curve, the crystallization drying of the biosaccharide in the biosaccharide equipment process is automatically monitored, the moisture content of the dried biosaccharide is accurately controlled, and the recrystallized crystals are accurately separated out in the drying process, so that the loss in the production process is greatly reduced, and the yield can be improved by 15% -25%.
Description
Technical Field
The invention belongs to the technical field of drying, and particularly relates to a crystallization drying method capable of accurately monitoring water content in a biological sugar preparation process.
Background
In each process of synthetic biological sugar, need carry out crystallization drying with intermediate product or final product, obtain semi-manufactured goods or finished product, and current crystallization drying method relies on the manual work to monitor mostly, if concentrated back crystallization process, cool off when having the micro-crystallization generally, this moment, just need the staff to pay close attention to the crystallization condition in real time, secondly, biological sugar's the most sample that adopts in the artifical certain time quantum production process of gathering of the degree of dryness detection, then detect, the defect that this method exists lies in: the sample is in the process of taking and transporting, or absorb external moisture, and the volume of taking the sample at every turn is not big, consequently, by external absorbing moisture, to whole model, its influence is great, leads to measuring precision to receive great influence to influence whole process production, influence the production efficiency of producing the line then.
Disclosure of Invention
The invention provides a crystallization drying method capable of accurately monitoring the water content in the process of preparing biological sugar, which aims to solve the problems in the prior art.
The invention is realized by adopting the following technical scheme:
the crystallization drying method capable of accurately monitoring the water content in the process of preparing the biological sugar comprises the following steps:
the method comprises the following steps: adding anhydrous sodium sulphate into the biological sugar treatment liquid for preliminary dehydration; primarily concentrating the primarily dehydrated treatment solution by a surface evaporation concentration method to form a primary concentrated solution;
step two: judging whether the moisture contained in the primary concentrated solution is in a preset range or not through a microwave signal detection device, and if so, entering a third step; if the current time is not within the preset range, repeating the operation of the first step;
step three: continuously heating the primary concentrated solution, and detecting whether crystals are separated out or not by an image scanning mechanism; if no crystal precipitation is detected, continuing heating; if crystal precipitation is detected; cooling and crystallizing the concentrated solution; after crystallization is finished, adding a solvent into the crystals for dissolving, then recrystallizing, ultrasonically crushing the recrystallized crystals, standing, calculating by using a microwave signal detection device to obtain a rough volume V of the precipitated crystals, calculating by using an image scanning mechanism to obtain an accurate volume V' of the precipitated crystals, and judging whether all the volumes of the precipitated crystals are recrystallized; if all crystals are separated out, discharging the solvent, and entering the step four;
step four: drying the crystals in the crystallization box, and performing online sampling inspection on the dried crystals; inputting the crystals meeting the dryness into a finished product library, and inputting the crystals not meeting the standard into a circulating drying area for circulating drying until the dryness meets the requirement.
Preferably, the microwave moisture measuring device comprises a conveying platform, wherein a crystal inlet and a crystal outlet are arranged on the conveying platform along the conveying direction of the crystal, and a first forming module and a first microwave moisture measuring instrument are sequentially arranged between the crystal inlet and the crystal outlet; the circulating drying area comprises a first drying channel connected with a crystal outlet of the conveying platform, a first drying box, a second forming module and a second microwave moisture measuring instrument are sequentially arranged on the first drying channel along the crystal conveying direction, the circulating drying area further comprises a second drying channel connected with the first drying channel, and the outlet of the second drying channel is connected with the crystal inlet of the conveying platform; a second drying box is arranged on the second drying channel; the tail end of the conveying platform and the tail end of the first drying channel are qualified product output ends; a first crystal pushing device is arranged on the opposite side of the inlet of the first drying channel; pushing the crystals from the conveying platform into the first drying channel through the first crystal pushing device; a second crystal pushing device is arranged on the side of the outlet of the first drying channel; pushing the crystals from the first drying channel into a second drying channel through the second crystal pushing device; a third crystal pushing device is arranged on the side of the outlet of the second drying channel, and the crystals output by the second drying channel are pushed to the inlet end of the conveying platform through the third crystal pushing device;
preferably, the method for performing online spot check comprises the following steps:
e1: placing the crystal on a conveying platform, conveying the crystal through the conveying platform, and forming through a first forming module in the conveying process; the cross section of the formed crystal is a rectangle with a set thickness;
e2: the molded crystal passes through a first microwave moisture measuring instrument which detects the moisture content of the crystal at regular time, and if the moisture content of the crystal is within a set range, the crystal is conveyed to a finished product warehouse through a qualified product output end; otherwise, stopping conveying the crystals in the crystallization box to the conveying platform; meanwhile, the drying time or temperature in the crystallization box is adjusted; conveying the crystals on the conveying platform to a circulating drying area for circulating drying until the crystals meet the requirement of dryness;
e3: and when the dryness of the crystals on the conveying platform meets the requirement, continuously conveying the crystals in the crystallization box to the conveying platform, and repeating the steps E1 to E3 to finish the online sampling inspection of the crystals.
Preferably, the circulation drying method comprises the following steps:
f1: the conveying platform outputs crystals with unqualified water content through detection, and the crystals are conveyed to the first drying channel through the first crystal pushing device;
f2: the crystal entering the first drying channel sequentially passes through the first drying box, the second forming module and the second microwave moisture measuring instrument; after detection, if the water content of the crystal is in a set range, outputting the crystal from a qualified product output end on the first drying channel; otherwise, the second crystal pushing device conveys the crystals to a second drying channel;
f3: the crystals entering the second drying channel pass through a drying box arranged on the second drying channel; after drying, the third crystal pushing device conveys the crystal to the conveying platform, and the steps F1 to F3 are repeated; and (5) finishing drying.
Preferably, the method for determining whether the water content in the preliminary concentrated solution is within the preset range by the microwave signal detection device in the second step comprises the following steps:
a1: taking a certain volume of standard concentrated solution, and taking a central point of the standard concentrated solution 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, measuring microwave signal change parameters of each point through a microwave signal detection device, averaging the microwave signal change parameters of each point obtained on each standard measuring surface, and forming a standard microwave signal change curve by each average value;
a2: taking the primary concentrated solution to be treated with the same volume as the standard concentrated solution, and taking the central point of the primary concentrated solution 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 at a plurality of points on an actual measuring surface, averaging the microwave signal variation parameters of the points obtained on each actual measuring surface, and forming an actual microwave signal variation curve by each average value;
a3: and comparing the actual microwave signal change curve with the standard microwave signal change curve, judging whether the actual microwave signal change curve is within the threshold value of the standard microwave signal change curve, if so, judging that the moisture content of the preliminary concentrated solution to be treated is within the set range, otherwise, judging that the moisture content is not within the set range.
Preferably, the method for detecting whether crystal precipitation exists or not by the image scanning mechanism in the third step comprises the following substeps:
b1: taking a sample solution with layered concentrated solution and crystals; shooting by an image scanning mechanism by taking the boundary of the concentrated solution and the crystal as a central line to obtain a sample solution image; converting the sample solution image into a standard gray image to obtain a gray value G1 of a concentrated solution area in the standard gray image; and gray value G2 of the crystal region in the standard gray image;
b2: taking a concentrated solution to be detected, obtaining a local image with the height of H from the bottom to the top 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 bottom edge of the actual gray image, taking the row of pixel points as a first base line, and upwards obtaining the gray value Gn of each pixel point in the actual gray image with the same width as the first base line, wherein the width of the gray value Gn is the width of the first base line, and the height of the gray value Gn is H;
b3: and comparing the gray value Gn of each pixel point in the detection area with the gray value G1 of the concentrated liquid area in the standard gray image and the gray value G2 of the crystal area in the standard gray image, if the gray value Gn of each pixel point in the detection area is within the threshold value of the gray value G2 of the crystal area in the standard gray image, determining that crystal precipitation exists, otherwise, determining that no crystal precipitation exists.
Preferably, the method for calculating the rough volume V of the precipitated crystal by the microwave signal detection device in the third step comprises the following steps:
c1: taking a sample solution with layered solvent and crystals; at the moment, the volume of the crystals in the sample solution accounts for more than 50 percent; taking the central point of the sample solution as a reference point; a plurality of second standard measuring surfaces extending outwards are arranged in a ring shape; taking a plurality of points on the second standard measuring surface, measuring the microwave signal change parameters of each point through a microwave signal detection device, averaging the microwave signal change parameters of each point obtained on each standard measuring surface, and forming a second standard microwave signal change curve according to each average value;
c2: gradually reducing the height of the crystal in the step C1 by taking 4-8cm as a section, and simultaneously supplementing a solvent with the same volume as the reduced crystal so as to ensure that the liquid level of the solution is the same as the initial liquid level; after each section is reduced and the solvent is supplemented, standing to ensure that the solvent and the crystal are layered; measuring a second standard microwave signal change curve at the moment, and repeating the steps to obtain a second standard microwave signal change curve corresponding to different crystals;
c3: taking the central point of the solution 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 at a plurality of points on the actual measurement surface, averaging the microwave signal variation parameters of the points obtained on each actual measurement surface, and forming a second actual microwave signal variation curve by each average value;
c4: comparing the second actual microwave signal change curve with each second standard microwave signal change curve; obtaining the actual height of the crystal contained at the moment; if the second actual microwave signal variation curve is between the second standard microwave signal variation curves of two adjacent sections; the actual height of the crystals contained at this time is determined as the lower section height of two adjacent heights; thus, a rough height S of the precipitated crystal is obtained, and then a rough volume V of the precipitated crystal is calculated.
For example; after comparison, the second actual microwave signal change curve is between the second standard microwave signal change curves corresponding to the crystal height of 30cm and the crystal height of 25 cm; at this time, the height of the crystal contained in the solution is determined to be 25cm, so that the crystal in the solution can be accurately obtained in the subsequent image recognition;
preferably, the method for calculating the precise volume V' of the precipitated crystal by the image scanning mechanism in the third step comprises the following steps:
d1: taking a second sample solution with the solvent and the crystals layered; shooting by an image scanning mechanism by taking the boundary of the solvent and the crystal as a central line to obtain a second sample solution image; converting the second sample solution image into a second standard gray image to obtain a gray value G3 of a solvent area in the second standard gray image; and gray value G4 of the crystal region in the standard gray image;
d2: moving the image scanning mechanism to the rough height H' obtained in the step C4, obtaining a local image with the height of H1 from bottom to top, and converting the obtained image into a second actual gray image; taking a plurality of pixel points which are horizontally arranged in parallel at the bottom edge of the second actual gray image, taking the row of pixel points as a second base line, and upwards obtaining the gray value Gn' of each pixel point in the actual gray image with the same width as the second base line, wherein the width of the second base line is obtained, and the height of the second base line is H1;
d3: searching a boundary; comparing the gray value Gn' of each pixel point in the detection area in the second actual gray image with G3 and G4; if the Gn '-G3 is less than or equal to 10, replacing the gray value Gn' in the second actual gray image with a gray value G3, and determining as a solvent gray value; similarly, if the value | Gn '-G4 | is less than or equal to 10, replacing the gray value Gn' with a gray value G4, and determining the gray value as a crystal gray value; after the gray value replacement of each pixel point in the area is completed, the gray value of the pixel point in the second actual gray image is divided into two parts, namely G3 and G4, and the joint of G3 and G4 is a boundary; calculating the distance from the boundary line to the bottom edge of the image, namely the height S' of the residual crystal; the total height of the precipitated crystals is SS = S + S', and if the amount of the precipitated crystals at this time is within the threshold value of the initial value, it indicates that the crystals are completely precipitated, otherwise, the crystals are not completely precipitated.
Compared with the prior art, the invention has the beneficial effects that:
according to the invention, through a detection mode of combining an image recognition technology and a microwave signal change curve, the crystallization drying of the biosaccharide in the biosaccharide equipment process is automatically monitored, the moisture content of the dried biosaccharide is accurately controlled, and the recrystallized crystals are accurately separated out in the drying process, so that the loss in the production process is greatly reduced, and the yield can be improved by 15% -25%.
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 schematic view of the structure of a drying apparatus according to the present invention;
FIG. 2 is an enlarged schematic view of A of FIG. 1;
FIG. 3 is a schematic view of the image scanning mechanism of FIG. 2;
FIG. 4 is a schematic view of the configuration of the circulation drying zone of the present invention;
fig. 5 is a schematic structural view of a first forming module according to the present invention.
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 example, the biosaccharide triacetyl monoacetone mannose was prepared by the following steps;
s1: and (3) synthesizing an intermediate material 2, 3.4, 6-diacetone mannose: putting mannose and dimethylformamide into a reaction kettle, stirring and dissolving at normal temperature, adding p-toluenesulfonic acid, dropwise adding 2-methoxypropene, uniformly mixing, stirring, tracking a thin layer, slowly adding triethylamine, ice water and dichloromethane, dehydrating and filtering a uniformly mixed reaction solution by using anhydrous sodium sulphate, concentrating a filtrate for at least crystallization, cooling to 5 ℃ for crystallization, adding ethyl acetate for recrystallization, and obtaining 2, 3.4, 6-diacetone mannose crystals;
s2: and (3) synthesizing an intermediate material of acetyldiacetone mannose: adding pyridine into a reaction kettle, adding crystal 2, 3.4, 6-diacetone mannose, cooling to 15 ℃, slowly adding acetic anhydride, stirring at normal temperature after dropwise adding, adding ethyl acetate for dissolving, adding water for extraction and washing, dehydrating and filtering organic phase anhydrous sodium sulphate, concentrating filtrate, refrigerating for crystallization, recrystallizing, and drying to obtain a dry product of the acetylacetone mannose;
s3: and (3) synthesizing an intermediate material of acetyl-monoacetone mannose: stirring and dissolving the reactant acetyldiacetone mannose in methanol, cooling by introducing a refrigerating fluid, slowly adding dilute sulfuric acid, after the reaction liquid becomes clear gradually after becoming turbid initially, neutralizing by using calcium carbonate after the reaction is finished, stirring the reaction liquid at normal temperature, filtering and concentrating the reaction liquid to crystallize, recrystallizing, and centrifuging the dried mother liquor to obtain the dry product acetyldiacetone mannose;
s4: and (3) synthesizing triacetyl monoacetone mannose: adding pyridine into the reactant acetyl monoacetone mannose in the previous step, introducing refrigerating fluid for freezing, slowly adding acetic anhydride, controlling the temperature below 25 ℃, keeping the temperature, adding ethyl acetate for dissolving, adding water for extracting and washing, dehydrating an organic phase by using anhydrous sodium sulphate, concentrating a filtrate at 60 ℃ to crystallize, cooling, crystallizing in a tank, heating the ethyl acetate until the ethyl acetate is completely dissolved, cooling to normal temperature, and recrystallizing to obtain a dry product of the triacetyl monoacetone mannose.
The reaction liquid generated in the step S1, the organic phase generated in the step S2, the reaction liquid generated in the step S3 and the organic phase generated in the step S4 can be processed by adopting the method;
example 1
Processing the reaction solution generated in step S1;
preparation before experiment:
(1) taking a container; the length, width and height are respectively as follows: 30cm 60 cm; adding a sample concentrated solution of a reaction solution generated in the step S1 concentrated in advance into a container, wherein the central point of the concentrated solution is taken as a reference point; 6 standard measuring surfaces extending outwards are arranged in a ring shape; taking 10 points on the standard measuring surface, measuring the microwave signal change parameters of each point through a microwave signal detection device, averaging the microwave signal change parameters of each point obtained on each standard measuring surface, and forming a standard microwave signal change curve by each average value; the standard microwave signal change curve is used for evaluating whether the primary concentrated solution meets the standard or not;
(2) heating and evaporating the concentrated solution in the step (1) until crystals are precipitated; shooting by an image scanning mechanism by taking the boundary of the concentrated solution and the crystal as a central line to obtain a solution image; converting the solution image into a standard gray image to obtain a gray value G1=189 of a concentrated solution area in the standard gray image; and gray value G2=216 of the crystal region in the standard gray image; the threshold range is plus or minus 10;
(3) adding ethyl acetate and crystallized 2, 3, 4, 6-diacetone mannose into a container; wherein the crystal 2, 3.4, 6-diacetone mannose accounts for 50 percent of the total volume of the solution; taking the central point of the solution as a reference point; the 6 second standard measuring surfaces extending outwards are arranged in a ring shape; measuring microwave signal variation parameters of each point on the second standard measurement surface at 15 points through a microwave signal detection device, averaging the microwave signal variation parameters of each point obtained on each standard measurement surface, and forming a second standard microwave signal variation curve by using each average value; gradually reducing the height of the crystal by taking 4cm as a section, and simultaneously supplementing a solvent with the same volume as the reduced crystal to ensure that the liquid level of the solution is the same as the initial liquid level; after each section is reduced and the solvent is supplemented, standing to ensure that the solvent and the crystal are layered; measuring a second standard microwave signal change curve at the moment, and repeating the steps to obtain a second standard microwave signal change curve corresponding to different crystal volumes;
(4) taking a picture by taking the boundary of ethyl acetate and crystal 2, 3.4, 6-diacetone mannose as a central line through an image scanning mechanism to obtain a second sample solution image; converting the second sample solution image into a second standard gray scale image, and obtaining a gray scale value G3=186 of a solvent area in the second standard gray scale image; and gray value G4=218 of the crystal region in the standard gray image;
as shown in fig. 1 to 5, the specific processing method includes the following steps:
the method comprises the following steps: adding anhydrous sodium sulphate into a reaction solution generated in S1 for primary dehydration; introducing the preliminarily dehydrated reaction liquid into a surface evaporation concentration device; preliminarily concentrating the preliminarily dehydrated treatment liquid by a surface evaporation concentration method to form a preliminary concentrated liquid, and introducing the preliminary concentrated liquid into a preliminary concentrated liquid storage tank; wherein the size of the primary concentrate storage tank is the same as the size of the container in (1);
step two: when the liquid phases of the primary concentrated solution and the sample concentrated solution in the primary concentrated solution storage box are the same, taking the central point of the primary concentrated solution to be processed as a reference point; 6 actual measuring surfaces extending outwards are arranged in a ring shape through a microwave signal detection device; measuring microwave signal variation parameters at 10 points on an actual measurement surface, averaging the microwave signal variation parameters of the points obtained on each actual measurement surface, and forming an actual microwave signal variation curve by each average value; comparing to obtain the actual microwave signal change curve of the primary concentrated solution within the threshold value of the standard microwave signal change curve, and finishing primary concentration of the primary concentrated solution at the moment;
step three: introducing the reaction liquid subjected to the primary concentration in the step two into a crystallization box, continuously heating the primary concentrated liquid for 14min, obtaining a local image with the height of 8cm from the bottom to the top by an image scanning mechanism, and converting the obtained image into an actual gray image; randomly taking 30 pixel points which are transversely arranged in parallel at the bottom edge of the actual gray image, taking the row of pixel points as a first base line, and upwards obtaining the gray value Gn of each pixel point in the actual gray image with the same width as the first base line, wherein the width of the gray value Gn is the width of the first base line, and the height of the gray value Gn is 8 cm; taking the average value Gn of the gray values Gn of all the pixel points1=210, determining that crystal precipitation exists within the threshold of the gray value G2 of the crystal region in the standard gray image, and continuously cooling and crystallizing the concentrated solution; taking the volume of the crystalline crystals herein as a standard volume; the height of the crystal in the crystallization box is 19.12 cm; after crystallization is finished, adding ethyl acetate into the crystals, heating and dissolving the ethyl acetate, then recrystallizing, carrying out ultrasonic crushing on the recrystallized crystals by an ultrasonic device, and standing, wherein the central point of the solution at the moment is taken as a reference point; 6 actual measuring surfaces extending outwards are arranged in a ring shape; measuring microwave signal variation parameters at 15 points on the actual measurement surface, averaging the microwave signal variation parameters of the points obtained on each actual measurement surface, and forming a second actual microwave signal variation curve by each average value; comparing the second actual microwave signal change curve with each second standard microwave signal change curve; the second actual microwave signal change curve is between the second standard microwave signal change curves of two adjacent sections 17 and 21; the actual height of the crystals contained at this time was found to be 17 cm; the rough height S =17cm of the precipitated crystals was thus obtained, and then the rough volume V =17 x 30cm of the precipitated crystals was calculated3(ii) a Mechanism for scanning imageMoving to a position 17cm away from the bottom, obtaining a local image with the height of 10cm from bottom to top, and converting the obtained image into a second actual gray image; randomly taking a plurality of pixel points which are transversely arranged in parallel at the bottom edge of the second actual gray image, taking the row of pixel points as a second base line, and upwards obtaining the gray value Gn 'of each pixel point in the actual gray image with the same width as the second base line, so as to obtain the gray value Gn' of each pixel point in the detection area with the width of the second base line and the height of 10 cm; finding a boundary line, wherein the size of the image is 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 = 53; the distance of the boundary line from the lowest edge of the picture is S = LN =1.39 cm; i.e. the height S' =1.39cm of the remaining crystals; when the total height of the precipitated crystals is SS = S + S' =18.39 within the set range, the crystals are completely precipitated;
step four: drying the crystals in the crystallization box, and performing online sampling inspection on the dried crystals; inputting the crystals meeting the dryness into a finished product library, and inputting the crystals not meeting the standard into a circulating drying area for re-drying until the crystals meet the dryness requirement;
the microwave moisture measuring device comprises a conveying platform, wherein a crystal inlet and a crystal outlet are arranged on the conveying platform along the conveying direction of crystals, and a first forming module and a first microwave moisture measuring instrument are sequentially arranged between the crystal inlet and the crystal outlet; the circulating drying area comprises a first drying channel connected with a crystal outlet of the conveying platform, a first drying box, a second forming module and a second microwave moisture measuring instrument are sequentially arranged on the first drying channel along the crystal conveying direction, the circulating drying area further comprises a second drying channel connected with the first drying channel, and the outlet of the second drying channel is connected with the crystal inlet of the conveying platform; a second drying box is arranged on the second drying channel;
the tail end of the conveying platform and the tail end of the first drying channel are qualified product output ends; a first crystal pushing device is arranged on the opposite side of the inlet of the first drying channel; pushing the crystals from the conveying platform into the first drying channel through the first crystal pushing device; a second crystal pushing device is arranged on the side of the outlet of the first drying channel; pushing the crystal from the first drying channel into a second drying channel through the second crystal pushing device; a third crystal pushing device is arranged on the side of the outlet of the second drying channel, and the crystals output by the second drying channel are pushed to the inlet end of the conveying platform through the third crystal pushing device; the method for performing online spot check comprises the following steps:
e1: placing the crystal on a conveying platform, conveying the crystal through the conveying platform, and forming through a first forming module in the conveying process; the cross section of the formed crystal is a rectangle with a set thickness;
e2: the molded crystal passes through a first microwave moisture measuring instrument which detects the moisture content of the crystal at regular time, and if the moisture content of the crystal is within a set range, the crystal is conveyed to a finished product warehouse through a qualified product output end; otherwise, stopping conveying the crystals in the crystallization box to the conveying platform; meanwhile, the drying time or temperature in the crystallization box is adjusted; conveying the crystals on the conveying platform to a circulating drying area for circulating drying until the crystals meet the requirement of dryness;
e3: and when the dryness of the crystals on the conveying platform meets the requirement, continuously conveying the crystals in the crystallization box to the conveying platform, and repeating the steps E1 to E3 to finish the online sampling inspection of the crystals.
The circulating drying method comprises the following steps:
f1: the conveying platform outputs crystals with unqualified water content through detection, and the crystals are conveyed to the first drying channel through the first crystal pushing device;
f2: the crystal entering the first drying channel sequentially passes through the first drying box, the second forming module and the second microwave moisture measuring instrument; after detection, if the water content of the crystal is in a set range, outputting the crystal from a qualified product output end on the first drying channel; otherwise, the second crystal pushing device conveys the crystals to a second drying channel;
f3: the crystals entering the second drying channel pass through a drying box arranged on the second drying channel; after drying, the third crystal pushing device conveys the crystal to the conveying platform, and the steps F1 to F3 are repeated; and (5) finishing drying.
Example 2
Processing the organic phase generated in step S4;
preparation before experiment:
(1) taking a container; the length, width and height are respectively as follows: 30cm by 60 cm; adding a pre-concentrated sample concentrated solution of the organic phase generated in the step S4 into a container, wherein the central point of the concentrated solution is taken as a reference point; 6 standard measuring surfaces extending outwards are arranged in a ring shape; taking 10 points on the standard measuring surface, measuring the microwave signal change parameters of each point through a microwave signal detection device, averaging the microwave signal change parameters of each point obtained on each standard measuring surface, and forming a standard microwave signal change curve by each average value; the standard microwave signal change curve is used for evaluating whether the primary concentrated solution meets the standard or not;
(2) heating and evaporating the concentrated solution in the step (1) until crystals are precipitated; shooting by an image scanning mechanism by taking the boundary of the concentrated solution and the crystal as a central line to obtain a solution image; converting the solution image into a standard gray image to obtain a gray value G1=149 of a concentrated solution area in the standard gray image; and gray value G2=206 of the crystal region in the standard gray image; the threshold range is plus or minus 10;
(3) adding ethyl acetate and crystalline triacetylmonoacetone mannose into a container; wherein crystalline triacetylmonoacetone mannose accounts for 50% of the total volume of the solution; taking the central point of the solution as a reference point; the 6 second standard measuring surfaces extending outwards are arranged in a ring shape; measuring microwave signal variation parameters of each point on the second standard measurement surface at 15 points through a microwave signal detection device, averaging the microwave signal variation parameters of each point obtained on each standard measurement surface, and forming a second standard microwave signal variation curve by using each average value; gradually reducing the height of the crystal by taking 5cm as a section, and simultaneously supplementing a solvent with the same volume as the reduced crystal to ensure that the liquid level of the solution is the same as the initial liquid level; after each section is reduced and the solvent is supplemented, standing to ensure that the solvent and the crystal are layered; measuring a second standard microwave signal change curve at the moment, and repeating the steps to obtain a second standard microwave signal change curve corresponding to different crystal volumes;
(4) shooting by an image scanning mechanism by taking the boundary of ethyl acetate and crystalline triacetyl monoacetone mannose as a central line to obtain a second sample solution image; converting the second sample solution image into a second standard gray-scale image, obtaining a gray-scale value G3=193 of the solvent region in the second standard gray-scale image; and the gray value G4=221 of the crystal region in the standard gray image;
the specific processing method comprises the following steps:
the method comprises the following steps: adding anhydrous sodium sulphate into the organic phase generated in S4 to carry out primary dehydration; introducing the preliminarily dehydrated reaction liquid into a surface evaporation concentration device; preliminarily concentrating the preliminarily dehydrated treatment liquid by a surface evaporation concentration method to form a preliminary concentrated liquid, and introducing the preliminary concentrated liquid into a preliminary concentrated liquid storage tank; wherein the size of the primary concentrate storage tank is the same as the size of the container in (1);
step two: when the liquid phases of the primary concentrated solution and the sample concentrated solution in the primary concentrated solution storage box are the same, taking the central point of the primary concentrated solution to be processed as a reference point; 6 actual measuring surfaces extending outwards are arranged in a ring shape through a microwave signal detection device; measuring microwave signal variation parameters at 10 points on an actual measurement surface, averaging the microwave signal variation parameters of the points obtained on each actual measurement surface, and forming an actual microwave signal variation curve by each average value; comparing to obtain the actual microwave signal change curve of the primary concentrated solution which is not in the threshold value of the standard microwave signal change curve, then reintroducing the primary concentrated solution into the surface evaporation concentration device for concentration, continuously detecting the water content after 30min, comparing to obtain the actual microwave signal change curve of the primary concentrated solution which is in the threshold value of the standard microwave signal change curve, and finishing the primary concentration;
step three: introducing the reaction liquid subjected to primary concentration in the step two into a crystallization box body, continuously heating the primary concentrated liquid for 18min, obtaining a local image with the height of 8cm from the bottom to the top by an image scanning mechanism, and converting the obtained image into an actual gray image(ii) a Randomly taking 30 pixel points which are transversely arranged in parallel at the bottom edge of the actual gray image, taking the row of pixel points as a first base line, and upwards obtaining the gray value Gn of each pixel point in the actual gray image with the same width as the first base line, wherein the width of the gray value Gn is the width of the first base line, and the height of the gray value Gn is 8 cm; taking the average value Gn of the gray values Gn of all the pixel points1=208, judging that crystal precipitation exists in the threshold of the gray value G2 of the crystal area in the standard gray image, and continuously cooling and crystallizing the concentrated solution; taking the volume of the crystalline crystals herein as a standard volume; the height of the crystal in the crystallization box is 21.14 cm; after crystallization is finished, adding ethyl acetate into the crystals, heating and dissolving the ethyl acetate, then recrystallizing, carrying out ultrasonic crushing on the recrystallized crystals by an ultrasonic device, and standing, wherein the central point of the solution at the moment is taken as a reference point; 6 actual measuring surfaces extending outwards are arranged in a ring shape; measuring microwave signal variation parameters at 15 points on the actual measurement surface, averaging the microwave signal variation parameters of the points obtained on each actual measurement surface, and forming a second actual microwave signal variation curve by each average value; comparing the second actual microwave signal change curve with each second standard microwave signal change curve; the second actual microwave signal change curve is between the second standard microwave signal change curves of two adjacent sections 20 and 25; the actual height of the crystals contained at this time was found to be 20 cm; the rough height S =20cm of the precipitated crystals is thus obtained, and then the rough volume V =20 × 30cm of the precipitated crystals is calculated3(ii) a Moving the image scanning mechanism to a position 20cm away from the bottom, obtaining a local image with the height of 10cm from bottom to top, and converting the obtained image into a second actual gray image; randomly taking a plurality of pixel points which are transversely arranged in parallel at the bottom edge of the second actual gray image, taking the row of pixel points as a second base line, and upwards obtaining the gray value Gn 'of each pixel point in the actual gray image with the same width as the second base line, so as to obtain the gray value Gn' of each pixel point in the detection area with the width of the second base line and the height of 10 cm; finding a boundary line, wherein the size of the image is 8cm by 10 cm; 302 pixels 378 pixels; the corresponding possible level L to a single pixel is 0.26 mm; boundary line to pictureThe number of the pixel points on the lowest edge is N = 55; the distance of the boundary line from the lowest edge of the picture is S = LN =1.39 cm; i.e. the height S' =1.43cm of the remaining crystals; when the total height of the precipitated crystals is SS = S + S' =21.43 within the set range, the crystals are completely precipitated;
step four: drying the crystals in the crystallization box, and performing online sampling inspection on the dried crystals; inputting the crystals meeting the dryness into a finished product library, and inputting the crystals not meeting the standard into a circulating drying area for re-drying until the crystals meet the dryness requirement;
the device comprises a conveying platform 400, wherein a crystal inlet and a crystal outlet are arranged on the conveying platform along the conveying direction of the crystals, and a first forming module 401 and a first microwave moisture measuring instrument 402 are sequentially arranged between the crystal inlet and the crystal outlet; the circulating drying area comprises a first drying channel 403 connected with a crystal outlet of the conveying platform, a first drying box 404, a second forming module 405 and a second microwave moisture measuring instrument 406 are sequentially arranged on the first drying channel along the crystal conveying direction, the circulating drying area further comprises a second drying channel 407 connected with the first drying channel, and the outlet of the second drying channel is connected with a crystal inlet of the conveying platform; a second drying box 408 is arranged on the second drying channel; the tail end of the conveying platform and the tail end of the first drying channel are qualified product output ends; a first crystal pushing device 409 is arranged on the opposite side of the inlet of the first drying channel; pushing the crystals from the conveying platform into the first drying channel through the first crystal pushing device; a second crystal pushing device 410 is arranged on the side of the outlet of the first drying channel; pushing the crystal from the first drying channel into a second drying channel through the second crystal pushing device; a third crystal pushing device 411 is arranged at the side of the outlet of the second drying channel, and the crystals output by the second drying channel are pushed to the inlet end of the conveying platform through the third crystal pushing device;
the method for performing online spot check comprises the following steps:
e1: placing the crystal on a conveying platform, conveying the crystal through the conveying platform, and forming through a first forming module in the conveying process; the section of the formed crystal is a rectangle with a set thickness;
e2: the molded crystal passes through a first microwave moisture measuring instrument which detects the moisture content of the crystal at regular time, and if the moisture content of the crystal is within a set range, the crystal is conveyed to a finished product warehouse through a qualified product output end; otherwise, stopping conveying the crystals in the crystallization box to the conveying platform; meanwhile, the drying time or temperature in the crystallization box is adjusted; conveying the crystals on the conveying platform to a circulating drying area for circulating drying until the crystals meet the requirement of dryness;
e3: and when the dryness of the crystals on the conveying platform meets the requirement, continuously conveying the crystals in the crystallization box to the conveying platform, and repeating the steps E1 to E3 to finish the online sampling inspection of the crystals.
The circulating drying method comprises the following steps:
f1: the conveying platform outputs crystals with unqualified water content through detection, and the crystals are conveyed to the first drying channel through the first crystal pushing device;
f2: the crystal entering the first drying channel sequentially passes through the first drying box, the second forming module and the second microwave moisture measuring instrument; after detection, if the water content of the crystal is in a set range, outputting the crystal from a qualified product output end on the first drying channel; otherwise, the second crystal pushing device conveys the crystals to a second drying channel;
f3: the crystals entering the second drying channel pass through a drying box arranged on the second drying channel; after drying, the third crystal pushing device conveys the crystals to the conveying platform, and the steps F1 to F3 are repeated; and (5) finishing drying.
The experimental equipment in the embodiment 1 and the experimental equipment in the embodiment 2 are the same, and each experimental equipment comprises a dewatering box 100 and a surface evaporation concentration device 200 connected with the dewatering box, wherein the surface evaporation concentration device is connected with a primary concentrated solution storage box 500, the primary concentrated solution storage box is connected with a crystallization box 300, and the crystallization box is connected with a conveying platform 400;
a first airflow interlayer 101 is formed outside the dewatering box, the first airflow interlayer is connected with a steam outlet of a steam generator 102, and a first condensate outlet 103 is further formed in the first airflow interlayer; the box body of the dewatering box is connected with an inlet of a steam generator through a pipeline; the pipeline is provided with a one-way valve;
the surface evaporation concentration device comprises a heater 201 connected with a dehydration tank, the heater is connected with a concentration tank, filler 202 with large specific surface area is filled in the concentration tank, a solution in the dehydration tank flows into the concentration tank from the top of the concentration tank after being preheated by the heater, a liquid film is formed by the internal filler from top to bottom, the bottom of the concentration tank is connected with a fan 203, an air flow passes through the filler from the bottom of the concentration tank upwards to gasify moisture in the liquid film, the top of the concentration tank is provided with a first air outlet, the first air outlet is connected with an inlet of a steam generator, and the preheated air flow is introduced into the steam generator for heating;
the upper top surface and the lower top surface of the primary concentrated solution storage tank are respectively provided with a plurality of microwave generators 501 and a plurality of microwave receivers 502, and the plurality of microwave generators and the plurality of microwave receivers correspond to each other one by one; the arrangement shape is arranged in a ring shape or other shapes, and is designed according to the use condition;
a second air flow interlayer 301 is arranged on the periphery of the crystallization box, a second condensate outlet 302 is arranged at the bottom of the second air flow interlayer, the top of the second air flow interlayer is connected with a steam outlet and a steam inlet of a steam generator through pipelines, and the box body of the crystallization box is connected with the inlet of the steam generator through a pipeline; the pipelines are provided with one-way valves; the bottom of the crystallization box is hinged with a sealing cover 303, the sealing cover is provided with an energy converter 304, the top of the crystallization box is provided with an ultrasonic generator 305, the crystallization box is also internally provided with a solvent precipitation pipeline 306, and the solvent precipitation pipeline is connected with a pump body and used for sucking out a solvent; a transparent window is arranged on one side of the crystallization box, the transparent window extends from the top of the crystallization box to the bottom of the crystallization box, an installation shell 307 is arranged outside the transparent window, a CCD image scanning mechanism is arranged in the installation shell, the CCD image scanning mechanism comprises a first driving motor 308, a screw 309 is connected to the output shaft end of the first driving motor, a nut 310 is connected to the screw, an installation plate 311 is fixed on the nut, a second driving motor 312 is fixed on the installation plate, a main transmission gear 313 is fixed on the output shaft of the second driving motor, and the CCD image scanning device further comprises a driven transmission gear 314, a rack 315 and a CCD scanning head assembly 316; the shell of the second driving motor is fixed on the mounting plate, and the output shaft of the second driving motor is 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, the CCD scanning head assembly is fixed on one side of the rack, 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 and the second driving motor are servo driving motors, and the CCD scanning head assembly can be accurately controlled by setting output parameters of output shafts of the servo driving motors.
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 (7)
1. The crystallization drying method capable of accurately monitoring the water content in the process of preparing the biological sugar is characterized in that: the method comprises the following steps:
the method comprises the following steps: adding anhydrous sodium sulphate into the biological sugar treatment liquid for preliminary dehydration; primarily concentrating the primarily dehydrated treatment solution by a surface evaporation concentration method to form a primary concentrated solution;
step two: judging whether the moisture contained in the primary concentrated solution is in a preset range or not through a microwave signal detection device, and if so, entering a third step; if the current time is not within the preset range, repeating the operation of the first step;
step three: continuously heating the primary concentrated solution, and detecting whether crystals are separated out or not by an image scanning mechanism; if no crystal precipitation is detected, continuing heating; if crystal precipitation is detected; cooling and crystallizing the concentrated solution; after crystallization is finished, adding a solvent into the crystals for dissolving, then recrystallizing, ultrasonically crushing the recrystallized crystals, standing, calculating by using a microwave signal detection device to obtain a rough volume V of the precipitated crystals, calculating by using an image scanning mechanism to obtain an accurate volume V' of the precipitated crystals, and judging whether all the volumes of the precipitated crystals are recrystallized; if all crystals are separated out, discharging the solvent, and entering the step four;
step four: drying the crystals in the crystallization box, and performing online sampling inspection on the dried crystals; inputting the crystals meeting the dryness into a finished product library, and inputting the crystals not meeting the standard into a circulating drying area for circulating drying until the crystals meet the dryness requirement;
and step two, judging whether the water contained in the primary concentrated solution is in a preset range by a microwave signal detection device:
a1: taking a certain volume of standard concentrated solution, and taking a central point of the standard concentrated solution 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, measuring microwave signal change parameters of each point through a microwave signal detection device, averaging the microwave signal change parameters of each point obtained on each standard measuring surface, and forming a standard microwave signal change curve by each average value;
a2: taking the primary concentrated solution to be treated with the same volume as the standard concentrated solution, and taking the central point of the primary concentrated solution 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 at a plurality of points on an actual measuring surface, averaging the microwave signal variation parameters of the points obtained on each actual measuring surface, and forming an actual microwave signal variation curve by each average value;
a3: and comparing the actual microwave signal change curve with the standard microwave signal change curve, judging whether the actual microwave signal change curve is within the threshold value of the standard microwave signal change curve, if so, judging that the moisture content of the preliminary concentrated solution to be treated is within the set range, otherwise, judging that the moisture content is not within the set range.
2. The crystal drying method capable of accurately monitoring the moisture content in the process of preparing biosaccharide according to claim 1, wherein: the microwave moisture measuring device comprises a conveying platform, wherein a crystal inlet and a crystal outlet are arranged on the conveying platform along the conveying direction of crystals, and a first forming module and a first microwave moisture measuring instrument are sequentially arranged between the crystal inlet and the crystal outlet; the circulating drying area comprises a first drying channel connected with a crystal outlet of the conveying platform, a first drying box, a second forming module and a second microwave moisture measuring instrument are sequentially arranged on the first drying channel along the crystal conveying direction, the circulating drying area further comprises a second drying channel connected with the first drying channel, and the outlet of the second drying channel is connected with the crystal inlet of the conveying platform; a second drying box is arranged on the second drying channel; the tail end of the conveying platform and the tail end of the first drying channel are qualified product output ends; a first crystal pushing device is arranged on the opposite side of the inlet of the first drying channel; pushing the crystals from the conveying platform into the first drying channel through the first crystal pushing device; a second crystal pushing device is arranged on the side of the outlet of the first drying channel; pushing the crystal from the first drying channel into a second drying channel through the second crystal pushing device; and a third crystal pushing device is arranged on the side of the outlet of the second drying channel, and the crystals output by the second drying channel are pushed to the inlet end of the conveying platform through the third crystal pushing device.
3. The crystal drying method capable of accurately monitoring the moisture content in the process of preparing biosaccharide according to claim 2, characterized in that: the method for performing online spot check comprises the following steps:
e1: placing the crystal on a conveying platform, conveying the crystal through the conveying platform, and forming through a first forming module in the conveying process; the cross section of the formed crystal is a rectangle with a set thickness;
e2: the formed crystal passes through a first microwave moisture measuring instrument, the first microwave moisture measuring instrument detects the moisture content of the crystal at regular time, and if the moisture content of the crystal is within a set range, the crystal is conveyed to a finished product warehouse through a qualified product output end; otherwise, stopping conveying the crystals in the crystallization box to the conveying platform; meanwhile, the drying time or temperature in the crystallization box is adjusted; conveying the crystals on the conveying platform to a circulating drying area for circulating drying until the crystals meet the requirement of dryness;
e3: and when the dryness of the crystals on the conveying platform meets the requirement, continuously conveying the crystals in the crystallization box to the conveying platform, and repeating the steps E1 to E3 to finish the online sampling inspection of the crystals.
4. The crystal drying method capable of accurately monitoring the moisture content in the process of preparing biosaccharide according to claim 2, characterized in that: the circulating drying method comprises the following steps:
f1: the conveying platform outputs crystals with unqualified water content through detection, and the crystals are conveyed to the first drying channel through the first crystal pushing device;
f2: the crystal entering the first drying channel sequentially passes through the first drying box, the second forming module and the second microwave moisture measuring instrument; after detection, if the water content of the crystal is in a set range, outputting the crystal from a qualified product output end on the first drying channel; otherwise, the second crystal pushing device conveys the crystals to a second drying channel;
f3: the crystals entering the second drying channel pass through a drying box arranged on the second drying channel; after drying, the third crystal pushing device conveys the crystal to the conveying platform, and the steps F1 to F3 are repeated; and (5) finishing drying.
5. The crystal drying method capable of accurately monitoring the moisture content in the process of preparing biosaccharide according to claim 1, wherein: the method for detecting whether crystal is precipitated or not through the image scanning mechanism in the third step comprises the following substeps:
b1: taking a sample solution with layered concentrated solution and crystals; shooting by an image scanning mechanism by taking the boundary of the concentrated solution and the crystal as a central line to obtain a sample solution image; converting the sample solution image into a standard gray image to obtain a gray value G1 of a concentrated solution area in the standard gray image; and gray value G2 of the crystal region in the standard gray image;
b2: taking a concentrated solution to be detected, obtaining a local image with the height of H from the bottom to the top 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 bottom edge of the actual gray image, taking the row of pixel points as a first base line, and upwards obtaining the gray value Gn of each pixel point in the actual gray image with the same width as the first base line, wherein the width of the gray value Gn is the width of the first base line, and the height of the gray value Gn is H;
b3: and comparing the gray value Gn of each pixel point in the detection area with the gray value G1 of the concentrated liquid area in the standard gray image and the gray value G2 of the crystal area in the standard gray image, if the gray value Gn of each pixel point in the detection area is within the threshold value of the gray value G2 of the crystal area in the standard gray image, determining that crystal precipitation exists, otherwise, determining that no crystal precipitation exists.
6. The crystal drying method capable of accurately monitoring the moisture content in the process of preparing biosaccharide according to claim 1, wherein: in the third step, the method for calculating the rough volume V of the precipitated crystal by the microwave signal detection device comprises the following steps:
c1: taking a sample solution with layered solvent and crystals; at the moment, the volume of the crystals in the sample solution accounts for more than 50 percent; taking the central point of the sample solution as a reference point; a plurality of second standard measuring surfaces extending outwards are arranged in a ring shape; taking a plurality of points on the second standard measuring surface, measuring the microwave signal change parameters of each point through a microwave signal detection device, averaging the microwave signal change parameters of each point obtained on each standard measuring surface, and forming a second standard microwave signal change curve according to each average value;
c2: gradually reducing the height of the crystal in the step C1 by taking 4-8cm as a section, and simultaneously supplementing a solvent with the same volume as the reduced crystal so as to ensure that the liquid level of the solution is the same as the initial liquid level; after each section is reduced and the solvent is supplemented, standing to ensure that the solvent and the crystal are layered; measuring the change curve of the second standard microwave signal at the moment, and repeating the steps to obtain a change curve of the second standard microwave signal corresponding to different crystals;
c3: taking the central point of the solution 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 at a plurality of points on the actual measurement surface, averaging the microwave signal variation parameters of the points obtained on each actual measurement surface, and forming a second actual microwave signal variation curve by each average value;
c4: comparing the second actual microwave signal change curve with each second standard microwave signal change curve; obtaining the actual height of the crystal contained at the moment; if the second actual microwave signal variation curve is between the second standard microwave signal variation curves of two adjacent sections; the actual height of the crystals contained at this time is determined as the lower section height of two adjacent heights; thus, a rough height S of the precipitated crystal is obtained, and then a rough volume V of the precipitated crystal is calculated.
7. The crystal drying method capable of accurately monitoring the moisture content in the process of preparing biosaccharide according to claim 6, wherein: in the third step, the method for calculating the accurate volume V' of the precipitated crystal through the image scanning mechanism comprises the following steps:
d1: taking a second sample solution with the solvent and the crystals layered; shooting by an image scanning mechanism by taking the boundary of the solvent and the crystal as a central line to obtain a second sample solution image; converting the second sample solution image into a second standard gray image to obtain a gray value G3 of a solvent area in the second standard gray image; and gray value G4 of the crystal region in the standard gray image;
d2: moving the image scanning mechanism to the rough height H' obtained in the step C4, obtaining a local image with the height of H1 from bottom to top, and converting the obtained image into a second actual gray image; taking a plurality of pixel points which are horizontally arranged in parallel at the bottom edge of the second actual gray image, taking the row of pixel points as a second base line, and upwards obtaining the gray value Gn' of each pixel point in the actual gray image with the same width as the second base line, wherein the width of the second base line is obtained, and the height of the second base line is H1;
d3: searching a boundary; comparing the gray value Gn' of each pixel point in the detection area in the second actual gray image with G3 and G4; if the Gn '-G3 is less than or equal to 10, replacing the gray value Gn' in the second actual gray image with a gray value G3, and determining as a solvent gray value; similarly, if the value | Gn '-G4 | is less than or equal to 10, replacing the gray value Gn' with a gray value G4, and determining the gray value as a crystal gray value; after the gray value replacement of each pixel point in the area is completed, the gray value of the pixel point in the second actual gray image is divided into two parts, namely G3 and G4, and the joint of G3 and G4 is a boundary; calculating the distance from the boundary line to the bottom edge of the image, namely the height S' of the residual crystal; the total height of the precipitated crystals is SS = S + S', and if the amount of the precipitated crystals at this time is within the threshold value of the initial value, it indicates that the crystals are completely precipitated, otherwise, it indicates that the crystals are not completely precipitated.
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Denomination of invention: Crystallization drying method for accurate monitoring of water content in the process of preparing biological sugar Effective date of registration: 20221206 Granted publication date: 20220524 Pledgee: China Minsheng Bank Limited Jinhua Branch Pledgor: SYNGARS TECHNOLOGY CO.,LTD. Registration number: Y2022980025200 |
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Denomination of invention: A Crystal Drying Method for Precise Monitoring of Water Content in the Preparation of Biological Sugar Granted publication date: 20220524 Pledgee: China Minsheng Bank Limited Jinhua Branch Pledgor: SYNGARS TECHNOLOGY CO.,LTD. Registration number: Y2024980011843 |