CN101306026A - Natural indigo prepared by froth flotation method and its preparation method and device - Google Patents

Natural indigo prepared by froth flotation method and its preparation method and device Download PDF

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CN101306026A
CN101306026A CNA200710074490XA CN200710074490A CN101306026A CN 101306026 A CN101306026 A CN 101306026A CN A200710074490X A CNA200710074490X A CN A200710074490XA CN 200710074490 A CN200710074490 A CN 200710074490A CN 101306026 A CN101306026 A CN 101306026A
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indigo
foam
flotation
preparation
indigo naturalis
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CN101306026B (en
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杨明
韩丽
王虎山
胡云江
郭朝均
张艳艳
蒋巧梅
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Ya'an Xunkang Pharmaceutical Co ltd
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D1/00—Flotation
    • B03D1/02—Froth-flotation processes
    • B03D1/028—Control and monitoring of flotation processes; computer models therefor
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D1/00—Flotation
    • B03D1/08—Subsequent treatment of concentrated product
    • B03D1/082—Subsequent treatment of concentrated product of the froth product, e.g. washing
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D1/00—Flotation
    • B03D1/14—Flotation machines
    • B03D1/24—Pneumatic
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D2203/00—Specified materials treated by the flotation agents; specified applications
    • B03D2203/005—Fine and commodity chemicals

Abstract

The invention provides an indigo prepared by adopting the froth-flotation method, which comprises the components by weight percentages as follows: 2.63%-5.51% of indigo blue and 0.13%-0.61% of indigo red. The invention also provides a preparation method and a device for the indigo. The preparation method for the indigo of the invention has the advantages that the operation and the management are convenient, the separation is not limited by environment or climate, and the running is stable and reliable. The preparation method is a novel technique for indigo separation; by adopting the novel technology for machining, the large scale production can be realized on the basis of ensuring the drug quality, in addition, the indigo product quality is increased; the preparation method has simple and convenient operation and low technical difficulty. The quality of the indigo which is prepared by the preparation method is higher than the pharmacopoeia standards obviously.

Description

A kind of Indigo Naturalis that adopts the foam flotation method preparation and preparation method thereof and device
Technical field
The present invention relates to the device of new preparation method and this method of employing of Indigo Naturalis, be specially adapted to the separation of Indigo Naturalis in the thick indigo.Belong to drug world.
Background technology
Indigo Naturalis is the leaf of acanthaceous vegetable acanthaceous indigo Baphicacanthus cusia (Nees) Bremek., polygonaceae plant polygonum tinctorium ait. Polygonum tinctorium Ait. or cruciferae isatis Isatis indigoticaFort. or dried powder or the agglomerate that stem and leaf makes through processing.Indigo Naturalis is lightly seasoned, cold in nature, and the effect of tool heat-clearing and toxic substances removing, removing heat from blood, arresting convulsion is usually used in the seasonal disease pyretic toxicity, ecchymosis haematemesis-spitting of blood. be useful on hemorrhage that bronchiectasis causes in recent years.Manufacturing procedure is mainly feedstock capture, soaking fermentation, beats indigo, washes in a pan flower etc., and because of raw materials used difference, some places are directly used semi-finished product " shallow lake " to add to stir behind the water and are Indigo Naturalis after the collection foam dries after beating indigo; And some places stir promptly " washing in a pan flower " after need adding other material (specimens of one's blood), and tradition processing all is to be finished by empirical pharmaceutical worker, and it is low to use this technical difficulty in the separation, does not possess general applicability; Modern Indigo Naturalis processing enterprise will purchase semi-finished product and put the certain water gaging of Chi Zhongjia, fully stir with electric blender, make liquid level produce a large amount of foams, fish for foam on the gauze sieve, put under the sunlight and tan by the sun drying, be Indigo Naturalis, be porous foam shape agglomerate this moment, reaching after the assay was approved through crushing screening, mix homogeneously, packing gets product.The later stage process is by stirring and produces metastable foam, by foam Indigo Naturalis is separated from a large amount of " the thick shallow lake ".There is report to adopt elutriation to prepare Indigo Naturalis at present, as utility model patent CN 2656010.Adopting the swirling flow isolation technics to develop Indigo Naturalis water flies automatic sorting device to carry out Indigo Naturalis refining, make Indigo Naturalis processing habitat processing method become modern mechanical production, greatly reduce labor intensity, enlarged production scale, saved production cost from the pure manual operations of tradition.But by buoyancy of water, not only taken Indigo Naturalis out of when water flies, also taken the less calcium carbonate of particle diameter out of, therefore, indigo content is lower than foam flotation method.
Foam flotation method is a kind of of foamet, be mainly used in and separate undissolved material, by the material of flotation this as non-surface-active agent, but can make itself and surfactant have various materials such as metal yin, yang ion, the dyestuff etc. of affinity by cooperation or other method, also have Ore particle and precipitation particles etc.It is according to the principle of surface adsorption, the mat bubbling makes the surfactant in the solution accumulate in gas-liquid interface to float and form froth bed to solution main body top, froth bed and liquid phase main body are separated, can reach the purpose of concentrated surfactant (at froth bed) and purification liquid phase main body.Foam separating technology just is used to the flotation of mineral a long time ago.Present this method also is widely used in separating of many insoluble substances and solable matter except being used for mineral floating, as the separation of solution metal cation, anion, protein, dyestuff etc., concentrate.
At present, it is ripe to be used for the correlation technique of industrialization ore separators of ion flotation, mineral floating.Be used for the also successfully exploitation of foam separator of waste water, sewage disposal industry, and in extensively applying to produce.Be used to concentrate, the foam separation device of isolated protein realized being moved towards the industrialization by laboratory at present basically.Foam separating technology is used for the extraction of natural drug, because natural drug and mineral and protein etc., no matter from the still function of of physicochemical property itself, all be distinct, foam separator is used for this frontier of natural drug, can reach the purpose of final extraction separation, be unexpected.Still do not have at present relevant report and adopt medical materials such as foam flotation method extraction, separating traditional Chinese medicine Indigo Naturalis, more do not have the relevant report of concrete segregation apparatus.
Summary of the invention
Technical scheme of the present invention has provided a kind of Indigo Naturalis that adopts the foam flotation method preparation; Another technical scheme of the present invention has provided and has adopted froth flotation to prepare the method and apparatus of Indigo Naturalis.
The invention provides a kind of preparation method of Indigo Naturalis, it is to adopt the foam floating flotating device operation, comprises the steps:
A, elder generation pump in the flotation column of foam floating flotating device after thick indigo is added the water stirring;
B, compressed air is sent in the flotation column by the micropore distributor of flotation column outside or bottom, formed froth bed;
C, foam through the water flushing after, by the broken bubble of bulb-breaking device, it is centrifugal or enter the sedimentation tank precipitation that broken bubble liquid enters centrifuge, is Indigo Naturalis after the collecting precipitation part drying.
Wherein, thick indigo adds water to be prepared into thick indigo concentration of slurry is 0.15-0.6g/ml in a step.To add the feed rate that pumps into flotation column after water stirs be 1.0～1.2m to thick indigo in a step 3/ h.Compressed air is 44.8L/h-5 * 10 by the gas flow of the micropore distributor of post outside or bottom in the b step 3L/h.Foam is that 100～200L/h should be 1.02L/h-200L/h through the water flow velocity of water flushing in the c step.The described broken bubble of c step or be centrifugal broken bubble.
The present invention also provides the Indigo Naturalis of described preparation method preparation, and it is characterized in that: containing indigo weight percentage is: 2.63%-5.51%, the weight percentage of indirubin is: 0.13%-0.61%.
The invention provides a kind of foam floating flotating device for preparing Indigo Naturalis, it is the intermittent foam floatation equipment, and this equipment comprises: air compressor (33), gas rotameter (34), bubbling area (35), froth zone (36), foam are collected bend pipe (37), product stock jar (38), gas distributor (39).Wherein bubbling area, froth zone are described flotation column.
The present invention also provides the foam floating flotating device of another kind of preparation Indigo Naturalis, and it is the continued operation foam separation equipment, and this equipment comprises flotation column (1), centrifugal bulb-breaking device (2), sedimentation tank (3), is connected to form with pipeline successively.Wherein, described flotation column (1) comprises housing (23), is equiped with gas distributor (24), charging shower nozzle (25), flushing water shower nozzle (26) in the post housing from bottom to top successively, and a downflow weir (9) is arranged outside post top, and a discharging opening (27) is arranged under it; One discharge gate (12) is arranged at the cylinder bottom, and pipeline connects the back discharges in flotation column 2/3 place, discharges by material storage barrel (13), with control liquid phase height; Air inlet pipe (7) is housed on housing links to each other, be used to carry compressed air with gas distributor (24).Wherein, gas distributor (24) is the rustless steel funnel of diameter less than column internal diameter, on carry out canvas and tighten with iron wire; Described canvas aperture is 500 orders.Wherein, centrifugal bulb-breaking device (2) comprises motor (28), case (29), impeller (30).
Wherein, thick indigo adds water and is prepared in the thick indigo concentration of slurry in a step, and the intermittent foam floatation equipment is 0.15-0.6g/ml, and optium concentration is 0.4g/ml; The continous way froth flotation equipment is 0.05-0.1g/ml.Compressed air is 44.8L/h～102.4L/h variable speed operation from small to large by the gas flow of the micropore distributor of post outside or bottom in the b step.
The foam of continued operation foam separation equipment is 0.01cm/s, i.e. 1.02L/h through the water flow velocity of water flushing in the c step.
The present invention also provides described foam floating flotating device to be used for preparing the application of Indigo Naturalis.
Effective ingredient such as that foam flotation method is utilized is indigo, indirubin can be by the character of optionally taking out of by foam, regulate and control by operating parameter, can change content indigo in the product, indirubin, satisfy product different quality demand: two kinds of equipment all can reach ideal effect, wherein, adopt the intermittent foam floatation equipment can also obtain more high quality of products, indigo weight percentage＞4%, but productive rate is lower; Foam adopts continous way froth flotation equipment products obtained therefrom to meet the pharmacopeia requirement, also meets enterprise market demand (productive rate is higher).
The preparation method of Indigo Naturalis of the present invention, convenient operation and management is separated the restriction that is not subjected to environment, weather, and is reliable and stable.Preparation method of the present invention is the isolating a kind of new technique of Indigo Naturalis, utilizes this new technique to process, and on the basis that guarantees quality of medicinal material, is produced on a large scale, and can improve the Indigo Naturalis product quality again, and this method is easy and simple to handle, and technical difficulty is low.The Indigo Naturalis quality of the inventive method preparation is apparently higher than standards of pharmacopoeia.
Description of drawings
Fig. 1 intermittent foam flotation unit figure;
Fig. 2 continous way foam floating flotating device flow chart;
Fig. 3 flotation column structural representation;
Fig. 4 bulb-breaking device structural representation;
Among the figure, 1, the froth flotation post, 2, bulb-breaking device, 3, the concentrate sedimentation tank, 4, pan feeding, 5, stirring pool, 6 centrifugal pumps, 7, air inlet pipe, 8, the flushing water inlet pipe, 9, the foam downflow weir, 10, supernatant, 11, the Indigo Naturalis finished product, 12, tailing outlet port, 13, material storage barrel, 14, the mine tailing sedimentation tank, 15, supernatant or separating part not, 16, mine tailing, 17, air intake valve, 18, gas flowmeter, 19, the charging valve, 20, the feed rate meter, 21, the flushing water valve, 22, the flushing water effusion meter, 23, the post housing, 24, gas distributor, 25, feed distributor, 26, the flushing water distributor, 27, foam outlet, 28, motor, 29, case, 30 impellers, 31, foam inlet, 32, the outlet of broken bubble liquid, 33, air compressor, 34, gas rotameter, 35, bubbling area, 36, froth zone, 37, foam is collected bend pipe, 38, the product stock jar, 39, gas distributor.
The relation of different foam maker inflation rates of Fig. 5 and gas holdup;
Relation (wherein, the Jg:1.5cm/s of Fig. 6 post height and Indigo Naturalis flotation; Jf:0.1cm/s; Jw:0.01cm/s);
The graph of a relation of Fig. 7 foam layer height and Indigo Naturalis flotation;
Fig. 8 foam flushing water speed is to the influence of Indigo Naturalis flotation;
Fig. 9 delivery rate is to the influence of Indigo Naturalis flotation.
The specific embodiment
[embodiment 1] the present invention prepares the equipment of Indigo Naturalis
With reference to Fig. 2, continuously acting production lines equipment of the present invention, is connected to form with pipeline by flotation column (1), bulb-breaking device (2), sedimentation tank (3) successively by technological process.Flotation column comprises housing (23), is equiped with gas distributor (24), charging shower nozzle (25) flushing water shower nozzle (26) in the post housing from bottom to top successively, and a downflow weir (9) is arranged outside post top, and a discharging opening (27) is arranged under it; One drainage conduit (12) is arranged at the cylinder bottom, and pipeline connects the back discharges in flotation column 2/3 place, discharges by material storage barrel (13), with control liquid phase height.Air inlet pipe (7) is housed on housing links to each other, be used to carry compressed air with gas distributor (24).Bulb-breaking device (2) is positioned at 5～10cm place, flotation column (1) top, comprises motor (28), housing (29), impeller (30).
Its operation principle and process are: pan feeding (4) adds water behind stirring pool (5) mixing, being pumped into the flotation column import by pump (6) evenly is distributed in the tower with shower nozzle (25) spray, simultaneously evenly enter in the post by tower bottom air inlet pipe (7) and gas distributor (24) with the gas-liquid volume ratio of 1～3cm/s 0.2～0.5MPa compressed air, because system self contains the foaming characteristic material, when a large amount of countless bubbles contact with feed liquid, promptly formed more stable foam, Indigo Naturalis is attracted on the foam simultaneously, the foam that forms is owing to the buoyancy of solution rises, along with foamy continuous generation, come-up, the Indigo Naturalis that is adsorbed on the bubble is just separated from thick indigo liquid, control suitable operating condition, be the bulky grain that is mingled with in the scumming, need add the water flushing in the froth bed, the floating foam of going up cat head to concentrate sedimentation tank (3) precipitation, is Indigo Naturalis (11) after the collecting precipitation drying after discharging opening (27) enters the broken bubble of bulb-breaking device (2); Supernatant (10) is discharged the back and flowed into liquid storage tank, and is recycling; Discharge gate (12) discharge liquor is got above it blue portion and is proceeded FLOTATION SEPARATION after material storage barrel (13) flows into mine tailing sedimentation tank (14) back natural sedimentation, shoals as if the supernatant blueness, can flow into liquid storage tank, and lower part can discard.
The index components assay method of [embodiment 2] Indigo Naturalis of the present invention
(1) " Chinese pharmacopoeia version in 2005 is with the indigo content of spectrophotometry in indigo reference.
1. indigo reference substance 20mg is got in the preparation of reference substance solution, accurate claims surely, puts in the conical flask, slowly adds sulphuric acid 15ml, stirs evenly gently with glass rod, puts in 80 ℃ of water-baths sulfonation 1 hour, stirs at any time, takes out cooling.Solution is slowly moved in the 200ml measuring bottle that fills suitable quantity of water, wash container and residue with water, washing liquid is incorporated in the measuring bottle, adds water to scale, shake up, filter, precision is measured subsequent filtrate 5ml, puts in the 50ml measuring bottle, add water and cause scale, shake up, promptly get (containing indigo 10 μ g among every 1ml).
2. the preparation precision of standard curve is measured reference substance solution 1ml, 2ml, and 3ml, 4ml and 5ml put respectively in the 10ml measuring bottle, add water and cause scale, shake up.According to ultraviolet visible spectrophotometry (" Chinese pharmacopoeia version appendix in 2005 VA), measure absorbance at 610nm wavelength place, be vertical coordinate with the absorbance, concentration is abscissa, the drawing standard curve.
With absorbance (A) concentration (C) is returned, must the standard curve equation be: A=0.0652*C+0.0031, r=0.9999, with absorbance (A) concentration (C) is mapped, get a straight line, the result shows that indigo concentration and absorbance linear relationship are good in 1.02～5.1 μ g/ml scopes.
3. it is an amount of that sample preparation methods and algoscopy are got Indigo Naturalis fine powder of the present invention, the accurate title, decide, by the method under the preparation of reference substance solution, from " putting in the conical flask ", to " precision is measured subsequent filtrate 5ml ", put in the 50ml-100ml measuring bottle (making absorbance between 0.20-0.45), add water to scale, shake up, measure absorbance at the 610nm place, read concentration indigo the need testing solution (μ g/ml) from standard curve, calculate, promptly.
(2) indirubin assay
" Chinese pharmacopoeia version in 2005 is recorded the content of using the tlc scanning determination indirubin, but the tediously long complexity of sample preparation methods (chloroform reflux, extract, 4 hours), and lamellae prepares problem such as became uneven and may cause its precision to reduce, problems such as poor repeatability, and now more bibliographical information adopts the content of HPLC method mensuration indirubin: Cao Hong etc. to report with high effective liquid chromatography for measuring indigo, the method of indirubin content: use high performance liquid chromatograph HP 1050-DAD system, indigo, the indirubin average recovery rate is 100.5% (RSD=1.7%) and 98.30% (RSD=2.5%); Sun Li has reported newly with the RP-HPLC method and has measured method indigo, indirubin content that indigo, indirubin average recovery rate is (99.0 ± 1.0) % and (104.2 ± 3.5) %.Wherein, the HPLC method of measuring indirubin is simple to operate, repeatability and average recovery are all better, so selection HPLC method is as the assay of indirubin.
1. chromatographic condition chromatographic column: Kromasil ODS-1 post (250mm * 4.6mm, 5 μ m); Detect wavelength: 285nm, column temperature: 30 ℃; Mobile phase: methanol: water (85: 15); Flow velocity 1.0ml/min.Under this chromatographic condition, the peak separating degree is more than 1.5, theoretical cam curve by indirubin greater than 3000.
2. the about 2mg of indirubin reference substance is got in the preparation of reference substance solution, and accurate the title decided 2.26mg, puts in the 200ml volumetric flask, adds N, and the dinethylformamide dissolving also is settled to scale, shakes up, and is standby.
3. the preparation of standard curve is under aforementioned chromatographic condition, and sample introduction 2.5 μ l, 5 μ l, 10 μ l, 15 μ l, 20 μ l detect successively, the record peak area.
With peak area value (A) sample size (C) is returned, getting the standard curve equation is: A=66.678*C-0.719r=0.9999, with peak area value (A) sample size (C) is mapped, get a straight line, the result shows that in 0.02825～0.226mg/ml scope indirubin sample size and peak area linear relationship are good.
4. sample preparation methods and algoscopy sample thief fine powder are an amount of, and accurate the title decides, and puts in the 25ml volumetric flask, add dilute hydrochloric acid and produce to there being bubble, add N, and the dinethylformamide dissolving also is diluted to scale, shakes up, and is standby.Under aforementioned chromatographic condition, sample introduction is measured peak area, calculates content.
The research of [embodiment 3] foam floating process of the present invention
The floatation process process is multifactorial combined process, and each factor both was closely connected mutually, influenced each other again, makes floatation process very complicated.Have only between each factor and work in coordination, and all be in best process conditions, could obtain good flotation effect.
(1) experiment material and instrument
Material: thick indigo is provided by Hengyuan Pharmaceutical Group Co., Ltd., Jiangyou City, Sichuan, indigo reference substance (Chinese biological goods calibrating institute), indirubin reference substance (Chinese biological goods calibrating institute), methanol (chromatographically pure), redistilled water, N, dinethylformamide, other reagent such as hydrochloric acid are analytical pure.
Equipment: DIONEX auto injection high performance liquid chromatograph (Chromeleon chromatographic work station, ASI-100 automatic sampler, P680A LPG-4HPLC pump, UVD 170U UV/VIS Detector, TCC-100 column oven); SHIMADZU uv-spectrophotometric instrument; LZB-4 glass rotameter (Zhejiang development flow-meter plant); ACO-007 type air compressor (ZheJiang Sunsun Industrial Co., Ltd.); TDL-5 type centrifuge (Anting Scientific Instrument Factory, Shanghai); FA1104 type electronics Libra (going up balance factory of Nereid section); RE-52C Rotary Evaporators (Shanghai Yarong Biochemical Instrument Plant); The automatic dual pure water distillator of SZ-93 (Shanghai Yarong Biochemical Instrument Plant).
(2) evaluation index and assay method
1, the selection of evaluation index and calculating
The intermittent foam floatation process is that index comprehensive is estimated this technology with purity ratio, the response rate, filters out the best intermittent foam floatation process condition of thick indigo serosity.Purity compares, response rate computing formula is as follows:
Figure A20071007449000091
Figure A20071007449000092
(3) intermittent foam flotation experiment
1, intermittent operation mode
The preparation of material liquid: get a certain amount of thick indigo, in mortar, ground five minutes,, take by weighing the thick indigo of constant weight, add water and be mixed with certain volume, stir evenly to mix homogeneously, standby.
2, segregation apparatus: experimental provision as shown in Figure 1.
3, operational approach
First crack gas, with disposable the pouring in the knockout tower of thick indigo of a certain amount of modulated good concentration and pH value, again with the gas velocity modulation to desirable value.Air is measured by spinner flowmeter, feeds pond liquid through gas distributor by gas distributor at the bottom of by tower, is dispersed into bubble in gas distributor.Bubble forms foam rise to liquid top, pond in liquid phase after, and foam rises along cat head, flows out cat head at last and enters catcher.Foam enters storage tank by cat head, can't pile up, during stable the discharge, stop the foam separation operation up to foam, and debris is discharged at the bottom of by tower.
4, result and analysis
(1) influence of air velocity
On equipment on the same stage, carry out intermittent operation under the room temperature, liquid level is 470mm, thick indigo concentration of slurry is 0.25g/ml, investigates the influence of different gas speed to separating effect.Investigation the results are shown in Table 1, table 2.
Table 1 is indigo-and gas speed investigates the result
Figure A20071007449000101
Table 2 indirubin-gas speed is investigated the result
Figure A20071007449000102
As shown in Figure 1, under the fixed air speed operating condition, along with the increase of air velocity, purity is than descending, because air velocity is accelerated, bubble time of staying in separation equipment is short, the surfactant adsorption time shortens, and liquid holdup increases simultaneously, and the impurity of carrying secretly increases, selectivity descends, so purity is than reducing.The increase of throughput can increase interfacial area, helps adsorbing more solute, and because of the increase of foam volume, the amount of carrying secretly also increases simultaneously, and solute enters foam solution with entrained liquids, so the response rate improves.
For intermittent operation, the operation of fixed air speed is comparatively irrational.In the beginning of whole bubbling process, material liquid bubbles abundant, and lower gas speed helps reaching isolating effect; But the foaming characteristic material in the material liquid is along with foam overflows, causing the debris foaming characteristic weakens, the foam stability variation, be easy to break, coalescence, original gas speed has not satisfied the needs that the promotion foam overflows continuously, has only this moment the air velocity of increasing could guarantee more successive generation of foam and discharge.Therefore, in order to obtain the comparatively ideal response rate and purity simultaneously, should adopt from variable speed operation.Adopt 44.8L/h～102.4L/h variable speed operation from small to large according to experiment and experience.
(2) investigation of input concentration
On equipment on the same stage, carry out 44.8L/h～102.4L/h variable speed operation under the room temperature, liquid level is 300mm, gets thick indigo raw material 105g, 175g, 280g, 350g, 420g thin up to 700ml, investigates the influence of different feeds concentration to separating effect.Investigation the results are shown in Table 3, table 4.
Table 3 is indigo-and concentration investigates the result
Figure A20071007449000111
Table 4 indirubin-concentration is investigated the result
Figure A20071007449000112
By table as seen, when concentration was low, purity was than higher, and the response rate is lower.Because when thick indigo concentration of slurry was low, foaming agent concentration with which was also lower, the foam of generation is bigger, and is unstable, the broken situation of coalescence is more, so the liquid entrainment amount is few, and purity is than higher, but because the foam total surface area is little, the material of absorption is few, and the response rate is low.When thick indigo concentration of slurry increased, foaming agent concentration with which was also higher, thereby a large amount of stable foam of easier generation, foamy coalescence phenomenon a little less than, so adsorbance increases response rate rising; Simultaneously, foam is carried a large amount of bulk solutions mutually secretly, in the process that rises along the tower wall, motion mode is real " piston flow ", to lack under the situation of low solution by the time ratio that identical vertical dimension is required, liquid is difficult for refluxing in the foam, when improving the response rate, has reduced the purity ratio.Take all factors into consideration, select the response rate and all preferable thick indigo of 280g of purity to be diluted to 700ml (being that concentration is the thick indigo serosity of 0.4g/ml) as optium concentration.
From gas speed investigate and the result of concentration investigation all as can be seen: closely similar with indirubin and the indigo curve of being done as index respectively, the two is an isomers in addition, has similar physicochemical property, can infer that both behaviors in floatation process are to indirubin and indigo adsorbing separation non-selectivity, so can only measure indigo content as the foundation of judging flotation effect fully in the investigation of process conditions, reduce workload with the pharmacopeia method.
(3) investigation of material liquid pH value
On the equipment, carry out 44.8L/h～102.4L/h variable speed operation under the room temperature on the same stage, liquid level is 300mm, input concentration is the thick indigo serosity of 0.4g/ml, five parts of raw materials are carried out acid adjustment and uncomfortable processing respectively, carry out bubbling under the same terms, investigate the influence of different material liquid pH separating effect.Investigation the results are shown in Table 5.
Table 5pH investigates the result
As seen from the figure, raw material pH value from 7.5 to 14 is provided with 5 levels.The pH value of raw material itself has been strong basicity (greater than 14), therefore need not be provided with than 14 higher levels; When pH value transferred to acidity, chemical reaction just took place and has generated carbon dioxide in the calcium carbonate in the thick indigo serosity, and great changes will take place for system, therefore is not provided with than 7.5 littler levels.
PH value is comparatively complicated to isolating influential effect: in the scope of investigating, purity fluctuates, changes little trend up and down after being hurried decline earlier than the increase along with pH value; The response rate increases to increase afterwards earlier with pH value and reduces, and overall variation is little.It seems that comprehensively the purity ratio and the response rate are all preferable during pH=8.8.
When transferring the pH of material liquid lowlyer, as pH=7～8 o'clock, gained foam filtrate becomes redness by yellow, and obtains to such an extent that the froth pulp color also changes, and is with rufous slightly.Consider it itself is, do not change the character of medical material as far as possible, and pH is little to response rate influence, therefore uncomfortable pH and the pH value of maintenance system itself as processing in production place.
(4) investigation of feed volume
On equipment on the same stage, carry out 44.8L/h～102.4L/h variable speed operation under the room temperature, input concentration is the thick indigo serosity of 0.4g/ml, investigates the influence of different feeds volume to separating effect.Investigation the results are shown in Table 6.
Table 6 feed volume is investigated the result
Figure A20071007449000122
In the intermittent operation, the different feeds volume has determined different liquid levels substantially, the same foam knockout tower increases feed volume, has just increased liquid level, can prolong liquid phase and gas phase time of contact, help adsorbing mass transfer, help purity than and the raising of the response rate; But can shorten foam layer height simultaneously, and cause the foam drain time to reduce, liquid holdup increases, and has influenced the purity ratio.Suitable liquid level should increase material absorption, guarantees that also certain foam layer height is beneficial to discharge opeing simultaneously.Comprehensive each index is selected the feed volume 1000ml that better mates with the foam separation device for use.
Comprehensive above-mentioned condition, thick indigo serosity froth flotation optimum process condition is: the changing the flow of QI-blood speed operation of 44.8L/h～102.4L/h scope, concentration is the thick indigo serosity of 0.4g/ml, adjust pH not, feed volume is 1000ml.Index components comprises indigo and indirubin, adopts ultraviolet visible spectrophotometry and HPLC method respectively.Evaluation index is the response rate and purity ratio.Three demonstration test results of best intermittent foam separating technology see Table 7.
Three demonstration test results of the best intermittent foam separating technology of the thick indigo serosity of table 7
As seen from the above table, thick indigo serosity intermittent foam separating technology is stable, feasible.The foam phase response rate is about 90%; The purity ratio is about 2.3; Final gained foam mutually in indigo purity be 5.51%, indirubin purity is 6.06 ‰ (indigo purity is 2.40% in the thick indigo of this batch, and indirubin purity is 2.85 ‰).
Above-mentioned test explanation, 1, thick indigo serosity has good foaming characteristic, indigo, indirubin is water insoluble, but effective ingredient such as indigo, indirubin can take out of by foam, have possessed the primary condition of flotation.2, respectively with the indirubin and the indigo flotation effect (response rate of being done as index, the purity ratio) curve is closely similar, the two is an isomers in addition, has similar physicochemical property, both behaviors in floatation process can only be surveyed indigo content (pharmacopeia method) as the foundation of judging flotation effect to indirubin and indigo adsorbing separation non-selectivity in the investigation of process conditions.3, under the intermittent operation mode, gas speed, input concentration, material liquid pH value, feed volume are to the influence of flotation effect, determined that thick indigo serosity intermittent foam flotation optimum process condition is: 44.8-102.4L/h changing the flow of QI-blood speed operation from small to large, thick indigo concentration of slurry is 0.4g/ml, adjust pH not, feed volume is 1000ml.This moment, the foam phase response rate was about 90%; The purity ratio is about 2.3; Final gained foam mutually in indigo purity be 5.51%, indirubin purity is 6.06 ‰ (indigo purity is 2.40% in the thick indigo of this batch, and indirubin purity is 2.85 ‰).
(4) continous way foam floating flotating device operation
1, continous way foam floating flotating device flow process:
1.1 flotation column
Test chamber flotation column external diameter 65mm, internal diameter 60mm, total height is 1.8m.Consider the requirement for height difference of different material to flotation column, flotation column segmentation manufacturing assembling, bubble generator cloth flexibly becomes in the unit separately, puts in the flotation column bottom.For the ease of observing the flotation situation in the post, adopt the glass manufacturing.The flotation column bottom connects flexible pipe and discharges the underflow mine tailing, with underflow valve control mine tailing flow velocity.Air connects flexible pipe by air compressor and is transported to bubble generator, regulates charged air pressure and flow with air relief valve, and spinner flowmeter shows flow of aerating air.Flushing water connects running water pipe by flexible pipe and feeds, ball valve control flushing water size, and spinner flowmeter shows the flushing water flow.Flotation stirs for the advanced agitator in ore deposit, is pumped into mine-feeding equipment again, enters flotation column.Indigo Naturalis continous way foam floating flotating device is seen Fig. 2, Fig. 3, Fig. 4.
1.2, foam maker
Because of the making factor, described foam maker is meant the gas distributor (being) among Fig. 2.The distributor that this test is adopted all belongs to gas and produces bubble by porous media, has used sand filtration rod, capillary tube and filter cloth in the research.The sand filtration rod: the aperture is 8～12 μ m; Capillary tube: the aperture is 0.3mm, radially distributes distributive law 5/cm 2Filter cloth: 500 orders, bilayer.
1.3 the mensuration of gas holdup
The method of measuring gas holdup in the flotation column has a lot, as pressure differential method, and electrical conductivity method, liquid level rise method etc.What preceding two kinds of methods obtained is the local gas holdup of flotation column.What the liquid level rise method was surveyed is whole gas holdup, simple and comparatively accurately directly perceived.This test adopts the liquid level rise method to survey the whole gas holdup of flotation column, investigates the influence to the flotation column gas holdup under different inflation rate situations of different distributions device.
ϵ g = Δh H × 100 %
Xiang Shizhong: ε g--whole gas holdup;
Liquid level is poor in the post of Δ h--inflation front and back, cm;
Liquid level in the H--inflation front pillar, cm;
1.4 bubble size and Determination of distribution
Research flotation column bubble size is a research foaming rule, the main means of check flotation column performance.The measurement of bubble size is the problem of a complexity.The observation procedure of bubble is a lot, can be divided into light, sound, methods such as electricity.But because bubble, granule, liquid are very complicated three-phase systems, and the method for using all has improper part aspect accuracy at present.As image method ((Photographic Method), bubble size distribution obtains by seeing through bubble image measurement that glass wall spreads out of, counting, its shortcoming is exactly the bubble generation distortion.In recent years, rule of thumb method such as Model Calculation is commonly used to study the bubble size and the inflation performance of flotation column.
In view of current experiment condition, this experiment adopts camera method to study bubble size and distribution.The bubble size is to obtain by the image by digital camera being imported into measure to add up after computer amplifies, and shortcoming is a bubble deformation, and is more time-consuming.During floating operation, after bubble stabilizes, focus, then shooting with scale.Under certain inflation rate feed concentration, take a picture, add up.
1.5 post float test process
1) takes by weighing an amount of flotation sample and pour in the agitator, add certain water gaging and be transferred to suitable concn.
2) open agitator, stir certain hour and make it even.
3) open air compressor machine, regulate air relief valve, inflation rate is stabilized in predetermined value.Turn on pump is given the ore deposit flotation.
4) regulate mine tailing flow velocity, flushing water speed and give ore deposit speed, make the flotation situation stable.Get the concentrate and tailings sample.
5) stablize the flotation certain hour after, close agitator, flotation concentrate and mine tailing are fed in the collecting vessel, no longer enter flotation column.Treat that flotation ends (not having foam to overflow) the pumping clear water.After the underflow flexible pipe goes out clear water, close pump and air compressor machine.Float test finishes.
6) after the off-test, flotation column injects the certain altitude clear water, allows foam maker still have a small amount of gas to pass through, and avoids foreign material to stop up.
2, the selection of foam maker
When other factors is determined, gas holdup and bubble size are mainly determined by foam maker in the flotation column, so gas holdup and bubble size are selected better suited foam maker when measuring different foam maker, in selected material, plastic plate and glass sand plate percent opening is lower and the aperture is bigger, so do not carry out DATA REASONING, capillary tube, sand filtration rod and filter cloth foam maker investigated.
2.1 different foam maker inflation rates and gas holdup concern (see figure 5)
As seen from Figure 5, the foam maker of three kinds of materials, along with the increase of inflation rate, originally whole gas holdup increases very fast, and after inflation rate reached 1.5cm/s, whole gas holdup increased slowly, maintains respectively about 18%, 19%, 21%; Inflation rate begins to occur turbulent flow greater than after 1.75 in the post, the fluid fluctuation is bigger, and foam--liquid surface instability is so inflation rate should not be excessive.Concerning these three kinds of foam makers, when inflation rate 1.5cm/s, become the bubble situation more satisfactory.Comparatively speaking, higher with the made foam maker gas holdup of filter cloth.
2.2 bubble size distribution
In the post floatation process, the bubble size not only influences the flotation rate and the response rate, but also influences the selectivity of flotation, as finding with the flotation column coal separation, flotation rate constant k and bubble mean radius Rb cube are inversely proportional to, and this has proved absolutely the property of crucial importance of bubble size.The flotation of different material has different requirements to the bubble size, is not that bubble is the smaller the better, and is too small because buoyancy is limited, also can influence flotation.The bubble size is relevant with foaming mode, hydrostatic pressure, surface tension, gas flow rate, the blowing pressure, fluid flow pattern etc.
By the bubble diagram picture of different materials foam maker, gas speed is 1.5cm/s, the actual size of statistics bubble.As can be seen, bubble diameter is approximate to be normal distribution, and capillary tube foam maker bubble mainly concentrates between 2～4mm, and average diameter is about 3mm; Mainly between 1～2, average diameter is about 1.5mm to the bubble size of sand filtration rod foam maker; Mainly between 0.6～1.4, average diameter is 1mm to filter cloth foam maker bubble size.And in same one-tenth bubble zone, the formed bubble of the latter is obviously more than the former two, and the bubble proportion of minor diameter is also obviously high, and promptly bubble mean diameter is little.
By on can find out that no matter the filter cloth foam maker still is all more excellent aspect the bubble size at gas holdup, at isolating system, grain diameter is less, it is higher to need high gas holdup and vesicle to carry out flotation efficiency, so select its foam maker as flotation column for use.
3, post float test
Adopt the laboratory flotation column, carried out the test of small-sized flotation column flotation Indigo Naturalis at laboratory.Test with the flotation column structure is as described in Figure 3, foam maker employing filter cloth foam maker, and process of the test is carried out according to aforementioned.Mainly carry out the optimization Test of flotation column operating parameter inflation rate, flushing water flow, delivery rate, flotation column height etc., amplifying for pilot scale provides foundation.In the process of the test, regulate aeration quantity, flushing water flow, underflow speed earlier, make the post flotation reach one than steady statue.
3.1 inflation rate is investigated
This is the most important operating parameter of flotation column flotation.It has determined size, the quantity (inflation rate) of bubble to a great extent, i.e. bubble surface area flux, thus influence the selectivity and the response rate of flotation.
The screening test of foam maker material shows, after inflation rate reaches certain value, if increase again, then make mixability increase in the flotation column, be unfavorable for flotation, situation as bibliographical information is similar, after Jg reached 1.75cm/s, the boundary of ore pulp froth bed was unclear, up and down fluctuation, and the ore pulp disturbance is difficult to obtain high grade product.So with reference to the front result of study, inflation rate adopts and makes the big and metastable value in interface of gas holdup, promptly gets its value and is 1.5cm/s.
3.2 the investigation of collecting district height
The flotation column height is crucial structural parameters, and it determines the cost of flotation column and the consumption of operation energy largely.During the test of post height, apparent inflation rate Jg=1.5cm/s, the apparent ore deposit speed Jf=0.2cm/s that gives, flushing water speed Jw=0.03m/s, other condition is the same.
Adopt the various combination mode, foam layer height is consistent, be 0.3m, the collecting district is respectively 0.8m, 1m, 1.2m and 1.5m, and each operation sampling dry weight 500g after adding water and stirring, carries out float test, and triplicate the results are shown in Figure 6.
As shown in Figure 6, the increase of flotation recovery rate and indigo content is the increase owing to the flotation column height, the cause that causes bubble one granule collision frequency to increase.But reaching the trend that still has increase behind the 1.5m, because of experimental condition is limit, further investigate, but flotation column height and response rate relation are very complicated, both made the fine grained that difficulty is floated mineral, is not high more good more yet.Data shows, being increased to a certain degree of flotation column height, and the response rate no longer increases, and increases to 2.3m from 2m as the post height, and the response rate changes not obvious.So tentative its highly is 2m when calculating in the back.
3.3 foam layer height is investigated
Granule-bubble incorporation body is in the buoyance lift process and in froth bed, and bubble annexs, breaking to cause the generation of desorption.
The flotation column foam layer height influences as shown in Figure 7 the Indigo Naturalis flotation, and total trend is that froth bed thickness height is favourable to content, and is unfavorable to the response rate.Coming off of hydrophilic granules arrives the kinetic energy release at interface and impulsive force, vibrated and the bubble merging at interface owing to foam/granule coalition.
Brief summary: the flotation column froth bed is too high, causes bubble carrying capacity to reduce, and the probability that comes off of attaching particles increases.The flotation of material of hydrophobicity difference needs lower froth bed thickness, so that increase the response rate.If require to obtain high content, can suitably increase the flotation column foam layer height.Take all factors into consideration the response rate and content, the selection foam layer height is 30cm.
3.4 foam flushing water speed
Flotation column foam flushing water is for getting rid of the hydrophilic granules that foam is carried secretly, promote during foam mutually foamy stable be crucial.Flushing water speed (Jw) also is the important operating parameter of flotation column.
Test has also confirmed, adopts positive bias can obtain better index.
Flotation column foam flushing water is characterized by the bias current coefficient:
α = Q b Q w = Q t - Q f Q w = 0.25 ~ 0.42
The bias current coefficient is a bias current amount (giving the poor of ore deposit and mine tailing flow) and the ratio of total flushing water flow.Figure is the Indigo Naturalis float test, works as Jg:1.5m/s, Jf:0.1cm/s, and post height: 1.5m, foam layer height: during 300mm, the foam flushing water influences to some extent to the indigo content of Indigo Naturalis flotation.
Along with flushing water speed (Jw) increases, content improves, but productive rate also decreases.Fig. 8 shows that there is extreme point in indigo content in the Indigo Naturalis, and as Jw less (not surpassing a certain ultimate value in flushing water speed, during as 0.02cm/s), along with Jw increases, the secondary enrichment strengthens, and mechanical entrainment reduces, and content improves; After Jw is bigger, surpasses this ultimate value, along with flushing water speed increases, because the foam that froth zone moves upward mixes with the intensive adverse current interception of the wash water of motion downwards, causes ore pulp circulation and recirculation, the back-mixing degree increases, the viscosity contact probability rises, and makes concentrate grade descend on the contrary.In a word, the flotation column result of the test shows that an amount of flushing water helps sorting.Flusher also is the important step of flotation column design, and total requirement is that what realization was mingled with under response rate ideal situation minimizes, and improves foam stability as far as possible and reduces the water consumption.Take all factors into consideration the response rate and content, selecting flushing water speed is 0.01cm/s, i.e. 1.02L/h.
3.5 delivery rate test
Above-mentioned test is at conventional delivery rate (J fBe 0.1cm/s) condition under carry out.The methods of the size of the disposal ability of flotation column and apparent inflation rate, aeration quantity, bubble size and distribution situation, foaming structure, foam layer height, mineral grain liberation degree of minerals, purpose mineral content, mineral proportion, mineral grain and distribution situation, ore pulp flow condition, ore pulp and bubble effect etc. have much relations, at present still do not have definite mathematical relationship, the flotation column treating capacity difference in the practical application is very big.At Jg 0.1cm/s, Jw 0.02cm/s, the high 1.5m of post under the condition, has investigated the situation that influences of delivery rate during foam layer height 300mm.
Along with delivery rate (J f) increase, the foam recovery rate descends, and content also descends to some extent, as Fig. 9.It should be noted that delivery rate has only a conventional half (0.05cm/s), the Indigo Naturalis response rate is higher, can reach 80%.This explanation bubble lazy weight under conventional delivery rate condition has caused the response rate not high.Therefore, the flotation column treating capacity need be mated with the number of bubbles of flotation column.Delivery rate increases must corresponding increase bubble surface area flux.
By above-mentioned test gained result of the test be: collecting district height is 1.5m, foam layer height is 30cm, delivery rate is 0.1cm/s (or 10.17L/h), flushing water speed is 0.01cm/s (being 1.02L/h), inflation rate is 1.5cm/s (being 152.6L/h), the Indigo Naturalis flotation recovery rate can reach more than 75% with this understanding, and indigo content is more than 4.0%.
4, pilot plant is amplified
4.1 the concrete parameter of pilot plant, material etc.
According to amplifying principle in proportion, consider and amplify the axial influence that mixes the holdup time in back, the granule time of staying is increased to 40min, and then minimum column length (flotation section) is 4.0m, again according to place of production practical situation, manufactured and designed with the rustless steel is material, diameter is 38cm, highly is the flotation column of 3m (flotation highly is 2m, and foam height is 1m), estimate that by the laboratory parameters operation treating capacity is 40kg/h, adjust again according to the pilot scale creation data.
4.2 middle test run data
In the pilot scale process, great number tested data shows that utilization laboratory screening parameter is carried out flotation, can not produce a desired effect, may be that the mixing situation increases after amplification, and due to the factor such as the design of post height is not enough, so flotation needs just can reach the required response rate by 2～3 times; Result such as table 8, table 9.
Test run data in the table 8
Figure A20071007449000191
Table 9 pilot plant test is table as a result
As can be seen from the above table, under this operating condition, indigo content reaches more than 4% in the product, but the productive rate and the response rate are lower.At the enterprise practical situation, its operating parameter is adjusted again, final operational factor and result are as follows:
Test run data in the table 10
Figure A20071007449000193
Table 11 pilot plant test is table as a result
Figure A20071007449000194
The result shows that treating capacity is about 35kg/h, and the products obtained therefrom quality all reaches requirement, and the response rate is also higher, and technological parameter is stablized feasible.
Concrete technological process: pan feeding (4) adds water behind stirring pool (5) mixing, being pumped into the flotation column import by pump (6) evenly is distributed in the tower with shower nozzle (25) spray, simultaneously evenly enter in the post by tower bottom air inlet pipe (7) and gas distributor (24) with the gas-liquid volume ratio of 1～3cm/s 0.2～0.5MPa compressed air, because system self contains the foaming characteristic material, when a large amount of countless bubbles contact with feed liquid, promptly formed more stable foam, Indigo Naturalis is attracted on the foam simultaneously, the foam that forms is owing to the buoyancy of solution rises, along with foamy continuous generation, come-up, the Indigo Naturalis that is adsorbed on the bubble is just separated from thick indigo liquid, control suitable operating condition, be the bulky grain that is mingled with in the scumming, need add the water flushing in the froth bed, the floating foam of going up cat head to concentrate sedimentation tank (3) precipitation, is Indigo Naturalis (11) after the collecting precipitation drying after discharging opening (27) enters the broken bubble of bulb-breaking device (2); Supernatant (10) is discharged the back and flowed into liquid storage tank, and is recycling; Discharge gate (12) discharge liquor is got above it blue portion and is proceeded FLOTATION SEPARATION after material storage barrel (13) flows into mine tailing sedimentation tank (14) back natural sedimentation, shoals as if the supernatant blueness, can flow into liquid storage tank, and lower part can discard.
Produce three batches according to process route of determining and condition, production equipment operational factor and data see Table 12 and table 13 respectively.
Table 12 service data
Table 13 production is table as a result
Figure A20071007449000202
The result shows that technological parameter is stablized feasible.
Above-mentioned test explanation, Indigo Naturalis of the present invention adopts identical preparation method, under two kinds of equipment (intermittent foam floatation equipment, continued operation foam separation equipment) condition, all can be prepared into steady quality, and the Indigo Naturalis that is higher than existing standards of pharmacopoeia, and convenient operation and management is separated the restriction that is not subjected to environment, weather, stable and reliable operation.
The comparative study of [embodiment 4] froth flotation and traditional Indigo Naturalis separating technology
The comparative study of froth flotation and existing Indigo Naturalis processing in production place technology
The froth flotation technology is to contain the suspension of solids, can add suitable surfactant, the collecting solid particle, make them obtain hydrophobicity, and then add suitable foaming agent, utilize the air bubbling, difference according to Ore particle and stone-like pulse particle properties, stone-like pulse is sunk, and Ore is with bubble floating, thereby reaches a kind of technology of purpose of separating.This technology maturation is applied in the suitability for industrialized production of sorting mineral, has that equipment is simple, characteristics such as easy operating, cost are low, good separating effect.
According to the froth flotation principle, can bubble in conjunction with thick indigo serosity and to take the character of effective ingredient out of, use for reference the application experience of smelting ore deposit industry, on existing research basis, this chapter utilizes froth flotation technical point indigo, indirubin in, enrichment Indigo Naturalis, and with existing Indigo Naturalis processing processing in production place technology, stir the indigo method and compare research, for the application and the popularization of foam separating technology provides foundation.
(1) experiment material and method
1, material and equipment
Material: thick indigo is by Hengyuan Pharmaceutical Group Co., Ltd., Jiangyou City, Sichuan, indigo reference substance (Chinese biological goods calibrating institute)
Equipment: SHIMADZU uv-spectrophotometric instrument; LZB-4 glass rotameter (Zhejiang development flow-meter plant); ACO-007 type air compressor (ZheJiang Sunsun Industrial Co., Ltd.); TDL-5 type centrifuge (Anting Scientific Instrument Factory, Shanghai); FA1104 type electronics Libra (going up balance factory of Nereid section);
2, Indigo Naturalis processing method
(1) stirs the indigo method
Adopt traditional craft to stir indigo, the thick indigo of every 50kg adds clear water 100～130kg and places water vat, and bamboo pole does not stop to stir along wall, and foam is floated in a large number, when treating that foam is piled up certain thickness, picks up foam drainage on toilet paper with the bamboo sieve, tans by the sun promptly under the daylight.
(2) elutriation
The permanent source of river, Sichuan oil Pharmaceutical has adopted voluntarily that the Indigo Naturalis water of development flies automatic sorting device, is that 2～3% thick indigo slurry is by 2.5m with concentration 3/ h flow velocity pumps into Indigo Naturalis water and flies the automatic sorting device removing impurities, again with the Indigo Naturalis slurry centrifuge dehydration that obtains to water content 55%, 80 ℃ of dryings of gained filter cake 7.5 hours to water content 30%, granulate, 100 ℃ of dryings 0.5 hour are promptly in SMH tunnel type far-infrared ray drying baking oven.
(3) foam flotation method
According to the pilot scale situation, control 2 kinds of different operating conditions and carry out froth flotation, operating condition 1: gas flow 4.0m 3/ h, feed flow 1.2m 3/ h, wash water flow 200L/h; Operating condition 2: gas flow 5.0m 3/ h, feed flow 1m 3/ h, wash water flow 100L/h.(operating condition 1 and 2 all is continous way froth flotations, the technological parameter difference)
Gained the results are shown in Table 14.
(2) mensuration of investigation index
" Chinese pharmacopoeia version in 2005 is with the indigo content of spectrophotometry in indigo reference.
(3) result begs for opinion
Result of the test sees Table 14.
Table 14 experimental study result
Figure A20071007449000221
*Thick indigo water content is 65%.
*Investigate the mensuration of index: according to " one one of Chinese pharmacopoeia version in 2005 is with the indigo content of spectrophotometry, the content of tlc scanning determination indirubin.
Stir the indigo method and adopt manual operations, labor intensity is big, and production efficiency is low, can not satisfy the modern production requirement, and unstable product quality; Effective ingredient such as that foam flotation method is utilized is indigo, indirubin can be by the character of optionally taking out of by foam, regulate and control by operating parameter, can change content indigo in the product, indirubin, satisfy product different quality demand: foam flotation method operating condition 1 can access high quality of products, but productive rate is lower; Foam flotation method operating condition 2 products obtained therefroms meet the pharmacopeia requirement, also meet the enterprise market demand.This method is easy and simple to handle, and technical difficulty is low.The Indigo Naturalis of preparation all can be met the need of market.

Claims (10)

1, a kind of preparation method of Indigo Naturalis comprises the steps:
A, elder generation pump in the flotation column of foam floating flotating device after thick indigo is added the water stirring;
B, compressed air is sent in the flotation column by the micropore distributor of flotation column outside or bottom, formed froth bed;
C, foam through the water flushing after, by the broken bubble of bulb-breaking device, it is centrifugal or enter the sedimentation tank precipitation that broken bubble liquid enters centrifuge, is Indigo Naturalis after the collecting precipitation part drying.
2, the preparation method of Indigo Naturalis according to claim 1 is characterized in that: thick indigo adds water to be prepared into thick indigo concentration of slurry is 0.15-0.6g/ml in a step.
3, the preparation method of Indigo Naturalis according to claim 1 is characterized in that: to add the feed rate that pumps into flotation column after water stirs be 1.0～1.2m to thick indigo in a step 3/ h.
4, the preparation method of Indigo Naturalis according to claim 1 is characterized in that: compressed air is 44.8L/h-5 * 10 by the gas flow of the micropore distributor of post outside or bottom in the b step 3L/h.
5, the preparation method of Indigo Naturalis according to claim 1 is characterized in that: foam is 1.02L/h-200L/h through the water flow velocity of water flushing in the c step.
6, the Indigo Naturalis of the described preparation method preparation of claim 1, it is characterized in that: containing indigo weight percentage is: 2.63%-5.51%, the weight percentage of indirubin is: 0.13%-0.61%.
7, a kind of foam floating flotating device for preparing Indigo Naturalis, it is the intermittent foam floatation equipment, and this equipment comprises: air compressor (33), gas rotameter (34), bubbling area (35), froth zone (36), foam are collected bend pipe (37), product stock jar (38), gas distributor (39).
8, a kind of foam floating flotating device for preparing Indigo Naturalis, it is the continued operation foam separation equipment, this equipment comprises flotation column (1), centrifugal bulb-breaking device (2), sedimentation tank (3), is connected to form with pipeline successively.
9, foam floating flotating device according to claim 8, it is characterized in that: described flotation column (1) comprises housing (23), in the post housing, be equiped with gas distributor (24), charging shower nozzle (25) flushing water shower nozzle (26) from bottom to top successively, one downflow weir (9) is arranged outside post top, a discharging opening (27) is arranged under it; One discharge gate (12) is arranged at the cylinder bottom, and pipeline connects the back discharges in flotation column 2/3 place, discharges by material storage barrel (13), with control liquid phase height; Air inlet pipe (7) is housed on housing links to each other, be used to carry compressed air with gas distributor (24).
10, foam floating flotating device according to claim 8 is characterized in that: centrifugal bulb-breaking device (2) comprises motor (28), case (29), impeller (30).
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CN107930861A (en) * 2017-11-07 2018-04-20 中国矿业大学(北京) A kind of wide grade mineral floating device of adjustable flotation height
CN108841480B (en) * 2018-06-29 2022-02-01 贵州省仁怀市水码头酿酒作坊 Fermentation device
CN108841480A (en) * 2018-06-29 2018-11-20 贵州省仁怀市水码头酿酒作坊 Installation for fermenting
CN110669354A (en) * 2019-10-29 2020-01-10 江苏省中国科学院植物研究所 Indigo manufacturing installation
CN111729353A (en) * 2020-08-06 2020-10-02 中国石油化工股份有限公司 Foam separation device and method for eliminating foaming of desulfurized amine liquid
CN111729353B (en) * 2020-08-06 2022-03-22 中国石油化工股份有限公司 Foam separation device and method for eliminating foaming of desulfurized amine liquid
CN114871000A (en) * 2022-04-26 2022-08-09 鞍钢集团矿业有限公司 Flotation dosing self-adaptive control method
CN114871000B (en) * 2022-04-26 2023-08-11 鞍钢集团矿业有限公司 Flotation dosing self-adaptive regulation and control method
CN114798184A (en) * 2022-05-16 2022-07-29 北京盈翔科技有限公司 Efficient foaming agent for copper-gold ore flotation and application method thereof
CN114798184B (en) * 2022-05-16 2024-01-23 北京盈翔科技有限公司 Efficient foaming agent for copper gold ore flotation and application method thereof

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